TECHNICAL

HIGHLIGHTS

196B

U.S. DEPARTMENT OF COMMERCE / National Bureau of Standards

UNITED STATES DEPARTMENT OF COMMERCE

C. R. Smith, Secretary

John F. Kincaid, Assistant Secretary for Science and Technology

NATIONAL BUREAU OF STANDARDS

A. V. Astin, Director 1968

Technical Highlights

of the

National Bureau of Standards

Institute for Basic Standards Institute for Materials Research

Institute for Applied Technology Center for Radiation Research

Annual Report, Fiscal Year 1968

For sale by the Superintendent of Documents, U.S. Government Printing Office Washington, D.G. 20402 - Price $1
Library of Congress Catalog Card Number: 6-23979
CONTENTS

INTRODUCTION 1 Management Progress 1 Center for Radiation Research Created. Reorganization

of Boulder Laboratories. New Institute Directors Named.

Special Programs 3

Research Associate Program. Foreign Scientist Visitation

Program.

Utilization of Federal Laboratories 5

Legislative Report 6

Flammable Fabrics Act. Fire Research and Safety Act. Standard Reference Data Act. TWO KEY STANDARDS PROGRAMS 9 The National Standard Reference Data System 9

History of the Program 10

Responsibilities of NBS. Operation of the System. General

Status of the Program. The Standard Reference Data Act. International Cooperation.

Current Data Project Activity 19

Nuclear Properties. Atomic and Molecular Properties.

Thermodynamic and Transport Properties. Solid State

Properties. Chemical Kinetics. Colloid and Surface

Properties.

Data Systems Design and Development 24

Information Services 25

The Standard Reference Materials Program 26

History of the Program 26

Current Activity 33

INSTITUTE FOR BASIC STANDARDS 39

Physical Quantities 39

International Base Units 40

Length. Time and Frequency. Temperature. Electric Current. Fundamental Physical Constants.

Mechanical Quantities 47

Electrical Quantities—D.C and Low Frequency 49

Electrical Quantities—Radio Frequency 51

High Frequency Region. Microwave Region. Electromagnetic Field Standards. New Calibration Services.

Thermal Quantities 56

Photometric and Radiometric Quantities 57

iii
INSTITUTE FOR BASIC STANDARDS—Continued

Physical Properties 61

Atomic and Molecular Properties. Solid State Properties.

Thermodynamic and Transport Properties.

Applied Mathematics 72

Technical Assistance to Others 73

Studies for Other Groups. Conferences and Symposia.

INSTITUTE FOR MATERIALS RESEARCH 79

Preparation and Characterization of Materials 79

Preparation , 79

Synthesis. Crystal Growth.

Characterization 83

Composition. Structure. Data on the Properties of Materials 98

Mechanical Properties and Strength oj Materials 98

Reactivity and Corrosion 102

Thermodynamics and Kinetic Data 105

Electric, Magnetic, and Optical Properties 113

Technical Assistance to Others 119

Advisory and Consulting Services 119

Conferences and Symposia 120

INSTITUTE FOR APPLIED TECHNOLOGY 123

Technological Measurements and Standards 123

Building Technology 124

Automatic Data Processing 128

ADP Standards. Consultative and Advisory Services.

Research. Computer Services.

Electronic Technology 132

Systems Analysis 134

Motor Vehicle Safety 135

Tire Systems. Occupant Restraint Systems. Braking

Systems.

Engineering Materials 137

Engineering Standards 139

Technological Innovation and Diffusion 142

Invention and Innovation 142

The Clearinghouse 143

CENTER FOR RADIATION RESEARCH 145

Radiation Measurement and Standards 145

Nuclear Physics Research 148

Facilities Operations 150

Technical Assistance to Others 152

Studies for Other Agencies. Conferences.

APPENDIXES 155

Organization of the National Bureau of Standards 155

Summary of NBS Staff 161

Financial Data 162

iv
APPENDIXES—Continued

Research Associates and Guest Workers 162

Advisory Committees 165

Statutory Visiting Committee 165

Technical Advisory Panels 166

Awards and Honors 171

Education, Training, and University Liaison 171

Publications 174

Publications in the Bureau's Series 174

Publication in Outside Journals 183

Patents 210

v

INTRODUCTION

Management Progress

The National Bureau of Standards has continuing responsibility in a number of areas under terms of the Organic Act which created it in

1901 and through subsequent amendments to the Act. In addition, as a

result of changing technology and through special legislative acts, new

and expanding activities have been undertaken over the years. Changes

in Bureau activity have occasionally resulted in redirection of administrative and management emphasis ; the most recent major reorganization came in 1964 with the formation of four Institutes to encompass

the various activities that existed at that time.

The significant changes that have taken place in the past fiscal year

are discussed below. In each case, the change was designed to make the

Bureau more responsive to needs of the commercial, scientific, and

industrial groups which it serves. Center for Radiation Research Created

A Center for Radiation Research was formed to provide more effec- tive management of the Bureau's large radiation facilities, previously

under two different Institutes in the NBS structure. With all of its major radiation-producing machines under central management the

Bureau will be able (1) to provide special services to all of its programs, (2) to carry out more vigorous basic research and (3) to share its unique resources with other Government agencies and with

universities.

Special radiation facilities at KBS include a ten megawatt nuclear

research reactor and a 100 million electron volt linear accelerator, as well as a number of other radiation-producing machines and sources. These facilities, especially the large machines, are used in a wide

variety of studies by various units in the Bureau, and are available to the Government and academic communities of the Washington area. NBS studies cover radiation measurement and standards, basic nature

of matter and radiation, and the effects of radiation on matter and

materials.

The new Center for Radiation Research is composed of a Reactor

Radiation Division, Linac Radiation Division, Nuclear Radiation Division, and Applied Radiation Division.

1
Reorganization of Boulder Laboratories

During the fiscal year the NBS Boulder, Colo., Laboratories were

unified, under a single, local management for the first time since 1964,

when the Bureau's programs were divided up between the Institute for

Basic Standards (IBS), the Institute for Materials Research (IMR),

the Institute for Applied Technology (IAT), and the Central Radio

Propagation Laboratory (CRPL). The last has since become part of

the Environmental Science Services Administration.

A reorganization which began in midyear was completed June 30,

bringing all of the Boulder elements into the NBS Institute for Basic

Standards, organized to provide "the central national basis for a complete, consistent system of physical measurement, coordinated with

those of other nations."

Transfer of the Boulder Cryogenics Division into IBS and the

appointment of a Deputy Director for IBS-Boulder to direct the activities of five research divisions and the services of three support divisions, created a common bond in fulfilling the IBS assignment to develop and maintain standards for physical quantities and for the

measurement of physical properties.

New Institute Directors Named

New Directors for the three NBS Institutes were named during the

year. The average age of the new Directors is 44, indicative of management policy to fill senior positions with young persons who are scientifi- cally well qualified but also attuned to the expanding and changing

role of science and technology in the Nation.

Dr. Ernest Ambler, Chief of the NBS Inorganic Materials Division was named to head the Institute for Basic Standards. Dr. Ambler, a Briton by birth, came to the United States in 1953, and joined NBS

the same year. He began performing magnetic research and nuclear

orientation studies at temperatures approaching absolute zero and,

within eight months after coming to the Bureau, completed the first nuclear alinement experiments to be conducted in the United States. Dr. Ambler received his B.A., M.A., and Ph. D. degrees at Oxford

University in 1945, 1949 and 1953. He shared in the 1964 Samuel Wesley Stratton Award for work demonstrating that the quantum mechanical law of parity conservation does not hold in weak interactions.

He was also honored for this work with a Department of Commerce

Gold Medal Award in 1957, the Washington Academy of Sciences

Award in 1957, and the John Price Wetherill Medal of the Franklin

Institute in 1962. In 1960, Dr. Ambler was named one of the ten out- standing young men in the Federal Government, receiving the Arthur

S. Fleming Award in recognition of his outstanding work in science. 2
Dr. John D. Hoffman heads the Institute for Materials Research. He

has been with NBS since 1954, when he joined the Polymer Structure

Section as a physical chemist. In 1956, a Dielectrics Section under Dr.

Hoffman's direction was established to investigate such areas as dielectric properties of polymers, precision dielectric measurements, and

theoretical studies on relaxation phenomena in molecular crystals. In

1964 he was named Polymers Division Chief. Dr. Hoffman received

his B.S. in chemistry at Franklin and Marshall College in 1942 ; and

in 1948 and 1949, he received his M.S. and Ph. D. degrees in physical

chemistry from Princeton University. Dr. Hoffman was presented the

1967 Samuel Wesley Stratton Award. He was corecipient, in 1961 of an NBS Special Act of Service Award. The Washington Academy of

Sciences awarded him a certificate of recognition in 1962 "for dis- tiftguished service in the science of polymer physics."

Dr. Lawrence M. Kushner was named Director of the Institute for

Applied Technology. Before becoming Deputy Director of the Insti- tute in July 1966, Dr. Kushner was Chief of the NBS Metallurgy

Division. He joined the Bureau in 1948 as a physical chemist in the

Surface Chemistry Section, later becoming Assistant Chief of the

Section. In September, 1956, he was appointed Chief of the Metal

Physics Section. Dr. Kushner's main scientific research interests are

in the relations of defects in the crystal structure of metals to the

metal's physical properties.

As a Commerce Science and Technology Fellow, Dr. Kushner

worked in the office of the Assistant Secretary of Commerce as a

Special Assistant for Legislation in 1964-65. Dr. Kushner was graduated from Queens College with a B.S. in chemistry in 1947. He re- ceived both his A.M. and Ph. D. in physical chemistry from Princeton

University.

Special Programs

Research Associate Program

The Kesearch Associate Program of the National Bureau of Standards makes it possible for qualified scientists and engineers from

industrial corporations, technical trade associations, professional societies, and other Government agencies to work on a full-time basis

for finite periods of six months to two years or more at NBS. They

work on research programs of mutual interest to the sponsoring

group and the National Bureau of Standards. Their salary continues

to be paid by their parent organizations.

The Research Associate Program has been in operation for over

fifty years but has received renewed emphasis since 1964. Primary

responsibility for the development of the program was given to the

NBS Office of Industrial Services late in that year. In the past, the

3
program was primarily aimed at serving the needs of researchers

from technical associations. The program is now being aimed directly

and primarily at industrial corporations performing research and

development. The acceptance by industry of this opportunity, as

reflected by success to date is most encouraging.

As of June 30, 1968, there were 61 Research Associates at NBS,

29 of whom came in during fiscal 1968. The total is approximately

twice as many as there were in November 1963. Further expansion

of the program is planned through the efforts of the NBS Office of

Industrial Services with participation by management and technical

staff from the three NBS Institutes. The ultimate goal is to have

about one Research Associate for every ten NBS professional staff members, or about 150 Research Associates.

An all-day meeting was held between representatives of NBS and

about 60 manufacturing concerns in the Pittsburgh area. The purpose was to introduce the Bureau and its services to a cross section of

industry in the area. The reactions to this meeting indicate that the

approach can be a most fruitful one to use in many cities of the U.S.

Foreign Scientist Visitation Program

For many years, the National Bureau of Standards has been en- gaged in international activities in various ways. It is in the interest

of this country to foster sound systems of standardization and meas- urement in other countries and for this reason NBS cooperates with

international laboratories and organizations engaged in pursuits

similar to its own. It is in this spirit that the Bureau receives qualified

workers from abroad or that NBS staff are sent to other countries.

A few examples illustrate the general principles listed above. NBS

staff are active in certain international organizations such as the

International Bureau of Weights and Measures, the International

Standards Organization and similar groups which create the defini- tions upon which most international systems, measurement, and standardization are based. These organizations are found in both developed

and less developed countries.

In the less developed countries, the role of NBS is usually to help

establish advanced systems in laboratories. NBS has been often called

upon to send experts or teams to various parts of the world where need

is felt for a standards laboratory or for a sound system of weights

and measures. Examples in the recent past are: Iran, South Korea,

Saudi Arabia, and Taiwan.

The Bureau recently participated in a cultural exchange with the

USSR on standards and norms. For this purpose a staff member of

NBS served as a member of the delegation going to the Soviet Union

and NBS received the Soviet delegation in December 1967.

4
As part of the international program, the Bureau in the last year

received 732 foreign visitors, 24 foreign guest workers from 16 countries, and six foreign trainees for periods ranging from 2 weeks to 6 months. Included among these guest workers are fellows from United

Nations, North Atlantic Treaty Organization, International Atomic

Energy Agency, and other national laboratories. NBS staff members

participated in a great number of international conferences, at many

of which they were asked to deliver papers or chair sessions. The operations described here constitute an effective way of trans- ferring technology to less developed countries. With the present importance of such transfer the relevance of all international exchanges

(documents, persons, instruments, or standard samples) cannot be

sufficiently emphasized.

Utilization of Federal Laboratories

During the 2nd session of the 90th Congress, the Subcommittee on

Science, Research, and Development of the House Committee on Sci- ence and Astronautics held a series of hearings on the Utilization of

Federal Laboratories. The purpose of the Subcommittee hearings,

chaired by Congressman Emilio Q. Daddario, was to determine "how

we can make the best use of our existing Federal laboratories." NBS

Director Allen V. Astin was invited to testify and did so on March 27,

1967. Excerpts of Dr. Astin's comments before the Subcommittee

appear below.

While the basic measurement mission has provided the prime focus

of NBS activities through the years, "the Bureau also has served

since its inception as a central resource of scientific and technical competence within Government. Other agencies have made extensive use

of the Bureau's competence and facilities, particularly in the exploratory stages of new technical endeavors, This has been a constantly

changing role that has involved the Bureau, at least temporarily, in

a great variety of technical activities, some of which have continued

and have grown to become major national programs involving new

Federal laboratories. ..."

"We do a considerable amount of work for other Federal agencies,

ranging from fairly fundamental research to testing and calibration.

A substantial part of the NBS annual budget—currently 40 percent

of the total—is made up of funds transferred to us from other agencies

for services rendered."

"NBS laboratories also serve State and local needs, primarily in

the weights and measures field." "NBS interactions with the academic community are varied and

growing. They include use of our laboratory facilities in a number of

ways."

5
"NBS works very closely with private standards making bodies, of

which there are some 500 in the United States." "In 1961, NBS sponsored the establishment of the National Conference of Standards Laboratories, and has acted as its secretariat ever

since. The NCSL is a continuing, nonprofit, laboratory-oriented organization to promote cooperative efforts toward solving common standards

and measurement problems. Its members include standards laboratories

of individual companies, universities, independent laboratories, and

those in other Government agencies."

"Finally, our laboratory facilities are shared with industry itself. The most effective mechanism is our Eesearch Associate Program,"

see page 3. Legislative Report

Four proposed legislative acts affecting the Bureau were considered

by the Congress during the fiscal year. The Flammable Fabrics Act

(PL 90-189) was amended on December 14, 1967. The Fire Eesearch

and Safety Act of 1968 became law on March 1, 1968. The Standard

Reference Data Act was signed into law on July 11, 1968. Also, a bill authorizing the Secretary of Commerce to conduct a study of the

metric system was under consideration. (This law was subsequently

passed by the Congress and signed into law August 9, 1968.)

Flammable Fabrics Act

The 1967 amendments to the Flammable Fabrics Act (PL 90-189)

make certain provisions for a more effective attack on the overall problem of deaths, injuries, and economic losses resulting from fires in- volving fabrics and related materials, and products made from them.

They extended the coverage of the Act to include all articles of wearing

apparel and, if the need is shown, items of interior furnishings. They

provide the authority for establishing standards and required levels of

performance, with certain operational safeguards; the conduct of in- vestigations of the extent of deaths, injuries and economic losses result- ing from fire involving garments and interior furnishings; research

into the flammability of fabrics and related materials ; the development

of test methods and revised or new standards ; training in the use of the

test methods and devices; and provisions for the enforcement of the

amended Act. Under the Act, the Department of Commerce, mainly through NBS,

is responsible for research into the flammability of materials and the

feasibility of reducing that flammability, development of test methods

and apparatus, training in their use, and for the establishment of

standards and regulations concerning fabrics and related materials as used in wearing apparel or interior furnishings. The legislation re- quires the Secretary of Commerce to consider the results of research

6
and investigations in determining that a hazard exists and that a standard or regulation, or a revision thereof, is needed to protect the public.

Fire Research and Safety Act

The Fire Eesearch and Safety Act of 1968 (PL 90-250) authorizes

the Secretary of Commerce to conduct, or through contracts or grants

to carry out

:

1. Investigations of fire causes, severity, frequency, or other pertinent factors;

2. Eesearch into the causes and nature of fires and the development

of improved methods and techniques for fire prevention, fire control,

and reduction of death, personal injury, and property damage;

3. Educational programs to inform the public of fire hazards and

fire safety techniques and encourage the avoidance of such hazards

;

4. Fire information reference services including the collection,

analysis, and dissemination of data and research results related to fire protection, control, and reduction of deaths or property loss.

5. Educational and training programs for among other things the

improved efficiency, operation, and organization of fire services; and

6. Demonstration projects in support of fire prevention, fire safety

principles in constructions, and improved fire services. Further, the Secretary is to support the development of fire safety

and protection engineering or science curriculums, and fire safety

courses, seminars, or other instruction materials and aids for courses of instruction. NBS will play a significant role in carrying out these

activities. Standard Reference Data Act

A National system for providing badly needed scientific data to

science and industry was authorized by the Standard Eeference Data

Act which became law on July 11, 1968.

The law authorizes NBS to coordinate the program. The Bureau has

had a standard reference data operation for three years, but additional

authority given by the new law will strengthen and increase the effec- tiveness of the system. The main purpose of the standard reference

data program is to make readily available to the Nation's scientists and

engineers data on the properties of matter and materials—melting

points, electrical resistance, strength, and many more. Such data are

essential for picking the proper material for making a space probe or

a toaster, or any other manufactured item.

7

TWO KEY STANDARDS PROGRAMS

The role of the National Bureau of Standards as a source of scientific and technical expertise to industry, commerce, science, and Government is clearly evident in two key programs designed to provide

highly reliable information and materials to users throughout the

world.

A STANDAED EEFEEENCE DATA PEOGEAM provides crit- ically evaluated quantitative information relating to a property of a

definable substance or system.

A STANTDAED EEFEEENCE MATEEIALS PEOGEAM provides well-characterized materials that can be used to calibrate a measurement system or to produce scientific data that can be readily

referred to a common base. These two programs have much in common, as their titles imply.

Both are the result of ready-made measurement. Both produce a highly reliable product which foster a user's capability to make meaningful measurements. Both are economically efficient—reference data

because they are not exhausted by continued use and reference materials because they are accurately reproducible on a mass production

basis. And most important, both serve a critical and wide-spread meas- urement need in the United States and are important in the development of new areas of international standardization.

THE NATIONAL STANDARD REFERENCE

DATA SYSTEM

Improvement in the effectiveness of the Nation's system for scientific and technical information is currently a matter of great popular

concern. Much is being said and written about the flow of information

from the generator to the user, and much is being done to try to speed

the process. The Chemical Abstracts Service of the American Chemical Society

is in the midst of a long-range program designed to increase the re- trievability of information within its concern [1]. The American Institute of Physics has embarked on a comprehensive study of means

to make the world's output of information in physics more readily

available to individual users [2] ; the Engineers Joint Council has

9
a similar program [3] . The Atomic Energy Commission, the Department of Defense, the National Aeronautics and Space Administration,

and other major Federal agencies are all increasing their efforts to improve the use of information generated within their technical

programs. The President's Office of Science and Technology and

the President's Science Advisory Committee maintain continuing ef- forts to review developments and to stimulate new initiatives for

improvement. Indeed, a report of the President's Science Advisory

Committee has provided basic guidelines for the development of

governmental activities since its appearance five years ago [4].

History of the Program

Government interest in all these activities is coordinated through

the Federal Council for Science and Technology by means of its Committee on Scientific and Technical Information (COSATI). The in- itiative of COSATI and its parent council led to establishment in 1963

of the National Standard Reference Data System, a federal interagency activity concerned with one aspect of the broad problem of

scientific and technical information—that of providing better access by

the American technical community to compilations of critically eval- uated data on the properties of substances.

Such compilations have been among the basic tools of scientists and

engineers throughout the history of technology,; each practitioner owns

at least one handbook containing table after table of data on the properties of the substances and systems that he deals with daily. Systematic

compilations of data also contribute in a fundamental way to progress

at the forefront of science. Samuel Goudsmit [5] recently emphasized

this importance with the following words

:

"Experimental results in measurements are the backbone of physics.

No theory is acceptable unless it agrees with the experimental data.

Conversely, a systematic study of experimental results can suggest new theoretical approaches. Tables and graphs of numerical data therefore play an important role in the progress of physics. ... It is thus

obvious that specialized data compilations are of great importance

and should have the full cooperation of those producing the data. It

is also clear that modern computer techniques can handle such data more efficiently than old tabulations could, especially since their number and variety are growing so rapidly."

Since the numerical data that result from measurements of properties

normally appear somewhere in the world's literature, why not let the

individual scientist or engineer look them up whenever he needs a value? There are two major reasons why this procedure is not efficient. First, it is often very difficult to locate a desired value among the millions of papers stored in a technical library; searching indexes, abstracts, and papers can consume many hours. Second, conflicting val^p-s

10
for the same property are often reported. Unless the user is a specialist

in the field, he will have difficulty deciding which value he should use. These inefficiencies translate directly into wasted effort and dollars. If the average scientist or engineer were to save only ten minutes a week that he now spends finding and evaluating data, the annual sav- ing to the Nation's research and development activity would be of the

order of $100 million. This estimate takes no account of the benefits of

having better data, evaluated by an expert in the field, at hand when

needed. Obviously, very significant economic benefits can be readily

obtained through a coordinated, comprehensive program for reviewing

the literature, extracting and evaluating the property data contained

therein, and disseminating them in convenient form.

Because of their usefulness and economic benefits, many compilations of data [6] have already been produced throughout the world.

However, existing mechanisms have not been able to keep pace with

the flood of new data appearing in the literature, except in a few specialized areas. Some compilations are "one shot" projects, resulting

in products that are never updated, others have been continuing

activities lasting many years. Some have been sponsored by missionoriented agencies of the United States Government; others, by pri- vate organizations. However, many newly recognized properties are not covered at all, and the time lag between the appearance of data

in original literature and their evaluation for inclusion in a critical compilation has been rapidly increasing. Even in the areas covered

by active projects there has been little coordination or standardization

of format and quality, and in some technical areas there is extensive

duplication.

Recognizing the deficiencies of the existing situation and the stake

of the U.S. Government in the financial support of the Nation's re- search and development activity, COSATI decided that a governmentwide coordinated effort was needed; thereupon it recommended that a proposed plan of action for increasing the level of effort of the

National Bureau of Standards in this field be expanded to encompass

the total Federal effort within all agencies, with administrative re- sponsibility assigned to NBS. Adopting this recommendation, the

Federal Council for Science and Technology and the President's

Office of Science and Technology promulgated a Federal policy

establishing the National Standard Reference Data System

(NSRDS).

The NSRDS is regarded as a subsystem within the concept of the

national measurement system [7], which is envisioned as comprising

a central core of national standards of measurement, a set of consist- ent instruments (calibrated through appropriate application of the

national standards), a body of reference data that provides users with readymade answers to questions on the properties of substances,

11

320-738 O—68 2
and finally the entire set of meaningful measurements made throughout science, technology, and the economy. From this viewpoint,

NSRDS is a portion of the activities leading to dissemination of

readymade data for use by the technical community of the United

States.

Responsibilities of NBS

In accepting the charge from the Federal Council for Science and

Technology, the Bureau has taken responsibility for (i) increasing

the availability of reliable reference data by sponsoring critical evaluation and data compilation projects as needed, (ii) coordinating

related work under the auspices of all Government agencies, (iii) establishing standards of quality for products of the system, (iv)

operating a national center for standard reference data, and (v)

establishing standards of methodology and such other functions as are required to ensure the compatibility of all operational components of

NSRDS. The goals of NSRDS are to be achieved through operation of an integrated network of data-evaluation centers and related projects

located wherever special tchnical competence for a particular project

may exist. Since data can be adequately evaluated only by specialists whose

judgments are accepted by their peers, each data center is to be con- cerned with a carefully delimited technical scope; normally it will

be established as an adjunct to the work of an individual or group

having an established reputation for competence and vigor.

Guidelines have been established to limit the boundaries of NSRDS

and restrict its program to a manageable size. The program is to be

concerned with (i) the data of physical science only (data relating to biological phenomena will be excluded) ; (ii) well-defined sub- stances only (substances whose composition, structure, and energy

content are well enough known that measurements of the property

under consideration do not wander erratically) ; and (iii) well-defined

properties that are intrinsic to the substance or system being studied

(properties that must be defined in terms of the system used for

measurement—such as Brinell hardness and Charpy breaking

strength—are excluded).

Operation of the System

Within the National Bureau of Standards the responsibility for

administering NSRDS has been assigned to the Office of Standard

Reference Data, created for that purpose within the Institute for

Basic Standards. Three major groups of activities within the Office

of Standard Reference Data have been initiated ; these are concerned

with (i) the planning and implementation of projects for compiling

12
data, organized into several broad technical areas ; (ii) an informationsystems design and research activity; and (iii) various specialized

information services to be provided to the technical community.

For program management the data-compilation projects of the

Office of Standard Eeference Data have been subdivided into seven broad subprograms : (i) nuclear properties, (ii) atomic and molecular

properties, (iii) solid-state properties, (iv) thermodynamic and trans- port properties, (v) chemical kinetics, (vi) colloid and surface properties, and (vii) mechanical properties. In each, responsibility for

developing a comprehensive, coordinated program has been assigned

to a program manager. -

1

Existing projects of other governmental and nongovernmental agencies are taken into account, and project priorities are determined by

consultation with groups of specialists from the academic world, Government, and industry. Some of the projects are conducted within the

experimental divisions of the Bureau, others in university laboratories or in other Government laboratories, and a few, by industry. None

is under the direct operational supervision of the Office of Standard

Reference Data, which is intended to provide program management

exclusively.

The raw material for any data compilation project is the results of

measurements by scientists and engineers throughout the world. Normally, these results are reported in the literature, but some will appear

in journals which may be obscure or difficult to obtain. Moreover, an

increasing fraction of results worth saving now appears in Government reports. In some areas (data on neutron cross sections are one example) many of the data generated in the laboratory never appear

in any report or publication. In such instances the compiler personally

may have to pry the data from the measurer. For a specific case, the

degree of comprehensiveness that can be achieved must be a practical

compromise between the desired 100 percent and the cost in time,

money, and effort of achieving that goal. For most existing projects

the comprehensiveness probably reaches 90 to 99.8 percent.

The procedure for "critical evaluation" varies widely from project

to project. In present practice in some data centers, the experimental

technique is reviewed, calculations are spot checked, values of the

fundamental constants are checked to ensure that the latest values were

used, the temperature scale is checked (if appropriate) and limits of

experimental uncertainty are independently assessed. In other centers,

the data evaluator may decide, for intangible reasons that he may find

difficult to formulate, that one particular value in the literature is "better" than another value. Such a judgment by a specialist of broad

experience should not be underrated ; the value obtained is much more

likely to be accurate than the result of unweighted averaging. Most

people agree that the first procedure provides a better "critical evalua13
tion" than the second. However, for the practical purposes to which

many compilations are applied, such a review is not justified, and the

second procedure, or an intermediate one, is employed.

The question arises then, what degree of critical evaluation is re- quired for a compilation to be considered "standard" reference data?

It is probably desirable to use the word "standard" sparingly ; it has

connotations that apply to few existing compilations. For the present,

when measurement results for most properties are uncertain and many

are in dispute, the shorter term "reference data" would avoid the implications aroused by use of the word standard. "Standard reference

data," the ultimate goal of NSRDS, are to be striven for constantly,

but perhaps not reached in many fields for years. Because of the variation in procedures for critical evaluation, all publications of NSEDS

are to describe the criteria used for judgment and the argumentation

used to derive the recommended values.

For each individual compilation project, requirements for continuity

must be examined. The overall program of NSRDS is designed to ensure continuity of effort in the production of data compilations

needed by scientists and engineers. In some areas a revised and updated compilation may be needed every six months; in others, only

every four or five years. In almost all areas, continuing literature re- view and indexing operations are required to maintain a current awareness of the state of development of the field. Therefore, most new

projects undertaken by NSRDS are expected to be long term, continuing activities, maintained as one component of the normal range of

professional activity of the program leader.

LITERATURE REVIEW BIBLIOGRAPHY

INDEXING INDEXED DIDLODRAPHY

Dm EXTRACTION — UNCRITICAL DATA COMPILATION

t

CRITICAL EVALUATION — CRITICAL REVIEW

CRITICAL DATA COMPILATION

CRITERIA

RECOMMENDATIONS

SOLUTIONS TO PRODLEMS

CORRELATIONS

Activities and products of data evaluation centers. 14
The broad types of activities and products that are normally associated with a data center are shown in the figure above. The left-hand

column represents activities, while the right-hand column indicates a product that may result from the corresponding activity on the left. Following the initial selection of relevant papers from the literature

(an activity basic to all evaluation and compilation projects), a bibli- ography may be prepared in which the literature to be evaluated is classified into several relatively broad categories. After the initial selection, the papers are indexed ; this process consists of assigning a number of key words or symbols to each paper to indicate the data

content of the reference. The indexed bibliography resulting from this

activity is very useful to many groups of specialists.

In consultations to determine the needs of the technical community

of the United States for data compilations of all kinds, the staff of the

Office of Standard Reference Data has often been told that an indexed

bibliography would satisfy most of the needs of the specialists, since

many would prefer to evaluate the data themselves and wish only to avoid the labor of locating the sources of the information. However,

this attitude does not prevail among those who need a particular value

for a calculation of some kind and are not themselves involved in

research in the field. The next step in the production of a critical compilation is the

extraction of data from the literature that has been selected. At this

stage an uncritical compilation could be issued, if determined to be

useful to the technical community.

The preliminary activities of literature selection, indexing, and

extraction of data lead finally to critical evaluation. The product of

this work is a critical review of the state of quantitative knowledge in some limited area of a field, or a compilation of critically evaluated

data. For NSRDS, a published product must contain sufficient argumentation for the user to know how results were obtained, as well as appropriate reference to the sources of the data used in the final evaluation.

The original emphasis in NSRDS was on the production of critical reviews and data compilations. Experience has shown that other

evaluated products are of vital importance as well, and data centers are now encouraged to pay considerable attention of them. Of special

significance are "criteria," which may be of three types: (a) criteria

for measurement methodology in the laboratory, (b) criteria for re- porting results in the literature, and (c) criteria for evaluating results already reported.

The physical form of the products of NSRDS activities may be anything considered convenient by the users to whom the product is di- rected ; that is, the product may be a monograph, looseleaf data sheets, a journal article, microfiche cards, IBM punch cards, punched paper

15
tape, magnetic tape, or any other physical form in which information

may be stored. The data-systems design and research activity of the Bureau's

Office of Standard Reference Data is concerned with the problems

of handling data throughout the entire flow process—from the time

measurements are first made in the laboratory, through disclosure

in some form to persons who may use the results (as a journal article, a laboratory report, or perhaps a magnetic tape), through review,

selection, and evaluation procedures in the data center, and finally to dissemination among members of the technical community who have

use for the evaluated product. The use of computers for all practical

operations is emphasized ; such applications to speed the flow of data

from the measurer to the user have only just begun.

Program decisions of the Office of Standard Reference Data have

relied heavily on the advice of a representative cross-section of the

American technical community. As overall program review committee

for the work of the Office, the Executive Committee of the Office of

Critical Tables of the National Academy of Sciences-National Research Council provides policy recommendations and is an important

channel of communication with many segments of the technical community. Program officers in other Government agencies have been consulted to determine the needs of their mission-oriented programs for

the products and services that the standard reference data system is intended to provide.

Considerable reliance has been placed on the recommendations of

panels of specialists in each of the technical areas where a program is being operated ; one or more meetings of ad hoc panels have been held

in each area. Some of these panels are existing committees of the NASNRC, established primarily for other purposes. Others have been

assembled directly at the request of the Bureau. These advisory panels

are now being organized on a continuing basis under the auspices of

the National Academy of Sciences-National Academy of Engineering.

The NAS-NRC Office of Critical Tables has provided frequent

advice on needs, priorities, and other operational details, and has also served as a channel of communication to various segments of the technical community in the United States and abroad. In all, more than

200 leaders of American science and technology have given generously

of their time and experience in helping to make NSRDS most re- sponsive to the needs of the technical community.

General Status of the Program

As a result of the recommendations of advisory panels, greatest

emphasis has been placed on initiation of new projects for evaluation

and compilation and on expansion of old ones, leaving to a future of

greater affluence the implementation of extensive and sophisticated

16
information services. Significant progress has been made, especially in

the areas of thermodynamic and transport properties and of atomic and

molecular properties; these two categories have been judged to be of

highest priority for additional effort. In the field of nuclear data, exist- ing activities sponsored by the U.S. Atomic Energy Commission provide nearly adequate coverage of the technical scope required, although

the level of effort needs to be increased to meet the rapid rate of appearance of new data.

More detail on the activities of the Office of Standard Reference

Data and on the status of specific projects under the cognizance of this

office are described in a recent report by the Office of Standard Reference Data [8],

The Standard Reference Data Act

Initial administrative responsibility for the National Standard

Reference Data System was given to the National Bureau of Standards

by the FCST. This assignment was made in recognition that many of

the broad elements of the proposed national program fell within

already-defined authorities which the Bureau had been exercising for some time. However, the early years of operation of the System

revealed that certain additional authority from Congress would provide increased efficiency in supplementing the program. Seeking such

authority, the Department of Commerce submitted appropriate draft

legislation to the 89th Congress. After public hearings before the Subcommittee on Science, Research and Development (House Committee

on Science and Astronautics), a revised bill was reported favorably

by the full Committee ; it was passed by the House of Representatives

in mid-August 1966. Although the bill did not move to completion in

the 89th Congress, it was resubmitted to the 90th Congress, further

revised by floor action in the House of Representatives, passed by the

Senate and signed into law on July 11, 1968.

The final version of the legislation contains the following provisions

:

( i) a declaration that it is the policy of the Congress to make critically

evaluated reference data readily available to scientists, engineers, and

the general public; (ii) a directive to the Secretary of Commerce to provide or arrange for the collection, compilation, critical evaluation,

publication, and dissemination of standard reference data; (iii) a

directive to the Secretary of Commerce to prescribe standard criteria

and procedures for the preparation and publication of standard refer- ence data, as may be necessary; (iv) authority for the Secretary, or a person or agency designated by him, to sell standard reference data

and to allow the proceeds to be used by the Bureau ; ( v) authority for

the Secretary to obtain copyright, on behalf of the United States as author or proprietor, for standard reference data prepared or made

available under the Act; and (vi) an authorization for appropriations

IT
to the amount of $1.86 million for the present fiscal year, and a requirement for annual authorization for subsequent appropriations.

The authorities indicated in items (iv) and (v) above offer NSRDS

new or modified channels by which to distribute reference data to users and the potential to use these same channels for recovering a

portion of the cost of the program. Study is already underway as to how NSRDS should act to utilize these authorities in the common good.

International Cooperation

Evaluation and compilation of data, on the properties of substances

has been a joint activity of the world's scientists for many years. The

International Critical Tables, produced mainly between 1920 and 1930,

contained contributions from scientists all over the world, coordinated

through the efforts of the National Academy of Sciences. The tables of

Landolt-Bornstein, originally German, now contain contributions by

scientists from many countries. Compilation and evaluation of neutron

cross section data have become a broad international effort, with participation by centers in the United States, Canada, the United Kingdom, France, the Soviet Union, and other countries.

The establishment of NSRDS in the United States has stimulated

additional interest among scientists in other countries on the possibility of developing cooperative programs with scientists in the United

States. Possible cooperation has been discussed with scientists from the

United Kingdom, France, Germany, the U.S.S.R., and Japan. Such

widespread interest leads immediately to the concept of a multilateral

international program, incorporating activities from all countries

wishing to participate. Indeed, multinational cooperation through sev- eral of the international scientific unions has been under way for many

years. The International Unions of Pure and Applied Chemistry and

Pure and Applied Physics and the International Astronomical Union

have been especially active. In June 1966 the International Council of

Scientific Unions created a Committee on Data for Science and Technology (now called CODATA) whose function is to promote international cooperation, to serve as a, channel of communication among

projects in various countries all over the world, to encourage more

scientists to undertake projects of this type, and to make recommendations about needs and priorities to persons responsible for funding such

projects in the various countries.

The second annual meeting of CODATA was held at the Headquarters of the Soviet Academy of Sciences in Moscow on May 31, and

June 1 and 2, 1967, and the third annual meeting in Frankfurt, Germany, June 28 and 29, 1968, both under the chairmanship of Frederick

D. Rossini, Vice President for Research at the University of Notre

Dame. The Chief of the Office of Standard Reference Data was invited

to attend both meetings as an observer and was thereby enabled to learn

18
about numerous data compilation activities in the U.S.S.R. and other

countries.

Membership in CODATA consists of National Members, Union

Members, Liaison Representatives, and Co-opted Expert members.

National Members, as of July 1968, represent Canada, France, Germany, Japan, United Kingdom, USA, and U.S.S.R. Italy and Poland

have indicated their desire to become members. There are eleven Union

Members, five Liaison Representatives and one Co-opted Expert Member—Dr. Guy Waddington, Director of the Office of Critical Tables

of the United States National Academy of Sciences. The Committee is served by a full-time executive staff under the directorship of Dr.

Christoph Schafer, with a Central Office located in Frankfurt,

Germany.

The First International CODATA Conference was held June 30 to July 5, 1968, at Arnoldshain, near Frankfurt, Germany. Approximately 100 scientists and administrators attended the conference, rep- resenting twelve countries.

The International Council of Scientific Unions, the unions themselves, and CODATA are all nongovernmental organizations; however, preliminary informal discussions have also been held regarding

the desirability and feasibility of conducting an international standard

reference data program under the auspices of an intergovernmental

organization, such as OECD, or one of the United Nations specialized

agencies, or a new agency created for the purpose.

Competence and interest in an international cooperative program

for compiling reference data are found in most of the technically developed countries. The products of such a program would benefit any

nation that conducts a research and development effort of any size, not

merely the most highly developed countries. International cooperation

in this area has been a tradition of the world's scientists for at least half

a century, but until recently no mechanisms for overall coordination

and support have existed. Many arguments now favor the vigorous

development of an international cooperative program.

Current Data Project Activity

Accomplishments of the past year, include: a) specific data compilation products published as a result of project efforts, and b) coordination and communication activities involving members of the Office of

Standard Reference Data, scientists engaged in data projects, scientific advisors to NSRDS, and representatives of the user community. These

accomplishments are described below under the headings by which

OSRD classifies its efforts. Nuclear Properties

The Office continued its direct sponsorship of the Photonuclear Data

Center. A supplement to the initial publication of this Center, "The

19
Photonuclear Data Index and Annotated Bibliography of Photonuclear Cross Sections," was published this year. The Office has continued fulfilling its responsibilities in this field by providing assistance to appropriate agencies. The program manager

in this area is a member of the Cross Section Evaluation Working

Group which has prepared a set of evaluated neutron cross sections. In addition, he is a member of the Cross Section Review Committee

of the Defense Atomic Support Agency, has been appointed to the

American Nuclear Society Standards Committee and is Chairman

of its Subcommittee on Nuclear Technology.

The Second Neutron Cross Sections and Technology Conference was held in Washington, March 1968. Sponsored jointly by NBS,

AEC, ANS, and APS, the Conference had as its Chairman the OSRD

program manager for nuclear data, who is also editor of the proceedings of the Conference.

Atomic and Molecular Properties

The Atomic and Molecular Properties area encompasses primarily

property characteristics of individual atoms or molecules rather than

of substances in any specific state of aggregation. A more explicit

indication of the scope of this area is given in the list below.

Major Topics in Atomic and Molecular Properties

Fundamental constants and prop- Information on molecular energy

erties levels derived from spectral data

:

Atomic energy levels a ) diatomic molecules Atomic spectral data b) polyatomic molecules Atomic and molecular x-ray spectral Other well-defined properties of data atoms and molecules Atomic and molecular collision data Transition probabilities Particle-surface interactions Computed functions Plasma properties Interatomic and intermolecular

forces Reference data in this area find application in two broad cate- gories—basic scientific research and the extension of theoretical un- derstanding on one hand, and technological problems, including

analysis and identification of substances, on the other.

General guidance for the Atomic and Molecular Properties program is provided by an advisory panel headed by Dr. E. U. Condon

of the University of Colorado. At the outset, the advisory panel recog- nized that special attention would be necessary in several areas, and

that subpanels of specialists for individual topics should appropriately

be convened to consider needs.

Four specialized advisory groups have met so far: (a) The con- tinuing advisory body on infrared spectroscopy is the Board of Management of the Coblentz Society. This group has met several times

at the request of the Office of Standard Reference Data to provide

20
advice and guidance of several sorts. One of its specific tasks, to prepare criteria for the evaluation of infrared spectra, has led to a report published in the August 1966 issue of "Analytical Chemistry".

In addition, the Board has given advice on the development of infrared spectral data compilation projects at various quality levels, (b)

An ad hoc advisory group on NMR spectroscopy, organized by Dr.

B. L. Shapiro, met in November 1967 in Washington, D.C., to discuss

data needs and possible compilation projects on chemical aspects of

NMR spectroscopy, (c) An ad hoc panel on the application of computers to spectral information was convened on July 24 and 25, 1967,

with Dr. E. K,. Lippineott as Chairman. In addition to recommendations to the Office of Standard Reference Data, this panel provided

discussions leading to a U.S. presentation at the 9th European Congress on Molecular Spectroscopy, held under IUPAC sponsorship

in Madrid, September 10-15, 1967. (d) An ad hoc panel on Raman

spectroscopy, with special concern for techniques involving laser

excitation, met in Washington, D.C., on May 24, 1968.

Most of the data projects in the Atomic and Molecular properties area have issued valuable products. During the past year, the following publications have appeared

:

Publication date

Title Author(s) Publication

Number

9/67 Bibliography of Atomic

and Molecular Processes

for July-December 1965. 9/1/67 Selected Values of Electric Dipole Moments for Molecules in the Gas

Phase.

9/25/67 X-Ray Wavelengths and

X-ray Atomic Energy

Levels. 10/67 Tables of Molecular Vibrational Frequencies, Part

2. 11/30/67 Selected Tables of Atomic

Spectra:

a. Atomic Energy

Levels—Second

Edition.

b. Multiplet Tables.

Si I, Data Derived from

the Analyses of Optical

Spectra.

12/67 Compendium of ab initio Calculations of Molecular Energies and Prop3/68 Tables of Molecular Vibrational Frequencies, Part

3. 4/68 Critical Review of Elec- tron Impact Ionization Cross Sections. 6/68 Tables for the Rigid

Asymmetric Rotor.

L. J. Kieffer ORNL-AMPIC-6.

R. D. Nelson, Jr.. NSRDS-NBS-10.

D. R. Lide

A. A. Maryott

J. A. Bearden NSRDS-NBS-14.

T. Shimanouchi... NSRDS-NBS-11.

C. E. Moore NSRDS-NBS-3

section 2.

M. Krauss. NBS Technical

Note 438.

T. Shimanouchi___ NSRDS-NBS-17.

B. L. Moiseiwitsch. Review of Modern

S. J. Smith Physics, 40, 238-353 (1968). R. H. Schwende- NSRDS-NBS-12.

man. 21
Thermodynamic and Transport Properties

There are 17 currently active projects in the NSEDS program on Thermodynamics and Transport Properties of which 12 are sponsored

by the Office of Standard Reference Data. The topics covered are

:

Chemical Thermodynamic Data on Inorganic Compounds.

Thermodynamic Data on Organic Compounds.

Properties of Molten Salts. Thermodynamic Properties of Ammonia.

Low Temperature Specific Heats. Thermodynamic Properties of Liquid Metals & Liquid Oxides. Phase Behavior in Binary and Multicomponent Systems at Elevated Pressures. Vapor-Liquid Equilibrium in Binary Mixtures of Non-Electrolytes at Low

Pressures. Properties of Electrolyte Solutions. Thermodynamic Properties of Metals and Alloys.

Binary Metal and Metalloid Constitution Diagrams.

Thermodynamic Functions of Cryogenic Fluids,

Thermal Conductivity of Selected Materials Including the Elements.

Viscosity and Thermal Conductivity of Mixtures in the Gaseous and Liquid

States. Transport Properties of Cryogenic Fluids. Thermal Conductivity of Solids at Low Temperatures.

The following reports have been published:

Selected Values of Chemical Thermodynamic Properties, Part 3, Tables for the First Thirty-Four Elements in the Standard

Order of Arrangement, D. D. Wagman, W. H. Evans, V. B.

Parker, I. Halow, S. M. Bailey and E. H. Schumm—NBS

Technical Note 270-3, Jan. 1968.

Thermal Conductivity of Selected Materials, Part 2, C. Y. Ho,

E. W. Powell and P. E. Liley—NSEDS-NBS-16.

Critical Analysis of the Heat Capacity Data of the Literature

and Evaluation of Thermodynamic Properties of Copper, Sil- ver and Gold from 0 to 300 K, G. T. Furukawa, W. G. Saba,

M. L. Eeilly—NSEDS-NBS-18.

Thermodynamic Properties of .Ammonia as an Ideal Gas,

L. Haar—NSEDS-NBS-19.

Annual Index of Worldwide Published Thermochemical Studies.—

As a part of its continuing program on the collection and evaluation of

chemical thermodynamic data, the Thermochemical Data Center at NBS has participated for several years in preparing the Bulletin of

Thermodynamics and Thermochemistry. This annual publication, pre- pared under the auspices of the International Union of Pure and

Applied Chemistry, Commission on Thermodynamics and Thermochemistry, contains listings of thermodynamic work in progress in

laboratories throughout the world and an index to the published

thermodynamic literature of the past year. The current issue of the

22
Bulletin includes over 2300 references, with about 8000 citations to chemical species in the index.

Solid State Properties

This NSRDS program effort embraces the activities of four data

centers covering such areas as crystal properties data, alloy properties

data, cryogenic properties data, and diffusion in metals and alloys.

These centers compile bibliographies and help stimulate the compilation of data related to their area of interest. The Alloy Data Center has now developed and made operational a computerized bibliographic system for the storage and retrieval of in- formation. Its description will soon be published. The Crystal Data

compilation is now in production with approximately 4000 data entries

of Volume I stored on tape for computer-controlled text composition.

Chemical Kinetics

This program area continues to emphasize the preparation and publication of critical review monographs on highly selective subjects.

