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PUBLICATIONS iffiJIimTk 0F STAND & TECH IIIIIII

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NBS SPECIAL PUBLICATION 260-97

/?e AU o*

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

Standard Reference Materials:

Summary of the Coal,

Ore, Mineral, Rock,

and Refractory

Standards Issued by the

National Bureau of

Standards

100 Radu Mavrodineanu and Thomas E. Gills

• U57

260-97

1985

c2
Tm he National Bureau of Standards was established by an act of Congress on March 3, 1901. The m Bureau's overall goal is to strengthen and advance the nation's science and technology and facilitate their effective application for public benefit. To this end, the Bureau conducts research and provides: (1) a

basis for the nation's physical measurement system, (2) scientific and technological services for industry and

government, (3) a technical basis for equity in trade, and (4) technical services to promote public safety. The Bureau's technical work is performed by the National Measurement Laboratory, the National Engineering Laboratory, the Institute for Computer Sciences and Technology, and the Institute for Materials Science and Engineering

The National Measurement Laboratory

Provides the national system of physical and chemical measurement;

coordinates the system with measurement systems of other nations and

furnishes essential services leading to accurate and uniform physical and

chemical measurement throughout the Nation's scientific community, in- dustry, and commerce; provides advisory and research services to other Government agencies; conducts physical and chemical research; develops, produces, and distributes Standard Reference Materials; and provides

calibration services. The Laboratory consists of the following centers:

• Basic Standards2 • Radiation Research

• Chemical Physics

• Analytical Chemistry

The National Engineering Laboratory

Provides technology and technical services to the public and private sectors to address national needs and to solve national problems; conducts research in engineering and applied science in support of these efforts; builds and maintains competence in the necessary disciplines required to carry out this research and technical service; develops engineering data and measurement

capabilities; provides engineering measurement traceability services; develops

test methods and proposes engineering standards and code changes; develops and proposes new engineering practices; and develops and improves mechanisms to transfer results of its research to the ultimate user. The

Laboratory consists of the following centers:

Applied Mathematics

Electronics and Electrical Engineering2 Manufacturing Engineering

Building Technology

Fire Research Chemical Engineering2

The Institute for Computer Sciences and Technology

Conducts research and provides scientific and technical services to aid Federal agencies in the selection, acquisition, application, and use of computer technology to improve effectiveness and economy in Government

operations in accordance with Public Law 89-306 (40 U.S.C. 759), relevant Executive Orders, and other directives; carries out this mission by managing

the Federal Information Processing Standards Program, developing Federal ADP standards guidelines, and managing Federal participation in ADP

voluntary standardization activities; provides scientific and technological advisory services and assistance to Federal agencies; and provides the technical foundation for computer-related policies of the Federal Government. The Institute consists of the following centers:

Programming Science and

Technology Computer Systems

Engineering

The Institute for Materials Science and Engineering

Conducts research and provides measurements, data, standards, reference

materials, quantitative understanding and other technical information funda- mental to the processing, structure, properties and performance of materials; addresses the scientific basis for new advanced materials technologies; plans

research around cross-country scientific themes such as nondestructive

evaluation and phase diagram development; oversees Bureau-wide technical programs in nuclear reactor radiation research and nondestructive evaluation; and broadly disseminates generic technical information resulting from

its programs. The Institute consists of the following Divisions:

Inorganic Materials Fracture and Deformation3 Polymers

Metallurgy

Reactor Radiation

'Headquarters and Laboratories at Gaithersburg, MD, unless otherwise noted; mailing address Gaithersburg, MD 20899.

: Some divisions within the eenter are located at Boulder. CO SfHfH
Standard Reference Materials:

rational bureau

of standards

LIBRARY Summary of the Coal, Ore, Mineral,

Rock, and Refractory Standards

Issued by the National Bureau of

Standards

R. Mavrodineanu 1

Center for Analytical Chemistry

National Measurement Laboratory

National Bureau of Standards

Gaithersburg, MD 20899

and

T. E. Gills

Office of Standard Reference Materials National Measurement Laboratory

National Bureau of Standards

Gaithersburg, MD 20899

Present Address: 227 Almeria Road

West Palm Beach, FL 33405

U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige, Secretary

NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director Issued September 1985
Library of Congress Catalog Card Number: 85-600577

National Bureau of Standards Special Publication 260-97

Natl. Bur. Stand. (U.S.), Spec. Publ. 260-97, 134 pages (Sept. 1985)

CODEN: XNBSAV

U.S. GOVERNMENT PRINTING OFFICE WASHINGTON: 1985

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402
Preface

Standard Reference Materials (SRM's) as defined by the National Bureau of Standards (NBS) are well-characterized materials, produced in quantity and certified for one or more physical or chemical properties. They are used to assure the accuracy and compatibility of measurements

throughout the Nation. SRM's are widely used as primary standards in many diverse fields in science, industry, and technology, both within the United States and throughout the world. They are also used extensively in the fields of environmental and clinical analysis. In many applications, traceability of quality control and measurement processes to the national measurement system is carried out through the mechanism and use of SRM's. For many of the Nation's scientists and technologists it is therefore of more than passing interest to know the details of the measurements

made at NBS in arriving at the certified values of the SRM's produced. An NBS series of papers, of which this publication is a member, called the NBS Special Publication - 260 Series , is reserved for this purpose.