Two manuscripts have been issued and a number are now being processed for publication. The two which have been issued are

:

NSRDS-NBS-9, "Tables of Bimolecular Gas Phase Reactions" by

A. F. Trotman-Dickenson and G. S. Milne.

NSRDS-NBS-13, "Catalytic Hydrogenation of Ethylene on

Metallic Catalysts" by J. Horiuti and K. Miyahara.

A third publication, "A Method for Estimating the Arrhenius A

Factors for Four and Six-Center Unimolecular Reactions" by H. E.

O'Neal and S. W. Benson has appeared in the Journal of Physical

Chemistry and is the byproduct of an intensive study on the kinetics

of gas phase unimolecular reactions. The effort concerning the evaluation and tabulation of reaction rate data has been enlarged to include

data sheet preparation on the kinetics of those reactions considered

important to related fields such as aerospace and air pollution.

Two data centers continue to perform a valuable service in compiling

and disseminating information in chemical kinetics and radiation

chemistry. The center treating the latter has compiled nine bibliographies in response to author requests and is stimulating the preparation of a data sheet on the decomposition of methane. It also publishes

a weekly reading list of articles in the field of radiation chemistry

appearing in the current literature.

The Chemical Kinetics Data Center plans to issue a bibliography of

kinetic data on reactions of nitrogen, oxygen, and the nitrogen oxides

as well as a compendium of rate coefficients of elementary reactions in

the light elements.

23
/ Colloid and Surface Properites

There are currently six active projects in this area under OSRD

sponsorship. The fields covered are the following

:

Critical Micelle Concentrations of Association Colloids. Electrical Properties of Interfaces. Surface Tension of Molten Salts. Light Scattering by Liquids. Surface Tension Data of Pure Liquids.

Physical Data Pertaining to Phase Transition Kinetics. In addition, there are three projects being carried out under the

auspices of the NAS-NRC Committee on Colloid and Surface Chemistry which will lead to critically evaluated data on heats of immersion, properties of monolayers, and surface tensions of colloidal

solutions. A report on the surface tension of molten salts is in the final stages of review and editing.

Data Systems Design and Development

The Data Systems Design and Development group (formerly called

Information Systems Design and Research) combines interest in computer programming, systems design and application, and data correlation. Earlier experience gained in design and application of a number

of general purpose computing programs (like OMNITAB) is now

providing guidelines for the preparation of general-purpose computer programs for data storage and retrieval, for file manipulation,

and for computer-assisted text preparation, editing, and printing.

There is close collaboration with the NBS Electronic Printing Section

in devising a variety of computer-based systems for more effective use of the Electronic Composing System at the Government Printing

Office. Work in this area can be grouped into three main activities: (a) development of general-purpose computer programs required

for the generation and updating of data files and the preparation of

publications.

(b) design of computer-based data files and retrieval systems which

provide accessibility to as wide a segment of the technical community

as possible.

(c) consultation and advisory services to data centers adhering to NSRDS.

Computer-Assisted Text Preparation and Editing.—Special effort

is being given to the writing of general-purpose compatible computer

programs to exploit the capabilities of the newest computer configurations. Programs and the subroutines they require are being written

in ASA Standard FORTRAN IV. The first release in this series is EDPAC. It contains five programs that have been used extensively at NBS over the last two years. These are called JUSTIFY,

SCRAMBLE, SEARCH, BLOCKSEARCH, and SUBSTITUTE.

24
The characteristics of EDPAC were outlined in some detail in the

NSEDS Newsletter of December 1967.

Automatic Typesetting and Composition of Data Tables.—Experience has been gained in writing computer programs to convert exist- ing data tapes for automatic typesetting of NSRDS publications. One

goal has been to design the programs, insofar as possible, for general

rather than specific applications.

Computerized Data Files.—The design and development of an ex- perimental computerized file of Standard Reference Data for remote

access via teletype has been undertaken. This work will draw on

experience with a variety of time-shared computer systems. Efforts

are being directed toward arranging the subject matter to make files attractive to university computing centers and commercial groups

offering time-shared computer service to schools and colleges. Plans

are to make the subject matter of general use to teachers of physics

and chemistry.

Information Services

Because the major available resources of the NSRDS program have

been applied to the production of compilations and critical reviews, the

development of a vigorous Information Service activity has been delayed. Nevertheless, groundwork for services has been laid and pilot

experience is being acquired. Four basic units of activity for Information Services have been identified : (a) Data File, (b) Compilation

Publication Services, (c) Inquiry Services, and (d) Analysis and

User Relations.

Data File.—The task of this activity has been to acquire known

world-wide data compilations and to organize the collection systematically. The File houses a collection of about 1000 reference data compilations, one of the most extensive collections in the world. General

planning of ultimate methods of indexing, storage, and retrieval

has begun.

Compilation Publication Services.—This activity acts as an editorial

intermediary between OSRD, associated data centers, other individuals

and groups producing data compilations on the one hand, and publishers on the other hand, including the Government Printing Office. In the present reporting period, 13 publications have been produced

and 20 are in process. Inquiry Services.—Plans have been developed for systematic handling of requests for data which may be addressed to any part of the

National Standard Reference Data System. Under these plans, replies

will be obtained by using all of the System's resources—the Data File,

the associated data centers, and experts in NBS. At the present time

25
only limited replies can be provided—referral to a data center or to a

specialist, provision of reference sources, or provision of a pertinent

data compilation or excerpt therefrom are the most common responses. More than 400 inquiries were handled in the past year, and only 28

responses were negative because of lack of information or the unavailability of a likely source of information.

Analysis and User Relations.—The mission of this unit is to provide

OSKD with an understanding of requirements, both present and

future, of NSRDS actual and potential users. It also has the responsibility for providing information on how best to meet user needs and

to develop feedback mechanisms for evaluating services provided. The

unit has a pilot study underway aimed at determining the needs of

scientists in finding and using data.

NSRDS News.—This newsletter first appears as a special section of

the monthly NBS Technical News Bulletin and then is reprinted separately and sent to more than 3200 interested individuals. Regular

features include an updated list of publications from the National

Standard Reference Data System, descriptions of data centers and

compilation projects, and other items of news. THE STANDARD REFERENCE MATERIALS PROGRAM

For more than 60 years, in an era marked by rapid and sweeping

technological change, certified Standard Reference Materials (SRM)

from the National Bureau of Standards have played a pivotal role in

providing a basis for order, stability, and control of the productive

process. In this time the gross national product has multiplied nearly

20-fold, from around $45 billion to some $850 billion. A high-technology civilization has developed, based in large part on the mass

production of goods and services, with requirements for ever-increasing accuracy of measurement, interchangeability of parts, and with

stringent performance criteria for materials of all types. Standards to establish and maintain these criteria form the basis of this technological

process, and NBS Standard Reference Materials stand in the forefront

of the thousands of standards produced and certified throughout the

world.

History of the Program

The Bureau's Standard Reference Materials program began in 1906

when four standard samples, as they were then called, were produced

and certified to help control the quality of cast iron in the U.S.A. With

this start the United States thus became the first country to have a

national standard materials program. Today, this program is being

significantly broadened in line with current needs of science and industry as shown by the more than 650 different SRM's now produced in more than 70 different categories.

26
Both industry and Government, in quest of better quality control,

smoother exchange of goods in commerce, clearer definition of per- formance characteristics, and more comprehensive measurement competences, rely on NBS Standard Eeference Materials as crucial refer- ence points in the establishment of an effective measurement system for

the entire Nation. Through the use of the Bureau's certified SRM's,

science and industry can make onsite calibrations and evaluations of

measuring instruments, methods, and systems in their own laboratories

and plants.

The NBS Office of Standard Reference Materials conducts its program on a self-supporting basis with the full cooperation of industry.

Outputs are increasingly in demand in such fields as metals, minerals,

chemicals, polymers, biological materials, gases, radioisotopes, ores, and ceramics. Among leading customers for some of the 650 cur- rently available SRM's are companies and organizations concerned

with aerospace, oceanography, pollution control, nuclear energy, clini- cal medicine, and such industries as steel, brass, aluminum, rubber,

glass, cement, petroleum,, automotive, chemical, plastic, pharmaceutical, and transportation.

In this day essentially all production is controlled by, and the quality

of output checked through, highly sophisticated instrumentation. Calibration of this equipment so that readings in widely separated plants

and between producer and customer may be referred to a common,

accepted base is one of the large roles played by SRM's. It is because

the properties of NBS—SRM's are, in general, certified on an absolute

basis that they are widely accepted as the primary standards with

which the intercalibration process may be undertaken with confidence.

Instruments calibrated range from pH meters costing $100 or less to automatic reading emission spectrometers ranging in cost upwards of

$75,000. Physical properties measured and certified range from micronsized particle distributions, through density, viscosity, dielectric properties, and Mossbauer effect, to extremely complex property certifica- tion such as thermal emittance. Certification for chemical composition

ranges from a steel SRM where only the carbon content is certified, to a very high purity zinc where more than 20 elements have been measured, some at the parts per billion level. As America's continuing technological revolution proceeds unabated, pressing demands for new Standard Reference Materials in- crease, exceeding resources currently available for their certification. In meeting its responsibilities, therefore, the Office of Standard Reference Materials necessarily exercises a continuous process of judgment

in deciding which new materials should be chosen for preparation and

in what order of priority, so as to serve the best overall interests of

the Nation's science and technology. This task is done only after exten-27

320-738 O—68 3
700

600

500

400

300 h

200

100

0

Number of Kinds of Standard Reference Materials

Available

191 1 1921 1931 194! 1951 1961 1968

sive consultation with various standardizing bodies, industry representatives, and other interested groups.

The total number of standard materials used by science and industry is far greater than the approximately 650 SRM's produced and

distributed by the Bureau, but these and the 120 now in production

have been selected for development on the basis of priority for purposes of technological progress. The NBS Standard Reference Materials serve, in fact, as essential benchmarks to which secondary industrial standard materials are related. In establishing the priority for

the production of a new Standard Reference Material, particular

emphasis is given

• where attainment of needed accuracy of analysis or measurement

of characteristics is not economically or technically feasible else- where, • where industry-wide standards for commerce are needed from a

neutral supplier not otherwise available, • where continuing availability of highly characterized material

from a common source is important to science or industry.

How the Standard Reference Materials program has both expanded

and changed with the times is apparent not only in statistics of the

program's growth but also in the extraordinarily demanding nature

of current applications of high accuracy new Standard Reference

Materials.

In 1910, for example, standards for a half a dozen elements certified to a fraction of a percent were good enough for steel industry needs

28
of the time. Now, in accounting for the uranium content in fuel rods

used in nuclear power plants it is necessary to have a uranium assay

standard certified to 1 part in 10,000. Similar highly accurate SKM's

are currently available from NBS.

Acute needs have developed for new Standard Reference Materials

useful in determining trace levels of many elements, particularly in

high-purity materials such as are used in the transistor and semiconductor industries. The nature of current requirements is illustrated

by the case of high-purity silicon, for which certification of elements

will be needed at or near the level of one part in a billion. In order to measure trace elements at these extremely low levels,

instruments like the spark-source solids mass spectrograph and techniques such as neutron activation analysis have been developed. While

such instruments and techniques are extremely sensitive in detecting

trace elements at the part per billion level, they are often not very

accurate, since until recently SRM's were not available to ferret out

sources of systematic error. Systematic errors of 300 percent, common

as little as 2 to 3 years ago in the use of the spark-source mass

spectrograph at the part per million (and lower) level have now been

reduced by a factor of 10 or more. One of the factors contributing to

this advance has been the issuance of high-purity platinum, gold,

NBS Standard Reference Materials (foreground) are used to analyze alloy

samples on an x-ray fluorescence device. Photograph furnished through the courtesy of the Research Laboratories of General Motors Corporation.

29
zinc, and other similar SRM's, where elements at these very low levels have been measured and certified at NBS. The application of these

SEM's to activation analysis and other sensitive techniques will have

a similar impact.

Standard Reference Materials contribute to progress in every arena

of action from the reaches of space to the depths of the ocean, enhancing the quality of life for Americans at work and at play, in factory

and field, in sickness and in health.

Recently, for example: • At the request of the College of American Pathologists and

the American Association of Clinical Chemists, the Bureau pre- pared a Standard Reference Material for cholesterol in human

blood, helping to correct a situation in which clinical determinations could vary by as much as 25 to 50 percent. This SRM is particularly important in research on the causes and prevention of

atherosclerosis. • For widespread applications in medical research and treatment,

NBS has prepared iodine and sodium tracers of known radioactivity. • To provide reliable analytical methods and standards for purposes of monitoring pollutants under the Clean Air Act, the

Bureau produced Standard Reference Materials for determining

amounts of sulfur in various fuel oils. • NBS-produced standards for detecting long term changes in the

concentration of carbon dioxide in air (having implications in

long range weather changes) are used by the Environmental Sci- ence Services Administration to calibrate monitoring equipment

ensuring that measurements taken over many years can be re- ferred to a common base. • The Bureau's reference materials for metallo-organics in oil are used by the Departments of Defense and Transporation and by

industry to determine engine wear and overhaul needs in trucks,

trains, and planes, allowing for efficient and safe overhaul schedules. By this means, catastrophic failures are averted, lives are

saved, and maintenance costs reduced. • U.S. Customs laboratories check their apparatus against the NBS

sucrose standard in order to levy uniform duties on imported

sugar, whose annual volume amounts to some $500 million. • Transfer of half-a-billion dollars worth of nuclear fuel from the

Atomic Energy Commission to private industry over a two-year

period was based on NBS assay standards. The international control and transfer of fissionable uranium and plutonium are dependent on these standards. These SRM's are vital in the area of

nuclear non-proliferation control.

30
• Microfilm reproduction systems—a business grossing at least $300

million a year—benefit from microcopy resolution test charts developed by the Bureau for evaluation purposes. The Department

of Defense and the General Services Administration use these

standards as a basis for a large portion of their contract

specifications. • Consumer-goods producers of all kinds, particularly in the garment and textile fields, look to the NBS unit known as the

"standard fading hour" as a means of putting all fading measure- ments on a common base. To extend the competence into the Nation's laboratories, the Bureau developed standard light-sensitive

paper and light-sensitive plastic chips. The chips serve to produce

controlled fading at a much accelerated rate, and thus facilitate more rapid tests under simulated natural conditions. • Nuclear instrument manufacturers have begun to utilize three new carbon-14 labeled solution SRM's for liquid scintillation

counting in the standardization and calibration of nuclear instru- ments. The new standards also are important to research workers

concerned with accurate measurements of low-energy beta emitters, and are widely used in medical research. • In cooperation with the electrical, electronics, and aerospace in- dustries, the Bureau has certified six new beryllium-copper alloy

SRM's for calibrating optical emission and x-ray spectroscopic

methods, to help meet critical needs for analytical reference

standards for these widely used alloys. Almost every high-reliability military, space, and oceanographic system uses berylliumcopper alloys in specialized electronics equipment and as components of microminiaturized circuitry. • A new zinc freezing-point Standard Reference Material with a purity approaching 99.9999 percent has been certified by NBS. The

General Conference on Weights and Measures has placed the

freezing point of zinc on a par with the boiling point of sulfur as a fixed point of the International Practical Temperature Scale.

The zinc point is expected eventually to replace the sulfur point on

the Scale.

It is readily apparent from the summary in table 1 that the program

in past years has strongly supported heavy industry—steel, copper,

rubber, etc. This is simply a consequence of the historical development

of this program over the years. However, as rapidly as fimds and re- sources become available, the SRM program is expanding to meet

national needs in health, air and water pollution, resource development and in other critical areas. Experts in each of these fields have

decried the lack of standards and have emphasized that progress will

necessarily be slow until these needs are met. Additional support from other interested Government agencies having direct missions in the fields of health and pollution control, if 31
Table 1. Present SRM Inventory

Category- No. of SRM's

available Typical use

1. Metals, Ferrous

2. Metals, Nonferrous

3. Ores, Cements, Ceramics

4. Organics, Organo-metallics

5. Primary SRM's for pH,

acidimetry, gases, highpurity metals.

6. Nuclear, Isotopic, Radioactivity.

7. SRM's for Thermodynamic

Properties.

8. SRM's for Rubbers, Plastics, Polymers.

9. SRM's for Various Physical

Properties (e.g., viscosity,

thermal emittance).

10. SRM's for Color Specification

and Control.

11. Miscellaneous Total

171

10136

84

35

68

1322

87

Quality control-steel industry.

Be-Cu alloy for aerospace, oceanography.

Control of fineness of cements.

Cholesterol for clinical control. Trace element determinations

in platinum, gold, zinc by

advanced techniques.

Determination of geologic ages by Pb isotopes. Calibration of resistance ther- mometers.

Molecular weight determinations. Control of viscosity of glasses.

50 International color system.

2 Specifications for microcopying. 669 Table 2. Work in process {1168) Percent Thousands

National concern area of total of dollars invested

1. Conservation and Resource Development 6. 0 $92

2. Defense 18. 2 281

3. Health 4.4 68

4. Education (Scientific Advance) 23. 5 363

5. PoUution 1. 3 20

6. Economic Growth 24. 9 385

7. Safety 4. 8 74

8. Space 12. 5 193

9. Consumer Interests 3. 0 46

10. Government Operations 1. 4 22

Total 100. 0 1, 544

forthcoming, will allow significant increases in the production and

certification of SRM's to support these areas. Similar contributions by the N~BS Office of Standard Reference

Materials are planned for other vital applications, including

:

• Standard Reference Materials to be certified in the range of 100

parts per billion for trace metallic elements in blood, tissue, and

botanical matter, as related to such life processes as enzyme catalysis, metabolism, reproduction, cell growth, and aging—for use by specialists in fields ranging from medicine to the food industry. • Preparation and calibration of gas SRM's for sulfur dioxide,

hydrocarbons, and carbon monoxide in air to facilitate measure- ments of some of the most important and highly significant pollu- tants in the atmosphere.

32
• Soda-lime glass SRM's representative of the chemical compositions of more than 90 percent of the flat glass and container glass

being manufactured ; a series of glass SRM's with trace impurities

graded at the 500, 50, 1, and 0.02 ppm as well as a "base level

blank.'* Also clay, plastic, and flint SRM's—all selected in cooperation with ceramics and glass industry representatives to meet

urgent research and production control needs.

Current Activity

The past year has been one of continuing growth in the SRM program, reflecting the increased capitalization in support of the work.

Over 43,000* units were sold to over 4,500 customers both in the United

States and throughout the world. Approximately 25 percent of sales are to foreign customers indicating the international importance of the

program. The dollar value of total sales for FY 68 was $1,022,500.

Table 3 shows how these sales were distributed among the major cate- gories of the SRM inventory.

Table 3. Fiscal year 68 Sales (By Major Category)

Sales Per- Category Units value in cent

sold thousands of total

of dollars sales

1. Metals, Ferrous 17, 543 $438. 1 42. 8

2. Metals, Nonferrous 3, 164 102. 7 10. 0

3. Ores, Cements, Ceramics 2, 812 46. 3 4. 5

4. Organics, Organo-Metallics 3, 019 65. 5 6. 4

5. Primary SRM's: pH, acidimetry, gases, high 5, 122 69. 6 6. 8 purity metals.

6. Nuclear, Isotopic, Radioactivity 1, 225 62. 0 6. 1

7. SRM's for Thermodynamic Properties 991 14.9 1.5

8. SRM's for Rubbers, Plastics, Polymers 4, 173 76. 8 7. 5

9. SRM's for Various Physical Properties 3,341 72.8 7.2

10. SRM's for Color Specification and Control 1, 206 27. 6 2. 7

11. Miscellaneous 1, 667 46. 2 4. 5 Total 43, 263 1, 022. 5 100. 0 During this reporting period 112 new and renewal SRM's were

produced, certified, and placed in stock. The 120 projects now in

progress will produce an additional 268 new and renewal SRM's. The

following pages give in detail the technical story of a representative

sampling of some of these new SRM's.

In a continuing assessment of the needs for SRM's throughout the

Nation and the world, in FY 66 the Office of Standard Reference Mate-

*Equivalent to 70,000 units on the old reporting base. The previous reporting

method distorts the average picture by overemphasizing unit sales of the micro- copy test charts. 33
rials identified 167 SRM's required which would cost $0,060,000 to produce. In FY 67 and 68, the corresponding figures are 226 SRM's at a cost of $12,328,000 and 251 SRM's at a cost of $15,084,000. Present

indications show little or no signs of leveling in demand for new SRM's ; indeed, as standards in the fields of health, air and water pollution, and other relatively new areas are further identified, it is expected

that this demand will move upward explosively.

The following examples have been selected from among the 112 new or renewal SRM's produced and certified during FY 68. The

technical work, spread across 13 technical divisions of the Bureau,

ranged from fairly simple chemical analyses to highly sophisticated

and complex physical and chemical measurements. A great deal of

this work is reported in detail in the NBS technical literature and in

various journals which are referenced in the appendix.

Certified Purity Cholesterol: SRM 911.—At the request of the College of American Pathologists and the American Association of Clinical Chemists, the Office of Standard Reference Materials is now issu- ing cholesterol of certified purity (purity 99.4±0.3 percent) as an NBS Standard Reference Material for use in standardizing clinical determinations of cholesterol. The purity of this cholesterol, estimated with 95 percent confidence,

has been determined by a combination of gas-liquid chromatography,

thin-layer chromatography, and mass spectrometry. The requirements

of the Cholesterol Certification Program of the College of American

Pathologists were utilized in certifying this cholesterol. These include

purification by the dibromide method ; determination of melting point

and carbon-hydrogen content; suitable reproducibility of results using the Liebermann -Burchard technique; examination by gas

chromatography, thin-layer chromatography, and mass, infrared, and

nuclear magnetic resonance spectroscopy ; and testing for the presence

of lathosterol. There is considerable uncertainty regarding the shelf-life of cholesterol. Therefore, the Bureau will continue to examine the stability

of this material over a 2-year period. Any significant changes in

purity that may appear will be reported to users. Platinum Standards: SRM 680 and €81.—Two new platinum standard reference materials, one of high purity and the other doped with

impurity elements at the 5 to 10 ppm level, have recently been issued by

the Bureau.

These standards are available in wire form. Doping was achieved

with a dozen impurity elements at the 5 to 10 ppm (by weight) con- centration level. Both standards are certified for silver, gold, copper,

iron, iridium, nickel, magnesium, oxygen, lead, palladium, rhenium,

and zirconium. In general, values range from a fraction of a part

34
per million in the high-purity platinum standard to about 10 ppm in

the doped standard.

Both standards have been extensively tested and found satisfactory

with respect to homogeneity. The following methods were used : optical

emission spectrography ; spark-source mass spectrography ; and elec- trical measurements, including electromotive force, temperature coefficient of resistivity, and residual resistivity ratio. The recommended

values of the concentrations of the various elements given on the provisional certificate were arrived at after analysis by one or more of

the following methods : optical emission spectrography, spark-source mass spectrography (isotope dilution), polarography, spectrophotometry, nuclear activation analysis, and vacuum fusion.

Sulfur in Residual Fuel Oil: SRM 1621 and 1622.—Of the sulfur

dioxide emitted to the air over the United States in 1963 (greater

than 23 million tons), about two-thirds stemmed from coal-burning

power plants and another 16 percent from residual fuel oil. The

Petroleum Products Survey of the U.S. Bureau of Mines indicates

that No. 6 fuel oil sold in the populous Northeastern area ranges

from 0.52 percent to 2.9 percent in sulfur content. In the West, the

maximum sulfur content exceeds 4 percent.

To provide a base for accurate analysis of fuel oil, NBS has certified two new standard reference materials intended for use in the

determination of sulfur in residual fuel oil. Sulfur was determined gravimetrically as barium sulfate after combustion in a Parr oxygen bomb using 1-gram samples. The method

used is similar to ASTM Method Designation D-129. It differed only

in that any iron present was removed with ammonium hydroxide before the precipitation of the sulfur as barium sulfate. Standard Light-Sensitive Papers: SRM 700b and 701b.—Standard

light-sensitive paper and booklets of faded strips of this paper are now

available for use in standardizing the dosage of the radiant energy

from commercial carbon-arc lamps. The standards in the 701b booklet

have been faded by exposure to the NBS master lamp in amounts cor- responding to stated numbers of "standard fading hours" of exposure

between 7 and 25. The standards were calibrated at NBS and the paper

from which the standards were prepared was made in the Bureau's

paper mill, and was dyed with the direct azo dye, Benzo Azurine G,

Color Index No. 24140.

The use of the light-sensitive paper standard is intended to correct for moderate variations in radiant flux. Given the same electrical operating conditions, and similar carbons, the radiant flux emitted by the

carbon-arc fading lamp is assumed to be reasonably well controlled

with respect to spectral distribution. By using NBS Standard Nos.

700b and 701b it is possible to translate clock hours of exposure in

lamps to "standard fading hours" (SFH) based on the average results35
Some of the many available Standard Reference Materials and associated

publications.

of 130 exposure tests using different carbon-arc lamps. Thus it is possible to express the dosage of radiant energy on a common basis in differ- ent laboratories.

Turbidimetric and Fineness Standard: SRM UJ^L.—A renewal of

the NBS Portland Cement, turbidimetric and fineness standard, designated NBS Standard No. 114L, has been prepared and certified. This

standard may be used to calibrate such devices as the Blaine Air

Permeability Apparatus according to Federal Test Method Standard

158, Method 2101, or ASTM Designation C204, and the Wagner

Turbidimeter according to ASTM Designation C115. It may also be

used to determine sieve residue with a No. 325 sieve according to ASTM

Designation C430. These tests are used throughout the cement industry

in the U.S. and abroad to control production of cement to specification

requirements. Many other uses are developing as the value of particle

size control is recognized in a given industry or application.

First issued about 35 years ago, more than a quarter of a million

units have since been distributed : No. 114X« is the fourteenth renewal

of this standard. The standard is now supplemented with calibrated

glass sphere standards which extend the particle size range for which

NBS standards are available.

Isotopw Standards for Lead: SRM 981-983.—Lend isotopic meas36
urements are used in measuring the age of rocks, meteorites, the earth,

and mineral deposits—the latter often of great economic importance.

Knowledge of the relationship of meteorites to the earth and understanding of the geologic origins of mineral deposits, can be gained

by the measurement of isotope ratios with accurate mass-spectrometric

techniques. To advance knowledge of the nature of geological processes

such as volcanic action, mountain formation, ore deposition, and the

chemical composition of the earth's interior, accurate comparison of

data from different laboratories is necessary. This requires standards

for calibrating mass spectrometers, now used extensively in this

important work, so that lead-isotope data can be compared on an

absolute basis. Three new lead isotope reference standards, designated NBS Nos.

981, 982, and 983, have been prepared. They will allow laboratories

to calibrate instruments over the range of isotopic compositions en- countered in nature, and to study the performance of their instruments.

They are also useful as "spiking" additions for determining lead, as well as for calibrating mass spectrometers.

NBS Microcopy Resolution Test Charts: SRM 1010.—Since December 1, 1967, the microcopy resolution test charts issued by KBS

have higher spatial frequencies than those issued previously. The old

type was designed in 1963 and had 21 patterns of black bars on a white

background ranging from 1 to 10 cycles/mm. These patterns were

arranged to permit the extension of the chart to include higher spatial

frequencies. The new type has five additional patterns with spatial

frequencies of 11, 12.5, 14, 16, and 18 cycles/mm.

American industry and Government spend about a third of a billion

dollars annually to microfilm records and preserve films. To assure

that the microfilmed images are of adequate quality to store the re- quired information, microfilm contracts generally stipulate that the

resolving power of the complete microfilming system be evaluated by

means of NBS microcopy resolution test charts. The charts are placed

in several locations on the camera copy board and are photographed

in the same manner as a document to be recorded. The resulting image

is then examined with a microscope. The number of cycles/mm in the

smallest pattern in which the bars can be counted with reasonable assurance is the resolving power of the system.

Oxygen-in-Nitrogen Standards: SRM 1601^-1609.—The NBS Office

of Standard Reference Materials prepared a new series of gaseous

standards containing concentrations of oxygen in nitrogen over the

range from about 1 ppm of oxygen up to the level of oxygen in the

atmosphere.

The new standards are supplied in units of 68 liters at a pressure of

500 psi in disposable gas cylinders. The preparation and certification of

the oxygen-in-nitrogen standards required the development of new and

37
modified analytical methods for determining oxygen in gases. These

methods made possible the certification of the oxygen contents of the

standards to one relative percent or better at all concentration levels. Standard Reference Metallo-Organic Compounds.—A series of

metallo-organic standards were developed at the request of the Division of Kefining of the American Petroleum Institute. At first, the

principal users of the metallo-organic standards were the railroad and

trucking industries. Here the analysis for metals in lubricating oils was

used as the basis for maintenance schedules and predictions of equipment failure. Agencies of the Department of Defense also utilize the

tmetallo-organics for safeguarding equipment and for minimizing

maintenance and repair costs. Newer uses include monitoring the

presence of catalyst metals and catalyst poisons in process streams. The amount of wear and the probability of failure of an internal

combustion engine may be determined by analyzing its lubricating oil for metals. Such analysis is done with the optical emission spectrometer. Because accurate predictions ordinarily are made on the basis

of trends in data accumulated over a period of time from a series of

determinations, it is necessary to have standard reference materials

for calibrating the apparatus. These standards must be stable, oil- soluble to the concentrations needed, and must not absorb an excessive

amount of water. They should yield solutions in lubricating oil which

are constant and which will not precipitate on standing.

The certificate furnished with each SUM gives the amount of the

metallic element of interest that is present, and also provides directions

for preparing a solution of known concentration in lubricating oil. References and Notes

[1] Tate, F., Chem. Eng. News 45, 78 (1967).

[2] Williams, V. Z., Hutchisson, E., Wolfe, H. C, Phys. Today 19(1), 45 (1966).

[3] Speight, F. Y., and Cottrell, N. E., The EJC Engineering Information Pro- gram—1966-67 (Engineers Joint Council, New York).

[4] President's Science Advisory Committee, Science, Government, and Infor- mation, January 1963 (Superintendent of Documents, Government Printing

Office, Washington, D.C. 20402).

[5] Goudsmit, S. A., Phys. Today 19(9), 52 (1966).

[6] Throughout "data" may be taken to mean the numerical results of measure- ment of the properties of substances.

[7] Huntoon, R. D. (Director of the Institute for Basic Standards, NBS),

Address to the Standards Laboratory Conference, NBS, May 1966 (Office of Technical Information and Publications, NBS, Washington, D.C. 20234).

[8] Brady, E. L., Ed., NBS Tech. Note 448, Status Report, National Standard

Reference Data System, April 1968 (Superintendent of Documents,

Government Printing Office, Washington, D.C. 20402).

38
INSTITUTE FOR BASIC STANDARDS

The Institute for Basic Standards (IBS), one of three institutes

which comprise the National Bureau of Standards, has as its first responsibility the provision of "the central national basis for a complete, consistent system of physical measurement properly coordinated

with those of other nations." As a second responsibility IBS develops

and maintains standards for physical quantities and for the measure- ment of physical properties. In concert with the Bureau's Institute for

Materials Research, and the Center for Radiation Research, IBS

shares the responsibility for providing physical data on the properties

of matter and materials.

Implicit in the assignment of the first responsibility is the recognition that there does exist a national system of measurement and that

this system is a centralized one, with a central laboratory which develops and maintains the national standards for physical measurement

and provides the starting point for a chain of measurement leading

from those standards to the ultimate users of the system. This chain

must provide for measurements of all necessary magnitudes, from the

properties of atoms to those of the universe.

From the point of view of the ultimate user who faces a measure- ment problem, such as finding the diameter of a ball bearing or the

melting point of a metal, the measurement chain can operate in two

different ways: (i) It can provide the user with a proven measure- ment technique or with a calibrated instrument, traceable back to the

national standards, with which he can measure the diameter or the

melting temperature, (ii) In the case of the melting temperature or

other similar properties, it can provide him with an immediately

available answer in the form of critically evaluated data which pre- vious investigators have obtained in measurements based on the

national standards.

As the Nation's central measurement laboratory, NBS exercises

leadership in both these measurement areas. In the Bureau's laboratories the acquisition of standard reference data by precise measure- ment goes on side by side with research to develop and improve the

national standards and associated measurement methods.

PHYSICAL QUANTITIES

The strength and utility of the national measurement system depend

fundamentally upon the existence of a complete, consistent system of

units and standards around which the system can develop. The In-39
ternational System of Units (SI), denned by the 11th and 12th General Conferences on Weights and Measures, is the base for the international system of measurement and for most national systems. Six

of these SI units—the kilogram, meter, second, degree Kelvin, ampere, and candela—are the arbitrarily chosen values of six quantities

of the physical world—mass, length, time, temperature, electric current, and luminous intensity. Consistent units for other quantities may

be derived from these, with appropriate values fixed by the units

selected for the basic six. The English system—pound, inch, second,

degree Fahrenheit, etc.—and other systems of units are related to the

SI units by definite conversion factors. The research at NBS on physical quantities is concerned with the

establishment of these units by international agreement, the realization

of the standards which represent them, and the development of a chain

of measurement from these standards to the multiples and submultiples needed by our technologically based society. These activities offer an exciting field of technical endeavor which reaches to the frontiers

of science and technology. Indeed, the state of sophistication of the

U.S. national measurement system is an important gage of the scope

and utility of our science and technology. The results of some of the

work in this area are described below; part of the effort involves a

collaboration with other groups, and is described in the Technical

Assistance to Others section.

International Base Units

Length

International Comparison of Laser Wavelengths.—A joint report on

independent measurements performed at the National Physical Laboratory, Physikalsich-Technische Bundesanstalt, and NBS on commercially available wavelength stabilized helium-neon lasers was pre- pared and published. The test results showed that unless a specific laser

is calibrated, the uncertainty in the wavelength is at least ±1 part in

107

. Agreement on a given stabilized laser can be within ±5 parts in 109. Laser Length Standard,.—The effect on laser output at 3.39 fxm of

placing a sample of low-pressure methane inside the laser cavity has

been investigated. Saturated absorption resulting in increased laser output power occurs when the laser is tuned to the center of the Doppler-broadened methane absorption line. A linewidth for the emission

peak in the laser output of 2 parts in 109 was obtained which is a step

toward demonstrating the feasibility of this technique as a highly ac- curate standard of length.

Laser Action on Non-Losing Transitions in an Atom.—The exact frequency at which lasing action takes place in a gas laser has been

40
NBS apparatus used for recent international comparison of laser wave-length.

shown to modify the frequency distribution in other, non-lasing lines

in the same laser. The detailed analysis of this phenomenon and the

phase coherence of a series of cascading transitions predicted an asymmetrical effect on the line shape of the cascading lines. Experiments

have been performed to demonstrate this asymmetry.

Time and Frequency

Atomic Second Adopted as International Unit of Time.—A new

definition of the international unit of time, the second, was adopted

Friday, October 13, 1967, in Paris by the 13th General Conference on Weights and Measures. The second has now been defined in terms

of a characteristic rate of electromagnetic oscillation of the cesium133 atom.

Speaking for the governments represented, which include those of

all the leading scientific and industrial countries, the Conference

agreed overwhelmingly that the moment had come to replace the

existing definition, based on the earth's orbital motion around the

sun, by an "atomic definition."

The Conference decided that

:

The unit of time of the International System of Units

is the second, defined in the following terms: "The second

is the duration of 9,192,631,770 periods of the radiation cor- responding to the transition between the two hyperfine levels of the fundamental state of the atom of cesium-133."

and abrogated the resolutions giving the earlier definition.

41
Time and Frequency Services.—Standard frequency and time broadcasts continued at VLF, LF, and HF from WWYL, WWVB, and

WWV in Ft. Collins, Colo, and at HF from WWVH in Maui, Hawaii. Antenna efficiency for WWVL was increased 30 percent by an improved ground system. Eadiated power from WWVH to the Far

East was increased with a corresponding decrease in interference on

the U.S. mainland by installing reflectors to modify the radiation

pattern.

Frequency-Time Dissemination Research.—Time and frequency

have the unique characteristic that NBS can distribute them to users by means of standard radio broadcasts. To meet the increasing needs

for accuracy in the methods of dissemination, research is underway

on new and improved methods. One potential time distribution system

being investigated is the use of satellites. Using the VHF trans- ponder aboard the ATS-1 satellite, clocks at NBS (Boulder, Colo.),

and NASA (Mojave, Calif.), Anchorage, Alaska, and Piteairn Island

in the South Pacific were compared with an accuracy of better than

10 /is. In other experiments a clock at NBS (Boulder, Colo.) was

compared with a clock at Goldstone, Calif., to an accuracy of about

5 fis by using the moon-bounce radar system developed by Jet Propulsion Laboratories.

Improvement of the NBS Frequency Standard.—Design and most

of the construction have been completed for major modifications to the

present NBS Frequency Standard. It is expected to have an accuracy

of about 5 X 10~13 and a precision of 1-2 X 10-13 for 1 s averaging

times. The design makes use of computer-optimized beam optics.

Improvement of the NBS Frequency Standard.—In order to exploit

effectively certain ideas relating to the stability of atomic frequency

standards, NBS and the Hewlett-Packard Company are jointly developing a new cesium beam tube. The design, which is based on the use

of computer-optimized beam optics, and most of the construction have

been completed.

Flicker Noise Sources in Electronic Devices.—A system has been

developed and tested for measuring the degradation in short-term fre- quency stability of a signal processed by various electronic devices.

Initial tests established the present state of the art for low noise, solid state devices and indicated that near the signal carrier, flicker noise

rather than normal thermal noise is the limiting behavior. The use of

this test system in the development of new signal processing dev^s

indicates conclusively that a 25 to 35 dB reduction in the flicker noise

level of conventional devices is possible by the use of relatively simple

design criteria. This reduction has been achieved in the construction of

two frequency multiplier chains to be used with the NBS Frequency

Standard.

42
Temperature

Josephson Effect Thermometer.—The need for accurate temperature

measurements in the 0.001 to 10 K region has been increasing steadily.

Since traditional methods are difficult to use, especially below 1 K, new concepts are being considered, one of which offers the promise of

a direct measure of absolute temperature without a calibration comparison. The concept is based on the measurement of thermal noise

detected with the aid of the Josephson effect, which occurs when two

superconductors are connected by a weak junction. Preliminary experimental results have demonstrated the feasibility of this type of

thermometer.

Device being investigated for absolute temperature measurement in the 0.001

to 10 K region. The arrangement of wires on the rectangular metal block is the adjustable Josephson junction (arrow) ; voltage bias and thermal noise

are supplied by the resistor (right).

Cerous Magnesium Nitrate Temperature Scale.—Cerous magnesium

nitrate (CMN) has been gaining widespread use as a medium for

obtaining and determining temperatures below 2 K. Since previous

studies on this salt have provided a temperature scale of somewhat

questionable reliability, a reinvestigation of the temperature scale was

undertaken, and a relation between the thermodynamic temperature

and the magnetic susceptibility of a single-crystal sphere of CMN

was deduced. The results disagree with earlier measurements, but are

in reasonable agreement with recent work obtained by a different

method.

43

320-738 O—68 1
Improved Thermometer Calibration Service.—An improved cali- bration service is now available for standard platinum resistance

thermometers. Recent improvements in techniques and apparatus per- mit a wider variety of such standard thermometers to be calibrated more accurately and in a much shorter time than before. The calibrations over most of the range from 10 to 900 K can now be made with

errors of less than 0.002 K. The turnaround time for this service has

been reduced to six weeks.

Nuclear Quadrupole Resonance Thermometer.—The nuclear quadrupole resonance frequency of 3

5

CI in KC103 in the temperature range

12 to 297 K has been measured. The frequency appears measurable to

sufficient accuracy to yield uncertainties of ±1 mK in the range 50

to 297 K, ±4 mK at 30 K, and ±10 mK at 20 K.

Liquid Hydrogen Vapor Pressure-Temperature Scale.—Using

germanium resistors as transfer thermometers, vapor pressures of

equilibrium liquid hydrogen in the temperature range 13.8 to 20.3 K

have been directly related to values of temperature on the Thermodynamic Temperature Scale as realized by the NBS Acoustical Thermometer. Thus a temperature Scale of liquid hydrogen vapor pressure versus temperature has been realized. The results were of particular

value to the Comite Consultatif de Thermometrie and aided in the

Comite's deliberations which resulted in a new International Practical

Temperature Scale. The new scale terminates at 13.8 K ; the previous

scale terminated at 90 K.

High Temperature Gas Thermometer.—The high temperature gas

thermometer at NBS reached operational status. It is a constant volume type, employing a 500 cm3 Pt-20 percent Rh bulb with helium

as the thermometrie fluid, and is designed to determine corresponding

values of temperature on the Kelvin thermodynamic and International

Practical Scale every 50 deg between 273 K and the gold point, 1336 K.

So far the apparatus has been used at 273 K and 373 K. The measure- ments were reproducible to within 1 ppm of the absolute temperature

(±0.0004 K at the steam point) for each of the initial pressures of

10, 20 and 30 cm Hg. The stability of the thermometer was demonstrated by repeatability of the results when the thermometer bulb was

cycled between 0 and 100 °C over time periods up to 6 days. Exact

values of thermodynamic temperature will be computed when measure- ments of apparatus characteristics are completed.

Improvement in Optical Pyrometer Calibrations.—The accuracy

with which high precision automatic optical pyrometers can be cali- brated has been improved by a factor of about 3. Typical standard

deviation uncertainties now range from about 0.3 deg at 1063 °C to 44
1.0 deg at 2000 °C and 4 deg at 3500 °C. A major factor in this improvement has been the development of a very stable blackbody which

can be operated to about 2500 °C and is used to transfer the International Practical Temperature Scale from the NBS Photoelectric Pyrometer to the test instrument. Another significant contribution in

reducing the uncertainties has been the development of a special type

composite filter whose transmittance is an insensitive function of

temperature. These niters are now being used in high precision commercial pyrometers and make the higher ranges of these instruments

significantly more stable. Copper-Point Blackbody.—The long-term instability of pyrometer

lamps used in high precision automatic pyrometers has created a need

for a stable inexpensive source of optical radiation for monitoring

these lamps. A simple furnace and blackbody, stabilized at the melting

temperature of copper, has been developed for this purpose. The source

requires no inert gas or vacuum, and utilizes only 225 watts to reach a melt about an hour after turn on. The blackbody can be stabilized at the copper point to within 0.1 °C for 10 min or longer. Using the

standard sample copper available from NBS, the radiance temperature

of this blackbody source has been determined to be 1083.3 °C with an

uncertainty of about 0.1 °C and a reproducibility (standard deviation

of a determination) of 0.01 °C.

Electron Density Determination from Spectral Line-Profiles.—The

number density of electrons in gases at high temperatures is a temperature sensitive quantity useful in measurements above 10,000 K for

many common gases. When the high temperature source contains some

hydrogen, the electron density can be obtained by determining the

spectral line profile of the Hg line at 4861 A and by using the theoretical calculations of Griem et al. The accuracy of 10 percent claimed for

these calculations has recently been confirmed by measurements on a high current atmospheric pressure arc in argon seeded with hydrogen.

Under conditions of thermodynamic equilibrium at atmospheric pressure, the maximum attainable electron density in argon is 2 X 1023 m-3 at 16,700 K. Arcs operated with higher axial temperatures exhibited

Hp line profiles which at their off-axis point of maximum broadening

agreed with the theoretical profiles for this electron density well within

10 percent uncertainty of the theory.

Electric Current

Absolute Ampere Determination.—The value of the NBS ampere was determined in absolute measure, using the recently modified NBS

Pellat-type dynamometer. The ratio of the NBS ampere (derived from

the units of emf and resistance as maintained by the NBS reference

standards) to the absolute or theoretical ampere (defined in terms of

45
the mechanical force between current-carrying conductors) was found

to be Anbs/A= 1.000010 ±0.000007. The stated uncertainty represents

the estimated probable error (50% confidence interval) resulting from

all known sources, the estimate being based on measurement repeatability. This result, together with other recent absolute determinations

of the electrical units will be considered by an International Committee later this year in reassigning the units of emf which are maintained

by the various national laboratories.

International Comparison of Capacitance Standards.—Three stable 10 pF fused-silica capacitors constructed in 1964 continue to be cir- culated to various national laboratories for comparisons of the unit

of capacitance. The most recently completed circuit was NBS, NSL

(Australia), ETL (Japan), and NBS. Values in the NBS laboratory

at the beginning and end of this circuit agreed within a part in 107

, indicating that the construction is adequate for international comparisons. The group of standards of this type held at NBS have now

been under observation for more than three years and appear to be

stable within this same limit. Interlab oratory Agreement of Electrical Measurements.—Statisti- cal experiment designs and methods for data analysis were provided

as part of the Bureau's collaboration with the Air Force on precision

electrical measurements. The designs are used in carrying on an interlaboratory comparison of calibrations and for methods of transporting

voltage standards.

Interlab oratory Transport of the Unit of Voltage.—The National

Bureau of Standards and the U.S. Air Force undertook a joint study

of the interlaboratory transfer of the unit of voltage. The two major

objectives of the program, both of which were achieved, were to reduce

the uncertainty of the assignment of the local unit and to reduce the

time required to make the assignment. Using the present method, six to eight weeks are generally required to assign the unit with a stated

uncertainty of 1 ppm. The techniques developed in this program

reduce the time required to about two to four weeks with an overall

uncertainty of approximately 0.5 ppm.

Fundamental Physical Constants

The Faraday.—An analysis was made of differing values of the

Faraday—most of which have been determined at KBS. Values obtained by silver deposition, iodide oxidation, oxalate oxidation, the

omegatron, and silver dissolution were reviewed. All values were

converted to the unified 12 C international scale of atomic weights

using the international atomic weights of 1967. The value determined

46
by dissolution of silver in aqueous solutions was shown to be least subject to uncertainties. A value of 96,487.0=1=1.6 coulombs per gramequivalent was recommended.

Laser Velocity of Light Measurement.—Important progress has

been made in the refinement of laser stabilization and control as applied to the measurement of the velocity of light. The method involves

measuring the difference in wavelength and frequency of two laser

lines very accurately and using these measurements to calculate the

velocity of light. Three important steps have been taken: (1) the 51

GHz photobeat between a pair of laser lines at 1.15 /mi has been measured, (2) the stability of the 30 m interferometer has been studied

using a laser which is locked to a stable 30 cm reference cavity, and

(3) apparatus has been developed which allows locking an auxiliary

laser at a known variable frequency offset from a reference laser. Mechanical Quantities

Adiahatic Saturation Psychrometer,—NBS has developed an

adiabatic saturation psychrometer for measuring the humidity of

gases. This instrument can also be used to determine the vapor content

of a vapor-gas mixture. The psychrometer behaves in accordance with

predictions deduced from thermodynamic considerations, and has considerable potential as a standard for meteorological use. Since it yields a direct measurement of "thermodynamic wet-bulb temperature," it should have application to measurement problems in engineering fields,

particularly in air conditioning. In the chemical engineering field, especially in several of the process industries, the instrument can be used to measure the vapor content of various vapor-gas mixtures.

Wide Range Vibration Generator.—Piezoelectric vibration generators (shakers) have been developed which produce motion suitable for

the calibration of vibration pickups over a frequency range of 1 to 60

kHz. These shakers incorporate highly elastic, highly damped coupled

resonators with overlapping resonant frequencies, and they produce

relatively good motion over a wide frequency range. Indications are

that these techniques can be extended to frequencies of at least 100 kHz.

The measurement of small amplitude, high frequency mechanical

vibrations is especially important in the scale model testing of large

complex structures such as space vehicles.

Hydrostatic High-Pressure System.—A cylindrical high-pressure

liquid container which uses a polyethylene liner to seal the highpressure liquid has been developed. The container can be pressurized in

almost any conventional piston and die press and used to perform

PVT and ultrasonic measurements on liquids and solids immersed in

47
liquids at pressures as high as 45 kbar. Electrical leads have been

brought into the high-pressure container in order to determine elec- trical properties of materials as a function of pressure. Ultrasonic

measurements with water pressurized in the liquid container were used

to compute the density of water at 22 °C to 12.6 kbar. The estimated

uncertainty of these measurements is 0.004 kbar.

Microphone Test Calibrations.—A new method for performing test calibrations on standard condenser microphones has been developed.

The method makes use of the reciprocal properties of NBS reference

standard microphones. Instead of making a direct comparison of the

test microphone against the reference standard using a third microphone as a sound source, the standard is used as a source and the test microphone as a receiver. Only one reading is necessary to measure

the response of the test microphone at each frequency rather than

two as previously required. Test calibration time is reduced by up to one-half.

Fatigue Crack Detector.—Fatigue tests of high strength aeronautical fasteners loaded in double shear require detection of the fatigue

crack in the fastener before catastrophic failure of the fastener occurs. A detector with associated circuits was developed which senses the

change in stiffness of the fastener while it is subjected to cyclic loads. The heart of the device is a linear-variable-differential transformer

whose output is recorded and which automatically causes termination

of the test a few hundred cycles after the crack initiates. In most cases, the resulting crack is too small to be visually detected but its presence

is verified using a dye penetrant.

Volume Changes Accompanying the Extension of Rubber.—As

part of the effort to determine how to include the effect of compressibility in a general, nonlinear, constitutive equation, the volume

changes accompanying extension of peroxide vulcanizates of natural

gum rubber have been measured with a dilatometer. These volume

changes, of the order of 10-4 cm3 /g for 100 percent extension, were measured with a precision of ±2 percent. Measurements of forceextension behavior and compressibilities were made on the same

samples. Though a constant compressibility described the results obtained using isotropic pressure, the volume changes accompanying

extension were not proportional to the isotropic part of the stress. Thus, the strain energy in extension cannot be separated into a sum

of two parts, one due to the shear and one to the dilatation.

Determination of Structural Damping.—Structures such as turbine

blades, air frames, and rocket housings require not only optimum

strength but also proper damping characteristics. A method to deter- 48
mine the damping coefficient of structural metals has been developed.

Vibration tests of mass-loaded, cantilever-beam specimens were made

in air and in vacuum. The method utilized a knowledge of the effects of mass-loading to normalize the experimental data to fit a nondimensional curve of transmissability—the ratio of free-end to fixed-end

beam displacements.

Cryogenic Flow Research.—A program is being developed for an

analytical and experimental verification of the performance of exist- ing flowmeters under well defined reproducible conditions. Work is also underway to develop recommended measurement practices for use of these meters in cryogenic systems, and to investigate new commercial metering devices. Implementation of these objectives

will provide Government and industry with a centralized research

facility for the study of cryogenic flowmetering problems. The program was established under sponsorship of NBS and the Compressed

Gas Association. The joint sponsorship by CGA provides international support for the program as this trade organization represents

six of the largest cryogenic producers in the United States as well as cryogenic producers in England, France, and Germany.

Swirling Flow Study.—The presence of swirling flow can at times

have significant influence upon the accuracy of flowmeters, including

turbine and differential-pressure types. However, the behavior of

swirling flow fields is not well known. Cooperative studies with the

University of Maryland Department of Mechanical Engineering on

turbulent, incompressible swirling fields in long, cylindrical, unobstructed pipes show that the angular momentum flux decays ex- ponentially along the pipe at a rate of about 3 percent per pipe dia- meter. Also, the rate of decay increases slightly as the Reynolds number decreases in the range from 200,000 to 12,500. Information from

these studies will aid in an improved description of swirling fields in

which the performance of flowmeters can be evaluated.

Electrical Quantities—DC and Low Frequency

Improved lOfiQO-Sl Resistance Calibrations.—For half a century

standard resistors of the "NBS Type" have been widely used in electri- cal standardizing laboratories in a range of nominal values extending

from 1 O to 1 Mo. Demands for better standards at kilohm resistance

levels having stability comparable to the l-O level are being met with

improved 10,000-0 standards recently developed by several manufacturers. NBS has developed methods and constructed apparatus for

calibrating these improved standards with a total measurement uncertainty of 1 ppm. This uncertainty applies to the calibrated value

(given to the nearest 0.001 O) in terms of the legal unit of resistance

maintained with l-O standards. To obtain this increased accuracy,

49
better methods for scaling resistance values have been developed utiliz- ing so-called "Hamon Devices" for multiplying resistance values

100-fold from 1 to 100 to 10,000 O. In practice, the accuracy of these

devices approaches the theoretical limit (ratio uncertainty a few

parts in 109 ). Cryogenic Parametric Amplifier-Detector.—A null detector for

audio-frequency capacitance bridges has been developed. The device,

which utilizes solid-state varactor diodes, permits an increase in meas- urement resolution up to a factor of five over conventional units. Operated at room temperature using a signal frequency of 104 rad/s, a minimum noise figure of 0.01 dB was obtained; at liquid nitrogen

temperatures, noise figures below 0.001 dB (referred to a room temperature source) were measured.

/Standard Cells.—Seventeen Vosburgh-type, saturated Weston standard cells were constructed and their emf's measured from 5 to 40 °C.

This type of cell (Bi added to Cd-Hg anode and double salt CdS04

* Na2 S04 -2H2 0 added at both electrodes) has an emf (1.018690 Y) at 25 °C which is almost the same as the conventional, saturated Weston

cell (1.018393 Y), but it has a lower emf-temperature coefficient: + 13.5 /aY/°C compared with —49 /*Y/°C for the conventional type.

This cell is expected to have a long-range emf stability.

Voltage-Ratio Measurements.—The "boot strapping" technique for

evaluation of inductive voltage dividers has been further improved

in accuracy and expanded in frequency coverage. It is now estimated

that an accuracy of 2 parts in 107 is obtainable for 5 and 10 kHz

calibrations, and a few parts in 108 for 400 and 1000 Hz calibrations.

Since it is a self-calibration method, the technique does not rely on any national standards, so it may be used by any laboratory with

equal validity.

High-Voltage Pulse Measurements.—A Kerr electro-optical system

for measurement of high-voltage pulses has been developed and cali- brated. This system permits time-resolved measurements of pulses

with peak amplitudes as high as 100kY. Simultaneous pulse divider

and Kerr system measurements of pulses as high as 100 kY have indicated that the Kerr system is accurate at least to the same degree as the pulse divider (to within 1 percent) . With further refinements, it is anticipated that the system will be useful as a standard for calibration of pulse dividers and that it will permit measurment of transient

voltages considerably in excess of 100 kY.

Stable 10 kV Power Supply.—A stabilized adjustable high-voltage

supply with a direct current capacity of 10 mA has been built for use 50
in an absolute volt determination. Its drift rate, measured over time

intervals greater than a minute and extending to more than 10 hr, is less than 1 part in 107/hr. For shorter times (1 s to 1 min) the peakto-peak: deviations from the mean are less than ±2 parts in 107 at 10 kV. Facilities are included to permit accurate measurement of the

output voltage of the supply against standard cells. Stark-Effect Voltmeter.—Work has begun on the development of

a voltage standard at the 10 kV level based on the Stark effect of

molecular radio frequency spectra. An ultimate precision of 1 part

in 106 is being sought ; absolute accuracy depends upon the accuracy

to which the electric dipole moment of the working molecule is known.

Initial experiments were performed with a beam maser spectrometer.

Following successful performance tests, the maser was modified for

Stark effect measurements on the TJHF spectra of hydrogen cyanide

(HCN), formaldehyde (H2 CO) and deuterated water (HDO).

Electrical Quantities—Radio Frequency

Radio Standards from 30 KHz up to and including microwave,

millimeter wave, and laser frequencies are provided by the Radio

Standards Physics Division, the Radio Standards Engineering Division, and the Time and Frequency Division of NBS, located at Boulder, Colo. These groups conduct basic and applied research leading to standards for important radio quantities (such as power, pulsed

quantities, attenuation, and noise) and to standards of frequency and

time. They also perform calibration and broadcast services which dis- seminate standards to industrial and Government laboratories.

High Frequency Region

$ MHz Noise Calibration.—A new calibration service for noise meas- urements at 3 MHz was completed and announced. The service is for

thermal and shot noise generators having a noise temperature in the

range from 75 K to 30,000 K. The service is capable of a maximum

uncertainty in the measured value of noise temperature of approximately 1 percent. This is the first announced service for noise in the

high frequency region and in coaxial systems. It uses a new technique

of measurement for which a patent has been issued. Noise is an important quantity in many areas of the radio electronics field. The

sensitivity of a receiver is ultimately limited by the noise which it generates internally and receiver sensitivity, in turn, directly influences

how soon a missile is detected or how well a deep space probe

functions.

Improvement in Coaxial Power Measurements.—A new rf-dc substitution calorimeter with automatically controlled dc reference power

51
has been developed that allows improved accuracies of measurement

in the lower power ranges. The new standard extends the range of the

existing coaxial reference standards in the frequency range below

1 GHz from 50 mW to 10 mW making possible the direct calibration

of 10 mW bolometer mounts. The measurement range of this new

standard is from 10 mW to 1 W at frequencies up to 4 GHz and

beyond. Maximum measurement uncertainty is 0.35 percent. This

standard was designed so that it can be connected to digital equipment

for direct automatic recording of measurement data.

Superconducting Transmission Lines.—A miniature, 80-foot coaxial

line (Nb inner conductor 0.01 in O.D., Pb outer conductor 0.034 in

I.D., polytetrafluoroethylene dielectric) has been anlyzed in terms of

the Gorter-Casimir two-fluid superconductivity model considering the

anomalous and classical cases (without relaxation effects) for the

normal component. The line attenuation 10s to 1016 Hz and the step

response from 1 to 100 ps have been calculated for the temperature

range 2.3 K to 10 K. This analysis, and its comparison with the

experimental results from other independent investigators have es- tablished the bounds between which the responses of physically real- ized superconductive lines will lie. Additionally, the results present

a method of identifying the purity of the conductors in a coaxial line

of this type. The study of coaxial transmission lines at superconducting temperatures is important because of their ability to transmit

pulses over long distances with minimum degradation of pulse shape

and also because of their potential for transmitting large amounts

of power with a minimum of loss. Automation of High-Frequency Power Measurements.—The highfrequency, coaxial bolometer calibration console was fully automated

with the addition of a small on-line computer. This enables the collect- ing, compiling, and computing of the output data from the console to yield the final calibration result. The calibration time has been

reduced by one-half, as has imprecision of the measurement. The

human error involved in compiling and computing the output data

has been eliminated.

Peak Pulse Power Calibrations.—Calibrations of coaxial peak pulse

power meters in the frequency range 300 to 500 MHz have been es- tablished in the range of 1 mW to 2.5 kW peak power. The pulse

width can be calibrated in the range from 2 to 10 /as with a pulse

repetition rate of 100 to 1600 pulses/s, and a maximum duty factor of

.0033. Peak pulse power measurements are important in the determination of output power from such devices as radar systems and pulsemodulated information transmission systems,

52
Portable Current Standard.—A small reference standard of radio

frequency current has been developed which can serve as a high ac- curacy, interlaboratory standard. The ammeter is unique and has no

precedence in principle of operation. It consists of a cylindrical, ellipsoidal silver reflector of infrared energy with a cylindrical thin-film

quartz heater along one focus axis and a heat sensing thermopile along

the other. The heater forms an extension of the center conductor of a

coaxial line, and the ellipsoidal reflector forms an extension of the

outer conductor. The ammeter has three times the current range of

previous devices, up to 10 times larger output for a given sensed cur- rent and unequaled broad-band frequency range. The prototype covers

the range from 0.5 to 5 A. The dc output corresponding to 0.5 A is approximately 1 mV and that corresponding to 5 A is approximately

100 mV for currents in the frequency range of dc to 1 GHz. The

ammeter is the first to use coaxial transmission line design which makes

it compatible with 50-O coaxial systems without introducing additional uncertainties. The ammeter may also be useful as a wattmeter

or voltmeter in special circumstances.

THERMOPILE

ELLIPTICAL REFLECTOR

NBS-developed reference standard for interlaboratory comparison of radio

frequency current. HF Electrodynamometer Accuracies Determined.—The high-frequency short-circuit ring electrodynamometer developed at the NBS

Boulder laboratories has been more accurately analyzed as a result of

a new technique for obtaining the ratio of the torque on the ring to the

current on the transmission line. Application of this technique to the

electrodynamometer has shown it to be capable of measuring currents

5f
over the frequency range 1 MHz to 1 GHz within the following limits

of uncertainty : at 1 A the uncertainty is within ±0.06 percent, and up

to 100 A it is within ±0.5 percent.

A New Standard of Voltage, Current, and Power.—A new standard

of voltage, current, and power, referred to as the "Bolovac," was developed for lumped-constant, coaxial, and other circuits operating in the

TEM mode. Its approximate ranges are 1 MHz to 20 GHz in frequency,

0.05 to 10 V, 5 mA to 10 A and corresponding power levels in 50-O sys- tems. A thin film conducting element located in the transverse plane of

the TEM mode is the principal sensing element of the device.

Broad Band Inductive Voltage Divider.—A new technique has been

devised for making broad band inductive voltage dividers of the 2 to

1 ratio type. This type of divider, which has a ratio of input voltage to output voltage of 2

n for cascaded transformers, has had until now a very high accuracy only at a fixed frequency. The new technique compensates for the voltage drop across the leakage impedance by placing

a small impedance between each transformer and ground. By making

this small impedance from the same type of cable used to construct the transformers, it can be made to compensate for the leakage impedance over all frequencies for which the transformers are usable ; i.e., 1 kHz to 1 MHz. The work shows that it is now possible to build a cascaded inductive voltage divider of this type with uncertainties in

the order of 10~5 over the entire frequency range.

Radio Frequency Standards Comparator.—An rf standards comparator, capable of providing standards of radio frequency at the

user level has been developed. The comparator consists of a voltmeter,

ammeter, power meter, and an impedance bridge combined in a compatible, 50-12, coaxial system in which the measured values of any one

instrument can be compared to results obtained from the other three. Intercomparison of the electrical quantities of power, impedance,

voltage, and current is possible over the frequency range from 30 MHz

to 1 GHz with a precision of about 0.1 percent. These quantities are

related mathematically, so that if any two are known the remaining

two may be computed ; if three are known, a redundancy exists which

permits a self-checking system. If all four quantities are known, a double redundancy exists which adds an extra degree of confidence

to the standards.

Microwave Region

Low Temperature Noise Standard.—An X-band (10 GHz) thermal

noise source has been developed. It consists of a waveguide termination

in a cryogenic environment along with temperature and pressure monitors and controls. The effective noise output at the room temperature

54
flange can be set to the boiling point of helium (4.2 K) with an

accuracy of ±0.03 K. The noise source can also be used with liquid

nitrogen as the coolant for which the effective noise output temperature is then approximately 77 K with an accuracy of ±0.16 K. Temperature stability is 0.002 K for helium, and 0.02 K for nitrogen. At

present, the useful accuracy of the standard is approximately 0.1 K;

the primary source of uncertainty is the insertion loss (approximately

0.001 dB) of mating room temperature flanges.

Microwave Noise Measurement.—A technique has been developed

for the comparison of low temperature microwave noise sources independent of their reflection coefficients. At a noise-source temperature

of approximately 77 K, noise-power output of sources with reflection

coefficients as high as 0.5 can be compared within uncertainty limits

of ±0.1 percent relative to a noise standard. This technique can be

applied at any microwave frequency range for which three-port cir- culators are available, and at higher noise-source temperatures.

Microwave High Power Measurements.—A technique has been developed for calibrating directional coupler bolometer units used for

high-power microwave measurements. The technique virtually elimi- nates mismatch errors, reducing the uncertainty in the calibration of

high coupling ratios from 15 to 1.5 percent. Because it employs existing

power measuring equipment and standards, it should lead to wide adoption and use by industry.

International Attenuator and Impedance Comparisons.—Attenuation measurements were compared with those of Sweden. The comparison was made on a variable attenuator in WR 90 waveguide at a frequency of 9.0 GHz. Agreement was within 0.03 dB for most values

measured. The first phase of an intercomparison of impedance standards with Italy has also been completed. The reflection coefficient magnitude of a WE. 90 fixed waveguide reflector was measured at 9.0, 9.8, and 11.2 GHz.

Electromagnetic Field Standards

Near to Far Field Antenna Pattern Calculations.—Work on the

establishment of methods to calculate far field antenna patterns and an- tenna gain from near zone data is rapidly approaching successful completion. The results of additional experimental data indicate a strong

probability of success. Computer programs have been developed which

allow the far field to be represented in a graphic projection of three

dimensions. Successful completion of this work will result in a signifi- cant saving in the cost of determining the far field of large aperture

antennas. 55
Measurement Capability m Field-Strength Calibrations.—The ca- pability for measuring field- strength and other precision receivers from

1 to 10 GHz has been completed and announced. This new service in- cludes calibrating such receivers for use as two terminal rf voltmeters,

calibration of signal attenuators, and calibration of overall receiver

linearity. The rf voltmeter calibration is performed in terms of coaxial

power standards, and attenuation and overall linearity measurements

are accomplished using the rf substitution method. With this new meas- urement capability, the frequency range of the field-strength receiver

calibration service is 30 Hz to 10 GHz.

New Calibration Services

The following is a complete list of services completed and an- nounced during FY-68:

• Reflection Coefficient Magnitude in WE 284 and WE 42 Waveguide, • Power Measurements of Bolometers and Bolometer-Coupler Units

in WE 284 Waveguide,

• Reflection Coefficient Magnitude for Non-Reflecting Waveguide

Ports in Waveguide Sizes WR 284, 187, 137, 112, 90, 62, and 42, • Phase Shift Measurements of Variable Phase Shifters in WR 90

Waveguide,

• Power Measurements of Bolometer Units in WR 28 Waveguide,

• Improved accuracy of Coaxial Impedance Standards in the range

1-8 GHz,

and the following, which have been discussed in detail above: • Peak Pulse Power, • 3 MHz Noise, • Extended Frequency Range for Calibration of Field Strength

receivers.

Thermal Quantities

Thermal Expansion Measurements.—Equipment is now available

to measure linear thermal expansion of solids from 10 K to 1,900 K.

Materials under consideration for standard reference samples (e.g., copper, fused silica, and sapphire) have been measured over this ex- tended temperature range. In the range from 10 to 1,200 K, a dual

interferometric apparatus was developed to measure the samples to an

accuracy of 1 fxm/m. From 1,100 to 1,900 K a comparative technique was developed with an accuracy of 30 /mi/m, the most accurate

available in this temperature range.

56
Photometric and Radiometric Quantities

Continuous Wave Laser Power Meter.—A photoelectric meter was

constructed for measuring the power output of CW lasers. The cali- bration factor of the meter was determined by four radiometric techniques: (1) a filter radiometer calibrated with an KBS lamp standard

of spectral irradiance, (2) a prism spectroadiometer similarly cali- brated, (3) a radiation thermopile calibrated with an NBS lamp

standard of total irradiance, and (4) an absolute radiometer calibrated

by eleccrical heating. The resulting calibration factors of the meter were consistent to ±2 percent. Although this work involved a particular 80-mW He-Ne laser operated at a 6328 A, the techniques are applicable to a much larger class of calibration problems. In addition,

the results obtained indicate the consistency of the calibrations of

NBS standards of spectral and total irradiance with each other and

with the electrical unit of power, the watt. Laser Energy Power Measurements.—A calorimeter containing

aqueous CuS04 and designed to measure pulsed laser energies to 10

J/em2 at peak power to 200 MW/cm2 has been developed. In the energy

range 1 to 100 J, a comparison with other energy measuring devices

indicates an accuracy of ±2 percent. Intercomparison of calibrated

calorimeters suggests a precision of 0.7 percent. In addition, the

average power of CW lasers can be measured in a similar manner with an indicated accuracy of ± 4 percent.

Infrared Laser Power Measurements.—A new type of calorimeter

utilizing an absorbing gas as the heat transfer medium has been de- signed and built. The device will be tested on a CW 50 W C02 -N2 -He

commercial laser. Initial calculations indicate that 100 and 1000 W

sources can be measured without major modification.

Production of Side-Bands on Visible Light.—Visible light from a helium-neon laser has been modulated at a microwave frequency of 10

GHz and the two resulting side-bands have been observed. The effect was produced by placing a crystal of KDP within the laser cavity

and also in a microwave cavity excited by a 10 GHz microwave

oscillator. The output light from the laser was observed to contain not

only the normal 6328 A red light, but also two sidebands, one at a wave

length corresponding to the frequency of the red light plus the micro- wave frequency, the other at the difference frequency. An output of

1012 photons per second was observed in this side-bands.

New Image Converter.—A new way of seeing and photographing

objects by invisible infrared and ultraviolet rays has been demonstrated. When energy from an object was focused on a special plate, a57
color change occurred at the image, making the image visible. The

plate, which may be used repeatedly, was prepared by laser exposure

of a high-resolution photographic emulsion in contact with mercury.

The standing wave pattern of interference of the incident and reflected beams was recorded in the emulsion which was then developed. The

color of such a plate is so sensitive to relative humidity that the slight

change in local humidity due to an infrared image is readily seen. The new principle has been demonstrated only under laboratory conditions but offers promise of very simple and economical devices for a number of infrared and ultraviolet applications.

Standard Detectors for the Vacuwrrb Ultraviolent.—An investigation

into the day-to-day reproducibility of the photoeleotron yield of

materials in the vacuum ultraviolent has been initiated. Given a material with adequate stability, a calibrated sample could serve as a transfer standard detector for use in this region. It has been discovered

that the yield of materials is extremely sensitive to the degree of surface

contamination present. Thus far, studies have eliminated some

materials from consideration because of excessive sensitivity to ambient

temperature or to storage history. Other materials are showing promise

for use either at ambient temperature or at temperatures sufficiently

high to preclude the influence of contamination from the vacuum sys- tem housing the sample.

Photodetector Calibration Service Expanded.—Calibration of

photodetector response can now be performed over the spectral region

0.35 to 1.8 fxm with a resolution of approximately 3.5 nanometers in the

visible region and 7 nm in the near infrared. The relative spectral re- sponse of a photodetector can be measured for unmodulated (dc) light, or for light modulated (ac) at ten fixed frequencies from 1 Hz to 1 kHz. The absolute spectral response can be measured at certain fixed

wavelengths. Uncertainties in spectral response are less than ±3 per- cent of peak response for relative measurements and less than ±5 per- cent of peak response for absolute measurements.

Infrared Spectral Radiance Calibrations.—A blackbody and spec- troradiometer have been developed which are capable of determining

the spectral radiance of 500 to 1300 K test blackbodies between about

1 and 4 /*m with an estimated uncertainty of 0.1 percent or the equivalent of 0.4 K, whichever is greater. The reference blackbody consists of

a 1.5 mm thick graphite cavity embedded in copper, and the spectroradiometer consists of an f/4 prism monochromator, a liquid nitrogencooled PbS detector, a "lock-in" amplifier, and means for precisely

orienting and translating the blackbody sources. The thermometer

presently being used to determine the blackbody temperature is a primary-calibrated platinum versus platinum-10 percent rhodium

58
Photodetector response is calibrated by this machine which measures detector output under monochromatic light swept across part of the electromagnetic

spectrum.

thermocouple. This work has been largely motivated by infrared re- quirements in the Department of Defense, and NBS is working with

the Newark Air Force Station to establish the capability of accurate infrared radiance calibrations.

Evaluation of Lenses for Aerial Color Photography.—Aerial color

photography is finding increasing application in agricultural and

geological surveys, mapping, and reconnaissance. To evaluate lenses for such uses, the camera calibration laboratory at NBS has been

equipped to expose color materials to test patterns illuminated by light

of the three primary colors employed in color photography. The

59

820-738 O—68 6
images can now be evaluated separately. Three normal color films and

one false color film have been used in the evaluation of resolving power,

chromatic aberration, and field curvature of seven lenses in wide use

or of advanced design.

Standard Nomenclature for Radiation, Light, and Color.—Members of the NBS staff directed efforts that led to the publication of

USA Standard Nomenclature and Definitions for Illuminating Engineering. Although this standard (ZT.1-196T) was developed for il- luminating engineering, it is of even greater interest in the fields of

photometry, colorimetry, and radiometry because it contains terms,

definitions, and symbols in these fields that are entirely consistent

with those adopted by committees of the International Commission

on Illumination, the International Organization for Standardization,

the International Electrotechnical Commission, and the SUN Commission of the International Union of Pure and Applied Physics. This

is the first standard published in this country, and possibly in the

world, that contains up-to-date terminology in the fields of photometry, colorimetry, and radiometry of such widespread acceptance that

it can reasonably be expected to remain authoritative for many years. Survey on Colorimetry.—A review of the field of colorimetry has

been completed and made available. This review includes, in addition

to subject matter retained from earlier documents, the most important

recent developments in colorimetry : the large-field supplementary ob- server system, the new sources that represent daylight, and the

treatment of colorimetry as a measurement science with associated

uncertainties.

Universal Color Language Applications.—The ISCC-NBS method

of designating colors, now known as the Universal Color Language,

has become the link between simple color designations (red, blue,

yellow, green) and the numerical specifications of color. It consists

of six levels of precision to supply the appropriate degree of accuracy

in color designation needed by science and industry. NBS utilizes this system to help those with color problems. Two examples of its use this year are the color designation system of the Manual of Photogrammetry of the American Society of Photogrammetry, and the

12-color code for highway signs in the Manual on Uniform Traffic

Control Devices for Streets and Highways. Special attention was di- rected to the needs of colorblind drivers ( about 3 percent of all drivers)

during the development of this new code.

Flattery Index Proposed for Lamps.—People and materials look worse than they really are under some lights, and better than they

really are under others. There is an international method for measur60
ing the degree to which a lamp succeeds in rendering object colors

truthfully. This method has now been modified to indicate how well a lamp succeeds in flattering them. This "flattery index" is under

study by the Committee on Color Rendition, Illuminating Engineering Society, for validification and refinement before being recom- mended for practical use. Theory of Chromatic Adaptation.—Two objects which look like

they have the same color to the eye (i.e., a matched pair) do not necessarily reflect light in the same wavelength pattern. If one stares at a

colored light of moderate brightness and then looks back at the

matched pair of objects, the match remains but the perceived color

changes. When this colored light is very bright, not only does the

perceived color change, but also the match is lost. In an attempt to understand these facts about color matching in terms of changes

occurring in the visual pigments of the eye, a mathematical study of

the bleaching of pigments in solutions was undertaken. It was found

that if the pigments absorb between 55 and 85 percent of the light to which they are most sensitive, it is possible to account for both the

match breakdown at high brightness and the match preservation at moderate brightness in terms of pigment bleaching alone.

PHYSICAL PROPERTIES

Approximately half of the activity within the Institute for Basic

Standards is related to the measurement of physical properties of

well-defined substances. The rapid growth of the physical sciences

has provided scientists with many new techniques for measuring "old"

physical properties and has made accessible many new ones. With new

techniques it has been possible to increase the precision of measurement, provide the scientific community with a greater range of refer- ence data, and characterize certain processes more fully. Examples of

these activities, drawn from current work, are given below.

Atomic and Molecular Properties

Absolute Electron Scattering Gross Sections.—Further development of electron scattering apparatus has now made possible the

absolute measurement of differential cross sections to an accuracy of

about 5 percent. Absolute measurements in helium for 2

XP excitation

and for elastic scattering have now been completed. Together with

very precise (about 1 percent) measurements of angular distributions,

the absolute measurements show that contrary to previous assumptions, the Born approximation is not valid at 400 eV, either in absolute

magnitude or in the shape of the angular distribution.

61
Radio Plasma.—The abnormal negative glow plasma in helium has

been adapted for a more thorough investigation of the microwave

cavity technique used to measure electron density in plasmas. The use

of this plasma, in combination with a low frequency microwave cavity,

has generated an acceptable situation for experimental and theoretical

investigations of the influence of longitudinal modes on the microwave

measurements. A double perturbation technique allows for evaluation

of the microwave field within the plasma and for an extension of the

cavity measurements beyond the limits of the simple perturbation

method. Present data indicate that use of the microwave technique as interpreted by the simple perturbation theory is more limited than

accepted in the literature due to the presence of excited longitudinal

modes not accounted for by the theory. The double perturbation tech- nique has in some situations extended the limits for the measurable

electron density by one to two orders of magnitude.

Absorption Spectra in Rare Gases.—Effort has been directed at the analysis of absorption profiles of resonances in the photoionization continuum; analysis of the energy position and profiles of the resonance structure for neutral argon has been completed. Work has

been facilitated by digitizing the transmission data and punching it onto paper tape suitable for computer processing, thus eliminating the

tedious job of hand data reduction. A least squares computerized

parameter fitting routine has been devised to analyze the data, taking

into account the smearing effect that the monochromator slits have on the transmission.

Regularities Among Atomic Oscillator Strengths.—During the

course of a critical compilation of atomic oscillator strengths from

data in the literature, many regularities among these data were detected and systematically investigated. Three principal regularities

have been found: (a) systematic dependency of oscillator strengths on

the nuclear charge for a given transition within an isoelectronic se- quence, (b) systematic variation of oscillator strengths in spectral

series with oscillator strengths usually rapidly decereasing with in- creasing quantum number, and (c) approximately constant oscillator

strengths for certain analogous lines in homologous atoms. These regularities have become a very useful and important tool for analyzing the

reliability of existing data and have made possible the determination

of many additional oscillator strengths by simple interpolation

techniques.

Theoretical Calculations of Atomic Oscillator Strengths.—Extensive calculations of atomic oscillator strengths have been made using

the method of configuration interaction to obtain the atomic wavefunctions. Such refined calculations have become necessary since recent 62
experiments show that configuration interaction effects may drastically change the oscillator strengths of certain transitions As many as 50 configurations are used to express the electron correlation, and /- values with an accuracy generally in the 25 percent range have been

computed for C I, C II, Al I, Si II and the magnesium and boron

isoelectronic sequences. Some more traditional configuration interaction calculations have also been made to study the absorption oscillator

strength distribution in perturbed Rydberg series. These latter calculations predict, for aluminum, the existence of an autoionizing state which takes up most of the oscillator strength.

Calculated Atomic Transition Probabilities.—The transition array

of atomic oscillator strengths has been calculated for Ti II using

methods which are an extension of Racah's method for energy level cal- culations. For the first time it was possible to include configuration

interaction in these calculations, and it was found that configuration

interaction strongly influences the energy level structure and the oscil- lator strengths for many of the atomic transitions. For a group of

transitions, the ^/-values which were calculated are within 10 percent

of the experimentally observed values, and in general within 30 percent of the observed values of King and Wobig. The calculations have

pointed out that some of the experimental values were obtained under

optically thick conditions.

Conversion of Translational Energy.—One of the most important

but least studied processes which occur in hot gases is the conversion

of translational energy of participating atoms and molecules to internal energy. This process is important in determining chemical reaction

rates and rates of collisional processes in stellar atmospheres and laboratory plasmas. A measurement technique has been developed involving resonance fluorescence which is applicable for certain simple cases, and which may provide important insight into the general significance

of the collisional transfer of translational energy to internal atomic

energy.

"Red-Shifted" Spectral Lines.—A "red-shifted" spectral line is usually interpreted as an indication that the emitter and the observer

are receding from each other. It has now been shown that red-shifted

lines can be formed by an emitting gas that is expanding toward the

observer with a positive velocity gradient. Although the resulting

apparent shift is too small to be of cosmological interest, this mechanism does appear to explain red-shifted lines seen in certain nebulae.

Atomic Spectra.—Accurate measurements in the vacuum ultraviolet region have resulted in improved wavelength and energy level data for the spectra CI i, CI n, S i, and Mg m. For CI i more than

63
1100 lines were determined to ±0.001 A, an accuracy sufficient for

reference standard wavelengths for most work in the region below

2000 A. Knowledge of the atomic energy level structure has been significantly improved for the complex spectra Tc i, Ce i, Pr hi, Pm i, Tm i, Tm n, and Th i. For several of these atoms the new results include the energies of some of the lowest and most important elec- tronic configurations. A large plane grating spectograph, with a resolving power of 500,000, has recently been completed and will be

used to observe complex spectra.

Photodetachment of Negative Ions.—The photodetachment of

H3 02~ (H2 0-OH_

) has been studied in detail because of its possible

importance in the control of electron density in the upper atmosphere.

The initial results lend increased support to the speculation that

water may play a significant role in the physics and chemistry of

the upper atmosphere.

Molecular Gas Laser Studies.—Studies have continued on the

fundamental processes involved in molecular gas lasers. More HGN"

laser transitions have definitely been identified and all of the known

DCN laser transitions have now been explained. Energy transfer

mechanisms as related to laser systems are also under study. Fluorescence lifetime measurements were made on the 001 level (the upper

laser level) of N2 0 in order to determine the rate of collisional deactivation of that level. Infrared fluorescence measurements were also made on several other molecules. Some double resonance measure- ments were made by using a 50 W C02 laser as a pumping source and

observing the effect on rotational levels monitored by means of a micro- wave spectrometer.

New Method for Sputtering by Low-Energy Ions.—Ultraviolet

absorption spectroscopy together with low temperature matrix isola- tion has been used to study the energy levels of selected metal atoms

and their oxides. In this connection a low-energy sputtering process was devised for the production of metal atom samples. The technique involves the production of low-energy rare gas ions in a micro- wave electrodeless discharge followed by the bombardment of a metal

sample by these ions. The process permits controlled production of

metal samples which may be difficult to produce by other methods

in a low temperature environment.

Grossed Beam Study of Photodissociation Gross Section of H2 +

.—

Crossed beam techniques have been used to study the photodissociation cross section of H2+ from 2537 A to 13,600 A. The method provides

a new tool for studying energy partition in dissociative collisions of

electrons with more complicated molecules, and gives fundamental

64
knowledge of the simplest molecule, H2+

, important in controlled

thermonuclear research, laboratory plasmas, and astrophysics. Calculations have also been made, and close agreement is found between

theory and experiment. Disparities can be attributed to differences

between actual and theoretical populations of the vibrational levels of H2\

Electron Impact Spectrometer for Air Pollution Studies.—Recent improvements in electron impact spectrometers at NBS have made

it possible to implement the suggestion that the characteristic energy

losses of electrons upon scattering be used as an analytical method.

Using the improved apparatus, carbon monoxide in air was detected

at concentrations of less than 100 ppm. This spectrometer is competitive in sensitivity with the best currently used instruments and

very considerable improvements in sensitivity and compactness are

possible.

Spectrum of the 010 Free Radical.—Using a new spectrometer

built for the study of free radicals, the microwave spectrum of the

CIO radical has been observed for the first time. Rotational transitions of the 2 n3/2 and 2 n1/2 electronic states of 35C10 and 37C10 were

measured. These studies gave new information on the A-doubling

parameter and the hyperfine constants, and an improvement by a

factor of ten for the values of the bond distance and dipole moment

for the states of the radicals.

Vibrational and Rotational Spectra of Simple Molecules.—Infrared

and microwave spectra have been studied in a number of molecules

which have features of special interest. New measurements have been

made of certain unusual transitions in the microwave spectrum of

HCN, OCS, CH3 CN, and HCCCN. The gas phase spectra of

CH3CI and CH3I have been studied in detail to determine the effect of certain vibrational and rotational interactions. These same transitions have been studied in matrix isolated solid spectra to determine

how the interactions differ in the solid phase. New infrared measure- ments have been made on gaseous HCN to improve knowledge of

the energy levels involved in laser action in the HCN laser. Molecular Energy Levels of Carbon Monoxide.—A detailed analysis of the vacuum ultraviolet absorption spectrum of carbon monoxide

has been completed. The so-called Fourth Positive System is the most

prominent feature of the spectrum in the region from 1100 to 1600 A.

It has particular significance because of the recent observation of

this band system in the solar spectrum. In addition to providing improved values for the energy levels and molecular constants of the

states of carbon monoxide involved in this transition, the analysis

established the existence of a maximum in the potential energy func65
Electron impact spectrometer for the study of the characteristic energy losses of electrons in gases. This device is now being investigated for use in air pollution studies.

tions of the first excited electronic state of CO. Knowledge of the

magnitude of this potential maximum is of interest because of the

great importance of the value of the dissociation energy of CO in

thermodhemical studies.

Alkali Molecular Spectra.—Several lines of the argon-ion laser excite definite vibrational-rotational levels in an upper electronic state of Na2 , Rb2 and N~aK, causing a relatively simple fluorescence spec- trum. Using a Fabry-Perot interferometer crossed with a spectrograph, this spectrum was investigated and molecular constants, potential curves and Franck-Oondon-factors were determined. This method

66
allows a high accuracy because single lines can be resolved. Since the

high laser intensity creates a high population in the upper molecular

states, one can measure the lifetime and angular-momentum coupling

condition of these states with level-crossing techniques.

Solid State Properties

Electron Paramagnetic Resonance.—A technique was developed for

the measurement of fast paramagnetic relaxation times which employs the Optical Faraday Rotation. This technique was used to measure the relaxation time of paramagnetic Eu2+ in CaF2 :Eu2+ at cryogenic temperatures.

Theoretical Magnetism.—It was shown that any theory of magnetism based on a one-particle distribution function, such as the Weiss

molecular field theory, is inconsistent if it assumes no correlation between spins. The consistency condition, a direct consequence of equilibrium fluctuations, was invoked to provide a measure of two-spin

correlations, thereby implying a two-particle distribution function

compatible with the one-particle Weiss distribution. The resulting

theory is exact at high temperatures for evaluating such inherently

two-particle quantities as heat capacity.

Various effective field techniques for the study of magnetism, appropriate for the Ising interaction, were examined with an infinite chain used as the basic cluster. These theories were found to offer no

substantial improvement over the analogous theories using very small

clusters. Nuclear Magnetic Resonance.—A new parametric nuclear spin sat- uration technique has been developed using 27A1 nuclei in ruby. With

the proper orientation of the tf-axis with respect to the external magnetic field and rf magnetic field, magnetic Am= ±2 nuclear spin transitions were observed. The theoretical calculation of this effect gave

excellent agreement with experiment, and indicated that Am=±3

and ± 4 magnetic transitions should be observable.

Field-Electron Studies of Adsorbed Atoms.—When atoms are adsorbed on a metal surface, the highest electron energy level of the atom

is shifted upward and broadened into a band which may be several

electron volts wide. Recently, it was predicted that the distribution

in energy of electrons field-emitted from a metal through single atoms

on the metal surface would reveal information about the shift and

broadening of the atomic energy level. Experiments conducted with

single strontium atoms on an oxygen-coated tungsten surface verified the theoretical prediction and established the feasibility of obtaining information about the interaction of atoms and surfaces with

this technique.

67
Electronic Characterization of High-Purity Metals.—A strong cor- relation between low temperature electrical resistance and chemical

purity has been shown for many metals. To exploit this fact an

eddy-current apparatus has been developed and refined to allow rapid

determination of the residual resistance ratio, which is the ratio of

the electrical resistance at the ice point to the resistance at liquid

helium temperatures. This contactless method works with bulk speci- mens and avoids both thin wires and soldered contacts. The method

is especially useful for production control or inhomogeneity testing.

A large number of metals have been tested for the NBS Standard

Reference Material program, including Ag, Al, Au, Cd, Cu, Mo, Pt,

Sn, W, Zn, and several noble metal alloys.

Characteristics of Slush Hydrogen.—Activities in the physical

characterization of liquid-solid mixtures of hydrogen (slush hydrogen) have continued. A densitometer has been constructed which

provides a traceable calibration for slush density instruments used

as secondary or transfer standards. At present, the most successful

density measuring instruments utilize nuclear radiation attenuation

techniques. A parametric study of the performance of a centrifugal

pump operating with slush hydrogen was made. It was found that

both fresh and aged hydrogen mixtures could be successfully pumped

and that performance and cavitation characteristics are the same when the difference in fluid density is considered.

Standard Reference Thermocouple Tables.—Printed and punched

card tables resulting from NBS research and analysis are available

in 1 K intervals from 4 to 280 K for ISA type E, K, and T low-temperature thermocouple materials. These tables have been smoothly joined

at 273.15 K to previous JSTBS high-temperature thermocouple tables. Properties of Solid Parahydrogen.—Dielectric-constant measure- ments along the melting line of solid hydrogen at pressures between

18 and 320 atm and temperatures between 14.4 and 22 K have led to the first calculation of the molecular polarizability (with an esti- mated precision of a few parts per 10,000) of this substance. New

measurements of the melting pressure were also obtained leading to accurate densities for the melting solid. Knowledge of these properties

is required for the design of efficient aerospace systems utilizing slush

hydrogen (liquid-solid mixtures).

Thermodynamic and Transport Properties

Specific Heats of Gaseous and Liquid Oxygen.—The specific heats,

Cy and ^saturation, of gaseous and liquid oxygen have been measured

from the triple point to room temperature at pressures to 350 atm. 68
They were combined with, earlier PVT measurements to produce what

is believed to be the most accurate and comprehensive thermodynamic

functions for this substance in the cryogenic temperature range. Accurate thermodynamic functions are required by the aerospace and gas

separation industries.

Refractive Index of Gaseous and Liquid Hydrogen.—The refractive index of liquid hydrogen has been measured with great precision over a very wide range of temperature and density. Data were obtained

at temperatures between 15 and 300 K and at pressures up to 233 atm

using a Fabry-Perot interferometer. The density and temperature dependence of the Lorentz-Lorenz function was also analyzed. The meas- urements are useful for the determination of fluid densities and mass

flow rates, and for providing new information on the interactions between molecules.

High-Speed Thermodynamic Measurements System.—The first phase of the High-Speed (millisecond time resolution) Thermodynamic Measurements System developed for research at high temperatures (1800 K to melting points) has become operational. This unique

system provides simultaneous dynamic measurement of specific heat,

electrical resistivity, and hemispherical total emittance of electrical conductors. Recording of the data is completely automated; up to 2000 data words can be measured and stored in digital form (with

0.01 percent resolution) in the core memory during an experiment of

subsecond duration. This information is retrieved immediately after

the experiment and processed by a remote-control, time-sharing computer. Data on molybdenum in the range 1800-2800 K have been obtained.

Quantum Mechanical Virial Coefficients of Helium.—The velocity

of sound in helium from 2 to 20 K obtained at NBS has been analyzed

and preliminary values of the second virial coefficient in this range have

been obtained. These values are better than previous ones and are of

importance to improvement of the International Temperature Scale. It was possible to obtain these improved values because accurate theoretical computations of the second virial for the Lennard-Jones

potential have yielded an appropriate form for the temperature dependence of the second virial. The calculations covered the complete

temperature range from near absolute zero to the classical region. By

separating the virial into Boltzmann and exchange terms, the suppression of statistical effects with rising temperature could be examined in

detail. The theoretical results have been compared with experiments

over the whole range leading to improvement of the intermolecular potential function for helium.

69
PVT Measurements in the Glassy State.—As part of a continuing

study of the influence of pressure, temperature, and volume history on the physical properties of glass-forming liquids and polymers,

specific volume measurements to 1000 bar along various isothermal

and isobarie paths into the glassy region on poly (vinyl acetate) have

been completed. These studies have helped to resolve several controversial points about the formation of glassy state, and the applicability of reversible thermodynamics to the glassy state. Theory of Transport Phenomena.—Such phenomena as frequency

dependence of sound velocity, nonlocal effects near the critical point,

and nonlinear dependence of viscosity on the rate of shear are not adequately explained by classical fluid dynamical theory, but require a

generalization of it. One generalization, which describes noninstantaneous, nonlocal, and nonlinear responses of flows to the thermodynamic

forces (gradients) , has been derived by statistical mechanical methods.

The conservation equations are unchanged in form, but new expressions are given for the pressure tensor and heat current vector. The new

expressions are determined by microscopic quantities (e.g., interparticle potential), and are the sum of reversible and irreversible parts.

The reversible parts are the average fluxes in a local equilibrium en- semble that includes nonlocal effects. The expression for the irreversible parts are the analog of the classical transport relations, and are

linear combinations of integrals over space and time of the thermodynamic forces multiplied by the correlations of fluxes averaged in a

local equilibrium ensemble.

Theory of Critical Phenomena.—A fluctuation theory of critical phenomena in fluids has been formulated and applied in several in- stances. The theory generalizes the Ornstein-Zernike theory of density

fluctuations to fluctuations of energy, pressure and similar functions.

It introduces an important new mathematical object, the critical eigenvector, which has several significant roles near the critical point. The

difference in molecular distribution functions in the liquid and gas

phase just below the critical point is proportional to this eigenvector,

and it is the most probable fluctuation in the molecular distribution

functions just above the critical point. It is known from experiments

that the specific heat at constant volume, while aparently infinite at the critical point, approaches infinity much more slowly than the

specific heat at constant pressure. This fact can be explained if the

molecular distribution functions have a certain asymptotic behavior,

which can be understood from the role of the critical eigenvector as the most probable fluctuation.

The Intermodular Potential and Experimental Data.—A method

to evaluate quantitatively the relationship between model intermo70
lecular potential functions and macroscopic experimental properties

has been developed. The method is valid for any potential function and

any property, provided the appropriate theoretical expressions are

available. A principal conclusion of this work is that a temperature

range exists where the experimental properties are insensitive to the

potential function. New results concerning the experimental precision

required in order to determine the potential function from these properties have also been achieved.

Light Scattering.—The change in the critical temperature of a binary mixture when an external electric field is applied to the fluid

has been studied by determining the change in the intensity of the light

scattered by concentration fluctuations (critical opalescence) as the

field is turned on. A theoretical description of the change with time of

the concentration fluctuation correlation function was made which re- lates the intensity of scattering to the binary diffusion coefficient. The

theory enables the binary diffusion coefficient of the mixture to be determined from these measurements.