This 260 Series is dedicated to the dissemination of information on different phases of the preparation, measurement, certification and use of NBS SRM's. In general, much more detail will be found in these papers than is generally allowed, or desirable, in scientific journal articles. This enables the user to assess the validity and accuracy of the measurment processes employed, to judge the statistical analysis, and to learn details of techniques and methods utilized for work entailing

the greatest care and accuracy. These papers also should provide sufficient additional information

not found on the certificate so that new applications in diverse fields not foreseen at the time the SRM was originally issued will be sought and found. Inquiries concerning the technical content of this paper should be directed to the author(s). Other questions concered with the availability, delivery, price, and so forth, will receive prompt attention from: Office of Standard Reference Materials National Bureau of Standards Gaithersburg, MD 20899

Stanley D. Rasberry, Chief Office of Standard Reference Materials

iii
OTHER NBS PUBLICATIONS IN THIS SERIES

Catalog of NBS Standard Reference Materials

(1984-85 edition), Catherine H. Hudson, ed., NBS

Spec. Publ. 260 (February 1984). $5.50* SN003-

003-02558-5.

Michaelis, R. E., and Wyman, L. L. Standard

Reference Materials: Preparation of White Cast

Iron Spectrochemical Standards. NBS Misc. Publ. 260-1 (June 1964). COM74-1 1061**

Michaelis, R. E., Wyman, L. L., and Flitsch, R., Standard Reference Materials: Preparation of NBS Copper-Base Spectrochemical Standards. NBS Misc. Publ. 260-2 (October 1964). COM74-

1 1063**

Michaelis, R. E., Yakowitz, H., and Moore, G. A., Standard Reference Materials: Metallographic

Characterization of an NBS Spectrometric LowAlloy Steel Standard. NBS Misc. Publ. 260-3 (October 1964). COM74-1 1060** Hague, J. L. Mears, T. W., and Michaelis, R. E., Standard Reference Materials: Sources of

Information, NBS Misc. Publ. 260-4 (February

1965). COM74- 11059

Alvarez, R., and Flitsch R., Standard Reference

Materials: Accuracy of Solution X-Ray Spectrometric Analysis of Copper-Base Alloys. NBS

Misc. Publ. 260-5 (March 1965). PBI68068**

Shultz, J. I., Standard Reference Materials: Methods for the Chemical Analysis of White

Cast Iron Standards, NBS Misc. Publ. 260-6

(July 1965). COM74-1I068**

Bell, R. K , Standard Reference Materials: Methods for the Chemical Analysis of NBS

Copper-Base Spectrochemical Standards. NBS

Misc. Publ. 260-7 (October 1965). COM74-

11067** Richmond, M.S., Standard Reference Materials: Analysis of Uranium Concentrates at the

National Bureau of Standards. NBS Misc. Publ. 260-8 (December 1965). COM74-1 1066** Anspach, S. C, Cavallo, L. M. Garfinkel, S. B. Hutchinson, J. M. R , and Smith, C. N., Standard Reference Materials: Half Lives of Materials Used in the Preparation of Standard Reference Materials of Nineteen Radioactive Nuclides

Issued by the National Bureau of Standards NBS Misc. Publ. 260-9 (November 1965). COM74-11065**

Yakowitz, H., Vieth, D, L., Heinrich, K. F. J., and

Michaelis, R. E., Standard Reference Materials: Homogeneity Characterization of NBS Spectrometric Standards II: Cartridge Brass and LowAlloy Steel, NBS Misc. Publ. 260-10 (December

(1965). COM74-1 1064** Napolitano, A., and Hawkins, E. G., Standard Reference Materials: Viscosity of Standard

Lead-Silica Glass, NBS Misc. Publ. 260-11 (November 1966). NBS Misc. Publ. 260-11** Yakowitz, H., Vieth, D. L., and Michaelis, R. E., Standard Reference Materials: Homogeneity

Characterization of NBS Spectrometric Standards III: White Cast Iron and Stainless Steel Powder Compact, NBS Misc. Publ. 260-12

(September 1966). NBS Misc. Publ. 260-12**

Spijkerman, J. L., Snediker, D. K., Ruegg, F. C,

and DeVoe, J. R., Standard Reference Materials: Mossbauer Spectroscopy Standard for the Chemical Shift of Iron Compounds, NBS Misc. Publ. 260-13 (July 1967). NBS Misc. Publ.