Critical Point Scaling Law.—The validity of the scaling law equation of state has been tested by an analysis of the data for the critical regions of C02 , Xe, 4 He and N2 0. This theoretically based equation

of state expresses the nonanalytic behavior of properties in the critical region through numerical exponents and a function, h (a?), of a single

variable which measures the difference from the critical point. The

analysis yielded values of the critical isotherm exponent and the criti- cal temperature based on a proposed form for A (a?), satisfying the

scaling law requirements. Taking experimental values for the co- existence exponent, a value of the critical isotherm exponent equal

to 4.6 ±0.1 was found to give a good fit for three classical substances,

and a value of 4.45 ±0.15 gives a good fit for 4He. For all substances* a value of about 4.4 for the ratio of the compressibility along the criti- cal isochore to that along the coexistence line is found. Although this

is much smaller than previously reported values, it agrees with the

value 4.9 for xenon determined by optical techniques.

Theory of Shock Wave Propagation in Crystals.—Shock compression experiments on solids provide a means for studying the interatomic forces under high pressure (to 106 bars) and high temperature

(to 104 K) conditions. A theoretical study has been completed in which

the relaxation process behind a shock front in a crystalline solid has

been modeled on a computer. This study provided information related to the interpretation of experimental data from this process in terms

of interatomic forces, and on the PVT relationships in the shock

compressed region.

71
APPLIED MATHEMATICS

The Institute for Basic Standards conducts a program in applied

mathematics and statistics to meet varied needs in the development of new measurement techniques and in the evaluation of the results of

measurement. The level of the mathematics involved makes it essential to conduct fundamental mathematics research on a fairly broad scale. Routmg for Maximum Flow.—A problem frequently arising in

operations research studies is that of routing so as to obtain a maximum flow from a "source" to a "sink" in a network whose individual

links have limited flow capacity. The standard method of solution

of this problem does not generally work if the various link capacities are incommensurable, and, if ratios of link capacities have large

denominators, a very great many computational steps may be required.

It was found that a slight and natural additional specification to the

algorithm enables one to obtain an upper limit on the computation

labor which is actually independent of the link capacities, namely,

the cube of the number of network nodes.

Mathematical and Statistical Tables and Handbooks.—A sixth

printing of Applied Mathematics Series 55—the Handbook of Mathematical Functions—was released in November 1967. With the sale of

the hard cover volume approaching 82,000, changes were submitted

for the seventh printing to be released in July 1968. A second edition

with additions and corrections of "Tables Relating to Mathieu Functions," initially printed by the Columbia University Press, was

released in August 1967.

Unified Treatment of Multidimensional Contingency Tables.—An

investigation of interaction in multidimensional contingency tables

has led to a unified treatment from an information-theoretic approach.

Under this approach the principle of minimum discrimination-information is proposed and used to generate hypotheses concerning secondorder and higher order interactions. It is shown that all classical hypotheses for contingency tables can be generated through the use of this principle when certain marginals are considered fixed. Behavior of Statistical Procedures.—The Bureau's Statistical Engineering Laboratory performed an extensive analysis of the properties

of Cochran-type tests for homogeneity of variance when the underlying distribution is not normal. Numerical results for small sample

sizes show that statistical procedures of this type can be seriously

misleading if used uncritically when the underlying distribution is not normal. For example, the sample range exhibits behavior different

from that predicted by the known approximations based on the fourth

72
moment when the underlying distribution is sufficiently discrete (as

often occurs when measurement data are severely rounded)

.

Matrix Representations of Groups.—A useful, comprehensive set of notes of Matrix Representation of Groups was completed. The notes

serve as a complete introduction to the subject and demand only a knowledge of elementary matrix theory from the reader. An appendix

on the elements of the theory of algebraic numbers is included.

Heat and Mass Transfer.—Significant work was performed on the

numerical solution of problems in coupled heat and mass transfer,

with nonlinear reaction kinetics in which the flux equations are based on the postulates of irreversible thermodynamics. A scheme for inte- grating the diffusional contribution to the transfer process was developed which effects economy of solution through permitting the use of

the maximum time step in each of the coupled equations.

Numerical Analysis.—New methods were developed for checking the

reliability of the results of numerical calculation. A new theory of

error bounds for Laplace's method of approximating definite integrals

containing a large parameter has been developed and illustrated by

numerical examples. In addition, the theorem of Piatetsky- Shapiro on

quadrature error bounds was extended and sharpened. Further, important new results were obtained on the computation of solutions of

second-order linear difference equations. Comparison theorems were

constructed which yield strict and very realistic bounds for the truncation error associated with the new method of computation.

TECHNICAL ASSISTANCE TO OTHERS

Studies for Other Groups

Fuel Oil Measurements.—A measurement service extended to the

Commerce Department's Maritime Agency has resulted in a signifi- cant saving of time and money. The Chairman of the Maritime Administration's Trail and Guarantee Survey Boards has expressed his

appreciation for the rapid determination of the heating value of fuel

oil which enabled M.A. to advise a steamship company and a shipbuilding corporation that economy trial reruns of a new $15 million cargopassenger vessel would not be required. The direct saving to the shipbuilder was about $10,000, but significant other cost savings in time

and equipment were also realized.

Commercial Tungsten-Rhenium Type Thermocouples.—The per- formance of commercially available W-Ke type thermocouples at temperatures up to 2300 °C has been studied, and existing commercial

73
temperature-emf tables for the thermocouples have been evaluated.

The investigation was performed for the American Society for Test- ing and Materials and will assist in the industrial standardization of

these thermocouples. W versus W-26 percent Re, W-3 percent Re

versus W-25 percent Re, and W-5 percent Re versus W-26 percent Re

thermocouples from two leading suppliers were investigated and

their temperature emf relationships were found to conform with the

suppliers' temperature-emf tables to within the equivalent of about 1 percent of the indicated temperature for the range 400 to 2100 °C.

Noise Control Guide.—Under the sponsorship of the Federal Housing Administration, NBS has completed an extensive investigation of

noise in multifamily dwellings. This investigation resulted in the

publication by FHA of a 421 page report entitled, "A Guide to Airborne, Impact, and Structure-borne Noise Control in Multifamily

Dwellings." Some 345 detailed architectural drawings show proper

construction and installation of wall and floor assemblies, building

equipment, appliances, heating, air conditioning, plumbing, and elec- trical systems required for adequate noise control and privacy. The

guide presents recommended sound insulation criteria for three grades

of multifamily dwellings and contains sound insulation data, fire ratings, and descriptive illustrations for 137 walls and 111 floor-ceiling

constructions.

Fluorescent 0rangeToProtect Hunters.—The state of Massachusetts

requires a hunter to wear "daylight fluorescent red or orange" garments

lest he be mistaken for game by other hunters. One fatal accident which

occurred two years ago involved a man wearing an inconspicuous,

slightly fluorescent, copper-colored vest, legal under the law. Inquiries

from several States have indicated a desire to revise present laws by

including color tolerances tight enough to assure that the fluorescent

orange worn by the hunter is sufficiently conspicuous to afford him

adequate protection. Samples of the fluorescent cloth have been meas- ured and recommendations issued for color tolerances which can be

met by currently available cloth. Electroluminescent Formation Lights.—Extensive development for

the Naval Air Systems Command has resulted in the use of flat, semiflexible, strip-type electroluminiscent (EL) lamps as formation lights on military helicopters. Incandescent lamps proved to be infeasible

for this application chiefly because of the severe vibrational environment. The linear geometry of the EL lamps has proven to be an added

advantage. Studies have begun to determine the feasibility of extending this t"pe of lighting to high-performance (mach 2) aircraft.

74
Microfilm Preservation.—Since microfilm is one of the most suitable

media for the storage of records of permanent value, NBS continually

investigates factors affecting the formation of blemishes on such films. Chemicals evolved by the cardboard cartons in which the films are

stored may react with image silver to form blemishes. Procedures have

been developed for testing the susceptibility of processed microfilm to blemish formation and for testing the relative blemish inducing potential of various carton materials. The effects of photographic process- ing and storage conditions are being established by these techniques.

Liquid Hydrogen Bubble Chamber Consultation.—Continuing consultation and advisory services were provided on three of the Nation's

large liquid hydrogen bubble chambers. Assistance has been given to the Atomic Energy Commission on the planning and cryogenic design

of the 12-ft chamber at the Argonne National Laboratory and to the

Brookhaven National Laboratory on the planning and safety analysis

of their proposed 14-ft chamber. Assistance was also given on the re- design and testing of the 500-liter bubble chamber at the Massachusetts

Institute of Technology. The latter chamber was earlier determined

to have initiated the fire and explosion at the Cambridge Electron Accelerator that resulted in the destruction of the Experimental Hall.

Studies of Explosives.—A study has been made for the Naval

Ordnance Laboratory of the heats of formation of stilbene and

hexanitrostilbene. The latter material is a solid explosive analogous

to TNT (trinitrotoluene) but having less sensitivity and a very low

volatility. This material is being investigated for possible extraterrestrial applications.

Holmium Total Neutron Cross-Section.—A collaborative effort with

experimenters at the Atomic Energy Research Establishment, Harwell, England, and theoreticians at the Oak Ridge National Laboratory has been undertaken to measure the total neutron cross-section

of oriented 165Ho in the energy range 2 to 135 MeV. The experiment

involved cooling a

165Ho single crystal to 0.32 K in an NBS 3He re- frigerator and measuring the neutron spectrum generated by the

Harwell sychrocyclotron with a time-of-flight spectrometer. The differential cross section of the oriented 165Ho oscillated in sign between

the measured energy limits in a manner consistent both with the nuclear optical model and with a model based on the Ramsauer effect. Conferences and Symposia

Thermometry Committee Meets at NBS.—NBS played host to the

Advisory Committee on Thermometry to the International Bureau

of Weights and Measures for the first half of its 1967 meeting on

September 5-8. The meeting was divided between NBS Gaithersburg

76

320-738 O—68 6
and National Research Council, Ottawa. Delegates from Australia,

Britain, Canada, France, Japan, Netherlands, Spain, U.S.A., U.S.S.R.,

and West Germany attended. In both institutions a day of laboratory

visits was scheduled to provide a break in the discussions which occu- pied a total of 4% days. Agreement was reached on the revision and

extension of the International Practical Temperature Scale to be

effected probably early in 1969.

Symposium on Wolf-Rayet Stars.—During the week of June 10-15,

1968, the American Astronomical Society, Harvard College Observatory, the NBS Joint Institute for Laboratory Astrophysics, and the

Smithsonian Astrophysical Observatory sponsored a working Symposium on Wolf-Rayet Stars. It was held at the JILA facility in

Boulder, Colo., and was attended by some 45 persons actively interested in the field. This class of star may make significant contributions

to understanding the phenomena that condition the state of other stars. They are thus of particular interest. A focus for the meeting concerned

the effect of mechanical input into the extended atmosphere. The case of the Wolf-Rayet stars appears to be one for which the whole line

spectrum, in the visual as well as in other regions, requires a model

departing from wholly radiative effects. The Wolf-Rayet stars probably represent the most extreme case of coupling between aerodynamics

and astrophysics to study the behavior of a hot gaseous atmosphere.

Colorimetry and Spectrophotometry Seminar.—Colorimetrists and

spectrophotometrists from university, industry, and Government lab- oratories participated in a 3-day seminar. Topics covered were: psychophysics of color vision, uniform color space, color-order systems,

spectrophotometry standards, photodetector response calibration,

photoelectric colorimeters, metamerism, and variability of color measurements. Attendees had the opportunity to visit the NBS colorimetry

and spectrophotometry laboratories and to discuss special problems

with Bureau experts.

Length Measurement Seminar.—Dimensional metrologists from

both industrial and Government standards laboratories participated

in a 5-day seminar. Topics covered were interferometric absolute

length measurements of gage blocks and diameter; interferometric

methods for calibration of flatness, surface texture, length, and angle

;

optical and mechanical methods for the calibration of surface planeness and angle. Experimental and statistical programs for determination of errors were discussed. Attendees had the opportunity to make

measurements on NBS equipment.

Seminar on Time and Frequency.—Thirty-six registrants from

private industry and several Government agencies attended a 3-day

76
seminar on Frequency and Time given by the NBS Time and Frequency Division during February 28-March 1, 1968. The seminar

included 2 full days of classroom lecture by various experts in the

Division and several laboratory demonstrations of state-of-the-art

equipment and measurement techniques. The latter included demonstrations of frequency stability measurement techniques, an actual

global time synchronization of atomic clocks to about 4^, and NBS

timekeeping techniques utilizing efficient weighting of individual

clocks. One full day was devoted to a visit to the NBS standard fre- quency broadcast stations at Ft. Collins, Colo.

High Frequency and Microwave Attenuation Seminar.—A seminar

in attenuation measurements was presented during March of 1968 for

eighteen people from Government and industry. The seminar included

definition of terms, discussion on attenuation standards, attenuation

measurement techniques, and measurement errors. The lecture sessions were supplemented with laboratory demonstrations.

Microwave Calibration Workshop.—A workshop on Microwave

Calibration Services was conducted in May 1968. Forty-six persons

attended from industrial and Government laboratories. The attendees were primarily technicians and engineers who are practicing metrologists. The workshop presentations were almost evenly divided between

lectures and demonstrations, and covered the subjects of frequency,

impedance, attenuation, phase shift, power, and noise.

Precision and Accuracy in Measurement and Calibration.—At a 4- day seminar, thirty-three participants representing 23 industrial and

10 Government standards laboratories obtained firsthand information on some of the statistical techniques in current use at the Bureau.

The Bureau reported experience in the development and use of statis- tical experiment designs especially tailored to the needs of calibration

laboratories for making economical intercomparisons among sets of

standards. Presentations by NBS statisticians were complemented by

reports from Bureau calibration laboratories that are implementing

the new computer-aided methods for data analysis, preparation of

calibration reports, and surveillance of the measurement ("production") process. Seminars on Statistics.—A series of 15 expository seminars for

chemists and physicists was conducted on the application of statistical techniques in the design, analysis, and interpretation of scientific data.

The series, planned jointly by the NBS Applied Mathematics and

Analytical Chemistry Divisions, served as a useful forum for consideration of the nature and value of the methods of statistics in scientific investigations.

77

INSTITUTE FOR MATERIALS RESEARCH

Emphasis in the Institute for Materials Research (IMR) is on

materials measurement methodology with particular concern for the

characterization of materials. This emphasis supports the unique mission to develop standards of measurement for the commercial, industrial, and educational communities of the Nation and to provide

research and consulting services to other Government agencies. About

25 percent of IMR's work is for other Government agencies.

Work falls into the following broad areas

:

1. Preparation and Characterization of Materials

2. Data on the Properties of Materials

3. Technical Assistance to Others.

PREPARATION AND CHARACTERIZATION

OF MATERIALS

This area includes such activities as the synthesis of new materials,

purification of materials, crystal growth, and the analysis of materials

with respect to chemical composition and structure. Outputs of these

activities are sample materials to be used for specific research purposes,

and the development of new techniques and procedures for preparing

or characterizing materials. Another output is a class of materials

called Standard Reference Materials. These are prepared and sold by

IMR and are used mainly by industry for the calibration of equipment.

Preparation

Synthesis

Synthesis of Alkaline-Earth Transition-Metal Oxides.—Oxide com- pounds of the alkaline-earths and elements of the first transition series have been investigated at elevated temperatures and controlled oxygen

pressures. Of primary interest is the influence of stoichiometry on compound formation, stability, and crystal structure which ultimately

may dictate the electrical and magnetic properties of the materials.

Phases in the systems SrMn03 -x, BaMn03±x, and BaFei_Y03_x reflect the importance of varying oxygen content (transition metal valence

disproportionation) and/or transition metal concentration.

Reacti/ve Intermediates in Chemical Synthesis.—Chemical trans- formations of inorganic compounds under energetic conditions have

been explored from the viewpoint of applications to synthesis of new

79
materials. Studies of the chemistry of inorganic fluorides in micro- wave discharges have demonstrated the synthesis of a number of new

oxyfluorides of boron, silicon, germanium, and phosphorus, and have

yielded information on the reactions of oxides and of polymers with

reactive molecular species. A significant chemical discovery is the observation that the complex chemical events in the discharges can be

rationalized hi terms of surprisingly few intermediates, conventional

reaction mechanisms, and chemically reasonable structures. The reactive intermediates produced in these discharges, or by thermal or photochemical excitation, represent novel chemical reagents that are difficult or impossible to obtain by other means.

Synthesis and Crystal Structure of a Trinuclear Complex.—The

complex 5&[triaquo-tri-/i (1,2,4, triazole (-N"!-N2 ) nickel] nickel

hexanitrate dihydrate has been synthesized from an aqueous solution

of M(X03 ) 2 and 1,2,4 triazole. Its crystal and molecular structure determination revealed that the material has a trinuclear complex

cation and is monoclinic. The structure was solved by the Patterson

and electron density Fourier methods. The material is one of a class of

inorganic compounds which contain two or more paramagnetic metal

ions per molecule. Such polynuclear species are well suited to detailed

study because the exchange coupling between paramagnetic ions in a

single molecule is greater than that between ions from neighboring

molecules. Therefore, the ions within a molecule behave as magnetically

isolated clusters. New Luminescent Materials.—Yttrium disilicate, Y2 Si2 07 (yttrialite) , occurs in both low- and high-temperature forms in nature. Hightemperature yttrialite, in the form of a fine powder, has been synthesized from precipitated gels in air at 1300 °C. When doped with

5 to 10 mol percent of europium or terbium, the material shows intense

luminescence when excited by ultraviolet light.

Gadolinium disilicate, a compound isostructural with high-temperature yttrialite, shows very high luminescence when doped with 10 mol

percent europium, the luminescent intensity stronger than that of

yttrium disilicate containing europium.

Yttrium may be replaced by cerium in Y2 Si2 07 under hydrothermal

conditions at 700 °C and 1 kbar. Up to 60 percent replacement of Y+3 by Ce+3 is possible without inducing phase transformations. Y2 Si2 07 containing 25 mol percent cerium shows a very intense bluish-white

lmninescence. The intensity decreases progressively with increasing

amounts of cerium.

New Method for Esterification.—Esterifications are among the most

commonly employed and important reactions of synthetic organic

chemistry, and many methods have been devised for effecting such

80
reactions. Nevertheless, there are enolic compounds, for example, that

have not been successfully esterified by any of these techniques. Difficult acylations can now be achieved by a novel reagent combination, an

anhydride (acetic, propionic, butyric, etc.) dissolved in 100 percent

syrupy phosphoric acid. Products are isolated by treatment with ice water or directly by extraction. In this way, croconic acid, which has

resisted all other methods, is converted into a crystalline diacetate

derivative. Other compounds, easily acylated by other methods, were

obtained for the first time as crystalline products.

High Pressure Polymerization.—Pressures of 10,000 to 20,000 atm

(about 10 to 20 kbar) have been used to convert fluoromonomers to new

polymeric materials having excellent physical properties combined

with thermal and oxidative stability. Gamma rays are often used to

initiate these reactions since they readily penetrate the thick-walled

steel vessels used to create the high pressure. New polymers prepared

include polyperfluorostyrene, poly-3,3,3,2-tetrafluoropropylene, poly3,3,3-trifluoropropylene, polyperfluoroheptadiene-1,6 and various co- polymers of the monomers of these polymers with tetrafluoroethylene.

Crystal Growth

Wide Solid-Solution Series of Apatite Compounds.—Crystals of

rare-earth fluoro-silicate apatites and oxyapatites of wide variations in

chemical composition were grown. These crystals are of interest for

detailed structure analysis of apatite, a stable phase with an exceptional

tendency to accommodate cations and anions of diverse shapes and sizes. Specific practical applications are not obvious, but apatites are

potentially useful laser hosts and could also be used for high temperature applications.

Sodium fluoride was found the most effective flux for growing the

fluoro-silicate apatites, and sodium tungstate is useful for silicate oxyapatites. Growth by isothermal evaporation at high temperature,

relying on spontaneous nucleation in 25 ml platinum crucibles, produced transparent crystals of Na2Ln8 Si6 024F2 (apatite, Ln=La, Pr,

Nd, Sm, and Gd) up to 8.0 mm in size with well developed faces. The

colors of the crystals were characteristic of each type of trivalent rare- earth ion. Unit-cell dimensions of all analogs were determined.

Europium and terbium doping of the gadolinium analogs produces

intensely luminescent crystals.

Crystallization of Ice.—Crystallization processes do not usually occur by the propagation of an interface of single shape. However, if the crystallization process is carefully controlled, as for example in

crystal growth, a simple interface shape can be retained.

81
A recent experiment has provided experimental confirmation of cur- rent morphological stability theory. Cylindrical crystals of ice of

known orientation were immersed in a bath of slightly supercooled

water. The crystal remained smooth during the initial stages of radial

growth, but eventually developed undulations. The growth rates of

these undulations were in good quantitative agreement with morphological stability theory.

Growth of Curved Crystals.—Studies of the growth of polymer

crystals from solution have shown several mechanisms by which the

direction of growth is rotated out of the plane of the nucleus. If crystals are grown from very dilute solutions at small supercoolings, rela- tively simple and planar crystals retaining the symmetry of the unit

cell result. For poly (4-methylpentene-l), as the solution concentration

and supercooling is increased, relatively more complex and curved

crystals result. The curvature, which is a characteristic common to sev- eral polymers, results from the combined effect of strain caused by

the molecular folds on the crystal surface and the subdivision of a

crystal into different fold domains. Such effects no doubt play a role

in the growth of structures with spherical symmetry (spherulites)

which dominate the morphology of melt crystallized commercial

polymers.

Simple planar crystals of poly (4-methylpentene-l) grown from very dilute solutions at small supercoolings. Studies on such crystals have shown several mechanisms by which the direction of growth is rotated out of the plane of

the nucleus. 82
Electrodeless Electrolysis.—An electrodeless electrolysis process was

developed in which electrolysis takes place in a glow discharge or a stream of electrons in vacuum rather than at the surface of the metallic

electrode. Silver chloride was used to produce a silver coating and a fused nickel salt was used to produce nickel powder. The principal

purpose was to further confirm the theory of electrolysis; however,

metal coating ceramics may become practical.

Characterization

Composition

Limits for Qualitative Detection and Quantitative Determination.—

Because of the numerous, inconsistent and restricted definitions of

a lower limit of detection in analytical chemistry, IMR examined the

statistical theory of signal detection and signal extraction. A series of

principles were evolved for unambiguously describing the sensitivity

of an analytical technique. Limiting sensitivity levels were defined for

(1) Lc which is the critical level below which a signal cannot be detected with a given probability, (2) LD, the a priori detection limit,

which together with Lc determines the probability of a correct detection, and (3) net signal limit which permits a statement of magnitude

in addition to detection.

New Goulometric Method for Boron Determinations.—Boron is com- monly determined by conversion to boric acid which is acidimetrically

titrated in the presence of mannitol. A new method has been developed

which carries out this titration coulometrically, resulting in an accu- racy of better than two-thousandths of a percent. This is a factor of

ten better than that obtained by conventional procedures. The method

is especially useful for, and has been applied to, the characterization

of primary standard boric acid. Because only small samples are re- quired, it is very advantageous for highly accurate microchemical

analysis. The new method is one of a series of coulometric procedures

developed in IMR ; each of these has a precision and accuracy about

ten-fold greater than those of the most refined conventional analytical

techniques.

New Neutron Generator Facility.—A new neutron generator has

been installed and the radiation shielding and pneumatic tube trans- port system have been upgraded to make this facility one of the finest of its kind. Using this new generator, methods have been devised for

the evaluation of systematic errors due to differences in self-shielding

of neutrons and self- absorption of gamma rays between the sample

and the standard. The system was calibrated with samples of known

density and composition, and by using the correction factors generated,

the element of interest may be determined accurately in any matrix

83
material. The general technique can be routinely applied to both trace and macro elemental determinations.

Using this facility, analyses have been performed for the determination of oxygen in metals and for metal in the metallo-organic

compounds with accuracy and precision comparable to many nonnuclear methods.

A-C Scanning Derivative Apparatus for Spectrometry.—An apparatus based on an a-c scanning derivative principle has been developed

which should greatly enhance the potentialities and usefulness of

flame emission and atomic absorption spectrometry. The new apparatus, which consists of a vibrating mirror or quartz plate operated at controlled frequencies, permits the repetitive scanning of a narrow

region of spectrum and in so doing offers significant improvement in

the precision and accuracy obtainable in both the emission and absorption modes.

Heretofore, a serious drawback in atomic absorption spectrometry

has been the need to use a separate source for each element. The use

of a continuum source has been restricted because such systems require some means for modulating or chopping the light beam as well as a higher resolution monochromator. The a-c scanning technique minimizes the need for high resolution instrumentation. This modification

should not only reduce the cost of instrumentation but should also

provide impetus for future development of multichannel methods by

which a large number of elements can be determined with a single

source. The advantage of the new technique has been demonstrated by the

successful determination of several elements in the presence of elements

which normally interfere when examined in the usual manner. For

example, barium can be readily determined in the presence of 1000-

fold excess of calcium. Lithium can be determined in sodium at less than 0.01 part-per-billion level. This development should facilitate the determination of trace ele- ments of importance in new materials and biological or environmental

problems.

Activation Analysis With the NBS Reactor.—The 10 MW nuclear

reactor at NBS began lowT power operation in December, 1967, and

will achieve full-power operation by November, 1968. Facilities have

been constructed for the irradiation of samples in the reactor for pe- riods of hours or days using a special sample suspension system through

the top shield plug of the reactor. Rapid (less than 2 s.) pneumatic

transfer facilities from various locations in the reactor core and from

the graphite thermal column allow the experimenter to choose widely

varying ratios of "fast" to "thermal" neutrons from a pure thermal

neutron spectrum in the thermal column facility to about 60 percent

84
greater-than-thermal neutrons in the reactor core. A "fast neutron converter" facility is in the development stage ; it will permit irradiations

with pure fission spectrum neutrons without thermalization. By choosing these ratios carefully, the experimenter can maximize a desired

nuclear reaction, or minimize a competing reaction.

High-Precision Flame Emission Spectrometery.—A new technique

of differential flame emission spectrometry was developed whereby a

precision of one part in a thousand was obtained over a concentration

gradient of a few parts per million to several percent. This 20 fold

improvement in precision is equivalent to or better than the present

classical chemical methods. To accomplish this improvement in precision, the various instrumental parameters were optimized. This technique was evaluated by the determination of 10 percent lithium in

glass beads which are to be used for neutron flux measurements. The

same approach can be applied to any analysis in flame emission or atomic absorption spectrometry and in any matrix such as biological

materials, and ferrous or nonferrous metals.

Trace Quantities of Yttrium in Rare Earths.—Trace quantities of

yttrium (Y) in other rare earths were determined with a ± 5 percent

precision at the 20 ppm level by utilizing the photonuclear reaction

89Y (y,n) 88Y. An analysis based on coincidence spectrometry utilizing

gamma ray decay rather than the more conventional analyses based on chemical reactions was necessary because of the close similarity of

the chemical properties of the rare-earth elements. Nuclear activation

analysis utilizing the 90Y isotope produced by neutron bombardment of

the stable, naturally occurring isotope 88 Y also was not utilized because

of the lack of gamma rays associated with the 90 Y decay.

Identification of Unstable Clinical Standard Compounds.—IMR

chemists have devised new methods of measuring the purity of a

series of unstable chemical compounds that are particularly significant to clinical calibration and measurement. Ordinarily, the

analysis for chemical purity is long and difficult when applied

to compounds such as urea, D-fructose, and uric acid, which are known to undergo decomposition if they are improperly treated. To

avoid this problem and yet obtain accurate chemical measurements, the

method utilizes formation of a chemical derivative that is much more

stable than the original compound.

Of particular importance is the technique of trimethylsilylation

which, when applied to the above compounds, yields derivatives that

are stable as gases when heated. These gases are then analyzed by gas

chromatography which serves to discriminate one compound from another. Of even greater importance is the fact that the technique per- mits separation of various contaminants which can then be fed into

85
a mass spectrometer and in a very short time their molecular weights

determined. The techniques of isolation and characterization can be

applied to as little as 10-9 g. Carbon Isotope Analysis.—A method has been devised for measuring the C

13/C12 ratio in C13 enriched samples by combining gas chromatographic separation techniques and analysis by means of a sensitive, differential gas density balance. A C

13 enriched sample of an

organic compound is burned to C02 and H2 0, the water separated

out on a gas chromatographic column, and then the density of the en- riched C02 compared to that of normal carbon dioxide. The minimum

detectable C

13 enrichment is about 0.02 percent of the natural abundance which suggests that the method will be applicable to geochemical

analyses. The technique is also applicable to the determination of stable isotopes other than those of carbon.

X-Ray Powder Patterns—Saline Series Standards.—In recent years

there has been a renewed interest in the recovery of a variety of commercial products from saline residues. More than one hundred com- pounds may be encountered in exploring various methods of separation of these salts. Identification of these anhydrous and hydrated

compounds is best accomplished with x-ray diffraction. Because this

method of analysis is dependent upon the availability of reference patterns, IMK has added over 50 new standard reference patterns of saline

compounds to several that were originally available in the Powder Diffraction File. In the next 2 years, another 50 such patterns will be

added in an effort to present an extensive ocean-salt series for those

who work with solids that accumulate from desalinization operations.

Nuclear Magnetic Multiple Resonance for Molecular Structure

Determination.—Development of double-resonance techniques to a

routine adjunct of high-resolution nuclear magnetic resonance meas- urements greatly enhance the power, utility, and versatility of n.m.r. in the determination of molecular structure. This has been demonstrated in 1MB, laboratories by measurements of n.m.r. parameters

for the silicon-29 nucleus in a number of inorganic and organic silicon

compounds. The silicon spectra, which are observed indirectly, fre- quently contain structural information not present in the commonly

observed proton or fluorine n.m.r. spectra of these compounds. The

method is being applied to a wide range of compounds of other nuclei

such as tin, lead, and mercury.

ElectronMicroprobe ColorPhotography.—A procedure for the color

representation of electron microprobe area-scan images has been developed. The net result is a means of showing microstructure in terms

of specimen composition. In order to obtain the color composite, x-ray

86
area-scans are prepared as positive black-and-white prints by photographing the cathode ray tube of a scanning electron probe microanalyzer. This procedure indicates the location of a particular element

in the microstructure by showing a bright spot whenever that element

occurs. The composite is obtained by combining up to three such

photographs using red, green, and blue filters interposed between

each photograph and the color film in a copy-camera. If rapid-development color film is used, the process is quite inexpensive. The color

method can be applied to any material from which characteristic

x-ray line scanning images and electron scanning images can be obtained. IMR has applied the method to archeology, biology, dentistry,

failure analysis, metallurgy, meteorites, and mineralogy.

An Automatically Operated Mass Spectrometer.—A two-stage 90°

sector mass spectrometer used for isotope ratio determinations has

been converted to automatic operation with the addition of a small

programmable calculator and suitable interfacing components. With

this conversion, samples as small as 10-12 g with isotope ratios of more

than 500 :1 have been analyzed and it is anticipated that samples sev- eral orders of magnitude smaller may be utilized in the near future.

In addition, the time for an analysis has been materially shortened

and the accuracy and precision obtained has equalled that expected

with much larger samples. The components necessary for this con- version were the calculator with its teletypewriter printout device,

digital control and command converters and a dual digital counter. With the use of this system the mass spectrometer may be programmed to collect data at predetermined times during a scan of the mass region of interest or, alternately, to repetitively collect data

representing the heights of as many as eight mass peaks, to calculate

the ratios of these peaks to each other and to readjust the time of

data collection to give constant, predetermined, counting statistics. New Concept of Microstandards.—The problem of isolating and

measuring extremely small quantities of matter in the region below

one nanogram is of growing importance to modern science and technology. The development of standards containing such small quantities of matter in exactly known quantity is therefore of considerable interest. The need for this is shown by the conspicuous absence

of standards for determining detection limits and performing quantitative calibration in the subnanogram region. These quantities are below the limit of weighability.

An important step toward the solution of these problems has been

made by IMR chemists. Spherical and chemically uniform beads of

ion exchange resin have been loaded with the ions obtained in water

from various electrolyte compounds. A technique has been found for

isolating individual beads of very small size, weighing to one trillionth

87
Components (teletypewriter printout device, digital control and command

converter, and a dual digital counter) to automate mass spectrometer being

used for isotope ratio determinations.

(10~12

) gram, in such a manner that all of the ions remain with the

bead. The method of "two dimensional dispersion" permits the identification of a single bead with a microscope and various procedures can then be used to measure the particle diameter. Instead of weighing

the bead, the weight is computed from the measured diameter, the

known chemical homogeneity of the material, and the independently

measured density of the beads. A single bead thus attains the role of a standard mass that can be reliably measured. With the use of conventional micromanipulation apparatus it can be transferred to a chosen

instrument requiring calibration for the type of matter contained by

the bead.

Analytical Chemistry of Com Syrups.—Recent technological developments in cornstarch hydrolysis have resulted in the industrial production of many new types of syrups that have expanded the use and

market for corn—the most valuable single crop in U.S. agriculture.

Relationships in the physical properties of corn syrups, developed some

years ago to characterize syrups for commerce and use, are now found

to be not entirely satisfactory for the new products. Furthermore, in- ternational controversy exists regarding the adequacy of some of these

relationships. To remedy this, a Research Associate program is being

conducted at KBS in cooperation with the Corn Industries Research

Foundation in order to evaluate with modern techniques the properties

of the broad range of syrup compositions now available.
Fundamental to the reliable measurement of many of the significant

properties of syrups is an accurate knowledge of their moisture content. Hence, prior to undertaking the study of other properties, methods for determining water in syrups are being evaluated. The standard

industrial method (mixing with filter-aid and drying in vacuum

oven) is found to be only slightly inferior in accuracy and precision,

but less satisfactory with respect to time required for analysis, to a new spectroscopic method employing the direct measurement of a water band in the near infrared. The much-used Karl Fischer titra- tion is found equally as reliable as the vacuum-oven method. Other

methods explored are attenuated total reflectance, thermogravimetry,

and colorimetry; these are somewhat less satisfactory, but adequate

for use in quality control.

Microanalytical Fluoride Determination.—An analytical method

for determination of very small amounts of fluoride has been devised.

Two commercial fluoride-sensing electrodes are used with one modified to accommodate 5 /d (y

1^ of a drop) of solution containing the

sample. By comparison with standards, as little as 0.2 ng of fluoride can be determined with a reliability of 1 relative percent. Since the

electrode is highly selective for fluoride ions, this constituent may be

determined in rather complex mixtures without separation. Accordingly, the new microchemical technique should be applicable to a

variety of analytical problems.

New Method for Trace Analysis of Oxygen in Gases.—A highly

sensitive and accurate absolute method has been found for the determination of trace amounts of oxygen in inert gases. In this method,

the gas is passed through a galvanic cell with silver and lead electrodes

that are covered with a film of potassium hydroxide solution. The cur- rent output of this cell depends on the rate of oxygen consumption,

which in turn is related to oxygen content and rate of flow of the gas, as well as to certain kinetic parameters.

Because of the time factor, the cell is not 100 percent efficient; hence, the laws of electrolysis cannot be applied as in coulometric procedures. To overcome this problem, the gas is passed successively

through several cells until the oxygen is essentially completely reacted.

Moreover, the measurement is conducted at two different rates of flow

to cancel the kinetic effect. The difference in total current for the two

experiments can then be equated to the absolute oxygen content by

use of quantitative electrolytic considerations. This method is very

simple to use, yet it provides analyses that are accurate to at least 1 part in 100 in the concentration range between 0.1 and 0.0001 mole

percent of oxygen.

89
New Method for Antimony Determination.—The accurate determination of antimony in steel at the 10 to 50 ppm level has presented numerous problems. Using a highly sensitive and selective spectrophotometric procedure, IMR chemists can now determine as little as

0.01 fig of this element. This work was initiated originally by requests

from the rotor steel industry to provide new Standard Reference

Materials with a certified antimony content. The need was based on

metallurgists' belief that trace amounts of antimony were directly re- sponsible for many of the cracking failures occurring in the rotor blades of turbine generators. The only interfering elements in the new

procedure are gold and thallium; their presence can be readily dis- cerned, however, and easily eliminated. Following dissolution of the

sample in a sealed glass tube at approximately 250 °C, antimony can be

determined in the resulting solution in 5 min or less. The expected ac- curacy is dz2 to 5 percent of the amount present.

Automatic Grid Scan for Electron Probe Microanalysis.—An auto- matic system for grid scanning and registration of x-ray counts,

installed by Institute scientists for the study of homogeneity of standard reference materials over micro areas, is a major step toward auto- mation of the electron probe microanalyzer. This system provides the

hardware for control of line and grid scans over matrices of selectable dimension up to 100X100 points, and readout of up to six numbers

which can represent time, x-ray counts, digitized target current, or monitor current measurement data. Output is presented in the form

of coded paper tape which can be printed on a teletypewriter, fed into

the memory of a multi-channel analyzer, or used for computation on NBS computers.

Improved Design of Clinical pH Electrode.—Glass microelectrodes

with tips small enough to be inserted into single cells are furnishing

increasingly useful results in studies of human physiology. These

electrodes make it possible to measure the concentrations of sodium

and potassium and to study the acid-base balance in living organisms.

Hence, they offer hope of future clinical applications in the monitoring of pathological conditions. It is often not possible to assure close uniformity of temperature throughout the measurement system comprising glass electrode, reference electrode, and living subject. Hence, some variability due to changes of temperature is difficult to avoid.

During the past year, a means was found to reduce or even eliminate

this source of error in systems containing pH microelectrodes. This

favorable result can be accomplished by careful choice of the inner

element and the inner solution from which the electrode is formed.

In the most suitable combination, these two components act together

to nullify completely the effect of fluctuations in the temperature of

90
the laboratory or operating room. The arrangement is applicable as well to the reduction of temperature effects in pH equipment used to monitor the acidity of industrial process streams. Time-Sharing Computations in Spectrochemical Analysis.—The

use of computers to facilitate analytical chemical operations has been

undergoing a rapid growth. A report prepared by chemists of the

Institute for Materials Research will serve as a guide to laboratories

desiring to avail themselves of time-sharing computers. The IMR

chemists are believed to be the first to use this type of computational

facility in spectrochemical analysis ; the methods they have developed

have elicited considerable interest, and other spectrochemical laboratories have recently installed terminals connected to time-sharing

computers.

Measurement Scales for Ionio Activity.—Electrical response of the

relatively new ion-sensing electrodes depends on the concentration of

a particular sort of ions present in the solution in which the electrode

is immersed. Ion-selective sensors have been designed for the measure- ment of some 10 different ions, both metallic and nonmetallic. They

facilitate the rapid measurement and control of ion concentrations

which are time consuming and laborious by conventional analytical

procedures. Nevertheless, the measured voltage of the ion-selective

electrode is not a direct measure of the desired concentration of the

ionic constituent but rather of its effective concentration or activity.

To enhance the accuracy and usefulness of the measurement, the elec- trodes require reference standards for ion activity. During the past

year, useful approaches to ion-activity standardization were investigated. The practical solution selected bases ion activities on the same

conventional numerical scale on which the national pH scale is established. It is now possible to assign standard values of ionic activity to reference solutions and thus to improve the accuracy of ion-selective sensors used for measuring concentrations of single ionic species.

Structure

Electron Microscopy Examination of Refractories.—An understanding of the physical and chemical properties of refractories can

lead to improved performance of these materials. The properties are known to depend on the manner in which the refractory components

are joined together; that is, on the microstructure of the refractory.

The microstructure is most commonly evaluated using the optical

microscope. However, because of the limited resolution of the optical

microscope (1 to 3 /mi) many details are lost and an improved tech- nique would be desirable. The Institute for Materials Research has

developed a superior method of examination in which thin sections of

91

320-738 O—68 7
refractories are examined by transmission electron microscopy. Speci- mens of periclase refractory have been examined in this manner and

details of the microstructure not capable of resolution in the optical

microscopy have been observed. The information so obtained is already

being put to commercial use in the development of periclase bricks

for the steel industry.

Single-Crystal X-Ray Diffraction at High Pressures.—A diamondanvil high-pressure cell for use to pressures of approximately 50,000

atm (about 50 kbar) has been constructed using only polycrystalline

beryllium as metal components. The cell is transparent to x rays and

permits observation of a large fraction of the x-ray diffraction pattern

of single crystals of high-pressure phases. The cell is used to determine the unit cell size and symmetry properties of any material whose

single crystals can be grown under pressure. This includes material

normally liquid at room temperature and at temperatures as high as approximately 300 °C under pressure. Included also are materials

which are gaseous under normal conditions with boiling points as low

as — 50 °C and materials which are solid under normal conditions but

have high-pressure polymorphs.

To determine the structure of the material, it is necessary to measure the intensities of the diffracted spots with precision. These intensities are affected by absorption in both the diamond anvils and the

beryllium metal of the cell. It is therefore necessary to correct the

observed values for this absorption. The appropriate corrections have

been calculated for all orientations of the cell and positions of the

diffracted spots, and have been verified by measurements on crystalline

bromine. Bromine, a liquid at room temperature and pressure, freezes

at about —13 °C at 1 bar. Its crystal structure has been determined

previously with crystals at low temperature. Using the beryllium cell, bromine was frozen at room temperature and approximately 5000 atm

(5 kbar). The symmetry properties and unit cell were found to be

consistent with those of the low temperature crystal. The intensities

calculated from the known structure were compared with the observed

intensities as corrected for absorption in the diamonds and the cell and good agreement was obtained.

Pressure Indicator for Use in the Diamond Cell.—A satisfactory

spectroscopic pressure indicator for use in the diamond-anvil highpressure cell has been developed. The calibrant consists of a spectroscopically thin slab of nickel dimethylglyoxime placed in the pressure

chamber between the diamond anvils with the material being studied.

The position of the pressure-sensitive absorption band in Ni(DMG) 2 is determined spectroscopically and can be used to define the pressure

to within ± 1/4: kbar. The calibration curve, determined by the freez- ing pressures of liquids at room temperature, is rigorously valid only

92
Crystal structures of materials at high pressure are determined by x-ray

diffraction in this assembly. Single crystals, grown in the beryllium diamondanvil high-pressure cell (center), are oriented in the x-ray beam by means

of the special goniometer head (left). X-ray diffraction precession patterns are recorded by the film located at the rear.

at room temperature to pressures of approximately 20 kbar, the freez- ing point of ethyl alcohol. An additional measurement on methyl al- cohol is available but the reported freezing point appears to be uncertain. If a reliable value for the freezing point of methyl alcohol

is reported, the range of utility of nickel dimethylglyoxime will be ex- tended to approximately 40 kbar. Although the calibration curve has

been determined only at room temperature, it appears most likely that

it can be applied at higher (to 100 °C) and lower temperatures by using

a linear correction.

Automated Diffractometer for Crystal StrucPwre Determinations.—

A single-crystal x-ray diffractometer and ancillary instrumentation

has been assembled to operate (1) on-line under direct control of a

remote, time-shared computer with communication via a full duplex

teletype channel requiring no special interface and (2) off-line under

paper tape control. This instrument is used in place of conventional

x-ray cameras for obtaining x-ray diffraction patterns needed in determining the structure of crystalline solids. The instrument orients a material sample in an x-ray beam and measures the intensity of the

diffracted beam. By eliminating the need for an operator to make

the angle settings and transcribe the data, the automated system

makes possible around-the-clock operations with increased speed and

accuracy. The system differs from others in that it has been designed

to operate both by reading a punched paper tape prepared by a com93
puter (off-line control), or by a direct link with, a remote computer

over a telephone line (on-line control). Crystallographers in IMR

now have new freedom in tackling structure determinations of great

complexity. The result is likely to be a more thorough understanding

of the structure of many more classes of materials.

XRAY67—A Program System for X-ray Crystallography.—Cooperative efforts by scientists in IMR, the University of Maryland, and

the U.S. Geological Survey have produced a general x-ray computing system, XRAY67, that includes all the programs required to solve structures using either x-ray or neutron diffraction data. The treat- ment of different diffraction data is similar with respect to symmetry,

settings, amount of data, number of parameters, and ease of use. This

system is designed to be used by scientists in laboratories involved in structure determination.

XRAY67 consists of a set of Fortran programs which share a com- mon data file and includes programs that permit : data reduction, the

calculation of electron density maps, least squares refinement of atomic

parameters, the calculation of bond angles and distances, and many

other calculations required in the determination of crystal structures. Dislocations in Crystals.—Deviations from a perfect crystal struc- ture such as dislocations and impurities are known to affect the

strength and other mechanical properties of the crystal. Hence, it is necessary to have an adequate theory of dislocations available for application to real substances. A step in the development of such a theory was the completion of a complex nonlinear dislocation theory for applications to interactions between dislocation groups and to concentrated distributions of dislocations.

Molecular Conformations by NMR.—The conformation (topography) of four 1,2 : 3,5-diO-benzylidene-a-D glucofuranose derivatives

have been determined by nuclear magnetic resonance. The proton spec- tra of the componds were recorded from solutions that were maintained in a magnetic field of 2.3 T., corresponding to a radio frequency

of 100 MHz. At this high field strength, many of the proton multiplets were resolved.

Proportional Detector for Mossbauer Spectrometry.—One problem

that has prevailed in the measurement of Mossbauer spectra is the

time required to obtain a high quality spectrum. Proportional detectors are used to detect radiation from the source but they have low

efficiency. A new detector has been designed which has a much larger

radiation sensitive area than has been used before. Serious diffi- culties in degradation of detector resolution were resolved by careful

positioning and sizing of the electrodes in the detector. 94
The detector was optimized to detect the x-rays produced by the

internal conversion process resulting from the decay of the Mossbauer

energy level in 57Fe. This was done by optimum selection of detector

thickness and by use of a methane-argon detector gas. This device can also be used to detect conversion electrons by replacing the detector window by a sample to be measured and by using a methanehelium detector gas. Mossbauer Spectrometry of Nickel Compounds.—The practical application of Mossbauer spectrometry to the study of nickel compounds

has been enhanced by the discovery of a practical source of radiation.

This source is produced from bremsstrahlung generated by the JSHBS

linear electron accelerator via the 62M(y,^) 61 Co reaction which decays

by beta particle to the 67.4 KeV Mossbauer level of 61M. A single line source was discovered by producing a chromium-nickel alloy with

composition adjusted to eliminate an internal magnetic field. As a re- sult of the discovery of this source, nuclear data such as the magnetic

moment ratio of the excited to the ground state and the nuclear radius

change during the nuclear transition have been measured.

The nuclear magnetic hyperfine interaction is large enough in 61Ni

to permit the measurement of the internal magnetic fields in nickel

compounds and alloys. Although the chemical shift is small compared

to the linewidth, it is possible to identify the formal oxidation states of nickel in chemical compounds.

Crystallography of Calcium Carbonates.—Three anhydrous calcium

carbonates—calcite, aragonite, and vaterite—are widely encountered

;

the existence of two hydrated forms, CaC03 -6H2 0 and CaC03 -H2 0

is less recognized. As a result, the possible role of the hydrated salts,

particularly in the formation of anhydrous salts, has been largely over- looked. The crystallography of calcium carbonate has been investigated

by IME scientists because of its possible relationship to calcium phosphate mineralization in tooth and bone. The crystal structure of

CaC03

• 6H2 0 was determined and was found to contain discrete ion

pairs, [CaCOs] , surrounded by water molecules. The occurrence of this

grouping in CaC03 6H2 0 accounts for the facility with which these

crystals grow. This is the first crystal in which this ion pair has been

found, and its structure has bearing on the structure of the [CaC03 ] ion pairs that are believed to exist in solution.

In parallel investigations, the structures of two hydrated calcium

sodium carbonates, CaNa2 (C03 ) 2 -5H2 0 (gaylussite) and CaNa2 (C03 ) 2 -2H2 0 (pirrsonite) were determined. The structure of gaylussite is of particular interest in that it contains [CO;i CaC03 ] ion

triplets.

95
Structure of Water.—It is generally accepted that the structure of

water around solutes has an important effect on the thermodynamic

properties of aqueous solutions. The forces between protein molecules

are greatly affected by these structures. NMR spectra were determined

for water absorbed in collagen, the main protein of connective tissue. These spectra show that the water molecules diffuse rapidly through

the pores, but do not rotate isotropically.

Polymer Characterization.—Physical properties such as viscosity

and plasticity are mainly dependent on the distribution of molecular

weights in the polymer sample. Techniques for fractionation have now

been developed for polyethylene, the commercially most important

plastic at present. Several instruments can be used for molecular weight

determinations of the fractions, provided they have been calibrated.

Variation of Unit Cell Dimensions.—It has been shown that the

orthorhombic unit cell dimensions of a given polyethylene are not

unique, but depend upon the physical history of samples crystallized

from either the melt or solution. Variations in cell dimensions result from variations in crystallization temperature, annealing temperature,

and annealing time as well as from deformation of the crystals. The

origins of the effects cannot be assigned with certainty but the observed changes are consistent with a mechanism involving strain

from the molecular folds on the crystal surfaces. Corresponding to the changes in dimensions are significant changes in unit cell density

and apparent changes in degree of crystallinity. The effects of cell variation no doubt play a role in the variation of many macroscopic

physical properties with physical history of commercial polymer

samples.

Stacking Faults in Alloys.—One basic parameter that determines

the mechanical properties of materials is the stacking fault energy.

Since technologically useful structural materials generally consist

of combinations of several different phases having different chemical

compositions, it is desirable to determine the effects of phase and

composition changes on the stacking fault energy. The electron microscope has been applied to a study of cubic and hexagonal phases in

several silver-tin alloys in order to establish the effect of phase and

composition changes in a simple system. Results indicate a near

equality in the stacking fault energy for these two related phases.

Quantitative Microscopy. An optical photographic scanner has

been constructed to evaluate photomicrographs taken from a wide

range of metallic and nonmetallic materials. Measurements characterizing the internal grain and phase structures are of great

96
importance in controlling the quality and uniformity of materials.

Machine-evaluated photographs are being compared among different

laboratories for the purposes of improving capability.

Adherence of Porcelain Enamel on Aluminum.—The Porcelain

Enamel Institute is sponsoring a Research Associate Program to in- vestigate the adherence of porcelain enamel to aluminum. The electron

microscope and electron probe microanalyzer have been applied to study the interface between the two materials. Some basic differences near the interface have been observed between porcelain enamelaluminum alloy systems showing good adherence with subsequent

spalling resistance and those combinations which fail. The electron

microscope shows a layer of foreign material present at the interface

of those systems which have poor adherence. The electron microprobe

also detects an enrichment of magnesium at the interface region on

certain alloys that exhibit poor coating adherence. Neither the layer nor magnesium buildup was observed on the systems having good

adherence.

Tapered-section through a porcelain enamel-aluminum alloy specimen as seen by the electron microscope shows (arrow) the presence of additional material at the interface. This material affects the degree of adhesion

coating.

97
DATA ON THE PROPERTIES OF MATERIALS

This program area includes making precise measurements of materials properties and the development of new measurement techniques.

It also includes fundamental investigations of physical phenomena of

importance to science and industry (corrosion, fatigue and fracture,

etc.). Establishing the laws relating the physical properties of materials to their characteristics is of prime concern. Theoretical work plays

a major role in this area. Mechanical Properties and Strength of Materials

Elastic Constants of Lower-Symmetry Tetragonal Crystals.—

A

complete analysis of the elastic constants of CaMo04 were made in

order to predict mechanical stability in applications such as a host

crystal for laser rods.

This analysis was also of scientific interest. Accurate determinations

of elastic constants of single crystals are based on resonance frequency

or wave velocity measurements. Wave velocity measurements can be

made upon small specimens and as a function of pressure ; however,

the analysis is complicated for low-symmetry crystals and some of the

elastic constants depend upon choosing the appropriate root of an

algebraic equation. Fortunately, the elastic constants appear linearly

in the expressions associated with the resonance technique ; therefore, no ambiguity arises. In this experiment the complete analysis extended

the elastic constant determination usually effective only for high-symmetry tetragonal single crystals to lower symmetry tetragonal single

crystals.

Properties of Electrodeposited Copper.—An IMR Industrial Research Associate, sponsored jointly by the American Electroplaters'

Society, Inc., The International Copper Research Association, and the

Copper Development Association, has obtained comprehensive data on the properties of electrodeposited copper. Types of plating baths

used in the program included sulfate, cyanide, pyrophosphate, fluo- borate, and amine. A total of about 150 sets of operating conditions were used, comprising variations in bath composition, temperature,

and current density. Properties measured and correlated include tensile

and yield strengths, modulus of elasticity, elongation, internal stress, fatigue limits, hardness, density, electrical resistivity, thermal expansivity, structure, and chemical composition. Effects of cold working and

annealing, and effects of cryogenic and elevated temperatures on some

of the above properties were also determined.

Ultra Stable Maraging Steel.—Measurements over a two-year period

of the temporal dimensional stability of a 12 percent Nickel maraging

steel heat treated to meet requirements for a gage block material

98
indicate that it is one of the most stable materials ever observed in the

continuing NBS gage block program. The long time dimensional sta- bility of this important new class of steels has never before been

reported. Stability of the two test blocks were —0.03 ^in/in/yr and

+0.10 /rni/in/yr respectively.

Studies of Fiber Reinforced Metals.—The problem of identifying

the constituents as well as their distribution in an aluminum-silicon

alloy containing sapphire fibers was solved, in part, with the use of

color photomicrography and the microprobe analyzer. Factors con- tributing to the strengthening of vapor-deposited copper reinforced

with tungsten wires were correlated with ductility, fracture types, and

resistivity measurements.

Microplasticity in Metals.—The accuracy of microstrain measure- ments has been improved by two developments. An IMR designed

specimen enables measurements to be made over a well defined gage

length, and precision measurements of temperature of the specimen

allow for the correction of temperature effects caused by loading and

unloading. Neither of these features have been indicated in reports

emanating from other laboratories.

Fatigue Cracking in Chromium Coated Iron.—Chromium diffusion

coatings on commercial Armco Iron lead to changes in microstructure,

stress distribution, and strength in the outer layer of the base material.

These factors affect the mechanism of fatigue formation. In coated

samples, the crack initiates below the Cr-rich zone, generally in the

grain boundaries where precipitated chromium carbides were dis- covered. Residual tensile stresses introduced below the coated layer by

the process are considered an accelerating factor for crack formation.

Fatigue Crack Propagation Under Constant Load Amplitude.—

A

theoretical-mathematical evaluation of fatigue crack propagation in

cyclic bending was completed. It was found that fatigue crack propagation can be expressed as a function of stress intensity factor. The

experimental results agree closely with the theoretical model. The

influence of localized (heterogenous) structural changes on the proposed model were also investigated. It appears that the length of

fatigue crack propagation and the rate of propagation cannot al- ways be expressed as a function of plastic zone size. This was related

to the anisotropic conditions of plastic deformation.

Fatigue Due to Reversed Bending and Reversed Torsional Loads.—

A recently completed investigation showed that fatigue damage due

99
to reversed bending loads did not reduce the resistance to fatigue

crack initiation under reversed torsional loads. The experiments were

conducted by stressing (bending) aluminum alloy specimens until a number of small fatigue cracks had developed, then determining the

number of stress cycles required to develop small cracks under reversed

torsion. It was found that this number was not significantly different

from that required to give equivalent damage in specimens that had

not been stressed previously. The reversed sequence was also investigated and it was found that prior stressing in reversed torsion did

not affect the resistance to crack initiation in reversed bending. The

results indicate that in alloys of this type the damaging effect of

fatigue stressing is limited to a relatively small proportion of the

crystals which are subjected to potentially dangerous ranges of stress.

Stress Rupture Characteristics of a Titanium Alloy.—In contrast

to some theories and some experimental observations on other metals

and alloys (e.g., copper and some steels), ductility of Ti-8Al-lMo-lV

increased with increase in test temperature and decrease in strain rate in creep tests with rupture times up to 10,000 hr. Although stress- rupture properties of this alloy were greatly affected by notches at low temperature, the presence of notches of varying notch geometries

had little or no effect on the behavior at elevated temperatures.

Improved Dental Cements.—Zinc oxide-eugenol (ZOE) cements

have found many applications in dentistry. This puttylike material

is more compatible with both the hard and soft tissues of the mouth

than other dental restorative materials. Previous investigations at 1MB, have shown that incorporation of c-ethoxybenzoic acid (EBA)

and certain additives to ZOE mixtures greatly improved the mechanical properties of these cements. Recent studies have shown that aluminum oxide acts as a reinforcing agent and further enhances mechanical and physical properties. The high strength and low solubility of the A12 03 reinforced

materials, as well as their ease of manipulation, suggested their use

for the final cementation of cast crowns and as insulating base. Cements based on the formulations developed at NBS have become

commercially available and have been well accepted by the dental

profession. Further modification of these products incorporating co- polymers of relatively low elastic moduli are showing considerable

promise as a rapidly intertable, long-duration temporary restorative.

A material of this type is of special interest to the Armed Forces

since the prolonged life of this material would permit delay of nec- essary definitive treatment. 100
Rabidly Fabricated Surgical Splint.—A large percentage of all in- juries incurred in combat are manifested as damage to facial structures. Among these, fractures of the mandible (jaw) commonly occur. The presently employed technics of splinting fractures of the mandible using archbars are not only traumatic to the oral tissues, but

are also time-consuming and require highly trained personnel and

specialized laboratory equipment and facilities. A polymeric material suitable for the rapid fabrication of splinttype appliances for the fixation and stabilization of fractures of the

mandible has been developed for the Department of Defense. The

doughlike product formed on the mixing of the powder and liquid can be readily adapted to the cervical third of the intact teeth. Polymerization occurs in the mouth within 4 to 7 min. at peak temperatures

not exceeding 50 °C. The polymerized product exhibits sufficient strength, rigidity, and dimensional stability to function as a splint.

Preformed, spring-like lingually inserted clasps prevent the buccal

displacement of the polymerized splint and serve also as anchor points

for interarch elastics. The use of the "rapid splint" precludes the need

for cast arch-bars and complicated wiring procedures.

Limited clinical tests for this application and for the stabilization

of alveolar fractures and avulsed teeth have been conducted successfully. The same polymeric material may find application as a hard

denture reliner, as an orthopedic splint and for the stabilization of

metal implants.

Rapidly fabricated surgical splint made from a dough-like polymer which

hardens in the mouth in 4 to 7 minutes.

101
Reactivity and Corrosion

Reaction of Oxygen Atoms with Olefins.—Studies of the reactions of

oxygen atoms with olefinic molecules at cryogenic temperatures have

been completed. They have relevance to problems of atmospheric pollution. The transition state model adopted for the initial stage of the

reaction is one in which the oxygen atom approaches the olefinic bond

in the plane of the molecule. Further, there is a force between the

oxygen and the hydrogen atoms attached to the olefinic carbons on

the O atom approach side. This interaction, though weak, is sufficient to inhibit the migration of the hydrogen atom in the passage from the

transition state to final products. The model has general applicability

and has been successful, for example, in predicting the course of reac- tion for 2-methyl-2-butene.

Second Layer Migration and Adsorption Displacement.—By combining a field emission microscope with a molecular beam apparatus

and operating the microscope at liquid helium temperatures, it was

possible to make detailed observations of second-layer migration of

hydrogen, nitrogen, and carbon monoxide on a tungsten surface. The

tungsten emitter was placed with its axis perpendicular to the molecular beam. The characteristics of the second-layer migration with

trapping on free sites were determined. The density of the free sites as well as surface geometry appear to be instrumental in the structur- ing of the sharp boundary shape as the migration progresses over the

surface. An unusual effect was that of the flow of nitrogen around the

100 planes of the tungsten surface, leaving them as uncovered islands

until most of the rest of the surface was completely nitrogen covered.

It has been known that carbon monoxide or nitrogen are capable

of replacing hydrogen adsorbed on tungsten. With the molecular beam

field emission microscope apparatus using sequential deposition and

field emission observations of the surface, it was found that the dis- placement occurs even at 4.2 K. The displacement is not complete,

however, and a relatively strong binding state of hydrogen remains

undisplaced.

Electron Interaction With Chemisorbed Diatomics.—Studies of

processes occurring upon electron impact on chemisorbed diatomics

have led to useful information in assessing the chemisorption process. The low energy (<75 eV) electron-impact conversion of a weakly

chemisorbed molecular y

species of nitrogen on tungsten to a more

strongly bound chemisorbed species has been Observed. This new state, designated as A, effectively doubles the concentration of strongly bound

nitrogen after the conversion from y to A by electron impact. Neither

N2+ nor N+ were detected with electron bombardment of the nitrogen

102
covered tungsten surface. In a mixture of 14N2 and 15N2 absorbed in

the y

state, isotopic mixing was not observed in the residual y state layer after electron impact.

Combination of Surface Measurement Techniques.—A technique has

been devised to enable low-energy-electron diffraction (LEED) and

field-electron microscopy (FEM) investigations to be made on a single

specimen. Since LEED primarily determines long-range single-crystal

plane surface structure and FEM detects and characterizes shortrange adsorption effects, the two individual techniques complement

each other. This removes some of the shortcomings of the techniques

when used separately, and enables meaningful adsorption sensitivity

comparisons to be made.

Microbial Corrosion of Iron.—An investigation of the anaerobic

corrosion of iron has shown that sulfate-reducing bacteria cause cor- rosion by a cathodic depolarization mechanism, utilizing phosphate

as an electron acceptor. Iron phosphite is produced as a result of this

corrosion process. The currently accepted theory is that sulfate is reduced with the production of iron sulfide. Stress Corrosion Studies.—The stress corrosion of aluminum alloy

extruded plates used in the aircraft industry occurs much more readily

when the plate is stressed in one direction with respect to the extrusion direction than in another direction perpendicular to this. Scanning electron microscopy revealed that crack initiation occurs in very

short times without regard to the stress direction, but that crack

propagation does, and this controls the time to failure.

The Reactivity of the Components of Tooth Structure.—A com- mon cause of failure of a dental "filling" is the inadequate seal be- tween the surfaces of the hard tooth tissue and the materials used to replace tooth structure lost through decay or accident. The need for a truly adhesive restorative that would enhance the quality of the

marginal seal has been recognized for many years. Lack of information regarding the chemical and physical characteristics of the

surfaces of tooth structure has retarded progress towards the

development of such a material.

An investigation of the reactivities of the components of human tooth

structure has as its objective the determination of those substances

that will bond to or modify tooth surfaces in the aqueous envinronment encountered in the oral cavity. Results obtained strongly suggest that the collagenous constituent, as well as the mineral portion

of tooth structure, presents a vast number of reactive sites to which

the bonding of a restorative may be achieved. A knowledge of the

103
substances that will bond at available or newly activated reactive sites may lead to the development of a biologically and mechanically suit- able adhesive dental restorative and a colorless transparent "painton" that could be applied to pre-carious decalcified areas to arrest tooth

decay in its initial stages.

Microscopic Studies of Corrosion.—The susceptibility to stress cor- rosion cracking of some commercial aluminum alloys is known to de- pend on the direction and magnitude of the applied stress and on the

temper of the material. The technique of transmission electron microscopy was applied to study directly the internal structures in alloys

subjected to different tempering treatments. The more resistant material was found to contain fewer defects and larger internal precipitate

particles. The observed directional corrosion susceptibility could be

correlated with internal boundaries in the material but not with other

structural characterises.

An electron microscope photograph of the internal structure of an aluminum

alloy subjected to stress-corrosion testing.

Adsorption of Polymers on Surfaces.—The adsorption of polymer

molecules on surfaces is being investigated for both technological and

scientific reasons. The nature of the interaction of these molecules with

surfaces is important to the field of adhesion, coatings, and composites.

104
Scientifically, it is important to understand the changes in the con- formation of a molecule upon its interaction with a surface and to establish the number of contacts of the long chain macromolecule with

the surface. The work which is still underway has provided significant

understanding of these parameters. As part of this study, the adsorption of a simple smaller molecule, stearic acid, was studied to help in- terpret the results obtained from polymers. Mercury was selected as a

substrate in order to provide a well-defined, smooth, and clean surface.

The measurements were carried out using stearic acid labeled with

radioactive C-14, and the development of new measurement techniques was required. The results showed a surprisingly high concentration of

stearic acid on the mercury surface, demonstrating the ready accessibility of the surface to these organic molecules.

Thermal Decomposition of Organic Aromatic Liquids.—The thermal

decomposition of biphenyl, phenyl ether, and their eutectic mixture

has been studied in the temperature region of 350 to 450 °C. The

eutectic mixture is a well known heat transfer liquid and is to be used

in many advanced type power generating systems including those

designed for use in remote installations. Detailed identification of the

20 or more decomposition products and measurement of their rate of

formation is being carried out. The products from the pyrolysis of bi- phenyl are: hydrogen, methane, benzene, 3 terphenyl isomers, and 5 quaterphenyl isomers. The eutectic mixture yields similar products

in addition to phenol and phenoxy ether type derivatives. Quantitative

analyses are performed by vapor phase chromatography of the liquid

and solid products. From the rate data of the decomposition of initial material and formation of products at various temperatures, activitation energies are calculated and compared. Data of this type are important in determining reaction mechanisms by which these fluids degrade thermally and in extrapolating the results to the conditions

of technological applicability.

Thermodynamics and Kinetic Data

Model of Two-Dimensional Polymer Crystallization.—A model of

two-dimensional polymer crystallization by chain folding was treated

by equilibrium statistical mechanics. The Laplace transform of the

partition function with respect to the length of the polymer chain was

obtained in exact analytical form. The model leads to thermodynamically well-defined chain- folded crystals. Under certain circumstances in the limit of an infinitely long polymer chain, the model

shows a second-order phase transition from an "extended-chain"

crystal to the chain-folded crystal.

105
Theoretical Chemistry.—Two physically dissimilar problems which

are identical from a mathematical point of view have been investigated.

They are

:

(1) The simplest nontrivial example of the excluded volume problem which arises in the discussion of the mean dimensions of chain

polymers. In this example, the only excluded volume restriction on the

overlap of units of the polymer chain which is considered is that no

unit of the chain can overlap the first unit. The effect of this restric- tion on the mean square end-to-end distance in the chain is evaluated

in the cases where the polymer chain is confined to a solution surface

and were the chain molecule is in solution.

(2) The time-dependence of the momentum autocorrelation function of a heavy isotopic particle in a harmonic crystal in the case where the crystal is treated as finite. It is shown that in the case of a one-dimensional crystal the momentum autocorrelation function is approximately a simple exponential. Explicit estimates of the accuracy

of this representation of the autocorrelation function are obtained and

are of interest because the heavy-particle-in-a-crystal system serves

as an example of a particle exhibiting Brownian motion.

Annual Index of Worldwide Published Thermochemical Studies.—

As a part of its continuing program on the collection and evaluation

of chemical thermodynamic data, the IMR Thermochemical Data Center has participated for several years in preparing the Bulletin of

Thermodynamics and Thermochemistry. This annual Bulletin, under

the auspices of the International Union of Pure and Applied Chemistry Commission on Thermodynamics and Thermochemistry, contains

listings of the thermodynamic work in progress in laboratories

throughout the world and an index to the published thermodynamic

literature of the past year. The National Bureau of Standards makes its principal scientific contribution to the Bulletin in the preparation of the index. Its con- tinuing program in the collection and critical evaluation of thermodynamic data provides a natural resource for this information as a

step in a more complete study which is carried out by the NBS

Thermochemical Data Center. The Bureau contribution covers the

general field of inorganic and metal-organic compounds and indicates

properties that were measured for each compound listed. Organic

compounds are covered by another group. The current issue of the

Bulletin includes over 2,300 references, with about 8,000 citations to chemical species in the index.

In the preparation of the Bulletin this year, all material was

originally entered on punched tape. Computer programs and techniques were then used for editing, sorting, arranging, and final output

106
of camera-ready copy. This serves as a pilot project for the eventual

mechanization of data handling and storage for the general files of

thermodynamic data material by the Center. Thermochemistry of Fluorine—Containing Oxidizers.—Several

fluorine containing compounds have important potential use as stor- able liquid oxidizers for special rocket propulsion problems. A study

of the heat of formation of chlorine trifluoride has resolved sus- picions that previous data were in error by several kilocalories per

mole, and has provided a more accurate value for the heat of formation. The extremely reactive gas was reacted with excess hydrogen

and a liquid water phase in a constant-pressure flame calorimeter,

giving a mixture of dissolved hydrofluoric and hydrochloric acids. The flame calorimetry technique has demonstrated its adaptability to

a number of problems of this kind with increasing accuracy and is being extended to chlorine pentafluoride and to trifluoramine oxide.

Chemical Kinetics Mass /Spectrometry.—A major objective of the

chemical kinetics mass spectrometry program has been the measure- ment of rate constants for the reactions of atoms with organic

compounds. The first series of measurements involved reactions of

atomic nitrogen with various olefins and acetylene. This work has now

been extended to reactions of atomic oxygen. Results have been obtained for a series of alkanes and alkyl halides from about 200 to 650 K.

Cracking of Hydrocarbons.—Decomposition of hydrocarbons at high temperatures has been studied by millisecond heating with a shock wave. In the initial step a carbon-carbon bond is broken, forming

two free radicals which may later react or further decompose. Detailed

studies have shown which bonds break, how rapidly this occurs, and the

relative importance of each route. Potential Energy Surfaces for Chemical Reactions.—Calculation of

rates of chemical reaction and reactive cross sections requires exact quantum mechanical calculation of the forces acting between molecules.

The contours of this "potential energy diagram" were calculated for

the HHD system. This is the first of several such surfaces which are being calculated as input to theoretical determination of reactive cross

sections for elementary processes. Calculations of such "exact" surfaces,

i.e., ones for which no approximations are made in the physics of the

system, are becoming competitive in cost with the experimental rate determinations.

Photoionization Mass Spectrometry.—The Mark I Photoionization

Mass Spectrometer utilizing a photon energy bandwidth of 1 A at any

desired wavelength throughout the vacuum ultraviolet region (1500

107

320-738 O—68 8
to 600 A) lias provided values of highest known precision and accuracy

for threshold measurements and thermodynamic properties for a number of gaseous molecules of importance to the understanding of

physical and chemical phenomena in terrestrial and extra-terrestrial

atmospheres. Also, the past year has seen the completion and initial operation of the Mark II Photoionization Mass Spectrometer with

optical and ion detection capabilities beyond those of the Mark I machine. This new and powerful tool was constructed for the study of

"ion spectroscopy" ; i.e., the detailed investigation of excitation processes of ions including the relationship of various spectroscopic phe- nomena to the modes and kinetics of ion formation and decomposition.

Preliminary experiments have already shown the feasibility of achieving significant advances toward these goals and toward still further

improvement in the determination of thermodynamic properties of

molecules and ions.

Mark II Photoionization Mass Spectrometer developed for the detailed investigation of excitation processes of ions. Vacuum Ultraviolet Fluorescence Studies.—Upon irradiation in the vacuum ultraviolet a molecule may dissociate and produce an elec- tronically excited fragment which fluoresces. The threshold energy

of the incident light needed to produce the fluorescence should give an upper bound for the dissociation energy of a molecule. This method

has been successfully applied to a number of cyanogen compounds and

the heat of formation of CN has been derived. Photodissociation processes to form electronically excited fragments have been correlated

108
with, the absorption processes and reactivities of electronically excited

fragments have been measured from studies of quenching of the

fluorescence.

Photolysis of Simple Molecules.—The nature of the particles into

which an excited molecule fragments has been investigated for such

molecules as CH4 and CH2 CO. A twin cell technique was used in

which two reaction systems are simultaneously but independently

irradiated. The photochemistry in the individual cells may then be

directly compared with respect to quantum yields and modes of fragmentation.

Superconducting Metal Compounds.—Studies are now in progress to determine the constitution and degree of atomic ordering in alloys con- taining metals of the platinum family. As a result of these studies,

several metal compounds have been discovered to lose their resistance

to the flow of an electrical current (superconductivity) at extremely

low temperatures. The new superconductors are Cr72 0s28 , Cr3 Ir, Cr3 Rh,

and Nb3 Os—all having the A15 or beta-tungsten type crystal structure. The temperature at which these compounds become superconducting

is found to be dependent on the degree to which each atom type tends

to segregate in occupying the available atomic positions. A high transition temperature is desirable for many practical applications.

Solubilities of Calcium Phosphates.—Measurements on the solubilities of CaHP04 , CaHP04 -2H2 0, Ca8 H2 (P04 ) 6 -5H2 0, £-Ca3 (P04 ) 2 , and Ca10 (OH) 2 (PO4 ) 6 have been carried out in the ternary system

Ca(OH) 2-H3 P04-H2 0 at various temperatures between 5 and 37 °C.

From these data it is possible to calculate the relative stabilities of

the calcium phosphates and to predict what reactions can take place

under the conditions of their occurrence. The data lend themselves

to the calculation of a self-consistent set of thermodynamic quantities

for this group of important inorganic compounds, which occur in

hard tissues such as tooth and bone and in many soft tissues. They

also have considerable industrial importance as fertilizers, in sugar

purification, in sewage treatment, as minerals, and in fluorescent lamps.

In all these connections, the solubility characteristics of the various

calcium phosphates determine the biochemical behavior or the conditions of manufacture or use. Vaporization of High Molecular Weight Organic Liquids.—The

rates of molecular vaporization of large organic molecules have been

measured. These molecules have molecular weights ranging from 500

to 2000 and are of the type used to plasticize polymeric materials.

Hence their ability to evaporate has a considerable technological importance. The results of the study demonstrate that the energy of

109
evaporation can be relatively small since these flexible molecules apparently coil up and evaporate approximately as spheres. An understanding of these processes has an application not only to the plasticization phenomenon but also to space and environment related questions as well as to the thermal decomposition of high polymers.

Reference Materials for Low Vapor Pressure Measurements.—Five

reference materials are being developed for calibration and checking

of equipment and techniques used in measuring vapor pressures in the

10"1 to 10"6 torr (1 torr= 133.32 N/m2

) range. These high purity

samples are cadmium, gold, silver, platinum, and tungsten. The materials will be suitable for a variety of pressure measurement methods

and will cover the temperature range 500 to 3000 K. The materials will

be particularly useful in the fields of high temperature chemistry and

refractory metals. Thirty laboratories from the United States, West

Germany, and Italy are cooperating in the program.

Equation of State in the Critical Region.—Studies around the criti- cal point in the gas-liquid region of a one-component system and in

the liquid-liquid phase separation of a two-component system con- tinue to be of interest to test recently proposed theories. Accurate

measurements on a liquid-liquid system are in excellent agreement

with those on one-component systems, indicating that a common basis

underlies the equations of state in the critical region of quite different

systems.

Melting Point of Aluminum Oxide.—The melting point of alu- minum oxide (A12 03 ) has been determined in controlled environments

in an attempt to explain the variance in seemingly reliable values

reported in the literature. Employing a modified quench technique,

melting point experiments have been conducted in specially designed

induction furnaces capable of heating small samples under blackbody

conditions to 3000 °C in vacuum, 2600 °C in helium or argon, and

2400 °C in air. The data indicate that the melting point of A12 03 in vacuum is 2051 °C (IPTS). Maximum overall uncertainty is esti- mated to be ±6 °C. Precision of the measurements is ±1.5 °C.

Although the alumina point has been suggested as a secondary temperature reference point, the investigation showed that environment

has a significant effect on the melting temperature. Vacuum conditions

are believed to give the most reliable indication of the melting point of

AI2O3 single crystal specimens (sapphire). On the other hand, each of

the various atmospheres, including air, yielded significantly lower

melting points. To fully resolve the problems related to this material

and other potentially useful secondary temperature standards, an

international task force has been formed under the auspices of the

Commission on High Temperatures and Refractories, International

110
Single crystal test specimens (sapphire) utilized in the precise determination

of the melting point of alumina (AI2O3). The specimen on the left exhibits

characteristics melting upon heating at 2052 °C; the specimen on the right

remains unmelted after treatment at 2050 °C. Union of Pure and Applied Chemistry. The task force, chaired by

an NBS staff member, consists of 13 scientists representing nine

countries.

Monte-Carlo Studies of Self-Interacting Polymer Molecules.—Analytical theories of the configurations of polymer molecules cannot

treat in an exact manner the mutual interference and attraction of

different parts of the molecule with each other. In order to investigate

these effects, polymer molecules were simulated by chain lattices. An

attractive energy was found for each lattice for which the two effects compensate each other. Also some of the parameters characterizing the

configurations were found to be independent of the lattice model that was used.

Diffusion in Metals.—The relation between two major types of diffusion measurements has been determined with greatly improved precision. From calculations based on the theory of atomic diffusion in

metals, a relationship between (1) tracer diffusion experiments in

homogeneous alloys and (2) interdiffusion experiments in nonhomogeneous alloys was proposed. This relation has been confirmed by ex- periments in AgCd alloys.

Interdiffusion often is important in practical applications but is difficult to measure accurately by direct means. The present work

shows in detail how to use tracer measurements, which are very ac- curate, to predict interdiffusion results. This work also has wide im111
plications for other diffusion applications, since it demonstrates the

importance of several previously neglected terms in the thermodynamic diffusion equations.

Heat Capacity of Material in Glassy, Crystalline, and Liquid

States.—The heat capacity of any glassy material has usually been as- sumed to be similar to, though uniformly slightly higher than, that of

the same material in the crystalline state. A more careful examination

of this assumption has been made by measuring and comparing precise values for the heat capacities of the model material diethyl

phthalate in the glassy, crystalline and liquid states. Although the

above assumption may be satisfactory for rough purposes, it is in- adequate when a precise comparison is needed. In the temperature

range from about 30 to 75 K, the heat capacities of diethyl phthalate

glass are lower than those for the crystal by more than the limit of

uncertainty of the measurements. Examination of existing litera- ture shows that this is also suggested for some half dozen other materials over discreet temperature ranges. The results for diethyl

phthalate also bear out recent indications that at the lowest temperatures investigated, around 10 K, the heat capacity of a glass is much

higher than that of the crystalline state of the same material. This

fact may be connected with aspects of the molecular structure of

glasses which also manifest themselves in other types of behavior

such as dielectric relaxation, ultrasonic absorption, nuclear spin relaxation and thermal conductivity. The diethyl phthalate data also show

unequivocally for the first time that the heat capacities for the an- nealed glass and for the quenched glass differ by more than the uncertainty of the measurements.

Actinometry.—In order to unravel the mechanism of chemical

events induced in matter by interaction with high energy radiation,

it is important to determine the relative importance of ionization of

the molecules versus the raising of the molecules to highly excited

states. Using as radiation source an argon resonance lamp which emits

photons of 11.6 to 11.8 eV energy, saturation ion currents induced in

various organic compounds were compared with saturation ion cur- rents in a compound having a well known quantum yield of ionization.

In this way ionization quantum yields for these compounds at the

argon resonance lines were accurately determined.

The photolysis of several hydrocarbons at the argon resonance lines was studied. The modes of decomposition of the molecules excited to neutral levels above the ionization energy as well as the ionic mechanisms occurring in the high energy photolysis were elucidated. The

measurement of saturation ion currents permitted the accurate determination of the quantum yields of the various product molecules.

112
Point Defects in the Alkaline-Earth Halides.—Based on current

theories of the properties of highly ionic crystals, methods have been

developed for semi-empirical calculations of the formation enthalpies

of vacancies and interstitials in the fluorite structure, and applied to CaF2 , SrF2 , and BaF2

. This represents the first successful excursion of

this kind of theory beyond the alkali halides. The calculated values

successfully account for the predominance of anion Frenkel pairs in

these substances, and give formation enthalpies in close agreement with

measured values. They also account for the measured enthalpy of solu- tion of NaF in CaF2

. One of the interesting results of these calculations

is to suggest that in CaF2 containing trivalent cations, cation vacancies

may exist in addition to anion interstitials. The latter are generally

accepted as the charge compensation species, but experimental re- search in the literature occasionally hints at the presence of cation

vacancies as well.

Electric, Magnetic, and Optical Properties

Dielectric Properties of Foliage.—The dielectric properties of

foliage have been measured in a coaxial cylindrical sample holder at frequencies from 105 to 4 X 109 Hz. Line admittances were determined

using transformer bridges below 2.5 X 10s Hz and a slotted line above

2.5 X 108 Hz. Values of both the real and imaginary parts of the dielectric constant were found to approach those of water at the highest

frequencies and to approach very high values (^104

) at the lower

frequencies. The data are of value to researchers interested in the

effects of foliage on electromagnetic radiation, and the method is generally applicable to a wide variety of biological materials. This data was needed by the Navy to solve communications problems in Vietnam.

Photoelastic Constants of Glasses and Single Crystals.—Techniques

using a combination of hydrostatic pressure and uniaxial loadinghave been used for the determination of the photoelastic constants of

glasses and single crystals. This combination is unique with the

Institute for Materials Research and represents a new development in

this area. The symmetry of a crystal determines the number of photoelastic constants, and the number of directions in which the crystal

must be stressed to evaluate all of the constants. Experimentally, the

problem resolves itself into determining the absolute changes in refractive index and the birefringence induced by stress. In the past,

determination of the absolute changes in refractive index have proved

to be most difficult. The use of hydrostatic stressing offers several

advantages: (1) the precision of measurement is much greater, (2)

the dependence of refractive index upon density may be determined

directly, (3) much higher stresses may be obtained, (4) loading is 113
uniform, and (5) the shape and orientation of the cut specimen

becomes much less critical. A knowledge of the photoelastic constants of single crystals and

glasses is of great interest because of optical distortion induced in

laser rods by thermal stresses. Thermo-Optical Studies on Glass.—A study of oxide glasses of

different types—silicates, borates, calcium aluminate, germanates, and

phosphates—is now being made to determine the effect of composition on the temperature coefficient of refractive index. An interferometric

method has been used for the measurements. All of the specimens are found to have positive coefficients of refractive index except for the

borate glass, which is slightly negative up to about 400° C. By combining data on the change of refractive index as a function

of temperature with data on its change with density, it is possible to separate effects on polarizability caused by (1) the change in temperature alone, and (2) the associated change in volume. It is found that

the temperature term is the more important one for the glasses studied

thus far. This is in contrast to the behavior of crystals, where the

volume term is of greater magnitude. The change in refractive index

of optical materials with temperature is of great importance to designers of optical systems that operate over wide temperature

ranges. Transverse Electroreflectance Using a New Modulation Technique.—

A new measurement technique has been developed which allows a

detailed study of the electronic band structure of semi-insulating

materials. In this method the sample is modulated by means of a large

electric field (10 to 100 kV/cm) ; the field is applied between two

evaporated gold electrodes on the front face of the sample as an a-c square wave of frequency 1 to 10 kHz. The technique has been used on a number of semi-conductors and insulators in collaboration with

Brown University. Because of the square wave form, one has a better

knowledge of the magnitude of the applied field. Hence it is possible to study quantitatively the change in position, magnitude and shape

of the reflectivity peaks and edges as a function of the field. Another

advantage is the opportunity to explore the polarization dependence

of the absorbed or reflected light. A wide variety of materials have

been studied. Excitons in CdS were investigated and similar meas- urements were performed on ZnS, ZnTe, Si, GaAs, Mg2 Si, Mg2 Ge,

and Mg2 Sn.

Development of Unique NMR/NQR Equipment.—The design and

construction of an NMR/NQR (nuclear magnetic resonance/nuclear

quadrupole resonance) spectrometer has recently been completed. It

is being used for NMR and NQR line shape studies, and for studies

114
of a variety of dynamic processes such as molecular diffusion, molecular rotation, and chemical exchange processes. The spectrometer,

which can be used to study dynamic processes which occur in the time

interval 10~5 to about 10+3 seconds, has several unique features. Its high power (15 kW) and fast recovery time (about 4 jus) make it possible to study dynamics of solids as well as liquids, and also very

slow motions in viscous systems (such as polymers) via the rotating

reference frame technique. The unit has a continuously variable fre- quency range of 2 to 28 MHz, which is necessary for pure quadrupole

studies, and its single coil design permits low (below 4K) and high

(above 1200K) temperature studies. A second unit has been built to study NQK line shapes and intensities. The intent of the work in this

instance is to develop methods for accurate temperature measure- ments below IK.

Analysis of Magnetic Resonance Data.—A major standards experiment concerned with improving the accuracy and interpretation of

data obtained in magnetic resonance experiments has been completed.

Measurements were made of ratios of electronic to nuclear ^-factors

which will make it possible to determine ^-factors to an accuracy of one part in a hundred million. In the analysis of resonance lines con- taining arbitrary mixtures of absorption and dispersion, a simple

correlation has been shown to exist between the degree of admixture

and a system phase or frequency shift, thus enabling one to obtain the

pure lineshapes by a simple and known adjustment of the spectrometer. This result is of considerable practical importance in NMR studies

of metals. In related work, lineshape distortions due to large resonance

signals and the concomitant errors in the observed second moments

have been analyzed. A simple line sharpening device is currently being

constructed, which should be capable of significantly improving reso- lution in magnetic resonance spectroscopy without the appreciable

losses in sensitivity inherent in other methods. Finally, several novel

techniques are now being developed which will make possible a direct

determination, to a high degree of accuracy, of the absolute number of

nuclear and electron spins which give rise to magnetic resonance lines. These methods will eliminate the many serious drawbacks encountered in spin concentration measurements which are made relative to standard reference materials.

Ultra Low Frequency Impedance Bridge.—Two models of a novel

ultra low frequency impedance bridge were completed and put into

use. These bridges make complex impedance measurements (magnitude

and phase) at frequencies from 10~3 Hz to 104 Hz with an accuracy of

better than 0.1 percent in magnitude and 10-5 rad in phase. Impedances

ranging from pure capacitive to pure resistive are easily and quickly

measurable. Key features of this new bridge are: (1) the use of an

115
operational amplifier rather than the ordinary passive impedance

ratio arms to provide two voltages equal in magnitude and 180 deg

out of phase to the standard and unknown arms of the bridge respectively, (2) the use of a high impedance detector, and (3) the

application of a quadrature voltage to a capacitor to balance the con- ductance of the unknown.

Fundamental NMR Studies of Inorganic Hydrides.— Recent broadline and pulsed nuclear magnetic resonance (NMR) studies of

H11 B(OC2H3 ) 2 and HCo(CO) 4 at IMR in conjunction with scientists at the University of Illinois, have led to a significant new understanding of the way in which fundamental magnetic interactions of nuclei

determine the shape of NMR absorption spectra and the magnitude of

spin-spin and spin-lattice relaxation times. One result of this work

is the demonstration, both experimentally and theoretically, that the

usual Van Vleck theory, which relates the second moment of an NMR

absorption spectrum to the bond distances between the interacting

magnetic nuclei, does not always apply if some of the nuclei have

spin quantum numbers greater than one-half.

A nucleus with a spin greater than y2 can have a quadrupole moment.

If the nuclear quadrupole coupling constant is large or comparable

to the NMR frequency, this quadrupole interaction must be considered.

This discovery has led to the reinterpretation of some NMR structural

studies with the result that some metal-hydrogen bond distances are

0.1 to 0.2 A longer than the values reported in the literature. The work also contributes a technique for using pulsed NMR techniques for determining quadrupole coupling constants for liquid

samples. An experimental demonstration of this technique was given

for H^BtOC'Hs),. The agreement between the pulsed NMR study

of the liquid and the more difficult, but more familiar, broad-line NMR

and NQR study of the solid is excellent. Exchange-Coupled Ions in Transition-Element Complexes.—Electron spin resonance spectra of pure and doped binuclear complexes

of transition metal ions have been studied to investigate the nature

of the metal-metal interaction in these materials. The first observation

has been made of resonance from exchange-coupled dissimilar metal

ions and information has been obtained concerning the bonding in

these materials. These studies are of particular interest since it now

appears likely that metal-metal "bonding" in a number of inorganic

and organo-metallic compounds may lead to interesting and practical

electronic properties in these materials.

Ferromagnetic Beryllium Compound.—The intermetallic compound

CrBe12 has been discovered to exhibit ferromagnetism below 50 K.

Susceptibility in the paramagnetic state and magnetization in the

116
ferromagnetic state have been measured. Ferromagnetism as large as observed in CrBe12 has not been found to occur in MnBe12 or FeBe12 or

in a number of other isomorphous Be compounds. Magnetic studies on these materials will add appreciably to our understanding of ferromagnetism in metals, particularly in the new class of itinerant ferromagnets, of which CrBe12 appears to be an example.

Soft X-Ray Spectroscopy.—Valence band emission spectroscopy

serves as a useful tool in understanding the electronic structure of

solids by providing information on the distribution in energy of elec- trons through the valence bands. In a recent study, the M2i3 emission band of paramagnetic nickel was measured under carefully controlled vacuum and temperature conditions. Previously unreported

fine structure was observed. Detailed comparison was made between

the observed spectrum, available band calculations, and the related

results of photoemission and ion neutralization experiments. These

comparisons strongly favored interpretation in terms of the independent particle model. Marked apparent discrepancies between the

soft x-ray and photoemission results, and between the L and M

emission spectra, were shown to be largely accountable on the basis

of different transition probability variations as a function of energy

through the valence bands. In another study, a striking correlation was found between the M2)3 spectrum of Ni in TiNi and the variation

of electronic specific heat as a function of electron per atom ratio

for bcc transition metal alloys.

Analysis of Ellipsometer Measurements.—The ellipsometer is an

optical instrument used to measure extremely thin films. However,

its use has been limited by the complicated calculations required to determine the refractive index and thickness of a film from the ellipsometer readings. For this reason, a general purpose computer program was developed to analyze ellipsometer readings. This program

can calculate the properties of either a clean surface or a film on a

surface, can correct for imperfect optical components or a tilt of the

reflecting surface, and can determine confidence limits for the

calculated values.

Polybutylisocyanate in Dilute Solution.—Measurements of the complex dielectric constant have been made on dilute solutions of fractionated polybutylisocyanate (PBIC) in CC1 4 . The measurements, which

were carried out at 23 °C and over a frequency range 0.05 Hz to 200

kHz, yielded relaxation times and dipole moments of PBIC as a

function of molecular weight where Mw varied from 2.5 X 104 to 13X106

. For low Mw (<250,000) the relaxation time data indicate

that the molecule is in a rigid rod conformation. As Mw increases, this

rodlike conformation can not be sustained and the effects of chain

117
flexibility accumulate with the addition of each monomer unit to the

chain. Finally at high Mw (>106 ) the dominent mode of relaxation

is a long-range Rouse-Zimm normal mode and the conformation of

the molecule is random coil. In both limits, for rigid rod and random

coil, the molecular dimensions and dipole moments were calculated.

High Accuracy 2-Fluid Dielectric Measurements.—Dielectric meas- urements were made on a series of solid polymer specimens using newly

developed capacitance cells and a 2-fluid method. This method involves

making four capacitance measurements—with the sample in the cell and with sample out in each of two fluids. The advantage of the method

is that the average sample thickness (a major source of error when

using older conventional methods) need not be measured independently. An increase of roughly an order of magnitude in the accuracy

of the measurements has been realized and standard specimens have

been prepared with dielectric constants certified to about 0.01 percent.

Pressure Effects on Dielectric Properties.—The investigation of the

dielectric properties of materials has been extended to include the ef- fects of pressure. Complex dielectric constant and volume measure- ments have been made using newly designed and constructed equipment on both solid and liquid samples over a wide temperature range at pressures up to 2X 107 kg/m2 (about 2000 atm.). The liquid measure- ments provide data on the density and temperature dependence of the

polarization. The solid measurements have been used to study the pres- sure dependence of orientational relaxation parameters. In both cases the data separate the effects of changing sample volume by means of a pressure change from those due to changing sample volume with

temperature.

Dielectric Constants of PhW04 and CaWO\.—The class of com- pounds having the scheelite structure has received considerable atten- tion as potential host crystals for laser applications. These scheelite- type crystals have been the object of numerous investigations, but the

dielectric constants of PbW04 and CaW04 have not been measured

heretofore. IMR scientists recently made such measurements at 24.5 °C

in air on single crystals grown by the Czochralski method.

Hall Mobility vn Semiconducting SrTi03 .—During the last four

years an intensive study of the electronic properties of SrTi03 has

been in progress. As part of this program a close look has recently

been taken at the temperature and donor-concentration dependence

of the Hall mobility in order to obtain information on the scattering

mechanism. Data on conductivity and Hall coefficient provide directly a measure of the electron mobility. Samples with carrier-concentrations

varying between 3.4Xl017/cm3 and 5.3Xl020/cm3 were investigated.

118
These carriers were obtained either by hydrogen reduction of the

strontium titanate or by doping with Nb or La. At high temperatures

(300 to 1200 K) the mobility shows an exponential behavior. It appears that the theory for scattering by optical phonons in the intermediate coupling range gives reasonable quantitative agreement with

the experimental results. At very low temperature (T<10K), scat- tering by ionized impurities limits the Hall mobility. The scattering

potential is strong, invalidating weak scattering approximations com- monly used. Existing partial-wave treatment gives a satisfactory description of the data.

TECHNICAL ASSISTANCE TO OTHERS

IMR gives technical assistance and advice on materials to other

Government agencies, and to science and industry. Arranging confer- ences and seminars to facilitate dissemination of new data useful in

solving materials problems is one of the services provided.