260-13**

Menis, O., and Sterling, J. T., Standard Reference

Materials: Determination of Oxygen in Ferrous

Materials - SRM 1090, 1091, and 1092, NBS

Misc. Publ. 260-14 (September 1966). NBS Misc.

Publ. 260-14**

Passaglia, E., and Shouse, P. J., Standard Refer- ence Materials: Recommended Method of Use

of Standard Light-Sensitive Paper for Calibrat- ing Carbon Arcs Used in Testing Textiles for Colorfastness to Light, NBS Misc. Publ. 260-15 (June 1967). (Replaced by NBS Spec. Publ.

260-41.) Yakowitz, H., Michaelis, R. E., and Vieth, D. L., Standard Reference Materials: Homogeneity

Characterization of NBS Spectrometric Standards IV: Preparation and Microprobe Characterization of W-20% MO Alloy Fabricated by Powder Metallurgical Methods, NBS Spec.

Publ. 260-16 (January 1969). COM74-1 1062** Catanzaro, E. J., Champion, C. E., Garner, E. L., Marinenko, G., Sappenfield, K. M , and Shields, W. R., Standard Reference Materials: Boric

Acid; Isotopic and Assay Standard Reference

Materials, NBS Spec. Publ. 260-17 (February

1970). Out of Print. Geller, S. B., Mantek, P.A., and Cleveland, N.

G., Standard Reference Materials: Calibration of NBS Secondary Standard Magnetic Tape (Computer Amplitude Reference) Using the Reference Tape Amplitude Measurement

"Process A," NBS Spec. Publ. 260-18 (November

1969). (See NBS Spec. Publ. 260-29.) Paule, R. C, and Mandel, J., Standard Reference

Materials: Analysis of lnterlaboratory Measurements on the Vapor Pressure of Gold (Certifica- tion of Standard Reference Material 745). NBS

Spec. Publ. 260-19 (January 1970). PB190071**

Paule, R. C, and Mandel, J., Standard Reference

Materials: Analysis of lnterlaboratory Measurements on the Vapor Pressures of Cadmium and

Silver, NBS Spec. Publ. 260-21 (January 1971). COM74-11359**

Yakowitz, H., Fiori, C. E., and Michaelis, R. E., Standard Reference Materials: Homogeneity

Characterization of Fe-3 Si Alloy, NBS Spec.

Publ. 260-22 (February 1971). COM74-1 1 357**

Napolitano, A., and Hawkins, E. G., Standard

Reference Materials: Viscosity of a Standard

Borosilicate Glass, NBS Spec. Publ. 260-23 (December 1970). COM71-00I57**

Sappenfield, K. M., Marineko, G., and Hague, J. L., Standard Reference Materials: Comparison

of Redox Standards, NBS Spec. Publ. 260-24 (January 1972). COM72-50058**

iv
Hicho, G. E., Yakowitz, H., Rasberry, S. D., and

Michaelis, R. E., Standard Reference Materials: A Standard Reference Material Containing

Nominally Four Percent Austenite, NBS Spec.

Publ. 260-25 (February 1971). COM74-1 1356"

Martin, J. F., Standard Reference Materials:

National Bureau of Standards-US Steel Corporation Joint Program for Determining Oxygen and Nitrogen in Steel, NBS Spec. Publ. 260-26

(February 1971). 85 cents* PB 81176620

Garner, E. L., Machlan, L. A., and Shields, W. R., Standard Reference Materials: Uranium

Isotopic Standard Reference Materials, NBS

Spec. Publ. 260-27 (April 1971). COM74-

11358**

Heinrich, K. F. J., Myklebust, R. L., Rasberry, S. D., and Michaelis, R. E., Standard Reference Materials: Preparation and Evaluation of SRM's 481 and 482 Gold-Silver and GoldCopper Alloys for Microanalysis, NBS Spec.