Advisory and Consulting Services

Collapsed Bridge at Point Pleasant, W. Va.—NBS is assist- ing in the investigation of the collapse of the highway bridge at Point

Pleasant, W. Va., on December 15, 1967. The eyebar in which the

initial fracture occurred has been identified and sent to NBS for

examination and laboratory testing of the material, in cooperation

with other interested parties.

Atmospheric Composition Studies.—NBS scientists are cooperating

with the Environmental Science Services Administration in their

studies of the possible variations in atmospheric oxygen content over

the oceans. NBS developed a reliable method for detecting the expected

small oxygen compositional differences and instructed ESSA per- sonnel in sampling methods. Samples collected during world-wide

cruises of the ESSA research ships will be analyzed in the NBS

laboratories.

Life of Postage Stamp Printing Plates Increased.—Recommendations for changes in the fabrication and heat treating procedures of

postage stamp printing plates have been made to the Bureau of

Engraving and Printing. Early and still preliminary reports indicate

that these procedures will increase the service life of the plates.

Analysis of Lung Tissue from Astronauts in Fatal Spacecraft

Fire.—IMR determined the trace contaminants in lung tissue taken

from astronauts killed in the fatal spacecraft fire, 119
On December 15, 1967, this structural member on the bridge at Point Pleasant,

W. Va., failed, sending 46 people to their death and injuring many others. The member, called an eye bar, was sent to NBS for analysis to determine

the type and cause of failure. Study has shown that initial brittle fracture occurred at 1 ; ductile fracture then occurred at 2 and 3. The peeling of the paint shows extensive deformation at 2 and 3 with a zone of almost no stress (where the paint remains) running in between. Results of this study should

provide important information on the cause of the tragedy and give indications of methods needed to insure the safety of similar bridges.

Naming of Synthetic Fibers.—IME advised the Federal Trade Commission on naming of manmade fibers according to the Textile Labeling Act. This keeps the consumer from being overwhelmed by a confusing array of names. Conferences and Symposia

Second Annual 1MBSymposium.—"Molecular Dynamics and Struc- ture of Solids," the second annual symposium of the Institute for Materials Research, was held October 16-19, 1967 in the NBS laboratories

at Gaithersburg, Md., and was attended by 250 university, Government, and industrial scientists from both the United States and

abroad. The goal of the symposium was the encouragement of interdisciplinary materials measurement science and technology. Topics

and speakers were selected so as to demonstrate the correlation of

various techniques for the study of molecular dynamics and structure of molecular solids. The Proceedings are being published.

Symposium on Mass Transport in Oxides.—IME and the Advanced

Research Projects Agency of the Department of Defense joined in

sponsoring this symposium to assess the concepts, theories, and experimental techniques currently applied in studies of mass transport in

120
oxides. Thirty papers were presented covering preparation of research

specimens, characterization and energetics of defects, lattice dynamics,

diffusion, and ionic conductivity. Panel discussions explored the need

for fundamental understanding in solving technological problems in mass transport, the improvement of accuracy in diffusion measurements, and the usefulness and selection of standard reference materials. The published Proceedings of the Symposium are available.

Symposium on Mechanical and Thermal Properties of Ceramics.—

Jointly sponsored by the American Ceramic Society, the American

Society for Testing and Materials, and IMR, this symposium emphasized the dependence of ceramic properties upon microstructure and

composition, and the importance of controlling these features of character to insure reliability in ceramics. Intended to provide a basis for

understanding property-character relationships as well as criteria for

the proper selection and use of ceramic materials, papers and discussion centered on properties of importance in structural and hightemperature applications—melting points, thermal expansion, thermal

conductivity, thermal radiation, elasticity, viscoelasticity, inelastic

deformation, and fracture. The published Proceedings of the Symposium are expected to be available in January 1969.

Material Failures Conference—"Must They Fail".—This conference

held at NBS reviewed the growing problem of service failures of

materials in view of the more stringent demands of today's space age

technology. It was jointly sponsored by IMR and the Washington

(D.C.) chapters of the American Society for Metals and the American

Society of Mechanical Engineers. Six technical speakers reviewed the

state of knowledge in the field ; Ralph Nader, well-known safety critic, was luncheon speaker.

Quantitative Electron Prole Microanalysis.—This seminar was held

June 12 and 13, 1967, to critically examine an important area of meas- urement in materials science. Twenty-five participants from the United

States and five foreign countries were brought together for an exchange

of ideas in the refinement of quantitative measurement in this area of

microanalysis.

Mass Spectrometry Workshop.—A workshop on Spark Source Mass

Spectrometry was held November 13 and 14, 1967, to examine the

factors that influence the precision and accuracy attainable in analytical determinations by the spark source technique. Seventy participants

from Government laboratories, universities, research institutes, and

industrial laboratories participated in the discussion which centered on calibration, quantitation, and standard reference materials suitable

for spark source work.

121

INSTITUTE FOR APPLIED TECHNOLOGY

The Institute for Applied Technology (IAT) addresses the Nation's

need for measurements and standards which relate to the artifacts of our society. Thus, the IAT programs are concerned with technological or "engineering" measurement and standards which deal with products, commodities, devices, processes or systems. Such measurements

and standards are the language of the market place for coupling user requirements with the performance capabilities of products, processes or services, and they bring order and quantification to man's use of

his technical skills. The Institute programs are oriented to industry, to the States and

regions of the country, and to all levels of Government. They bridge

the interface between science and its application to society's needs,

and by coupling science and technology with the daily activities of

commerce, industry, and Government, they stimulate economic progress. IAT activities fall into two major categories—Technical Measurements and Standards, and Technical Innovation and Diffusion.

A substantial portion of the work done in the entire Institute program is under the classification of technical assistance to other parts

of the Bureau, other Government agencies, and to industry. The work

in motor vehicle safety research and technical analysis is virtually

all done for others. In other fields, a lesser but still substantial volume

of IAT work is done at the request of others.

TECHNOLOGICAL MEASUREMENTS AND STANDARDS

This category covers the Institute effort for the broader extension of

the national measurement system into the engineering and technological fields. It is a program to apply principles of good measurement,

rather well defined in the science area, to the determination of per- formance or other significant characteristics of products, systems and

devices important either in commerce or to Government needs. In

essence, the objective is to find ways by which standards can be developed for items, systems, and devices which are not readily eval- uated in terms of existing measurement methods.

The performance concept introduces man into the measurements

and standards process, and the whole idea centers on the belief that

products, processes, services, and systems can be described and their

performance can be measured in terms of user's requirements without

regard to their physical characteristics, design, or method of their

320-738 O—68 9 123
creation. Key to this method is the identification of measureable per- formance criteria for meeting the user's requirements, thereby cou- pling subjectively derived needs with objective technical measurement

methods.

As the complexity and technical sophistication of articles of com- merce increase, it becomes increasingly difficult to define those characteristics of a product which best measure its performance. The virtue

of the performance concept in measurement and standards development is that it stresses the end to be attained, and leaves the means to obtain the desired end wide open.

Today many complex products are actually complete "systems",

and the only feasible way to evaluate them is in terms of their per- formance against criteria established to meet the user's requirements.

The concept encourages innovation when producers can meet the per- formance required by whatever design of product will do the job.

The idea of performance criteria also has ramifications beyond

those concerned with articles of commerce. Our national welfare depends critically on making informed decisions related to complex

social and economic policies and programs. To do this, one needs to define criteria of performance for these policies and programs and be

able to measure or predict possible benefits and costs of alternative

actions. Through the techniques of systems analysis and operations

research, technology has provided a means for helping such decisionmaking.

Institute activities in technological measurements and standards

range from the development of performance criteria and test methodology for individual items to the study and analysis of complex

systems such as a multi-State transportation network.

Program elements include seven areas

:

1. Building Technology

2. Automatic Data Processing

3. Electronic Technology

4. Systems Analysis

5. Motor Vehicle Safety

6. Engineering Materials

7. Industrial and Consumer Products

Building Technology

Buildings represent a large portion of the existing tangible wealth

of this country. Annual building production continues in the range of

$100 billion, with an effect on every village, town, or city. And we are

still faced with the need to produce in the next 30 years or so as many buildings as we now have, with an industry which has never

really entered the mass-production stage and is still heavily dependent on hand craftsmen techniques. Spiraling construction costs have ac- 124
celerated the move to the industrialization of the building process, although these costs are only part of the total, which is heavily in- fluenced by the cost of land and by tax, financial, and other social

burdens. Nonetheless, the changes taking place are already generating

pressure for advanced techniques for better measurements and updated standards. There is a greater need for standardization of test procedures and innovation needs to be encouraged by implementing

the use of the performance concept for evaluating complex components. During the past year the IAT Building Technology program

has accelerated efforts in this direction.

Activity has centered on improving the normal building code,

standard and specification process by continued development of the

technological base and measurement procedures needed for the process to function. Work on new methodologies has been initiated to bring

about changes in the process whereby innovation in building systems

and components will be encouraged. As an example, a study was

initiated to determine how a broader use of performance based standards might open the way for the introduction of cost-reducing innovations into the design of low-cost housing. The project involved a comprehensive definition of the performance concept and the various

steps that must be taken from the determination of user requirements to the issuance of performance standards.

The building technology program continued the traditional lab- oratory and field support provided to Federal agencies, State, and

local Government groups concerned with building construction and

technology. Technical consultation and advice was made available to industry, and the staff continued to work closely with the many

private standards-making groups throughout the country.

Structural Performance of Multifamity Building System.—Load

tests on a one-story portion of a new low-cost building system were

arranged in a manner that simulated the structural response expected

of a three-story unit. The laboratory tests showed that the prefabricated system did in fact produce a structure which complied with the

intent of a local building code. The test section was subjected to simulated dead, live, and wind load trials. Individual components were

also tested to obtain data on their behavior. Results obtained provided

the performance criteria for evaluating the structural safety of this and similarly innovative building systems.

High Temperature Thermal Conductance of Soils.—It is antici- pated that space nuclear power systems, on re-entry impact burial in

the earth, may have a maximum steady-state temperature as high as 1700 °C. A little information is available on the thermal conductivity

of soils at temperatures of 100 °C, but essentially nothing is known

125
about what happens above 500 °C. In order to provide the high temperature data needed in the safety evaluation of such power systems,

tests were developed for thermal conductivity measurements on soils and other granular materials at hot-side temperatures near 1700 °C.

Using apparatus specifically designed for the purpose, thermal con- ductivity values have been established for a number of natural or

artificial samples representative of subsoils found on most of the

earth.

Continuous HCl Analysis for Smokes.—Polyvinyl chloride is a com- mon plastic used as a construction material. When it burns, hydrogen

chloride is present in the smoke and a continuous, recording, analytical

method was required for the monitoring of smoke tests. It was found

that scrubbing the HCl from the smoke in a microscrubber, and analysing it by means of a specific ion electrode, is a satisfactory method for

determining the HCl present to a sensitivity of 20 ppm of HCl.

Reducing Flood Damage in Alaska.—Four thousand residential structures suffered approximately $29 million damage in a disastrous

flood in Fairbanks, Alaska, in August 1967. The NBS Building Kesearch Division was asked by the United States Senate Public Works

Committee to assist the stricken residents. An KBS team consisting of

a mechanical engineer and a materials technologist was sent to Fairbanks in the company of Senator Ernest Gruening and staff members

of the Public Works Committee. Recommendations were made to facili- tate drying of homes for early rehabilitation with a minimum removal

of water soaked materials. Based on an asessment in May 1968, the

services provided by the National Bureau of Standards resulted in an

estimated reduction of flood losses in the amount of $5 million.

Effects of Air Pollution on Building Materials.—The presence of

sulfur dioxide and ozone contaminants in urban atmospheres affects both people and materials. As part of the task of estimating economic

losses caused by these contaminants, their effect on the chemical and

physical properties of paints, plastics, and asphalts is being evaluated.

Through laboratory tests, samples have been subjected to a simulated

natural exposure of light and humidity along with controlled amounts

of sulfur dioxide and ozone. Measurements were then made of the

changes in color, tensile strength, brittleness, and chemical structure induced by the tests. Short term tests show that vinyl plastics absorb

sulfur dioxide and show a loss of strength. The adsorption is dependent on humidity and light. As they develop, the studies should increase our knowledge of the interrelationship of the effects of weather variables

and air contaminants.

126
Scenes such as these were common after the August 1967 flood which caused

$29 million damage in Alaska. Significant reductions in losses due to flood damage were realized through services provided by an NBS team of building

systems experts.

Computer Simulation of Building Fires.—The complex interactions

of a building and a fire are being studied with the aid of computer

simulated models. A major problem has been the development of a building description of manageable size and form suitable for use on

the computer. Another problem has been how to determine air move- ments induced by fires. Hot gases produced by fire tend to rise and mix

with other gases in a room or building and knowledge of this motion

is important for the early detection of fires. To provide preliminary

information on this phenomenon, Kesearch Associates of the Factory

Mutual Engineering Corporation (working at NBS with Bureau staff) ran a parallel experimental-theoretical in-motion study in a closed

model room in which a hot spot on the floor was used to simulate a fire. The theoretical prediction was obtained by a computer calculation. By

highlighting the information required for a successful calculation,

guides to future research were obtained.

Performance Criteria for Exterior Walls.—A comprehensive study was made of the performance characteristics of exterior walls for one- and two-family houses. Using newly developed apparatus and new test procedures, combined compressive and racking tests, and transverse strength tests were developed to determine the criteria for measuring

the strength properties and associated elastic or permanent deforma127
tions of such walls. Criteria were suggested for evaluating surface

flammability of the interior components of the walls. In the area of the

environmental requirements, new criteria were developed which

covered maximum limits for air penetration of the walls and for the

temperature difference between the room air and wall surface. Many

other characteristics were included in this total evaluation study : the

effects of weathering on color change, chalking, erosion, peeling and

cracking of surfaces, washability, etc., as well as criteria related to

resistance to impact and abrasion. The investigation revealed the

paucity of information available for determining the performance

requirements of exterior walls. Conference of States on Building Codes and Standards.—Staff support was given to a number of States in organizing a National Conference of States on Building Codes and Standards. Modeled after the

National Conference on Weights and Measures, the new group of state representatives used NBS facilities for a first meeting in May 1968.

Organization of working committees is underway for study of code

requirements, standards, enforcement, etc., with the objective of

obtaining more uniform standards among the States. A majority of the

States do not have research facilities, and thus the NBS building

technology program findings will serve in support of the States in the

National Conference.

Automatic Data Processing

The NBS Center for Computer Sciences and Technology completed its second full year of operation in fiscal year 1968. Established

by a Commerce Department Order in September 1965, it carries out

the responsibilities of the Secretary of Commerce under Public Law

89-306 (the Brooks Bill) for broad ADP standards development, consultation, and assistance to Federal agencies and supporting research

in matters relating to the use of computers in the Federal Government.

This mission necessitates close interaction with ADP managers in the

General Services Administration and the Bureau of the Budget, who

share responsibility under the Law for improving the use of computers

in Government.

The Center program covers four areas : ADP standards (both Federal and in cooperative efforts with industry in the voluntary commercial area), consultative and advisory services, research, and

computer services. ADP Standards

Federal Information Processing Standards.—On March 11, 1968,

President Johnson approved the first Federal standards for ADP. The

128
standards are the USA Standard Code for Information Interchange,

and implementation of the code on perforated tape and magnetic tape.

This action opened the way for important applications which require

computers to talk to each other, to send each other messages, and to consult each other's files. Additional Federal standard recommendations in process include type fonts for optical character recognition,

forms layout, COBOL programming language, and data elements and

their coded representation.

Voluntary Commercial Information Processing Standards.—The

first international standard in the information processing field was

approved by member nations of the International Standards Organization—ISO Recommendation 646—which covered Six and Seven

Bit Coded Character Sets for Information Interchange. The Center

continued to work with the USA Standards Institute on a wide range

of information processing standards aimed at improving compatibility

between and within data processing installations. Projects include

standards for magnetic tapes, disc packs, punched cards, data trans- mission, tape labels and formats, programming languages, operating

systems, remote control user procedures, data elements and codes, computer terminology, program documentation, flowchart symbols, optical

character recognition, keyboards, and interfaces.

Measuring Compliance With Information Processing Standards.—

Routines are being prepared to analyze and test FORTRAN and

COBOL compilers. In the hardware area, measurement procedures

and test equipment were developed for laboratory certification of unrecorded standard reference digital computer tape samples. Under a

cooperative arrangement with the General Services Administration,

a magnetic media testing and evaluation facility is being established

for long term operation at the KBS Gaithersburg site. Dissemination of Information on Standards Activities.—Through

distribution of three issues of an Information Processing Standards

Tech Memo, ADP circles were kept aware of the status of voluntary

and Federal standards work going on at the Center.

Consultative and Advisory Services

These services have been extended to more than 30 Federal agencies with computer related problems. The subjects range from re- viewing proposed specifications for computer systems; conducting

systems studies; evaluating, designing and developing software and

hardware; to monitoring installation and systems performance on

a continuing basis. 129
In addition to assistance on specific problems, the Center provides

general help through

:

a. Development of techniques to be used as guidelines for those

conducting feasibility studies, computer selections, or computer performance evaluations. These guides result from the

experience gained in the performance of consulting services to other agencies.

b. Operation of a Technical Information Exchange which provides Government agencies access to collections of formal lit- erature in the ADP field, publications of manufacturers and

suppliers, and resumes of Government sponsored projects.

c. Automated information storage and retrieval systems developed for three of the collections, (1) the formal literature, i.e., books, proceedings, reports, serials, and periodicals, (2) res- umes of government sponsored projects, and (3) publications

that are available from the manufacturers and suppliers of

ADP systems and services. Also, search tools in the form of

a computer-produced bibliographic citations list and KWIC

(Key Word in Context), personal and corporate author, subject category, and report number indexes are prepared monthly.

Research

For many years the Bureau has conducted research in computer

science fields of particular utility in Government operations. The Center has continued this basic work, and has undertaken a variety of

major projects this past year. Selective Information Extractor.—A software system was developed

to provide a simple language enabling nonprogrammers to query large

files and to produce formatted output. From simple file descriptions

and an ordinary English request, this system generates a complete

COBOL program to process the user's files and to produce the desired

reports. The system was written in COBOL to achieve machine

independence.

Low-level Programming Language.—A programming language re- sembling an assembly language in format is being developed for problems which presently can only be adequately approached in true as- sembly languages. This language provides a small but complete basic

instruction set, including some commands not usually found in assembly languages. Flexibility is gained by using parameters to modify

basic instruction types, and by permitting a very general form of

operand addressing. This approach is intended to avoid the almost

prohibitive intricacy and cost of assembly language programming for

third generation digital computers with their multiplicity of registers,

130
word formats, and instruction types. The language makes no reference

to hardware registers, and it is in many respects machine-independent.

Career Referral System.—Research was undertaken aimed at es- tablishing an automated Government-wide system able to identify all eligible employees with the requisite qualifications for a vacancy anywhere in the Federal Government.

"Magic"—A Display System—-This display system is used in con- junction with an experimental computer for applications such as computer aided design of structures, electronic circuit organization and

file information retrieval.

Console of "Magic II" with drawing of a circuit element on the cathode-ray

tube. Time-Share System.—A time shared user project was carried out with the Center's experimental computer MOBIDIC. The project

dealt with real time remote computer control of temperature and elec- trical current as related to the Hall effect. Automated Fingerprint Classification.—A procedure has been

developed, under the sponsorship of the Federal Bureau of Investigation, for determining by computer whether two fingerprint impressions were made by the same finger. The procedure uses the X and Y

coordinates and the individual directions of the minutiae (ridge

endings and bifurcations) . The identity of two impressions is established by matching the impressions in terms of the relative distances

131
and relative angles of the minutiae. This matching procedure promises

to be useful in an automated system in which a file of minutiae data

corresponding to thousands of fingerprints of known individuals is searched. Thus the identity of an unknown person may be established

using only one of his fingerprints.

Computer Services

The Computer Services Division of the Center provides computer

time and programming within NBS and for many other Government

agencies. The present multi-access computer, a TJNTVAC 1108, is operated in a batch-processing mode using a priority arrangement

under which users can obtain either special service or deferred turn- around service. At the end of FY 1968, two high-volume and five medium-volume remote terminals were fully operational. Output of

publication quality is provided to both microfilm and hard copy of

either printed or graphical material. A small-scale programmable

computer provides a full range of conversion services between magnetic tape and punched paper tape.

Data processing services were provided to over 60 organizations

including 9 executive departments and 18 agencies of the Government, the Congress, state and local governments, quasi-government

organizations and universities. Programming and consultative services are also provided in support of NBS technical activities. This

effort is largely in assisting KBS scientists with problem formulation

and in writing FORTRAN" programs.

Electronic Technology

The electronics industry is among the fastest growing and most

heavily research-oriented in this country. In the context of R&D funds

spent within the industry, NBS activities are relatively small. Yet the

Bureau contribution has a broad pervasive influence in the field. Emphasis is placed on the characterization of basic building blocks, that is, acquiring the "nuts and bolts" knowledge needed for advances in the

technology. An example of this kind of activity is the effort given to studies of the yield, performance, and reliability of discrete and inte- grated semiconductor devices. The NBS Electronics Instrumentation

group, working with materials such as germanium and silicon, develops measurement techniques and test procedures for information on resistivity and lifetime, detection and identification of flaws, control of material properties in processing, and correlation of the properties of devices with materials characteristics. In the past year there

has also been an expansion in participation with national and inter- national standards groups.

Characterization of Germanium for Nuclear Radiation Detectors.—

Semiconductor nuclear radiation detectors have been extensively used

132
for about eight years. Uncontrolled variations in the quality of ger- manium intended for this application have occurred during this period

for reasons which are not well understood. Crystals are presently

selected on the basis of room temperature resistivity, photoconductive

decay lifetime, and etch pit density, but use of these parameters does

not always permit discrimination between material suitable for detec- tor fabrication and material which is not. A comprehensive program is underway with the objective of developing methods for the early identification of material suitable for fabrication into lithium-compensated detectors. The program involves

material evaluation, device fabrication, and device evaluation utilizing

both "good" and "bad" material. Material properties being determined

include routinely measured properties such as room temperature

resistivity, photoconductive decay lifetime, etch pit density, and other

less commonly measured properties such as Hall mobility and drift

mobility at low temperatures, infrared absorption in the 11 /mi region,

lithium precipitation and drift rates, x-ray topography, and composition by means of neutron activation or mass spectrograph^ techniques.

Fabrication of gamma-ray detectors from the material and testing

of the detectors is also part of the measurement program. Presently

38 germanium crystals contributed by various domestic suppliers and

national laboratories are being studied.

Because of the large number of specimens, an automatic computercontrolled system for making low temperature Hall effect measure- ments was built in cooperation with the NBS Computer Center. This

system enables a run to be made between 20 and 300 K in about 4 hr. Apart from the study, the automatic system is used to make measure- ments on specimens sent from a national laboratory specifically for

Hall measurements.

Standard Method for Measuring the Resistivity of Silicon Wafers.—

The technical basis for a standard method of measuring the resistivity

of silicon wafers was developed in cooperation with Committee F-l

of the American Society for Testing and Materials. The method is an improved version of the four-probe technique most widely used in the

industry. The improvements, based on work which has been underway

since 1960, permit comparative measurements to be made with a standard deviation of less than 1 percent over much of the resistivity range

of commercial interest. Some of the features of the new method can be applied to calibration procedures for use on production equipment and hence will also enable improved control at various stages in the processing of wafers.

Increased emphasis on requirements for control of the processing has

led to extension of the work to include measurements on epitaxial or

diffused layers with a variety of surface conditions,

138
Systems Analysis

In any program for promoting the application of technology to complex problems of industry or Government, the use of systems

analysis or operations research is almost a mandatory requirement.

The NBS Technical Analysis Division seeks to develop, test, and dis- seminate systems analysis techniques which are applicable to public

sector problems in terms of program planning, resource allocation, and

program execution.

The IAT systems analysis group is the largest such organization

within the civilian agencies of the Government. It serves other agencies

in the solution of their specific systems analysis problems, and helps

these agencies to develop their own capacity to tackle complex systems

problems. It also conducts research on cost-benefit analyses for Government programs.

Application of Systems Analysis to Highway Maintenance.— Considering highway maintenance as a system composed of three levels

:

(1) national, (2) state, and (3) operational, a study was conducted on the feasibility of applying systems analysis or operations research

methods to the solution of problems at those levels. It was determined

that in general the operational level, where measures and interactions are better defined, was more amenable to the application of analytic

techniques. A computerized simulation model of a typical highway

maintenance operational unit was developed to provide highway

maintenance management with a quantitative means of evaluating

the effect of different job-scheduling and resource-allocation policies on the productivity of the unit.

Systems Analysis and Problems of the City.—The Department of

Housing and Urban Development asked the NBS technical analysis

group to serve as "technical coach" on a project to determine whether

quick and inexpensive application of systems analysis to selected city

problems is feasible. The project is under the direction of the International City Managers' Association. Three cities are involved in the

test. In East Lansing, Michigan, the project involves calculating optimal fire station locations. At Poughkeepsie, New York, comparison

of possible city actions related to building code compliance was initi- ated. Model neighborhoods were studied, using cost to owner, cost to occupant, and cost to city measures of value. In Charlotte, North

Carolina, through in-depth interview techniques, user perceptions of

value and distance to public service facilities were studied.

Ship Operation Simulation.—An event-oriented simulation repre- senting the operation of a commercial shipping fleet was developed at the request of the Maritime Administration. The event occurrence is 134
the entry of a ship into port for cargo to be discharged and loaded.

The simulation can consider several networks to provide for the trans- shipment of cargo between adjoining networks. The simulation has

proved useful in evaluating alternative shipping routines, schedules,

and ship design configuration.

Progress in Transportation Simulation Studies.—Significant re- finements in computer simulation models were made in the continuing

studies of the Northeast Corridor Transportation Project of the Department of Transportation. Flexible preprocessors and post processors have been developed which aid in the application of the computer

models to transportation planning analysis. Modification of new methods for evaluating interurban transportation studies has advanced to the point where run-teams have been organized to assemble all the

models developed for the entire Northeast Corridor system, and to

exercise the complex of models in solving transportation planning

problems.

Safeguarding Fissionable Nuclear Materials.—The advent of pri- vate ownership of fissionable nuclear material beginning in 1970

creates a need for methods to prevent possible diversion of these materials to other than peaceful uses. One problem is to determine the

level of material losses which is acceptable in nuclear fuel process sys- tems, such knowledge being necessary in accounting for total disposition of the fissionable materials. NBS systems analysts are studying

all nuclear fuel process systems to develop a process model which

will trace the flow of nuclear material through all stages of each

process, and which will include a capability for assigning acceptable

loss rates at each stage of the process. Demand Forecasting Models.—The IBS Operations Research Section collaborated with the IAT Technical Analysis Division in logical

analysis of and numerical experimentation with variants of several

travel-demand forecasting models prepared by contractors for the

Department of Transportation. The result was improved model versions in a number of cases, as well as significant computational simplifications. Such work has great value in providing a better basis for

planning the extensive transportation networks of the future.

Motor Vehicle Safety

During FY 1968 the Bureau continued to provide technical assist- ance to the National Highway Safety Bureau (NHSB) of the Department of Transportation in its development of motor vehicle safety

performance standards. Research is being performed in the areas of

tire systems, occupant restraint systems and braking systems.

135
Tire Systems

A significant breakthrough was made in the development of instrumentation to measure the temperature of a running tire on a vehicle.

Thermistors or thermocouples embedded in the tire carcass are con- nected to a miniaturized solid-state transmitter mounted on the wheel

rim. To assist the consumer in making an informed choice in the purchase of tires, methods are being developed to measure the speed capabilities, traction, mileage, impact resistance, and endurance properties

of tires. Extensive road and laboratory testing of a large sample of

passenger car tires will serve as a technical data base for this uniform

quality grading system.

Temperatures created in tires during use are measured by a thermistor inserted

in the tire shoulder. Antenna being mounted on car is part of a radio telemetry system used in the heat measurement.

Occupant Restraint Systems

The important research program involving human subjects con- tinued at Holloman Air Force Base. The performance of 1968 model

year production seats and restraint systems under collision conditions

using anthropomorphic dummies was evaluated on the Daisy Decelerator at this facility. An important observation made during the research

conducted on human subjects was the amount of restraint contributed

by the legs during a 15 g deceleration accounting for as much as 55

136
percent of the subject's kinetic energy. An improved laboratory test was developed to measure more realistically the abrasion of seat belt

webbing occurring during use. Braking Systems

A laboratory for the evaluation of complete braking systems and

their components is nearing completion. In operation are two types

of brake lining testing machines, a Friction Materials Test Machine

(Chase-Link type) and a Friction Assessment Screening Test Machine (FAST) . A special purpose double-ended dynamometer is ready

for installation and check out. It is capable of testing complete braking

systems of motor vehicles up to light size trucks, including the new

skid limiting devices. A popular American make sedan with front

wheel disc brakes has been instrumented and is being used for correlation of vehicle road performance and laboratory testing. Laboratory

test procedures for evaluating hydraulic brake fluids are being criti- cally examined with respect to actual service performance require- ments. Safety requirements were developed for standards relating to the packaging and labeling of brake fluids. Engineering Materials

IAT provides advisory, consultative, and laboratory investigation services relating to selected engineering materials. The laboratory

work is mainly for the development of test procedures which can be

used by other testing laboratories. The staff responsible for this program works with national and international groups to establish standards for these materials. Services also include establishing a technical

base for other Government agencies to set purchase specifications.

Magnetic Tapes for Satellite Recorders.—One of the most important

causes of NASA satellite malfunctions is the early failure of flight

tape recorders. NBS has undertaken studies of the changes of physical

and chemical characteristics of tapes during use and also of the interaction of tapes and recording head surfaces. Advances have been made

in two areas. Previously unused techniques have been applied to measure such properties as stiffness, surface hardness, and surface energy

of tapes. The detection of very small amounts of foreign material on

head surfaces by contact angle measurements, fluorescence, and in- frared absorption spectroscopy were included in the study. Also, an

informal liaison with satellite tape recorder manufacturers, magnetic

tape manufacturers, and a number of NASA engineers concerned with

satellite tape recorder problems has been established and NBS is gradually becoming a clearinghouse for information related to satellite magnetic tape and materials problems,

137
Evaluating the Stability of Record Papers.—The stability of paper

is greatly dependent on the chemical modifications of the cellulose that occur during the manufacturing process, and on the interaction of

cellulose with additives such as papermaker's alum (aluminum sul- fate) . Sensitive methods for the estimation of aluminum and of sul- fate have been adapted to paper pulp-aluminum sulfate systems in or- der to ascertain the distribution of aluminum and of sulfate, and the

effect of this distribution on stability. As file copies of most letters and manuscripts are made on manifold (carbon copy) paper, a special

study was made of the stability, as measured by laboratory aging, of a

representative group of these papers. Although acidity, as measured

by a standard pH method, is an important factor in predicting stability, the study shows that a pH value alone can be very misleading, and

that some laboratory aging procedure must be used in conjunction with

acidity measurements.

Stability of Record Paper.—Differential Thermal Analysis (DTA)

,

a technique for studying the thermal behavior of materials as they

undergo physical and chemical changes during heating, has been found

useful in ranking record papers in order of their relative stabilities. Most papers and related carbohydrate materials exhibit a typical decomposition pattern, and the temperature at which one of the peaks

occurs appears to be related to stability, as measured by laboratory

aging. This can be correlated with the acid content of the paper. A

study of the effect of chemical modification of cellulose on the DTA

pattern is in progress. In another series of tests, crosslinking of cellulose, as measured by the development of wet strength, has been found

to occur during laboratory aging, and there is some evidence that cross- linking occurs during natural aging. This could have an important

bearing on the evaluation of changes in the physical properties of

paper during aging. Data could be interpreted as indicating degradation when, in fact, they might represent a change in the chemical

structure that would not be related to stability.

Measuring the Durability of Paper.—The durability of paper is an

elusive property that is difficult to measure in the laboratory. Some

progress has been made, however, in the evaluation of durability

through the development of a flexing device that uniformly destroys

the physical structure of the paper. The rate of destruction, as meas- ured by changes in rheological properties due to flexing, may be taken

as a measure of relative durability. For specific end uses, durability can be greatly improved by incorporation of specially selected additives in the paper.

138
Precision of Standard Paper Test Methods.—As part of a study of

the precision of standard methods used in the paper industry, an

evaluation was made of the precision of the bursting strength method

from data published over the past 40 years. It was found that no

significant change in within-laboratory precision had occurred during

this period. It was concluded that one or more standard reference materials would be needed to effect a substantial increase in precision.

Human subject slams into the water brake of the Daisy Decelerator in a simulated 15 g automotive collision. He is restrained by automotive lap belt and shoulder harness on the NBS experimental seat. Data recorded includes

seat belt load, sled velocity and deceleration and human kinematic motion.

Flammable Fabrics Research.—The amended Flammable Fabrics

Act broadened the coverage of items to include fabrics used in interior

furnishings as well as those used in wearing apparel. Data acquired

by NBS under the terms of the original Act, and information on

individual cases gathered by the HEW Public Health Service are under review to determine whether new or revised standards and

regulations are needed to protect the public. Tests on fabrics other

than those used for clothing have been initiated as part of the program to see that the standards not only cover furnishings, but are also kept current in terms of items on the market.

Engineering Standards

Product Standards.—During 1967 the Institute broadened its efforts to provide improved technical services to the public and to State and

Federal Government agencies in product standardization. It operated

a Testing Laboratory for the General Services Administration's Federal Supply Agency which conducted work leading to more meaning139

320-738 O—68 10
ful specifications for commodities purchased by the Government.

Product standards were revised by the Office of Engineering Standards Services to meet current needs of the consumer and industry.

Amendments to the procedures for developing voluntary product

standards were formally announced in May 1968. These provided for

the more effective development of standards, particularly those relat- ing to the quantities in which consumer products are sold at retail, and

restated the numerical percentages definition of a consensus determination. During FY 1968, five proposed standards were circulated for

comment, and 24 others were transmitted for committee approval of

which 14 were later recommended for final acceptance. The review of

older standards continued and 155 were examined to determine

whether they should be withdrawn, revised, or revalidated. The col- lection of published standards has been expanded and now includes

between 15,000 and 20,000 individual items which are being listed for

publication in a reference index. These standards represent the output

of more than 350 standards-making organizations or other groups.

Fair Packaging and Labeling.—During FY 1968 staff members

were intensively engaged in carrying out NBS responsibility under

the Fair Packaging and Labeling Act. With the cooperation and

assistance of State and local weights and measures officials, other Federal agencies, and industry trade associations and committees, the

Office of Weights and Measures investigated some 135 different types

of packaged consumer commodities for evidence of undue proliferation. One hundred major industries are in various stages of a process

to reduce and simplify the quantities in which consumer commodities

are packaged. The packaged goods produced by these industries

account for more than 60 percent of annual consumer expenditures for

products covered by the Fair Packaging and Labeling Act and firm

commitments have been received from about one third of them.

An important aspect of the fair packaging and labeling activity is to make sure that the customer can easily find and read the statement

of net quantity on the package. Legibility depends among other things on the contrast between the color of the print and that of the background. A method of stating the color-contrast requirement, suitable

for inclusion in packaging regulations, and capable of being used as a guide by graphic artists engaged in labeling design, has been pre- pared by IBS mathematicians for the NBS Office of Engineering

Standards Services.

New State Standards.—This fiscal year NBS presented new State

standards to nine States—Delaware, Connecticut, Ohio, Illinois, Tennessee, New Mexico, Utah, California, and Oregon. (The tenth State,

Kentucky, was scheduled to receive standards officially on July 19,

1968.) Provision is being made for ten additional States to receive

140
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Typical results of voluntary steps by industry to reduce the number of product

package sizes since enactment of the Fair Packaging and Labeling Act on

July 1, 1967. Industry has taken steps to cut the number of package sizes of 14 basic items. Eleven of these have made specific reductions of 289 sizes to 104. Sixty-five other industries have informed the U.S. Department of Commerce they are working on plans to consolidate package sizes. standards—Maine, Pennsylvania, West Virginia, North Carolina,

Georgia, Florida, Wisconsin, Missouri, Arkansas, and Hawaii—and

manufacture of the third set of precise physical standards and in- struments is underway. Recipients of the latest set will include:

Vermont, New Jersey, Alabama, Indiana, North Dakota, Oklahoma,

Texas, Wyoming, Idaho, and Maryland.

Basic laboratory training (two weeks) has been completed for 15

State laboratory technologists at various State laboratories and at the NBS Weights and Measures Laboratory. The first Regional Laboratory Training Seminar (intermediate training) at Madison, Wisconsin, attended by technologists from Ohio, Illinois, and Wisconsin, was also conducted by the Office of Weights and Measures.

Technical Training.—During the past fiscal year, 25 training courses were conducted throughout the country for State and local weights

and measures officials. A one-week seminar was held at NBS for offi- cials having supervisory responsibilities, and over 40 officials repre- senting 33 jurisdictions attended. Other forms of training conducted

by NBS officials included : ( 1

) assistance to the States in field testing

operations, (2) special purpose training for foreign visitors, Federal

agencies, and private industry, and (3) training of State laboratory

personnel (at both the State lab and NBS)

.

141
National Conference on Weights and Measures.—The 53rd National Conference on Weights and Measures held in Washington during June, accomplished a task of considerable magnitude in adopting

a Model State Packaging and Labeling Regulation. The development

of such a Model Regulation was complicated by the existence of in- dividual regulations covering packaged consumer commodities issued

by the Food and Drug Administration and the Federal Trade Commission, both pursuant to the Fair Packaging and Labeling Act. The

States, with their obligation to provide labeling standards for all packages, found it necessary to create a document that included the

stipulations of the two Federal regulations and, in addition, wholesale and institutional packages. Under the terms of the Fair Packaging and Labeling Act, requirements of the States with respect to consumer package quantity labeling cannot be less stringent than or

inconsistent with the Federal requirements.

The Conference heard Lawrence C. McQuade, Assistant Secretary

of Commerce for Domestic and International Business, report on vital

economic developments within the Nation, and Dr. A. V. Astin, Director, National Bureau of Standards, discuss activities of the Bureau

during the past year. Present were delegates from 40 States and the

District of Columbia and, in addition, many businesses, industries,

and consumer groups interested in weights and measures supervision.

TECHNOLOGICAL INNOVATION AND DIFFUSION

Technological innovation may be denned as that process whereby means are devised and applied for stimulating new technologies,

channeling them in promising useful directions, and exploiting their use for purposes other than those for which they were originally developed. Technological diffusion, in the context of the IAT programs,

is largely restricted to disseminating the results of Government

sponsored R&D.

Invention and Innovation

The Office of Invention and Innovation is the IAT activity which

helps to develop an environment conducive to technological change. Its basic program has three aspects : providing a national basis for formulation of climate-setting Federal policies, offering assistance to in- ventors, and education.

In FY 1968, the Office assumed responsibility (as assigned by

the Assistant Secretary of Commerce for Science and Technology) for

the program, planning and budgeting activity of the Department of

Commerce Technology Program. Department programs included in

this responsibility are the Patent Office, Office of State Technical

Services, the KBS Clearinghouse for Federal Scientific and Technical

Information and the Office itself. m
Invention Policy.—The Office of Invention and Innovation con- tinued to assist other organizations (such as the Organization of

American States, the Arms Control and Disarmament Agency, Committees of the U.S. Senate) to further the work of the Commerce Secretary's Panel on Invention and Innovation. Seminars for universities

and professional organizations have been held throughout the country. A new Secretarial panel on the problems associated with the

allocation of venture capital has been established. The National In- ventors Council has embarked on a comprehensive assessment of the

inventor and his relationship to society.

Invention Programs.—The number of states holding invention ex- positions and inventors' seminars increased to 24 during fiscal 1968 and

several other states are planning to join this effort during the coming

year. The programs are organized and conducted by state organizations

and universities and are aimed at facilitating the licensing, development, and exploitation of inventions. NBS provides assistance in

planning and undertaking the expositions and also provides speakers

and experts for the seminar programs.

Education for Innovation.—The Bureau is working with the

American Society for Engineering Education and the National

Science Foundation to survey opportunities for encouraging innovative design projects in the engineering schools. The program started

from recommendations of the National Inventors Council and at this

stage is directed primarily to an analysis of opportunities for bringing public sector problems into engineering curricula.

The Clearinghouse

A second major activity in the category of Technological Innovation and Diffusion is the IAT program for the dissemination of tech- nical information. This program centers around the Clearinghouse for

Federal Scientific and Technical Information which is the central

point of contact in the Federal Government for disseminating the

results of Government-sponsored R&D to industry, commerce, and

the general public. In addition to the Clearinghouse, the Institute

maintains certain specialized technical information centers covering

engineering standards, weights and measures, instrumentation, and

computer sciences.

The output of the Clearinghouse increased substantially during FY

1968. The Clearinghouse journal UJS. Government Research and Development Reports {USGRDR) announced 37,100 titles. There are now over 547,000 titles in the Clearinghouse collection. Also, over 2

million copies of research reports were distributed to more than

70,000 customers. 143
Document Announcement.—The Clearinghouse began announcing

unclassified/unlimited Department of Defense technical reports to Defense Documentation Center (DDC) users through the USGRDR.

Under a DDC/Clearinghouse agreement all registered DDC users

receive one copy each of USGRDR and its companion publication

USGRDR INDEX.

In January 1968 the title of the USGRDR/Index was changed

from Government Wide Index to Federal Research <& Development

Reports (GWI) to U.S. Government Research <& Development Reports Index ( USGRDR-I) . Changes in the format of the journal and

index were made to improve presentation and readability.

The publication of the separate announcement journal Technical

Translations terminated with the December 30, 1967 issue. Technical

translations are now announced in the USGRDR.

In an experiment with a new announcement mechanism, Clearinghouse Announcements in Science and Technology (OAST), over 1,000

Air Force technical personnel and NBS scientists participated in a test as subscribers to a method for scanning the flow of information in 46

separate fields of technology. Reports resulting from research in

defense, space, nuclear energy, transportation, area development,

education, and other national programs were included. More than 85

percent of the participants reported that CAST opened up new information sources and saved them valuable time. The results of the

experiment, which ran for 6 months, will be used in the development of

a new Clearinghouse announcement medium beginning in FY 1969.

New Document Input.—The Clearinghouse expanded its coverage in

acquiring technical information from Federal agencies and from pri- vate organizations. Documents were acquisitioned from the Department of Transportation and the British Road Research Laboratories on highway safety research; from the Department of Housing and

Urban Development on urban transportation ; from the Office of Economic Opportunity on research in the social sciences and summaries of

Federal programs for FY 1967 in each State ; from the Federal Communications Commission on magnetic tapes containing radio station

licencee data ; from the Federal Aviation Agency on aircraft accident

reports and briefs of accidents in the field of U.S. Civil Aviation. In

the private sector reports were received on area development planning from the American Institute of Planners and the Metropolitan

Council of Governments.

Clearinghouse Computer.—An IBM 360-20 computer was installed

which is programmed to handle processing of orders received for

documents.

144
CENTER FOR RADIATION RESEARCH

The Center for Eadiation Research (CRR) was created in March

1968 by consolidation of the Radiation Physics Division of the Insti- tute for Basic Standards with the Reactor Radiations Division of the

Institute for Materials Research. With this action, the extensive

radiation facilities at NBS were placed under a single management

with responsibilities different in some respects from those of the three

Bureau Institutes. Because the Center contains unique facilites and

competences, it not only has the responsibility for carrying out the

Bureau's mission in the area of radiation, but also for making available its resources and capabilities to other Government agencies, in- dustry, and universities. This policy of facility sharing ensures effi- cient utilization of large multi-purpose facilities such as the reactor and linear accelerator by making them available to a broad segment

of the scientific community.

Radiation of concern to CRR is that produced by radionuclides, re- actors, and particle accelerators with energies between 5 keV and 300

MeV. In this range, the Center provides national leadership in accurate and uniform techniques of measurement of radiation and its interaction with matter, and serves as a national resource providing facili- ties and competence for the development and use of radiation for

investigating properties of atoms, nuclei, and materials. Current programs can be grouped roughly as follows

:

1. Radiation Measurement and Standards

2. Nuclear Physics Research

3. Facilities Operations

4. Technical Assistance to Others

Approximately 20 percent of the Center's work is supported by other

Government agencies.

Radiation Measurement and Standards

Neutron Sowrce Standards.—The precision of the calibration service for neutron sources by the manganous-sulfate bath method has

been improved from a random uncertainty of 0.6 percent to 0.2 percent. This was accomplished by improving the manganese-56 detection system. The new system continuously counts the saturated bath

by circulating the activated solution past a gamma scintillation detector which is shielded from the neutron source. 145
Neutron Energy Transfer.—Calculations of energy transfer to matter by neutrons from thermal energies to 18 MeV have been carried

out for a number of important compounds and mixtures including

tissue. These calculations differ from nearly all previous calculations

in that all detailed neutron reaction processes are included. The work

has demonstrated the importance of usually neglected neutron-induced charged-particle reaction processes, which are very effective for

delivering neutron energy to materials.

Neutron Gross Sections.—The total neutron cross sections of iron,

carbon, and lead have been measured in the neutron energy range 0.7 to 4.4 MeV. The neutron time-of-flight method was employed, with

the NBS electron linear accelerator used as the pulsed neutron source. The energy resolution varied from 0.4 percent to 2 percent ; the overall uncertainty on the absolute cross section values was ±2.5 percent,

and the statistical accuracy of each point was about ±1.5 percent. The

results are in general agreement with earlier data from other laboratories. The measurements revealed much new fine structure in iron and

lead, as well as a new resonance in carbon. Data are now being used for

shielding calculations at other Government laboratories, where they

have helped to resolve some annoying discrepancies.

Response of Silicon Detectors to Monoenergetic Electrons.—The

response of silicon semiconductor detectors to monoenergetic electrons

in the energy region from 0.25 to 1.00 MeV has been systematically

investigated. This was accomplished by exposing silicon transmission

detectors to normally incident electrons with energies of 0.25, 0.50,

0.75, and 1.00 MeV. When the detector thickness was less than the

incident electron range, the pulse-height distributions produced by

electrons were characterized by an absorption peak and a relatively

broad escape peak which is associated with transmission and reflec- tion of electrons. Taking into account the resolution of the detectors,

which were used at room temperature, comparisons were made between the experimental pulse-height distributions and Monte Carlo

results calculated for the same conditions. Good agreement was found

between theory and experiment at 0.75 and 1.00 MeV; however, un- explained differences appeared in the position of the escape peak at

0.25 and 0.50 MeV.

High-Energy Electron and Photon Absorbed Dose Standard.—

A

project was initiated to establish a service for calibrating measuring

instruments in terms of absorbed dose produced with monoenergetic

electron and bremsstrahlung beams between 1 and 50 MeV. A new

calorimetric design and measuring technique was devised to reduce

or eliminate uncertainties caused by temperature gradients, a basic

problem affecting accurate calorimetric measurements. Although the

146
calorimeter was intended for measuring absorbed dose, the principles are applicable to calorimetry in general. Calculations concerning the

performance of the calorimeter revealed a mathematical identity con- cerning heat transfer and its electrical analog.

Cobalt-60 Source Calibration.—The total power output of a cobalt60 gamma ray source furnished by the National Research Council,

Ottawa, Canada was determined. A total absorption calorimeter was

used for the measurement. An accuracy of 0.1 percent was obtained.

The source will also be measured at the national laboratories in Canada

and the USSR and at the International Bureau of Weights and

Measures in order to assess the measuring capability of the four

laboratories.

Solid State Dosimetry.—An investigation was carried out of the

temperature dependence of photocurrents produced by x and gamma

rays in silicon radiation detectors of different types used for exposure rate measurements under the dc mode of operation. The different

temperature dependence of short-circuit currents produced in p-n,

p-i-n, and surface barrier type detectors was found to be due to the

different structure of these detectors rather than to a different temperature dependence of their basic electronic properties. The results of this investigation indicate the possibility of developing an exposure rate meter with silicon radiation detectors showing only a very

small temperature dependence over a chosen temperature range.

Ferrous-Sulfate Dosimeter Studies.—Since July 1967 the Bureau

has provided a quarterly service of mailing Fricke dosimeter units

to those requesting assistance with absorbed-dose measurements in

high-energy electron beams. The purpose is to promote uniformity

of absorbed-dose calibrations among the users of electron beams in

the energy range 5 to 50 MeV. In connection with this service, ex- perience has been gained in the preparation, shipping, and evaluation of large numbers of Fricke dosimeters, and information has been

gathered on the types of high-energy electron machines in use in this

country. Results of the studies indicate there is a reasonable degree

of uniformity among participating users of high-energy electron

beams, with only a few exceptions.

Radioactivity Standards.—During the past year, 366 radioactivity

standards were sold, 36 source calibrations were performed, and the

complete stock of radium solution standards was recalibrated. New

standards produced were a cadmium 109-silver 109 ay

_ray kit" point

source, a tin 113-indium 113 y-ray solution source, and a 10-8 g radium

source in solution for radon testing. Radium standards in solution

form have been reissued at the 10~9 g radium level. The half-lives of

147
two states in neptunium-239 have been measured and a new method

of calibration for the disintegration rate of cadmium 109 has been

developed utilizing a thin-walled well-type scintillation crystal.

Procedures have been developed which enable the determination of

activities by means of scintillation spectrometers to accuracies of the

order of 1 percent. The 113 Sn radioactivity standards (with an uncertainty of ±2.2 percent) were produced with the aid of these techniques. A determination of radioactivities present in certain Antarctic

soil by means of gamma-ray spectrometry was made.

The Bureau participated in experimental work in connection with

the development of an ASTM standard procedure for determination of

radium in water, as well as the intercomparison of cobalt 57 sources among pharmaceutical laboratories and national laboratories in the

U.S. and Canada.

Electron Interactions.—The revamped 500-keV electron accelerator

has been used for measurements on the response of thermoluminescent

materials to electrons, and on atomic binding effects in Moller scat- tering. The latter experiment revealed prominent, but theoretically

unpredicted, structure in the inelastic spectra and increasing agreement

with the Moller cross section for increasing atomic numbers.

Other measurements were made on electron response to radiationsensitive dye systems and work is currently being pursued on x-ray

spectral data, especially those related to cross section or production

efficiency determinations of characteristic radiations.

Monitoring of High Energy Electron Beams.—A nonintercepting

technique for measuring the integrated current of pulsed high-energy

electrons is being developed, employing ferrite toroids as pulse trans- formers. The system provides stable and reproducible results when

compared with a Faraday cup. Nonlinear effects due to changes in pulse

length and amplitude are being investigated. A simple, radiation hard

beam position monitor has been developed. The sensitivity is suffi- cient to permit beam position measurements with an accuracy of

better than 1 mm at pulsed beam currents less than 1 mA.

Nuclear Physics Research

Electron Scattering.—Experiments in progress include inelastic

scattering from 12C, concentrating on the excitation region 17-27

MeV ; inelastic scattering from low-lying levels of 16 0 ; and an experiment attempting to measure the charge form factor of the proton to very high accuracy at low momentum transfer. Collaborative research

programs using the NBS electron scattering facility are in progress

with research teams from five universities. The multidetector "ladder"

counter system employing semiconductor detectors has been brought

into operation with excellent results. A number of other laboratories

148
throughout the world are adopting similar systems for their electron

scattering programs, The design aim of an overall resolution capability of 0.1 percent has been achieved. At this resolution, experiments

can be performed with electron beam current of about 3 /xA. Heavy-Ion Spectrometer Experiments.—The electron and photon

disintegration cross sections of 4He are being measured with the NBS

heavy-ion spectrometer and NBS linac. The mass identification fea- ture of the heavy-ion spectrometer makes possible an unambiguous

determination of the 4ILe(y,p)T, 4He(e,^e') and 4He(y,n) 3He,

4He(e,we') 3He cross sections. This measurement will substantially improve the precision of total and different (in angle) cross sections

from threshold to 50 MeV for proton reaction and from 24 MeV to 100 MeV for neutron reaction.

The Nuclear Three-Body Problem.—Calculations of the photodisintegration of 3H and 3He have been extended using a more consistent

model based on a ground state wave function that is an exact solution

of the three-body Schrodinger equation with separable potentials of

the Yamaguchi type. The final states contained interactions between

nucleon pairs. Calculations were carried out for both the YamaguchiSitenko-Kharchenko and Tabakin sets of interaction parameters.

Since the wave functions used have also been employed to describe the

scattering of neutrons by deuterons, the theoretical model serves as a means of relating two types of experimental data. Investigations are underway to check the validity of the model for calculating the three

alpha particle break-up of 12C. In a separate investigation the problem of constructing a practical

calculational scheme for off-energy-shell two-body amplitudes was

undertaken which avoided the use of integral equations. The off- energy-shell two-body amplitudes are used as input to the Faddeev

formulation of the three-body problem. It was found that the cal- culation could be done with a differential equation similar to the

Schrodinger equation but containing an extra inhomogeneous term. Nuclear Structure Studies by Electron and Photon Excitation.—

The program to investigate nuclear states by exciting them with elec- trons and photons is continuing. Nuclear levels in the isotope 179Hf

have been investigated and a report on this nucleus is being prepared.

Further levels in isotopes of Au and Ir are being investigated and

other elements will be studied in the future. An apparatus for investigating elastic and inelastic scattering of electrons at 180° has been

installed and should be operating shortly. This apparatus will provide

experimental tests of established nuclear force and structure theories

by investigating how low atomic number elements behave in interactions where non-nuclear excitation scattering is at a minimum.

149
"Large Angle Inelastic Electron Scattering.—Data taken on the in- elastic scattering of 200- and 400-keV electrons at large angles from

various targets has been analyzed and a report published. These results show disturbing deviations form the available theoretical calculations

and are being investigated further. In particular, the incident electron

energy is to be extended from 400 keV upwards to 4 MeV by utiliza- tion of the 1.5 and 4.0 MeV NBS electron accelerators. Nuclear Spectroscopy.—The asymmetry of beta particles from ori- ented thulium 170 and praseodymium 142 nuclei implanted in iron

foils by the NBS isotope separator has been used to measure the effec- tive internal magnetic fields for these nuclei. Beta spectroscopy under

the conditions of cryogenic nuclear orientation has been aided by the

development of thick silicon detectors and preamplifiers which function well at temperatures of 1.5 K. The effect of polarizing fields, foil angles, and scattering on electron spectra have been investigated.

Optimum conditions for the apparatus have been determined for

sustained maximum orientation and for accurate thermometry using

the anisotropy of a

57Co gamma ray measured by germanium detectors. The Photonuclear Data Center.—The first Supplement to Miscellaneous Publication 277, Photonuclear Data Index, was published and

circulated to workers in the field. This supplement covered data added

to the Center's files in the period January 1, 1965 through April 1967.

Each entry in this index supplies quantitative data about the specific

type of experimental information given in each reference to the litera- ture cited. The complete index to data in the Center's files has now been

put on magnetic tape, making possible automatic searches using a small computer, for reference to any one or all of nine specific types

of information.

Facilities Operations

Linear Accelerator.—During fiscal year 1968 in excess of 1500 hr

of beam time were provided for experiments using the NBS linac. This was 57 percent of the scheduled beam time. Numerous modifications to the accelerator and beam-transport equipment have been ac- complished to improve beam quality and reduce maintenance problems. The chief maintenance problems continue to be associated with

the fact that round-the-clock operation is not possible. Despite this,

beam has been provided at under $200 per hour of beam-on-target time.

Experiments using the accelerator include programs in electron

scattering, photoneutron production, production of heavy ions, meas- urement of neutron total absorption cross sections, studies in beam

monitoring, programs in activation analysis, and production of radioactive sources for materials studies using Mossbauer sources and for

150
studies of photonuclear reactions. Programs in electron and x-ray- beam dosimetry, accelerator research, and production and use of monoenergetic positron and photon beams are in preparation. Collaborative

programs with groups from six different universities are or will soon

be in operation.

A major improvement during the year for time-of-flight experiments

has been the development of enhanced short pulse linac operation.

Beam pulse lengths of three to five nanoseconds and beam currents in excess of two amperes at the end of the accelerator are now possible.

Delivery of energy analyzed beams (2 percent) in excess of one ampere to experiments with these pulse lengths is routine.

NBS Reactor.—On December 7, 1967 the National Bureau of Standards Reactor (NBSR) achieved criticality for the first time. This was the culmination of more than nine years of planning and over four years of construction. The NBSR, a high-flux, tank type, heavy

water cooled and moderated machine will operate initially at a power

of 10 MW (thermal) and will have a flux of 1014 n/cm2 /s. Several

months of low power testing are required to determine the characteristics of the reactor before operating at high power. When NBSR be- comes fully operational, it will be used for neutron diffraction and

scattering experiments in the area of materials research and for studies in radiochemistry.

Jp MeV Accelerator.—The experimental flexibility of the NBS 4- MeV Van de Graaff accelerator has been increased by the addition

of a new 18-in. diameter electron scattering chamber. This chamber,

which may be used for electron scattering experiments, dosimeter ir- radiations and charged particle detector calibrations, provides such

features as a remotely operated target viewing system to determine

incident beam position, scattering ports every 30° from 0 to 180°, and

complete electrical insulation for current measurements. The acceler- ator system has also been equipped with a beam centering feedback

system to automatically maintain beam location, independent of small

changes in the operating parameters of the accelerator. Further updating of the accelerator voltage stabilizing system is also underway.

Isotope Separator.—The new electromagnetic separator has been

used for the preparation of pure, thin, mass-identified sources of stable

and radioactive isotopes. Sources which were made with the isotope

separator were used in Mossbauer, photonuclear reaction, nuclear orientation, and range distribution studies. The ion implantation of sulphur

in semiconductors such as gallium arsenide and cadmium sulfide re- sulted in the production of materials with desirable properties. An

investigation of the radiation damage to metal chelates has been

started. 151
Reactor operators using fuel handling tools to lock fuel elements into the core of the NBS reactor. Control room can be seen in the background. Technician on left is observing the operation in the core through a periscope.

Synchrotron Move.—During this year the major effort of moving

the NBS 180-MeV synchrotron from the Washington site to Gaithersburg was essentially completed. Efforts are now underway to achieve or better the beam currents previously available before experimental

programs using the accelerator resume. Technical Assistance to Others

Studies for Other Agencies

Standard Nuclear Instrument Module System.—The standard Nuclear Instrument Module (NIM) System, developed in conjunction

with the National Laboratories of the U.S. Atomic Energy Commission, has had a tremendous impact on the entire nuclear instrumentation field and has revolutionized the manner in which experiments are performed in nuclear physics. Practically all modular nuclear in- 152
strumentation currently produced in the United States is in accord- ance with this standard. The NIM System is also the dominant

modular nuclear instrumentation system worldwide. The NIM System

development was undertaken as a result of an NBS report issued in

December 1963 that pointed out interchangeability problems that ac- companied the advent of transistorized modular instruments and rec- ommended that a coordinated effort be initiated to produce a standard module system to reduce these difficulties. Specifications for

standard modules to assure mechanical and electrical interchangeability were drawn up in 1964 ; laboratory and industry utilization began

at the end of that year. By 1966 the NTM System had been adopted by

practically all U.S. nuclear instrument manufacturers and was responsible for a considerable export market in nuclear instruments.

Radioactive Contamination of Materials.—An extensive study is being carried out on behalf of the USAEC to determine the extent of

low-level contamination in chemical reagents and commercial materials, including the study of variations with time, nature, manufacturing practice and geographical origin. Over 500 samples have been

studied to date. Conferences

Molecular Dynamics and Structure of Solids Conference.—The

Molecular Dynamics and Structure of Solids Conference was held at the National Bureau of Standards site in Gaithersburg, Md., on

October 16-19, 1967. Sessions were attended by approximately 250

people from Government, industry, and universities. Objectives of the

symposium were to

:

Encourage interdisciplinary cooperation by demonstrating the cor- relation of various techniques applied to the study of molecular dynamics and structure of solids. Stimulate among participants an appreciation of techniques outside

their own specialties.

Promote a more complete understanding of the materials of

interest. Neutron Cross Sections and Technology Conference.—The second

conference on "Neutron Cross Sections and Technology" was held at the Shoreham Hotel, Washington, D.C., on March 4-7, 1968. Approximately 350 persons from Government, universities, and industry at- tended the Conference. The purpose of the second conference was to provide a common meeting area for the exchange of information

among nuclear scientists and engineers interested in neutron cross sec- tions. The conference program was designed to consider all aspects of

neutron cross sections, the need for accurate measurements, and their

determination by theoretical and experimental techniques and their

applications.

153

APPENDIXES

ORGANIZATION OF THE NATIONAL BUREAU

OF STANDARDS 1 The Bureau is headed by a Director who is appointed by the

President with the advice and consent of the Senate. The Director is assisted in the overall management of the Bureau by a Deputy Director. In addition there is an Associate Director for Administration

who is responsible for the planning and operation of facilities and of

administrative management services in support of the Bureau's technical programs.

Technical program activities are conducted in three Institutes and

a Center for Radiation Research. Each is headed by a Director who

is responsible for the development and direction of research programs

and central national services essential to the fulfillment of a broad

segment of the Bureau's mission. These major organizational units

are:

(1) The Institute for Basic Standards, which includes 12 divisions

(5 in Boulder, Colo.), each serving a classical subject matter area of

science and engineering ; also 3 administrative divisions serving technical divisions located in Boulder, Colorado

;

(2) The Institute for Materials Research, which consists of 6

divisions, organized primarily by technical field

;

(3) The Institute for Applied Technology, which includes 16

divisions oriented to high-technology industries ; and

(4) The Center for Radiation Research, which includes 4 divisions

concerned with the theory and application of radiation.

DIRECTOR

Allen V. Astin

DEPUTY DIRECTOR

I. C. SCHOONOVER

Assistant to the Deputy Director

P. H. Kratz

1 As of June 30, 1968. 155

320-738 O—68 11
OFFICE OF THE DIEECTOE

Assistants to the Director

G. E. Auman

C. K COATES

A. G. McNish

Legal Advisor

A. J. Farrar

Office of Industrial Services

G. S. Gordon

Office of Public Information

A. V. Gentilini

Office of Academic Liaison

S. Silverman

Office of Engineering Standards Liaison

A. A. Bates

Office of Program Development and Evaluation

E. D. Huntoon

M. B. Wallenstein

E. E. Ferguson

Senior Eesearch Fellows

C. ElSENHART

K. Shuler

Technical Support Units Eeporting to the Deputy Director

Coordinator of Special International Programs L. L. Marton

Office of Technical Information and Publications W. E. Ttllet

Library Division E. L. Tate

Instrument Shops Division F. P. Brown

Measurement Engineering Division G. F. Montgomery

OFFICE OF ASSOCIATE DIEECTOE FOE

ADMINISTRATION

E. S. Walleigh

Deputy Associate Director

P. H. Schrader

Patent Advisor

D. Eobbins

156
Accounting Division J. P. Menzer

Administrative Services Division G. W. Knox

Budget Division J. E. Skillington

Management and Organization Division J. T. Hall

Personnel Division G. E. Porter

Plant Division H. Graham

Supply Division G. B. Kefover

INSTITUTE FOE BASIC STANDAEDS

Director

E. Ambler

Deputy Director

Vacant

Deputy Director, Institute for Basic Standards/Boulder 1 B. W. Birmingham, Acting

Coordinator for Measurement Services

H. L. Mason

Office of Standard Reference Data E. L. Brady

Atomic and Molecular Data Information Services Design

Chemical Kinetics Mechanical Properties

Colloid and Surface Chemistry Nuclear Data

Information Services Solid State Properties

Thermodynamics and Transport Data

Applied Mathematics E. W. Cannon

Numerical Analysis Statistical Engineering

Operations Research Systems Dynamics

Electricity Division

Resistance and Reactance

Electrochemistry

Electrical Instruments

C. H. Page

High Voltage

Absolute Electrical Measurements

Metrology Division

Optics Metrology Branch

Photometry

Image Optics and Photography

Colorimetry and Spectrophotometry

T. R. Young, Acting

Length Metrology Branch

Length

Engineering Metrology

Mass and Volume Branch

Mass and Volume

Mechanics Division Sound

E. C. Lloyd, Acting

Engineering Mechanics

Rheology

1 Located at Boulder, Colo. 157
Mechanical Measurements Branch

Pressure Measurements Vacuum Measurements

Vibration Measurements

Humidity Measurements

Fluid Mechanics Branch

Fluid Meters

Hydraulics

Aerodynamics

Heat Division R. P. Hudson

Heat Measurements Statistical Physics

Cryogenic Physics Molecular Energy Levels Equation of State Temperature

Radiation Thermometry

Atomic Physics Division K. G. Kessler Spectroscopy Infrared and Microwave

Spectroscopy Far Ultraviolet Physics

Electron Physics

Atomic Physics

Plasma Spectroscopy

Radio Standards Physics Division 1 H. S. Boyne, Acting

Solid State Electronics Quantum Electronics Plasma Physics

Radio Standards Engineering Division 1 H. M. Altschuler H F Calibration Service H F Electrical Standards

H F Impedance Standards M W Calibration Service M W Circuit Standards Electromagnetic Field Standards

Time and Frequency Division 1 J. A. Barnes Frequency-Time Dissemination Frequency-Time Broadcast Services Research

Atomic Frequency-Time

Standards

Laboratory Astrophysics Division 1 L. M. Branscomb

Cryogenics Division 1 D. B. Chelton, Acting

Cryogenic Technical Services Cryogenic Data Center

Cryogenic Properties of Solids Properties of Cryogenic Fluids

Cryogenic Systems Cryogenics Metrology

Cryogenic Fluid Transport Process Administrative Services Division 1 B. F. Betts Supply Office Services Drafting Services Instrument Shops Division 1 R. S. Perrill Instrument Shop I Instrument Shop II Welding-Sheet Metal Shop Glassblowing Shop

Plant Division 1 E. A. Yuzwiak

Construction-Maintenance Special Services Custodial Services Section

1 Located at Boulder, Colo. 158
INSTITUTE FOR MATERIALS RESEARCH

Director

J. D. Hoffman

Deputy Director

H. E. Sorrows

Office of Standard Reference Materials W. W. Meinke

Analytical Chemistry Division W. W. Meinke

Radiochemical Analysis Microchemical Analysis

Spectrochemical Analysis Analytical Mass Spectrometry

Electrochemical Analysis Organic Chemistry

Analytical Coordination Chemistry Activation Analysis

Separation and Purification Polymers Division Polymer Dielectrics Polymer Chemistry

Polymer Crystal Physics

Molecular Properties

R. R. Stromberg, Acting

Dental Research

Polymer Characterization Polymer Interfaces Thermophysical Properties

Metallurgy Division E. Passaglia

Engineering Metallurgy Corrosion

Alloy Physics Metal Physics

Lattice Defects and Microstructures Electrolysis and Metal Deposition

Crystallization of Metals

Inorganic Materials Division . J. B. Wachtman

Inorganic Chemistry Physical Properties

Inorganic Glass Crystallography

High Temperature Chemistry Solid State Physics Section Physical Chemistry Division. Thermochemistry

Surface Chemistry

Elementary Processes

J. R. McNesby, Acting

Mass Spectrometry

Photo Chemistry

Radiation Chemistry

INSTITUTE FOR APPLIED TECHNOLOGY

Director

L. M. Ktjshner

Deputy Director

Vacant

NBS/GSA Test and Development Division P. J. Franklin

Manager, Engineering Standards M. W. Jensen

Office of Engineering Standards Services D. R. Mackay

Product Standards Section Information Section Mandatory Standards Section 159
Office of Weights and Measures M. W. Jensen

Office of Invention and Innovation D. V. DeSimone

Innovation Studies Program Invention Programs

Engineering Education Program

Office of Vehicle Systems Research P. J. Brown

Clearinghouse for Federal Scientific and Technical Information H. E. Sauter Document Distribution and Reproduction Branch

Automated Systems and Services Branch

Administrative Operations Branch

Joint Publications Research Service Documents Processing Branch

Product Evaluation Division S. B. Newman

Plastics and Textiles Paper Evaluation

Fibrous Systems Fabric Flammability

Viscoelastic Materials

Building Research Division J. R. Wright

Structures Materials Durability and Analysis

Fire Research Codes and Standards

Scientific and Professional Liaison Building Systems

Sensory Environment Branch

Environmental Engineering Psycho-physics

Building Transport Systems

Electronic Instrumentation Division M. G. Domsitz

Semiconductor Characterization Instrumentation Applications Electron Devices Semiconductor Processing

Technical Analysis Division W. E. Cushen

Corridor and Highway Studies Economic Analysis

Systems Analysis and Human Development of New Methodology

Factors

Center for Computer Sciences and Technology H. R. J. Grosch

Office of Information Processing Standards J. O. Harrison, Jr. Technical Information Exchange M. R. Fox

Computer Services Division W. B. Ramsay, Acting.

Systems Research and Development Division E. C. Marden

Information Processing Technology Division J. P. Nigro

CENTER FOR RADIATION RESEARCH*

Director

C. O. Muehlhause, Acting

Deputy Director

R. S. Caswell, Acting

Radiation Theory Health Physics Reactor Radiation Division R. S. Carter, Acting Reactor Operations Neutron Solid State Physics

Engineering Services Radiation Effects

'Reports to the Deputy Director, NBS

160
Linac Radiation Division J. E. Leiss, Acting

Linac Operations Photonuclear Physics

Radiation Physics Instrumentation Electronuclear Physics

Nuclear Radiation Division H. H. Landon, Acting

Nuclear Physics Radioactivity

Nuclear Spectroscopy Section Applied Radiation Division J. W. Motz, Acting

X-Ray Physics Dosimetry

FIELD ESTABLISHMENTS

Institute for Basic Standards

Metrology Division Field Station : Visual Landing Aids Field Laboratory

Time and Frequency Division Field Stations : Standard Frequency Station WWV-WWVL-WWB

Standard Frequency Station WWVH

Laboratory Astrophysics Division Field Station: Poor Man's Relief Mine, Four-Mile Canyon

Areata, California Fort Collins, Colorado Maui, Hawaii

Boulder, Colorado

Institute for Applied Technology

Office of Weights and Measures Field Stations

:

Master Railway Track Scale Depot Clearing, Illinois

SUMMARY OF NBS STAFF AS OF JUNE 30, 1968

Washington Boulder Total

Full-time permanent staff 1 2, 939 580 3, 519

Other staff 2 305 48 353

Total paid staff 3, 244 628 3, 872

Research associates—guest workers 131 16 147 Total NBS staff 3, 375 644 4, 019

Professional Staff With Academic Degrees:

Phvsicists 395 114 509

Chemists . 272 7 279

Engineers _ __ 172 89 261 Mathematicians. 49 7 56 Other _ 128 5 133

Total _ 1,016 222 1, 238

1 Includes Post Doctoral Research Fellows.

2 Summer, Youth Opportunity Corps, Part-Time, Intermittent and Temporary.

161
FINANCIAL DATA FOR FISCAL YEAR 1968

Obligations incurred in thousands

of dollars Program and source of financing (rounded) Supported by NBS Appropriations

Operating programs:

Research and technical services $32, 283

Civilian industrial technology 139

Special foreign currency program 444

Construction and facilities programs:

Plant and facilities 894

Construction of facilities 2, 996

Total obligations, NBS appropriations 36, 756 Supported by other funds 1 From other Federal agencies 24, 036 From other sources 4, 392

Total obligations, other funds 28, 428

Total program 65, 18

1

1 Work supported by other funds consists of research and development pro- grams for other Government agencies; consultative, advisory, and technical

services, the performance of various tests and calibrations, and the manufacture

and sale of standard reference materials for other Government agencies and the

public.

RESEARCH ASSOCIATES AND GUEST WORKERS

Research Associates and Their Sponsors

During Fiscal Year 1968

AiResearch Manufacturing Company

Simpson, Mr. Anthony U. American Cyanamid Company

Hodgson, Dr. William G. American Dental Association Argentar, Mr. Harold

Bowen, Mrs. Joy C. Bowen, Dr. Rafael L. Brown, Dr. Walter E. Carlson, Mr. Elmer T. Caul, Mr. Harold J. Gregory, Mr. Thomas M., Jr. Kingsbury, Mrs. Pamela

Mabie, Mr. Curtis P., Jr. Manuszewski, Mr. Richard C. McDowell, Mr. Hershel

162
American Dental Association—Continued

Moreno, Dr. Edgard C. Paffenbarger, Dr. George C. Palcic, Miss Julia M.

Patel, Mr. Prafull Wallace, Mrs. Betty M.

Waterstrat, Mr. Richard M. American Electroplaters Society

Johnson, Mr. Christian E. American Society for Testing and Materials de Groot, Mr. Johan H.

Evans, Mrs. Eloise H. McMurdie, Mr. Howard F. Morris, Mrs. Marlene C. American Society for Testing and Materials (Concrete and Concrete Ref- erence Laboratory)

Anderson, Mr. Harry G., Jr. Atkinson, Mr. George O., Jr. Dise, Mr. John R. Johnson, Mr. Marlin C. Katz, Mrs. Anne K.

Liskey, Mr. John F. Markus, Mr. Walter

McCarthy, Mr. Dennis D.

Seiler, Mr. James F., Jr. Spring, Mr. Curtis B. Sturm, Mr. William F. Wallace, Mr. Dennis R. American Viscose Division (FMC Corporation)

Oneal, Mr. Glen, Jr. Asphalt Roofing Industry Bureau

Crowe, Mr. Thomas A. Greenfeld, Mr. Sidney H. Bethlehem Steel Corporation

Swanson, Mr. Kenneth R. Calcium Chloride Institute Tomes, Mr. Lewis A. Consumers Union of U.S., Inc. Kanagy, Dr. Joseph R. Control Data Corporation

Buckland, Mr. Stanley F., Jr. Com Refiners Association, Inc. Thomas, Mr. James H. Vomhof, Dr. Daniel W.

Cornmg Glass Works

Justice, Mr. Benjamin

163
Dow Chemical Company

Grenley, Mr. Dallas G. Hamilton, Mr. Robert M.

O'Dell, Mr. William W., Jr. Eastman Kodak Company

Prsybylowicz, Dr. Edwin P. Electrical Testing Laboratories, Inc. Mohan, Mr. Kshitij

Factory Mutual Research Corporation

de Ris, Dr. John N. Kapprafe, Mr. Ronald M.

Orloff, Mr. Lawrence

Rockett, Dr. John A. Torrance, Dr. Kenneth B. International Business Machines Corporation

Cleveland, Mr. Norman G. Shelton, Mr. Carl A. F. Japan Electronic Industry Development Association Yamadori, Mr. Yuji

Manufacturing Chemists Association

Brucksch, Mr. William F., Jr. Clark, Mr. Joseph E. Herndon, Mr. John L., Ill Martin Marietta Corporation {Research Institute for Advanced Studies)

Mengelberg, Dr. Hans-Dieter

Ministere des Postes et Telecommunications {France)

Anquetil, Mr. Phillippe L. Nippon Electric Company {Japan)

Inawashiro, Mr. Tutonra Owens-Corning Fiberglas Corporation

Fitch, Mr. WiUiam E. Porcelain Enamel Institute Burdick, Mr. Milton D.

Gugeler, Mr. Lauren A. Rushmer, Miss Margaret A. Structural Clay Products Institute Johnson, Mr. Paul V. Watstein, Mr. David

Underwriters Laboratories, Inc. Castino, Mr. Guy T.

U.S. Navy Marine Engineering Laboratory

Arora, Dr. Om P.

U.S. Steel Corporation

Martin, Mr. John F. 164
Foreign Guest Workers and Their Sponsors

During Fiscal Year 1968

Name Country Sponsor

Martins, J. Walters Brazil CAPES (Brazilian NSF).

Cohen, Agda Artna Canada Nuclear Data Project, Oak Ridge, Tenn. Herman, J. A Canada National Research Council,

Canada.

Herman, K. M Canada National Research Council,

Canada.

Goonetilleke, H. L Ceylon Dept. of Commerce, Colombo,

Ceylon.

Quinn, Terrence J England National Physical Laboratory.

Artru, Madame M. C France Observatoire de Paris, Meudon.

Hanauer, Jean-Pierre France Delegation Generale a la Recherche

Scientifique et Technique, Paris. Guetrot, Alain France Delegation Generale a la Recherche

Scientifique et Technique, Paris. Haddad, Roger J France Delegation Generale a la Recherche

Scientifique et Technique, Paris. Boisrobert, C. Y France Delegation Generale a la Recherche

Scientifique et Technique, Paris. Straub, Johann Germany Institut fur Technische

Thermodynamik.

Hussmann, E Germany NATO Fellow. Dajani, Khawla Iran American University.

Goldschmidt, Zvi Israel None.

Natali, Sergio Italy None, employee of Institut of Physics, Univ. of Bari, Italy.

Inamatsu, Teruko Japan National Research Laboratory

of Metrology, Japan.

Kaarls, R Netherlands Dutch Service of Weights and

Measures.

Olaussen, Leif K Norway Norwegian Government.

Adil, Syed M. F Pakistan United Nations Fellow. Angeles, Rosalie Philippines American University.

Czyz, Wieslaw Poland American University NSF Grant.

Youssef, Samir UAR International Atomic Energy

Agency.

Radovanovic, Dusan Yugoslavia National Academy of Sciences. ADVISORY COMMITTEES

STATUTORY VISITING COMMITTEE

The Statutory Visiting Committee was established by Act of Congress to advise

the Secretary of Commerce and the Director of NBS. This committee is appointed

by the Secretary of Commerce. It meets at the call of its chairman. Dates indicate expiration of appointment.

Dr. Robert L. Sproull, Vice President Academic Affairs, Cornell University

(1971), Chairman

Dr. Paul C. Cross, President, Mellon Institute (1969)

165
Dr. Elmer W. Engstrom, President, Radio Corporation of America (1968)

Prof. Norman F. Ramsey, Department of Physics, Harvard University (1970)

Dr. E. R. Piore, Vice President, Research and Engineering, International Business Machines Corporation (1972)

TECHNICAL ADVISORY PANELS

The panels advisory to the National Bureau of Standards were established in 1959 under the terms of a contract between the National Bureau of Standards

and the National Academy of Sciences. The Advisory Panels are responsible to the National Academy of Sciences-National Academy of Engineering-National

Research Council, Division of Physical Sciences. One panel is established for each of the three Institutes of the Bureau, and one panel for each of the major

divisions within the Institutes. The advisory panels to the Institute for Applied

Technology are appointed by the President of the National Academy of Engineering. All other panels are appointed by the President of the National Academy

of Sciences. The divisional panels ordinarily have eight members although by

special arrangement a few have more or less. Terms are usually three years.

Institute for Basic Standards

Advisory Panel to Institute for Basic Standards

Prof. John Todd, California Institute of Technology

Dr. William G. Amey, Leeds & Northrup Company

Dr. J. H. Webb, Eastman Kodak Company

Prof. S. R. Beitler, American Society of Mechanical Engineering

Prof. John Ross, Massachusetts Institute of Technology

Dr. Wade L. Fite, University of Pittsburgh Dr. Norman D. Coggesehall, Gulf Research & Development Company

Dr. Bruce H. Billings, Aerospace Corporation

Dr. Peter T. Demos, Massachusetts Institute of Technology

Dr. Paul D. Coleman, University of Illinois Advisory Panel to Applied Mathematics Division

Prof. John Todd, California Institute of Technology, Chairman

Prof. Francis J. Anscombe, Yale University

Prof. Philip J. Davis, Brown University

Prof. Charles R. DePrima, California Institute of Technology

Dr. Ralph E. Gomory, International Business Machines Corp.

Prof. M. H. Martin, University of Maryland

Dr. J. Barkley Rosser, University of Wisconsin

Prof. John W. Tukey, Princeton University

Advisory Panel to Electricity Division

Dr. William G. Amey, Leeds & Northrup Company, Chairman

Prof. Raymond M. Fuoss, Yale University

Prof. H. N. Hayward, University of Illinois Mr. William J. Johnson, Philadelphia Electric Company

Prof. George B. Hoadley, North Carolina State University

Prof. Clyde A. Hutchison, Jr., The University of Chicago

Dean R. B. Lindsay, Brown University Mr. Douglas C. Strain, Electro Scientific Industries, Inc. 166
Advisory Panel to Metrology Division

Dr. J. H. Webb, Eastman Kodak Company, Chairman

Prof. Isay A. Balinkin, University of Cincinnati Mr. B. R. Buus, General Electric Company

Dr. Alsoph H. Corwin, The Johns Hopkins University Mr. J. K. Emery, The Van Keuren Company

Dr. Robert E. Hopkins, University of Rochester

Mr. Louis Pclk, Dayton, Ohio

Mr. Eric J. Schneider, Engis Equipment Company

Dr. George J. Zissis, University of Michigan

Advisory Panel to Mechanics Division

Prof. S. R. Beitler, American Society of Mechanical Engineering, Chairman

Prof. Lynn S. Beedle, Lehigh University

Dr. B. B. Dayton, Consolidated Vacuum Corporation

Prof. Cyril M. Harris, The Columbia University

Prof. Arthur T. Ippen, Massachusetts Institute of Technology

Dr. Harry P. Olson, Radio Corporation of America

Prof. R. S. Rivlin, Lehigh University

Dr. M. E. Shank, Pratt & Whitney Aircraft Advisory Panel to Heat Division

Prof. John Ross, Massachusetts Institute of Technology, Chairman

Prof. G. B. Benedek, Massachusetts Institute of Technology

Prof. Howard W. Emmons, Harvard University

Dr. E. F. Hammel, University of California Dr. John P. McCullough, Mobil Oil Corporation

Dr. James W. Moyer, Northrop Corporation

Prof. John G. Phillips, University of California Dr. Howard Reiss, North American Aviation Science Center Advisory Panel to Atomic Physics Division

Dr. Wade L. Fite, University of Pittsburgh, Chairman

Prof. C. O. Alley, University of Maryland

Prof. Kurt Dressier, Princeton University

Dr. Leo Goldberg, Harvard College Observatory

Prof. Richard C. Lord, Massachusetts Institute of Technology

Prof. Robert Novick, Columbia Radiation Laboratory

Prof. W. E. Spicer, Stanford University

Advisory Panel to Radio Standards Engineering Division

Dr. Paul D. Coleman, University of Illinois, Chairman

Dr. George Birnbaum, North American Aviation Science Center

Prof. Sanborn C. Brown, Massachusetts Institute of Technology

Dr. C. Lester Hogan, Motorola, Inc. Dr. A. O. McCoubrey, Varian Associates Mr. Frank McGinnis, Sperry Gyroscope Company

Dr. J. A. Pierce, Harvard University

Dr. Bernard M. Oliver, Hewlett-Packard Company

Mr. Theodore S. Saad, Sage Laboratories, Inc. Mr. D. F. Schmit, Radio Corporation of America

Prof. J. H. Van Vleck, Harvard University Mr. C. E. White, AVCO Corporation

167
Advisory Panel to Laboratory Astrophysics Division

Dr. Bruce H. Billings, Aerospace Corporation, Chairman

Prof. W. R. Bennett, Jr., Yale University

Dr. James E. Drummond, Boeing Scientific Research Laboratories

Dr. John W. Evans, Air Force Cambridge Research Laboratory

Dr. Wade L. Fite, University of Pittsburgh

Dr. George H. Herbig, University of California Dr. John A. Hornbeck, Sandia Corporation

Prof. Robert Novick, Columbia University

Institute for Materials Research

Advisory Panel to Institute for Materials Research

Dr. Robert L. Sproull, Cornell University, Chairman

Dr. William O. Baker, Bell Telephone Laboratories

Prof. John Bardeen, University of Illinois Dr. Arthur Bueche, General Electric Research Laboratory

Dr. N. B. Hannay, Bell Telephone Laboratories, Inc. Dr. Raymond F. Boyer, Dow Chemical Company

Prof. Roman Smoluchowski, Princeton University Dr. J. H. Crawford, Chairman, University of North Carolina

Advisory Panel to Analytical Chemistry Division Dr. N. B. Hannay, Bell Telephone Laboratories, Inc., Chairman

Prof. Walter J. Blaedel, University of Wisconsin

Mr. M. D. Cooper, General Motors Corporation

Dr. Edward C. Dunlop, E. I. Du Pont de Nemours & Co. Dr. John F. Flagg, American Cyanamid Company

Prof. George Morrison, Cornell University

Prof. L. B. Rogers, Purdue University

Dr. Ralph E. Thiers, Duke University Medical Center

Advisory Panel to Polymers Division

Dr. Raymond F. Boyer, Dow Chemical Company, Chairman

Dr. J. J. Hermans, Chemstrand Research Center

Dr. Fraser P. Price, General Electric Research Laboratory

Dr. William P. Slichter, Bell Telephone Laboratories

Prof. Walter Stockmayer, Dartmouth College Dr. Howard W. Starkweather, Jr., E. I. Du Pont de Nemours & Co. Dr. Duane F. Taylor, University of North Carolina

Prof. Bruno H. Zimm, University of California

Advisory Panel to Metallurgy Division

Prof. Roman Smoluchowski, Princeton University, Chairman

Dr. Walter A. Dean, Aluminum Company of America

Dr. G. J. Dienes, Brookhaven National Laboratory

Dr. Julius J. Harwood, Ford Motor Company

Dr. Richard A. Oriani, United States Steel Corp. Dr. Robb M. Thomson, Advanced Research Projects Agency

Prof. David Turnbull, Harvard University

Dr. H. G. F. Wilsdorf, University of Virginia

168
Advisory Panel to Inorganic Materials Division

Dr. J. H. Crawford, University of North Carolina, Chairman

Dr. George J. Bair, Corning Glass Works

Dr. Joseph E. Burke, General Electric Company

Dr. Harris M. Bnrte, Wright-Patterson Air Force Base

Dr. Theodore L. Brown, University of Illinois Dr. J. S. Kasper, General Electric Company

Prof. John L. Margrave, Rice University

Prof. Alan M. Portis, University of California Dr. Elias Snitzer, American Optical Company

Advisory Panel to Physical Chemistry Division

Dr. Norman D. Coggeshall, Gulf Research & Development Company,

Chairman

Prof. Kyle D. Bayes, University of California Dr. Hartwell F. Calcote, AeroChem Research Laboratories, Inc. Dr. F. G. Ciapetta, W. R. Grace and Company

Dr. R. E. Fox, Westinghouse Electric Corporation

Prof. Robert Gomer, The University of Chicago

Prof. B. S. Rabinovitch, University of Washington

Dr. Bruno J. Zwolinski, Texas A&M University

Institute for Applied Technology

Advisory Panel to Institute for Applied Technology

Prof. C. West Churchman, University of California, Chairman

Mr. Kenneth C. Allen, Hobart Manufacturing Company

Dr. Robert A. Hechtman, McLean, Virginia Dr. Leon Podolsky, Pittsfield, Massachusetts

Prof. Philip Morse, Massachvisetts Institute of Technology

Dr. William W. Eaton, Washington, D.C.

Dr. W. J. Harris, Jr., Battelle Memorial Institute Dr. Carl H. Madden, U.S. Chamber of Commerce

Dean Joseph R. Passonneau, Skidmore, Owens & Merrith Mr. Jacob Rabinow, Bethesda, Maryland

Mr. Paul Strassman, National Dairy Products Corp.

Dr. Michael Witunski, St. Louis, Missouri

Advisory Panel to Building Research Division

Dr. Robert A. Hechtman, McLean, Virginia, Chairman

Mr. Edward N. Davis, Underwriters' Laboratories, Inc. Dr. J. Vincent Fitzgerald, Tile Council of America, Inc. Prof. Hoyt C. Hottel, Massachusetts Institute of Technology

Mr. William H. Lindsay, Jr., Department of Licenses & Inspections, Phila- delphia Mr. Joseph H. Newman, Tishman Research Corporation Mr. Alwin B. Newton, Borg-Warner Corporation Mr. Raymond C. Reese, Toledo, Ohio

Dean Charles E. Sehaffner, Polytechnic Institute of Brooklyn

Dr. J. A. Stavrolakis, American Standards, Inc. Mr. Herbert H. Swinburne, Nolan, Swinburne and Associates Mr. Charles H. Topping, E.I. Du Pont de Nemours & Co. Mr. T. E. Werkema, The Dow Chemical Company

169
Advisory Panel to Electronic Instrumentation Division Dr. Leon Podolsky, Pittsfield, Massachusetts, Chairman

Mr. J. A. Cafflaux, Electronic Industries Association Mr. Ralph E. Clarridge, IBM Corporation Mr. Ivan G. Easton, General Radio Company

Mr. Edward S. Hill, Metals and Controls, Inc. Dr. C. H. Hoffman, Illinois Institute of Technology

Dr. Robert Jeffries, Data Control Systems, Inc. Mr. H. J. Luer, Bell Telephone Laboratories Dr. Russell H. Lyddane, General Electric Company

Mr. John S. Norton, Honeywell, Inc. Mr. Peter R. Perino, Statham Instruments, Inc. Dr. Robert Pritchard, Stanford Electronics Laboratories Mr. Robert I. Scace, General Electric Company

Mr. Samuel H. Watson, Radio Corporation of America

Dr. Richard C. Webb, Colorado Instruments, Inc. Advisory Panel to Technical Analysis Division

Prof. Philip Morse, Massachusetts Institute of Technology, Chairman

Prof. Russell L. Ackoff, University of Pennsylvania

Prof. George B. Dantzig, Stanford University Mr. Leslie C. Edie, Port of New York Authority Mr. Martin L. Ernst, Arthur D. Little, Inc. Dr. Hugh J. Miser, The Travelers Research Center, Inc. Mr. David Novick, The Rand Corporation

Prof. Thornton L. Page, Wesleyan University

Dr. George Pettee, Research Analysis Corporation

Prof. Gustave J. Rath, Northwestern University

Prof. R. F. Rinehart, U.S. Naval Postgraduate School Advisory Panel to Center for Computer Sciences and Technology

Dr. William W. Eaton, Washington, D.C., Chairman

Mr. John Diebold, The Diebold Group, Inc. Mr. Robert B. Forest, DATAMATION Magazine

Prof. Walter F. Frese, Harvard University

Dr. Cuthbert C. Hurd, Computer Usage Company, Inc. Mr. James D. Gallagher, McCall Corporation

Dr. Adrian McDonough, University of Pennsylvania

Dr. Jack Moshman, EBS Management Consultants, Inc. Dr. Charles A. Phillips, Business Equipment Manufacturers Association

Prof. Alan J. Rowe, University of Southern California

Prof. John Tukey, Princeton University

Dr. Willis H. Ware, The Rand Corporation

Center for Radiation Research

Advisory Panel to Center for Radiation Research

Dr. Peter T. Demos, Massachusetts Institute of Technology, Chairman

Dr. John S. Blair, University of Washington

Mr. Casimer J. Borkowski, Oak Ridge National Laboratory

Dr. Marshall R. Cleland, Radiation Dynamics, Inc. Dr. Charles J. Mullin, University of Notre Dame

Dr. George F. Pieper, National Aeronautics and Space Administration

Dr. W. C. Roesch, Pacific Northwest Laboratory

Prof. Erwin F. Shrader, Case Institute of Technology

170
AWARDS AND HONORS

Recognition of the Bureau's contributions to science and technology often takes

the form of awards and honors from Government, academic, professional, and

industrial groups. The following list reflects such recognition bestowed on Bureau

staff members during fiscal year 1968 1

: Recipient

Alexander, S. N.

Astin, A. V.

Brenner, F. Cecil

Cutkosky, Robert D.

Harris, Forrest K. Hoffman, John D. Hougen, Jon T. Jensen, Malcolm W.

Marsden, Charles P., Jr. Meinke, W. Wayne

Meyerson, Melvin R.

Stiehler, Robert D.

Williams, Morgan L.

Award

Harry Good Memorial Award, American Federation of Information Processing Societies Commendation Plaque, National Conference on Weights and Measures

Distinguished Alumni Award, University of Utah Alumni Association Notable Services Award, Apparel Research

Foundation

Scientific Achievement Award, Washington

Academy of Sciences Edward Bennett Rosa Award

Samuel Wesley Stratton Award

Coblentz Society Award

Commendation Plaque, National Conference on Weights and Measures Hands of Cooperation Award, National Forest Products Association Award of Merit, American Society for Testing

and Materials

American Nuclear Society 1968 Special Award

for Industrial Applications for Radiation

Techniques

George Kimball Burgess Award, Washington

Chapter of the American Society for Metals

Award of Merit, American Society for Testing

and Materials

Bissell Award, Washington Section of the American Welding Society

EDUCATION, TRAINING, AND UNIVERSITY LIAISON

A broad employee development program, ranging from broad surveys to very

detailed treatment of a new or specialized area of research, is available to all staff members. Courses and seminars are implemented primarily through the NBS Graduate School and non-Government educational and training facilities. The programs cover education through postdoctoral research, and are offered at both the Boulder and Gaithersburg Laboratories. The primary objectives are to increase employee knowledge, skills and efficiency in assigned duties and

to prepare Bureau staff members to respond to the rapidly changing technology

at all levels. Programs also include emphasis on maintaining liaison with the

public, industry, commerce and science.

1 Commerce Department Medal Awards, previously distributed in February of eacb

year, will now be distributed in October. The 1968 listing of award recipients will appear

in the 1969 Technical Highlights.

171

320-738 0—68 12
In addition, the Bureau is becoming more and more involved with projects

in the community interest. The Hood College Program for Women at the National Bureau of Standards, supported by the National Science Foundation,

has made expert instruction and facilities available to five participating small

liberal arts colleges. A course in science of metals for high school teachers using Bureau expertise and facilities, in cooperation with the American Society for Metals was given in the Fall Semester. In addition to numerous seminars offered

at the division and institute level, there is a weekly Scientific Staff Meeting at which current topics of broad interest to the Bureau are presented. These are open to the public and are attended by members of the universities, industry

and Government community, as well as by NBS personnel. Speakers are drawn

from the outside community as well as from within the Bureau. Monthly

colloquia under the joint sponsorship of the National Institutes of Health and

the National Bureau of Standards are also offered, with each institution alter- nating as host. NBS Graduate School

The NBS Graduate School curriculum includes graduate and undergraduate

courses in the physical sciences, mathematics and specialized branches of engineering. A series of scientific colloquia and seminars designed to update and

continue the education of the postdoctoral scientist are led by research leaders from the Bureau and from other research centers and universities. In addition,

general staff development courses are offered, such as Scientific Russian, Supervision and Management, Reading Improvement, Technical Report Writing, and

administrative and clerical conferences and workshops.

Two special programs, designed for technicians and subprofessional laboratory

personnel, offer courses both in-house and in cooperation with the Montgomery

Junior College leading to two NBS Technician Certificates and/or the A. A. degree at the Montgomery Junior College. Surveys periodically redetermine

course offerings and keep the program in step with the changes and variations

in educational requirements and the changing technology. Graduate degrees

based partly on credit obtained for courses or thesis research carried on under

the NBS Graduate School Program have been earned by 4 Bureau employees

this year, bringing the total to 346 graduate degrees earned at 45 different universities since the establishment of the educational program in 1908. The Graduate School at Boulder is associated with the University of Colorado

in a Joint-Course program and Adjunct Professor Plan. Various graduate depart- ments of the NBS Graduate School at Boulder and the University offer courses which mutually benefit the Government and the University.

Postdoctoral Research Associateships

The National Bureau of Standards, in cooperation with the National Research

Council, National Academy of Sciences-National Academy of Engineering, offers a number of awards for postdoctoral research. These awards provide young scientists of unusual ability and promise an

opportunity for fundamental research in various branches of the physical,

engineering, and mathematical sciences. Applications are evaluated by a Board

of Selection appointed by the National Research Council. The NRC-NBS Post- doctoral Research Associateship program has been in existence since 1954. There

have been 173 awards made during these years ; currently there are 26 in residence. 172
Postdoctoral Research Associates on Duty During Fiscal Year 1968

NAME UNIVERSITY NBS ADVISER

Anderson, Robert u. oi KsdiLii. ^-DerKtuey^ T. Carrington

Balling, Ludwig TTJxI V <XL LI Jtt. u. Mockler

oanni, ivevni TTTlcll Q T\7"Q V Vf\ dbx LI o. lviesnKov Cooper, Martin Brandeis University TV /T O M. fe. Ureen

Davis, Douglas TT\J . nfUl -TlUllUd Florin a TT TT Aun

±1. is.. Ukabe

DeLancey, George TTu. nfoi xibtbijurgn PH+oViiiT-trh ±1. User

Duerst, Richard U. Ul v^ellll. V, JJtJX ft. cloy ) U. ±» . Kokoszka

Ensign, Thomas yj . ui vv y uiiniig l. Unang

f lCKext, -f reaericK L/lcgUIl kjlid/Lc U 111 V cl 31

u

y sx. Jrowell Fong, Jeffrey Stanford University TT „„ 11. User

uroiuD, otepnen KyULHilLUlcX \J 111 V cl bl \jy r>. ioiemer Gould, Harvey TTu. nfoi Palif v^aiii. fRorlrolo^ ^jjerKeiey^ burner Greenhouse, Jeffrey u. oi v^am. ^JDerKeiey,/ W.J. L/anerty

Hadley, Steven u. oi v^aiii. ^-L/avisj T> TT/->ll^-« K. Heller

Hartl, Werner Columbia University K. Howard

Hettche, Leroy Carnegie L. Irwin

Hoegy, Walter U. of Michigan i\/r M. cb. Ureen

ixeiiy, lvODerir ju. u. oi oani. ^-DerKeieyj U. iviuehlhause Latanision, Ronald Ohio State University A. W. Kurt

McAlister, Archie TTu . nfoi 1\iviaryianci To T*T/1 Q 11 A j . uutniii

Miller, Tvennetn Iowa State University M. Krauss Manson, Steven Columbia University A. W. Weiss

Negas, Taki Ohio State University K. fe. Kotn

Osgood, Charles TT nf Polif ^"RQT.VolmT^ u. oi v^ani. ^.DerKeiey; M. Newman

Parke, William George Washington University T> WJ TT ^. TT^n.rl K. w. Mayward

Pechukas, Philip U. of Chicago onuier

Plummer, Earl Cornell University K. JJ. Young

Pong, William U. of Cincinnati T? "P 1\/Tq /-Irlckn XV. Jr. lviaaaen

Ponzini, Robert Michigan State University G TV/Too Ti \r mr C5. IVieSllKOV Pringle, Wallace tx/tthp IVll 1 W.J. Liaiierty

Radebaugh, Ray Purdue University JJ. Uhelton

Raveche, Harold TT nf r^oli'fn^m' o (1 o Tnll a 1 u. oi ^aniornia ^.L/ajoiia,/ ±v. onuier

Retajczyk, Theodore tx/tthp IVll 1 J . 1 aylor

Robertson, Baldwin Washington University K. KuDin

Shirk, James u. oi uani. ^rserKeiey; A TV IT *D«*-i« A. M. ±3ass Stemmler, Rosemarie U. of Illinois M. Newman

SnlliTravi OU.111 V <xll, Tlnnalrl T-JUIldlU ~\7 Ck T\ r\ PvTlllt" TTv»1'\fO'rC31'f"\7' v txiiLici uii v yj in v ci si \jy T?TV. rV. A 1\TVdlllJJtJI QTnnor

Sullivan, Peter Rensselaer Polytechnic Inst. J. D. Hoffman

Veillon, Claude U. of Florida M. Margoshes

Weisman, Irwin U. of California (Berkeley) L. H. Bennett

Williams, Harry U. of Virginia M. Danos

Zalewski, Edward U. of Chicago R. A. Keller Non-Government Education

Non-Government education falls into three categories . . . full-time (3 to 12 months) graduate study and research assignments at universities and research

centers; full-time (less than 3 months) attendance at institutes, seminars, short concentrated courses and workshops ; and part-time, job related academic

courses at universities and in industry. In the last year 452 staff members at Washington and Boulder were trained through non-Government facilities, and

173
13 career employees were selected for full-time graduate study or research as- signments at universities and research centers. Participants in approved full- time training programs receive full salary and expenses, including tuition, fees, travel, and per diem, as well as transportation of family and household effects. In addition, 434 staff members, mostly from technical divisions, attended job- related courses on a semester basis, and shorter concentrated courses at universities and in industry.

Interagency Training

Courses made available through the Interagency Training Programs are an

additional effective means of improving program operations for NBS personnel. Courses are offered at Government facilities in Supervision, Management, Office Skills and Practices, and specialized programs. This pooling of agency resources

offers broader employee development opportunities at a saving to the Government. During 1968, 212 National Bureau of Standards employees took advantage of the interagency offerings.

PUBLICATIONS*

PUBLICATIONS IN THE BUREAU'S SERIES

During the year NBS publications totaled 998 published papers and

documents.

Of the formal publications, 111 appeared in the Journal of Research,

and 546 in the journals of professional and scientific societies. Also,

249 summary articles were presented in the Bureau's monthly

Technical News Bulletin.

In the nonperiodical series, 86 documents were published : 10 in the

Monograph series, 3 in the Handbook series, 11 in the Miscellaneous

Publication series, 3 in the Special Publication series, 44 in the Technical Note series, 11 in the National Standard Reference Data Series,

and 7 in the Building Science Series.

Journal of Research. Contains full research papers, including laboratory data,

experimental procedures, and theoretical and mathematical analyses. Advances

in measurement standards and techniques . . . physical constants . . . properties of materials . . . instrumentation . . . radio propagation.

The Journal is published in three separate sections . . . A. Physics and Chemistry, issued six times a year. Annual subscription : Domestic, $6 ; foreign, $7.25 ; single copy, $1.00. B. Mathematical Sciences (Name changed from Mathematics and Mathematical

Physics to Mathematical Sciences effective January 1968), issued quarterly.

Annual Subscription : Domestic, $2.25 ; foreign, $2.75 ; single copy, 75 cents.

C. Engineering and Instrumentation, issued quarterly. Annual subscription:

Domestic, $2.75 ; foreign, $3.50 ; single copy, 75 cents. Publications for which a price is indicated are available by purchase from

the Superintendent of Documents, U.S. Government Printing Office, Washington,

D.C. 20402 (foreign postage, one-fourth additional). The NBS non-periodical

series are also available from the Clearinghouse for Federal Scientific and Technical Information, Springfield, Va. 22151. Reprints from outside journals and

the NBS Journal of Research may often be obtained directly from the authors

174
Volume 71A (Phys. and Chem.), No. 4 (July-Aug. 1967)

Kinetics of crystallization in multicomponent systems: I. Binary mixtures of

w-paraffins. John I. Lauritzen, Jr., Elio Passaglia, and E. A. DiMarzio.

Kinetics of crystallization in multicomponent systems : II. Chain-folded polymer

crystals. John I. Lauritzen, Jr., and Elio Passaglia. Infrared absorption spectra of 2-oxo-l, 3-bis(phenylhydrazono) derivatives and

related bis- and tris-phenylhydrazones. Alexander J. Fatiadi.

Dielectric constant of n-hexane as a function of temperature, pressure, and

density. Frederick I. Mopsik. Heat capacities and related thermal data for diethyl phthalate crystal, glass,

and liquid to 360 °K. S. S. Chang, J. A. Horman, and A. B. Bestul. Heats of formation of aluminum diboride and a-aluminum dodecaboride. Eugene

S. Domalski and George T. Armstrong.

Effect of environment upon the melting point of A1203. S. J. Schneider and C. L. McDaniel.

Volume 71A (Phys. and Chem.), No. 5 (Sept.-Oct. 1967)

Zeeman effect in positronium annihilation at low temperatures. William C. Saunder and Richard D. Deslattes. Surface-layer relaxation in the dielectric spectrum of CaF2 doped with GdF8. A. D. Franklin, S. Marzullo, and J. B. Wachtman, Jr. Thermal expansion of rutile from 100 to 700 °K. Richard K. Kirby.

Mass spectrometric study of photoionization. VII. Nitrogen dioxide and nitrous

oxide. Vernon H. Dibeler, James A. Walker, and Susan K. Liston. Ionization constants of substituted benzoic acids in ethanol-water. G. M. Brauer,

George Durany, and Harold Argentar.

Dissociation constants of some substituted nitrophenols in aqueous solution at 25 °C. R. A. Robinson.

Volume 71A (Phys. and Chem.), No. 6 (Nov.-Dec. 1967)

William Frederick Meggers, A Tribute. Karl G. Kessler. The second spectrum of ytterbium (Yb n). W. F. Meggers. (Edited by Charlotte

E. Moore.)

An improved description of technetium spectra (Tc I and Te n), 2000 to 9000 A. W. R. Bozman, W. F. Meggers, and C. H. Corliss. Lifetimes of energy levels in neutral iron. C. H. Corliss and J. L. Tech.

Transition probabilities in argon I. C. H. Corliss and J. B. Shumaker, Jr. The fifth spectrum of praseodymium. Victor Kaufman and Jack Sugar.

Fundamental energy levels of neutral promethium (Pm i). Joseph Reader and

Sumner P. Davis. Volume 72A (Phys. and Chem.), No. 1 (Jan.-Feb. 1968)

Reactions of uranium with the platinide elements. I. The uranium-ruthenium

system. John J. Park. Reactions of uranium and the platinide elements. II. The uranium-rhodium

system. John J. Park. Reactions of uranium and the platinide elements. III. The uranium-iridium

system. John J. Park and Lyle R. Mullen. Phase relations between palladium oxide and the rare earth sesquioxides in air. C. L. McDaniel and S. J. Schneider. Preparation and purification of some oxidation products of perylene. Alexander J. Fatiadi. 175
Electron spin resonance spectra of polymer radicals in aqueous solution. Roland

E. Florin, Fred Sicilio, and Leo A. Wall. A mass spectromemtric study of the BeO-BeF2 system at high temperatures.

J. Efimenko. Laser induced Roman spectra of some tungstates and molybdates. R. K. Khanna,

W. S. Brower, B. R. Guscott, and E. R. Lippincott.

Valence—only correlation in LiH and BeH+. W. A. Sanders and M. Krauss. Thermalization by elastic collisions : positronium in a rare gas moderator. William C. Sauder. Density fluctuations in fluids having an internal degree of freedom. Raymond

D. Mountain.

Volume 72A (Phys. and Chem.), No. 2 (Mar.-Apr. 1968)

Constant pressure flame calorimetry with fluorine II. The heat of formation

of oxygen difluoride. Reatha O. King and George T. Armstrong.

The heat of formation of boron carbide. E. S. Domalski and G. T. Armstrong.

Solubility of tris(hydroxymethyl)aminomethane in water-methanol solvent mixtures and medium effects in the dissociation of the protonated base. Paul

Schindler, R. A. Robinson, and Roger G. Bates. Calibration of the nickel dimethylglyoxime spectral shift at pressures to 20

kilobars for use in spectroscopic pressure measurement. Helen W. Davies. Second virial coefficient of He4 in the temperature range from 2 to 20 °K. Marjorie E. Boyd, Sigurd Y. Larsen, and Harmon Plumb.

Diffusion rates in inorganic nuclear materials. A. L. Dragoo.

Effect of oxide additions on the polymorphism of tantalum pentoxide. (system Ta205-Ti02 ) . J. L. Waring and R. S. Roth.

Effect of statistical counting errors on wavelength criteria for x-ray spectra. John S. Thomsen and F. Y. Yap.

Thermodynamic properties of ammonia as an ideal gas. Lester Haar. Volume 72A (Phys. and Chem.), No. 3 (May-June 1968)

Jump rates for point defects in special positions held by a trapping center of noncubic symmetry. H. S. Peiser and J. B. Wachtman, Jr. The thermodynamics of the ternary system : water-potassium chloride-calcium

chloride at 25 °C. R. A. Robinson and A. K. Covington. Force field for SiF4. Ira W. Levin and Stanley Abramowitz.

Blemish formation in processed microfilm. C. I. Pope. Absolute isotopic abundance ratios of common, equal-atom, and radiogenic lead

isotopic standards. E. J. Catanzaro, T. J. Murphy, W. R. Shields, and E. L. Garner. Role of nickel in Al-10 percent Si composites containing nickel-coated sapphire

whiskers. H. Yakowitz, W. D. Jenkins, and H. Hahn.

Volume 71B (Math, and Math. Phys.), No. 2 and 3 (Apr.-Sept. 1967)

Poineare's conjecture is amplified by a conjecture on free groups. Roger D. Traub.

Construction of EPr generalized inverses by inversion of nonsingular matrices. John Z. Hearon. A generalized matrix version of Rennie's inequality. John Z. Hearon.

Polar factorization of a matrix. John Z. Hearon. Two classical theorems on commuting matrices. Morris Newman.

A converse to Banach's contraction theorem. Philip R. Meyers,

^-transforms (II). F. M. Ragab.

176
Criterion for the stability of numerical integration methods for the solution of systems of differential equations. Abbas I. Abdel Karim.

Discrete complex functions with prescribed boundary values and residues. Elmor L. Peterson. Numerical solution of second-order linear difference equations. F. W. J. Olver.

Indefinite integrals involving Bessel functions. B. A. Peavy.

Volume 71B (Math, and Math. Phys.), No. 4 (Oct.-Dec. 1967)

Calibration designs based on solutions to the tournament problem. R. C. Bose and J. M. Cameron. Bounds for the solutions of second-order linear difference equations. F. W. J. Olver. Notes on automorphic functions : An entire automorphic form of positive dimension is zero. Marvin I. Knopp.

Solving equations exactly. Morris Newman.

A system of equations having no nontrivial solutions. Hansraj Gupta.

Remarks on cut-sets. J. W. Grossman. A pseudo primal-dual integer programming algorithm. Fred Glover. Properties of a useful biorthogonal system. L. V. Spencer and P. Flusser. On even matroids. W. T. Tutte. Matrices of class J2. John S. Maybee.

Partially isometric matrices. John Z. Hearon. Symmetrizable generalized inverses of symmetrizable matrices. John Z. Hearon. Optimum branchings. Jack Edmonds.

Systems of distinct representatives and linear algebra. Jack Edmonds.

Bounds for the number of generators of a finite group. Morris Newman.

Volume 72B (Math. Sci.), No. 1 (Jan.-Mar. 1968)

Means and the minimization of errors. Michael Aissen. On Taylor's theorem. O. Ohisha.

Principal submatrices III : Linear inequalities. R. C. Thompson.

The diophantine equation P(co, y) = (xy-\-d)z. Charles F. Osgood.

A note on the G-transformation. H. L. Gray and T. A. Atchison. The distribution of the sample correlation coefficient with one variable fixed. David Hogben.

Solutions of the time-dependent Klein-Gordon and Dirac equations for a uniform

electric field. Vernon W. Myers.

Analysis of a market split model. J. M. McLynn, A. J. Goldman, P. R. Meyers,

and R. H. Watkins.

Citation searching and bibliographic coupling with remote on-line computer access. Franz L. Alt and Russell A. Kirsch. Simple analytic expressions for the total Born approximation cross section for pair production in a coulomb field. L. C. Maximon.

Volume 72B (Math. Sci.), No. 2 (Apr.-June 1968)

The probability of an equilibrium point. K. Goldberg, A. J. Goldman, and M. Newman.

On spaces and maps of generalized inverses. John Z. Hearon and John W. Evans.

Differentiate generalized inverses. John Z. Hearon and John W. Evans.

Principal submatrices V: Some results concerning principal submatrices of ar- bitrary matrices. R. C. Thompson.

Mathematical basis for the plasma kinetic equations (BBGKY). John J. Sopka.

177
On the diffusion of an ion sheet in Poiseuille flow. Stephen Jarvis, Jr. A class of thickness-minimal graphs. Arthur M. Hobbs and J. W. Grossman. Volume 71C (Engr. and Instr.), No. 3 (July-Sept. 1967)

Procedure for high precision density determinations by hydrostatic weighing. Horace A. Bowman and Randall M. Schoonover with Appendix by M. W.

Jones. Study of the storage stability of the barium fluoride film electric hygrometer

element. Frank E. Jones. Torsion creep of circular and noncircular tubes. Leonard Mordfin.

Digitized low-frequency phasemeter assembled from logic modules. John E. McKinney.

Volume 71C (Engr. and Instr.), No. 4 (Oct.-Dec. 1967) Measurements of the thermal conductivity and electrical resistivity of platinum

from 100 to 900 °C. D. R. Flynn and M. E. O'Hagan.

Thermal conductivity and electrical resistivity of Armco iron. T. W. Watson,

D. R. Flynn, and H. E. Robinson.

Heat flow in a right circular cylinder with internal heat generation—applica- tions to the determination of thermal conductivity. D. R. Flynn.

Radiation-induced acoustic cavitation ; apparatus and some results. Martin

Greenspan and Carl E. Tschiegg.

Design of a new Kossel pattern generator. D. L. Vieth and H. Yakowitz.

The near-zone magnetic field of a small circular-loop antenna. Frank M. Greene. Volume 72C (Engr. and Instr.), No, 1 (Jan.-Mar. 1968)

Acceleration due to gravity at the National Bureau of Standards. D. R. Tate. Deflection of thin circular elastic plates under symmetrically distributed loading. A. F. Kirstein and R. M. Woolley.

A dynamic method for determining the vapor pressure of carbon dioxide at 0

°C. J. L. Edwards and D. P. Johnson. An adiabatic saturation psychrometer. Lewis Greenspan and Arnold Wexler. An injection method for self-calibration of inductive voltage dividers. Wilbur

O. Sze. Bolometric voltage and current (Bolovac) standard for high and microwave

frequencies. M. C. Selby.

An admittance meter technique to measure the complex permeability at VHF.

A. L. Rasmussen and 0. M. Allred. Volume 72C (Engr. and Instr.), No. 2 (Apr.-June 1968)

Analysis and design of an oscilloscope deflection system with a calculable trans- fer function. D. M. Stonebraker. Calculation of substitution error in barretters. Stephen Jarvis, Jr., and John W.

Adams.

Analysis of n-degree elliptical elastic rings of nonuniform cross section. R. A.

Mitchell. Applications of coaxial chokes to a-c bridge circuits. D. N. Homan.

Creep rupture properties of Ti-8Al-lMo-IV alloy. W. D. Jenkins and W. A. Willard. TecJmiccU News Bulletin. This monthly publication summarizes the current

research, development, and test activities of the Bureau. The articles are brief, with emphasis on the results of research and their significance, chosen for their 178
importance to other scientists, engineers, and to industry. Resumes of longer research reports, important national and international conferences on funda- mental science in which the Bureau has represented the Nation, and bibliography

of all publications by members of the staff as published are included. The Bulletin is designed to give a succinct account of the current work of the Bureau. (Annual subscription: domestic, $3.00; foreign, $4.00.)

Monographs. These are usually contributions to the technical literature which

are too lengthy for publication in the Journal of Research. They often provide

extensive compilations of information on subjects related to the Bureau's technical program. Until July 1959 most of this type of material was published in the Circular series.

25. Section 5. Swanson, H. E., McMurdie, H. F., Morris, M. C, Evans, E. H., Standard x-ray diffraction powder patterns. August 31, 1967. 55 cents.

32. Supplement. Corliss, C. H., Revision of the NBS tables of spectral-line intensities below 2450 A. July 7, 1967. 30 cents.

35. Supplement 1. Brombacher, W. G., Bibliography and index on vacuum and

low pressure measurement January 1960 to December 1965. May 31, 1967. 65 cents.

101. Reed, R. P., Mikesell, R. P., Low temperature mechanical properties of copper and selected copper alloys, a compilation from the literature. Dec. 1, 1967. $2.75. 102. Peterson, R. L., Effects of finite lattice heat capacity on spin lattice relaxation, theory and numerical analysis. Aug. 1, 1967. 25 cents.

103. Pontius, P. E., Cameron, J. M., Realistic uncertainties and the mass meas- urement process, an illustrated review. Aug. 15, 1967. 20 cents.

104. Nimeroff, I., Colorimetry. Jan. 1968. 35 cents. Supersedes Circular 478.

106. Rosenberg, S. J., Nickel and its alloys. May 1968. $1.25. (Supersedes NBS

Circular 592.)

108. Corliss, C. H., Tech, J. L., Oscillator strengths and transition probabilities for 3288 lines of Fe I. Mar. 1968. 45 cents.

110. Tipson, R. S., Infrared spectroscopy of carbohydrates, a review of the litera- ture. June 1968. 30 cents. Handbooks. These are recommended codes of engineering and industrial practices, including safety codes, developed in cooperation with the national organizations and others concerned. In many cases the recommended requirements are given official status through their incorporation in local ordinances by State and municipal regulatory bodies.

81. Supplement 2. Safety rules for the installation and maintenance of electric supply and communication lines. Mar. 1968. 5 cents. 103. Moffitt, J. K, Tabulation of data on receiving tubes. Sept. 29, 1967. $1.25.

( Supersedes Handbook 83.

)

104. Moffitt, J. K., Tabulation of data on microwave tubes. Sept. 29, 1967. $1.25.

( Supersedes Handbook 70.) Special Publications. (Formerly Miscellaneous Publications.) As the name implies, this series provides material of a particular nature and quality in fields of the Bureau's competence. It includes proceedings of NBS-sponsored national and international conferences devoted to the state-of-the art, as well as precision measurement and calibration volumes, NBS Research Highlights, and other

special publications appropriate to this grouping.

179
250. 1968 edition. Mason, H. L., Editor, Calibration and Test Services of the National Bureau of Standards, May 1968. $1.75. Supersedes Misc. Publ. 250, 1965 edition. 295. Lee, R. W., Worral, R. W., Ed., Electronic composition in printing, pro- ceedings of a Symposium held at the National Bureau of Standards June 15-

16, 1967. Feb. 1968. 70 cents. 297. Koeser, R. L., Editor, Report of the 52d National Conference on Weights

and Measures 1967. May 1968, $1.25. Miscellaneous Publications

260. 1968 Edition. Standard Reference Materials: Catalog and price list of standard materials issued by the National Bureau of Standards. Jan. 31, 1968. 45 cents. (Supersedes Misc. Publ. 260—1967 Edition.) 260-13. Spijkerman, J. J., Snediker, D. K., Ruegg, F. C, DeVoe, J. R., Standard

Reference Materials : Mossbauer spectroscopy standard for the chemical shift iron compounds. July 28, 1967. 40 cents. 260-15. Passaglia, E., Shouse, P. J., Standard Reference Materials : Recom- mended method of use of standard light-sensitive paper for calibrating carbon

arcs used in testing textiles for colorfastness to light. July 21, 1967. 20 cents. 277 Supplement 1. Photonuclear data index, January 1965 through April 1967.

Oct. 1967. 45 cents. 278 Supplement. Glennon, B. M., Wiese, W. L., Bibliography on atomic transition

probabilities May 1966 through December 1967. April 1968. 30 cents. 287. Franklin, A. D., Editor, Calculation of the properties of vacancies and

interstitials, proceedings of a conference Shenandoah National Park, Va. May

1-5, 1966. Nov. 17, 1967. $2.50. 288. Hartman, J. E., Directory of United States standardization activities. Aug.

1, 1967. $2.00. (Supersedes Misc. Publ. 230.)

291. Proceedings of the 1966 standards laboratory conference. May 9-12, 1966, Gaithersburg, Maryland. July 13, 1967. $1.00. 292. Stern, K. H., Bibliography of Liesegang rings (second edition). Sept. 1, 1967. 40 cents. 293. Technical highlights of the National Bureau of Standards, Annual Report

1967. Nov. 1967. 55 cents. 294. Joseph, J. A., Editor, Operations research, proceedings of a conference for Washington area government agencies, April 20, 1966 held at Museum of Natural History, Smithsonian Institution, Washington, D.C. Dec. 1967. 25 cents. National Standard Reference Data Series. NSRDS provides quantitative data on the physical and chemical properties of materials, compiled from the world's

literature and critically evaluated. Reports fall into eight categories: general; nuclear properties ; atomic and molecular properties ; solid state properties

;

thermodynamic and transport properties ; chemical kinetics ; colloid and surface

properties ; and mechanical properties of materials.

3. Section 2. Moore, C. E., Selected tables of atomic spectra ; atomic energy

levels and multiplet tables ; Si I. Nov. 30, 1967. 20 cents.

9. Trotman-Dickenson, A. F., Milne, G. S., Tables of bimolecular gas reactions.

Oct. 27, 1967. $2.00.

10. Nelson, R. D., Jr., Lide, D. R., Jr., Maryott, A. A., Selected values of electric dipole moments for molecules in the gas phase. Sept. 1, 1967. 40 cents. ( Supersedes the data on dipole moments included in Circular 537)

.

11. Shimanouchi, T., Tables of molecular vibrational frequencies, Part 2. Oct. 1967. 30 cents. 180
12. Schwendeman, R. H., Tables for the rigid asymmetric rotor : transformation

coefficients from symmetric to asymmetric bases and expectation values of Pa2

, PE

4

, and Pz6

. June 1968. 60 cents.

13. Horiuti, J., Miyahara, K, Hydrogenation of ethylene on metallic catalysts. June 1968. $1.00.

14. Bearden, J. A. X-ray wavelengths and x-ray atomic energy levels. Sept. 25, 1967. 40 cents.

16. Ho, O. Y., Powell, R. W., Liley, P. E., Thermal conductivity of selected materials, Part 2. Feb. 1968. $2.00.

17. Shimanouchi, T., Tables of molecular vibrational frequencies, Part 3. Mar.

1968. 30 cents.

18. Furukawa, G. T., Saba, W. G., Reilly, M. L., Critical analysis of the heat- capacity data of the literature and evaluation of thermodynamic properties

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Alley, C. O., Bender, P. L., Information obtainable from laser range measure- ments to a lunar corner reflector, Book, IAU-IUGG Symposium 32 on Continental Drift, Secular Motion of the Pole, and Rotation of the Earth, 32, 86-90

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1963, pp. 815-821 (Natl. Assoc. Corrosion Engr., Houston, Tex., 1966).

Arenhovel, H., Hayward, E., Scattering of plane polarized photons by the giant resonances of nuclei, Phys. Rev. 165, No. 4, 1170-1174 (Jan. 20, 1968).

Armstrong, G. T., Calorimetry, Encyclopaedic Dictionary of Physics, 2d Supplementary Volume, pp. 1-8 (Pergamon Press Inc., New York, N.Y., Oct.

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Co., New York, N.Y., 1967). Armstrong, R. W., NBS dynamic seat belt tester, Proc. 10th Stapp Car Crash

Conf., 6571st Aeromedical Research Laboratory, Alamogordo, N. Mex., Nov. 8-9, 1966, pp. 38-45 (Society of Automotive Engineers, New York, N.Y.,

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Astin, A. V., Standards of Measurement, Sci. Am. 218, No. 6, 50-62 (June 1968)

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Ausloos, P., Lias, S. G., Gas-phase radiolysis of hydrocarbons, Book, Actions

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1967) . Ausloos, P., Lias, S. G., Photoionization of cycloalkanes in the gas phase. A study

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England, 1967).

Ausloos, P., Scala, A. A., Lias, S. G., Ion-molecule reactions in the condensed-phase

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Barbrow, L. E., The metric system in illuminating engineering, Ilium. Engr. 63, No. 11, 638-640 (Nov. 1967).

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Frequency 5, No. 6, 15-20 (Nov-Dec. 1967). Bates, R. G., Hydrogen-ion concentration, Encyclopedia of Chemical Technology,

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(Feb. 1, 1968). Bean, B. L., A method of producing sturdy specimens of pressed powders for use

in X-ray spectrochemical analysis, Appl. Spectry. 20, No. 3, 191-193 (MayJune 1966). Bean, B. R., Warner, B. D., Some radio-physical considerations in studies of the

fine scale structure of the atmosphere, Proc. Intern. Conf. Fine Scale Structure

of the Atmosphere, Moscow, USSR, June 1965, pp. 215-224 (1965). Beaty, E. C, Patterson, P. L., Mobilities and reaction rates of neon ions in neon, Phys. Rev. 170, No. 1, 116-121 (June 5, 1968).

Beckett, C. W., Status of properties research in the kilodegree range, Book, The

Characterization of High-Temperature Vapors, Ed. J. Margrave, Chap. 1, pp. 3-15 (John Wiley & Sons Inc., New York, N.Y., 1967). Bekkedahl, N., Crystallization of natural rubber, Rubber Chem. Technol. 40, No. 3, xxv-vlvii (June 1967). Bender, P. L., Laser measurements of long distances, Proc. IEEE 55, No. 6, 1039-1045 (June 1967).

Bender, P. L., Radio reflection by free radicals in earth's atmosphere, Science 158, No. 3807, 1487-1488 (Dec. 15, 1967).

Bennett, H. S., F center in ionic crystals: semi-continuum polaron models, Phys.

Rev. 169, No. 3, 729-745 (May 15, 1968).

Bennett, J. A., To avoid fatigue failures, pay attention to details, Current Engr.

Pract. 9, 12-16 (Sept. 1966).

Bennett, L. H., Swartzendruber, L., Watson, R. E., Hyperfine fields and electronic structure of CsCl type ternary alloys of the first transition series, Phys. Rev.

165, No. 2, 500-505 (Jan. 10, 1968).

Bennett, L. H., Nuclear magnetic resonance in sodium thallide, Acta Met. 14, No. 8, 997-999 (1966). Bennett, L. H., Nuclear magnetic resonance in zintl intermediate phases LiCd

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Berendt, R. D., Winzer, G. E., Burroughs, C. E., A guide to airborne, impact and

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Berger, M. J., Energy deposition in water by photons from point isotropic sources,

J. Nucl. Med. Suppl. 1, 15-25 (Feb. 1968).

Berman, H. A., West, E. D., Rosner, A. G., Anomalous heat capacity of TiNi,

J. Appl. Phys. 38, No. 11, 4473-4476 (Oct. 1967).

Bevan, A. W., Jr., Daniel, A. C, Mahler, R. J., Indication of the effect of a magnon

energy gap on the 19 F relaxation rate in antiferromagnetic CoF2 , Physics

Letters 25A, No. 7, 555-556 (Oct. 9, 1967).

Billick, I. H., Dishon, M., Weiss, G. H., Yphantis, D. A., Numerical solutions of the Lamm equation. IV. Rotor slowing experiments, Biopolymers 5, 1021-1028

(1967).

Billick, I. H., Schulz, M., Weiss, G. H., Quasi-equilibrium sedimentation experi- ments with rotor deceleration, J. Phys. Chem. 71, No. 8, 2496-2502 (July 1967)

.

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Blandford, J. M., A progress report on the NBS-ARF apparel materials evaluation

project, First Annual Conf. Apparel Research Foundation, Washington, D.C., Nov. 29-Dec. 1, 1967 (Apparel Research Foundation, Washington, D.C.,

20036, 1967).

Bleicher, M. N., Knopp, M. I., Lattice points in a sphere, Acta Arith. X, 369-376,

(1965).

Bloss, R. L., The measurement of strain, (Proc. 22nd Annual ISA Conf. Chicago,

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Bowen, R. L., Development of an adhesive restorative material, (Proc. 2nd

Workshop, Adhesive Restorative Dental Materials, University of Virginia,

Charlottesville, Va., Dec. 8-9, 1965), Book, Adhesive Restorative Dental

Materials, No. 2, Chapt. 4, p. 225 (U.S. Public Service Publ. 1494, Superin- tendent of Documents, U.S. Government Printing Office, Washington, D.C.,

20402, 1966, $1.00).

Bowen, R. L., Argentar, H., Diminishing discoloration in methacrylate accelerator systems, J. Am. Dental Assoc. 75, No. 4, 918-923 (Oct. 1967).

Bowman, H. A., Gallagher, W., Schoonover, M. R., The development of a working

density standard (Proc. 20th Annual ISA Conf., Oct. 4-7, 1965). Bowman, R. R., Remarks on the paper "Field strength above 1 GHz: Measure- ment procedures for standard antennas", Proc. IEEE 53, No. 2, 216 (Feb.

1968). Bozman, W. R., The application of computers in printing scientific manuscripts,

Book, New Techniques in Office Operations, Chapt. 13, pp. 120-124 (The

Business Press, Elmhurst, 111., Mar. 1968). Brady, E. L., Wallenstein, M. B., The National Standard Reference Data System,

Science 156, No. 3776, 754-762 (May 12, 1967)

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Frady, G., Mclntyre, D., Myers, M. E., Jr., Wims, A. M., Critical scattering of perfluoroheptane-isooctane system, (Proc. Conf. Small-angle X-ray Scattering,

Syracuse University, Syracuse, N.Y., June 1965), Book, Small-angle X-ray

scattering, Ed. H. Brumberger, pp. 425-448 (Gordon and Breach, Science

Publ., Inc., New York, N.Y., 1967).

Branscomb, L. M., The misinformation explosion: Is the literature worth reviewing? Sci. Res. 3, No. 11, 49-56 (May 1968).

Branscomb, L. M., The role of atomic collision processes in astrophysics, Book,

The Physics of Electronic and Atomic Collisions: Invited Papers from the

Fifth International Conference, Leningrad, U.S.S.R., July 17-22, 1967, Ed.

L. M. Branscomb, pp. 12-31 (Joint Institute for Laboratory Astrophysics,

University of Colorado, Boulder, Colo., 1968).

Branscomb, L. M., Twenty years of physics: Atoms, molecules, and electrons, Phys. Today 31, No. 5, 36-39 (May 1968).

Brauer, G. M., New developments in zinc oxide-eugenol cement, Ann. Dentistry

26, No. 2, 44-50 (June 1967).

Braun, W., Lenzi, M., Resonance fluorescence method for kinetics of atomic

reactions. Reactions of atomic hydrogen with olefins, Discussions Faraday

Soc. 44, 252-262 (June 1967).

Breen, D. E., Keller, R. A., Intramolecular energy transfer between triplet states of weakly interacting chromophors. I. Compounds in which the chromophors

are separated by 1,2, and 3 methylene groups, J. Am. Chem. Soc. 90, No 8, 1935-1940 (Apr. 10, 1968).

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Brehm, B., Gusinow, M. A., Hall, J. L., Electron affinity of helium via laser photodetacbment of its negative ion, Phys. Rev. Letters 19, No. 13, 737-741

(Sept. 25, 1967).

Brenner, A., Metzger, W. H., Jr., Determination of the composition of complexes

and their instability constants by calorimetry. III. The complex in fuzed sodium

molybdate and molybdenum trioxide, J. Electrochem. Soc. 115, No. 3, 258-261

(Mar. 1968).

Bridges, J. M., Wiese, W. L., Comparison of the Stark widths of the Balmer

lines H0 and Ha, Proc. Seventh Intern. Conf. Phenomena in Ionized Gases, Ed. B. Perovic and D. Tosic, III, 165-167 (Gradevinska Knjiga Publ. Co., Belgrad, Yugoslavia, 1966).

Bridges, J. M., Wiese, W. L., Experimental determination of transition probabilities and Stark widths of S I and S II lines, Phys. Rev. 159, No. 1, 31-38 (July 5, 1967).

Broberg, J., Leiss, J., Scrack, R. A., Wyckoff, J. M., On-line handling system for the NBS linac, IEEE Trans. Nucl. Sci. NS-11, No. 3, 331-337 (June 1964).

Brombacher, W. G., 40 years of precise measurement, Instr. Control Systems 40? No. 9, 87-92 (Sept. 1967).

Brooke, R. L., Cruz, J. E., Current distribution and impedance of lossless con- ductor systems, IEEE Trans. Microwave Theory Tech. MTT-15, No. 6, 358-364 (June 1967).

Brown, D. W., Wall, L. A., The radiation-induced copolymerization of tetra- fluoroethylene and 3,3,3-trifluoropropene at high pressure, J. Polymer Sci. Part A-l. Polymer Chemistry 6, No. 5, 1367-3179 (May 1968).

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Brown, R. L., Brennen, W. R., Spin-relaxation effects on the EPR spectrum of gaseous nitrogen atoms, J. Chem. Phys. 47, No. 11, 4697-4705 (Dec. 1, 1967).

Brown, R. L., Dittmann, S., Vibrational relazation and quenching in the yellow

nitrogen afterglow, Chem. Commun. 21, 1144-1146 (Nov. 8, 1967).

Brown, W. E., A mechanism for growth of apatitic crystals (Proc. Intern. Symp.

Composition Properties and Fundamental Structure of Tooth Enamel, London,

England, Apr. 1964), Book, Tooth Enamel, pp. 11-14 (John Wright and Sons,

Ltd., Bristol, England, 1965).

Brualdi, R. A., Newman, M., Proof of a permenental inequality, Quart. J. Math.

17, No. 67, 234-238 (Sept. 1966).

Bullis, W. M., Coleman, J. A., Characterization of germanium and silicon for nuclear radiation, Book, Nucleonics in Aerospace, Ed. P. Polishuk, pp. 166-175

(Plenum Press Inc., New York, N. Y., 1968).

Bur, A. J., Roberts, D. E., High polymeric materials, 1964 Digest of Literature on Dielectrics 38, 231-260 (National Academy of Sciences-National Research

Council, Washington, D.C., 1964).

Burley, G., The "memory effect" in silver iodide, Acta Cryst. 23, Part 1, 1-5

(July 1967).

Bussey, H. E., Instrumentation and measurement, Digest of Literature on

Dielectrics Publ. No. 1496, 30, 1-21 (1966).

Butterfield, M. A., Care and preservation of the new media-equipment needs, Proc. A Pioneer Presentation of a National Symposium on the Impact of Auto- mation on Documentation, Denver, Colo., Apr. 27-29, 1967, pp. 60-64 (1968).

Butterfield, M. A., Optical character recognition as an archival tool, Proc. A

Pioneer Presentation of a National Symposium on the Impact of Automation

on Documentation, Denver, Colo., Apr. 27-29, 1967, pp. 101-111 (1968). Caldwell, B. P., Kubelka-Munk coefficients from transmittance, J. Opt. Soc. Am.

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Campbell, P. G., Wright, J. R., Asphalt hardening by gaseous oxidants: The

relationship between softening point and chemical changes as measured by

IR spectroscopy, J. Mater. 2, No. 3, 581-596 (Sept. 1967).

Canfield, L. R., Johnston, R. G., Codling, K., Madden, R. P., Comparison of an

ionization chamber and a thermopile as absolute detectors in the extreme

ultraviolet, Appl. Opt. 6, No. 1, 1886-1888 (Nov. 1967).

Cannon, E. W., Digital computers, Encyclopedia of Physics, Ed. R. M. Besancon,

pp. 124-125 (Reinhold Publ. Corp., New York, N. Y., 1966).

Cassidy, E. C, Time resolved studies of spectra produced by electrically exploded

wires, Naturwissenschaften 55, No. 3, 125-128 (1968). Cassidy, E. C, Abramowitz, S., Time-resolved spectroscopic studies of exploding

wires in controlled atmospheres, Appl. Spectry. 21, No. 6, 360-364

(Nov.-Dec. 1967).

Catanzaro, E. J., Absolute isotopic abundance ratios of three common lead reference samples, Earth and Planetary Sci. Letters 3, No. 4, 343-346 (1968). Chamberlain, G. E., Simpson, J. A., Mielczarek, S. R., Kuyatt, C. E., Effect

of double scattering on cross-section measurements at large momentum transfer,

J. Chem. Phys. 47, No. 10, 4266-4267 (Nov. 15, 1967).

Chang, S. S., Bestul, A. B., Heat capacities for atactic polystyrene of narrow

molecular weight distribution to 360° K, J. Polymer Sci. 6, Part A-2, 849-860

(1968). Chang, T., Yang, G., Temperature dependence of paramagnetic relaxation of Mo5+ in Ti02 , J. Chem. Phys. 48, No. 6, 2546-2549 (Mar. 15, 1968).

Chappell, S. E., Humphreys, J. C, Motz, J. W., Berger, M. J., Seltzer, S. M.,

Response of silicon transmission detectors to monoenergetic electrons, IEEE

Trans. Nuclear Sci. NS-15, No. 3, 359 (June 1968).

Chappell, S. E., Sparrow, J. H., The average energy required to produce an ion

pair in argon, nitrogen, and air for 1- to 5-MeV alpha particles, Radiation Res.

32, No. 3, 383-403 (Nov. 1967).

Childs, G. E., Hanley, H. J. M., Applicability of dilute gas transport property

tables to real gases, Cryogenics 8, No. 2, 94-97 (Apr. 1968).

Chilton, C. J., Conner, J. P., Steele, F. K., A comparison between solar X-ray

emission and VLF sudden phase anomalies, Proc. IEEE 53, No. 12, 2018-2026

(Dec. 1965). Chivers, H. J. A., Hargreaves, J. K., The use of multiple antennas in studies of absorption at conjugate points, Proc. Symp. High Latitude Particles and the

Ionosphere, Alpbach, Austria, 1964, pp. 257-264 (Academic Press Inc., New.

York, N.Y., 1965).

Christ, B. W., Giles, P. M., Metallurgical uses of the Fe57 Mossbauer effect in metallic iron and plain carbon steels, Book, Advances in Mossbauer Methodology 3, 37-65 (Plenum Press Inc., New York, N. Y., Jan. 1967).

Christ, B. W., Smith, G. V., Strengthening of polycrystalline iron by nitrogen, Trans. ASM 60, 732-734 (1967).

Christ, B. W., Smith, G. V., Yield and flow stress increase in pure polycrystalline iron during 600° C treatment after wet hydrogen purification, Scripta Met. 1, No. 3, 123-130 (1967).

Christensen, R. G., Cassel, J. M., Volume changes accompanying collagen

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PATENTS

The following U.S. Patents have been granted to Commerce inventors and

assigned to the United States of America, as represented by the Secretary of the Department noted in parentheses

:

Hoynes, Dagfin S. No. 3,329,957, July 4, 1967. Antenna System Employing Hu- man Body as Radiator (Commerce).

210
Armstrong, Richard W. No. 3,331,228, July 18, 1967. Combination Lock (GSA)

.

Brack, Stephen D. No. 3,331,656, July 18, 1967. Chemically Crimping Nylon

Fibers Through Formation of Disulfide Bonds Therein (Commerce).

Weitzel, Daniel H. No. 3,339,948, September 5, 1967. Pipe Coupling (Air Force).

Selby, Myron C. No. 3,354,411, November 21, 1967. Coaxial Transmission Line

T-Junction Having Rectangular Passageway Dimensioned Beyond Cutoff for Higher Order Modes (Commerce)

.

Jones, Frank E. and Castle, Alfred B. Sr. No. 3,354,544, November 28, 1967. Method

and Apparatus for Making Electrical Elements (Navy )

.

Kekopoulos, Gregory and Buckley, Arthur, No. 3,360,262, December 26, 1967. Apparatus for Moving and Aligning Limp Pieces of Material (Commerce).

Brenner, Abner No. 3,366,562, January 30, 1968. Method of Conducting Electrolysis

in a Solid Ionic Conductor Using an Electron Beam ( Commerce)

.

Lhermitte, Roger M., Shreeve, Kenneth H. and Erdahl, Robert J. No. 3,366,951, January 30, 1968. Waveform Averaging and Contouring Device for Weather

Radars and the Like (Commerce)

.

Torgensen, John L. and Peiser, H. Steffen No. 3,371,036, February 27, 1968. Method and Apparatus for Growing Single Crystals of Slightly Soluble Substances (Commerce).

Wall, Leo A. and Pummer, Walter J. No. 3,371,064, February 27, 1968. Fluoro- phenyl Vinyl Ethers and Their Polymers (Navy )

.

Leiss, James E., Penner, Samuel and Pararas, John L. No. 3,375,387, March 26, 1968. Fluid Cooled Multi-Foil Beam Window for High Power Beam Tubes

( Commerce )

.

Boynton, Ira D. and Bode, Robert H. No. 3,378,257, April 16, 1968. Apparatus

for Moving and Orienting Limp Pieces of Materials ( Commerce )

.

211

U.S. GOVERNMENT PRINTING OFFICE: 1968 O—320-738