Publ. 260-28 (August 1971). COM71-50365**

Geller, S. B., Standard Reference Materials: Cali- bration of NBS Secondary Standard Magnetic Tape (Computer Amplitude Reference) Using

the Reference Tape Amplitude Measurement

"Process A-Model 2," NBS Spec. Publ. 260-29 (June 1971). COM7I-50282

Gorozhanina, R. S., Freedman, A. Y., and

Shaievitch, A. B. (translated by M. C. Selby), Standard Reference Materials: Standard

Samples Issued in the USSR (A Translation from the Russian). NBS Spec. Publ. 260-30 (June

1971). COM7I-50283**

Hust, J. G., and Sparks, L. L., Standard Reference

Materials: Thermal Conductivity of Electrolytic Iron SRM 734 from 4 to 300 K, NBS Spec. Publ. 260-31 (November 1971). COM71-50563**

Mavrodineanu, R., and Lazar, J. W., Standard

Reference Materials: Standard Quartz Cuvettes,

for High Accuracy Spectrophotometry, NBS

Spec. Publ. 260-32 (December 1973). 55 cents* SN003-003-012I3-I Wagner, H. L., Standard Reference Materials: Comparison of Original and Supplemental SRM 705, Narrow Molecular Weight Distri- bution Polystyrene, NBS Spec. Publ. 260-33 (May 1972). COM72-50526**

Sparks, L. L., and Hust, J. G., Standard Reference

Materials: Thermoelectric Voltage, NBS Spec.

Publ. 260-34, (April 1972). COM72-50371**

Sparks, L. L., and Hust, J. G., Standard Refer- ence Materials: Thermal Conductivity of

Austenitic Stainless Steel, SRM 735 from 5 to 280 K, NBS Spec. Publ. 260-35 (April 1972.) 35 cents* COM72-50368**

Cali, J. P., Mandel, J., Moore, L. J., and Young, D.

S., Standard Reference Materials: A Referee Method for the Determination of Calcium in Serum, NBS SRM 915, NBS Spec. Publ. 260-36 (May 1972). COM72-50527**

Shultz, J. I. Bell., R. K. Rains, T. C, and Menis,

O., Standard Reference Materials: Methods of Analysis of NBS Clay Standards, NBS Spec.

Publ. 260-37 (June 1972). COM72-50692**

Richmond, J. C, and Hsia, J. J., Standard Refer- ence Materials: Preparation and Calibration of Standards of Spectral Specular Reflectance, NBS Spec. Publ. 260-38 (May 1972). COM72-

50528**

Clark, A. F., Denson, V.A., Hust, J. G., and

Powell, R. L., Standard Reference Materials: The Eddy Current Decay Method for Resistivity Characterization of High-Purity Metals, NBS

Spec. Publ. 260-39 (May 1972). COM72-50529**

McAdie, H. G., Garn, P.D.,and Menis, O., Standard Reference Materials: Selection of Thermal

Analysis Temperature Standards Through a Cooperative Study (SRM 758, 759, 760), NBS

Spec. Publ. 260-40 (August 1972.) COM72-

50776** Wood, L. A., and Shouse, P. J., Standard

Reference Materials: Use of Standard LightSensitive Paper for Calibrating Carbon Arcs Used in Testing Textiles for Colorfastness to

Light, NBS Spec. Publ. 260-41 (August 1972) COM72-50775**

Wagner, H. L. and Verdier, P. H., eds.. Standard

Reference Materials: The Characterization of Linear Polyethylene, SRM 1475, NBS Spec. Publ. 260-42 (September 1972). COM72-

50944*

Yakowitz, H., Ruff, A. W., and Michaelis, R. E., Standard Reference Materials: Preparation, and Homogeneity Characterization of an Austenitic Iron-Chromium-Nickel Alloy, NBS Spec. Publ. 260-43 (November 1972). COM73-50760**

Schooley, J. F., Soulen, R. J., Jr., and Evans, G. A.,

Jr., Standard Reference Materials: Preparation and Use of Superconductive Fixed Point

Devices, SRM 767, NBS Spec. Publ. 260-44 (December 1972). COM73-50037**

Greifer, B., Maienthal, E. J., Rains, T. C, and

Rasberry, S. D., Standard Reference Materials: Powdered Lead-Based Paint, SRM 1579, NBS

Spec. Publ. 260-45 (March 1973). COM73-

50226**

Hust, J. G., and Giarratano, P. J., Standard Refer- ence Materials: Thermal Conductivity and

Electrical Resistivity Standard Reference Materials: Austenitic Stainless Steel, SRM's 735 and

798, from 4 to 1200 K, NBS Spec. Publ. 260-46 (March 1975). SN003-003-0I278-5*

Hust, J. G., Standard Reference Materials: Electrical Resistivity of Electrolytic Iron, SRM 797, and Austenitic Stainless Steel, SRM 798, from 5

to 280 K, NBS Spec. Publ. 260-47 (February

1974). COM74-50I76** Mangum, B. W., and Wise, J. A., Standard Refer- ence Materials: Description and Use of Precision Thermometers for the Clinical Laboratory, SRM 933 and SRM 934, NBS Spec. Publ. 260-48 (May 1974). 60 cents* SNO03-O03-OI278-5

Carpenter, B. S., and Reimer, G. M., Standard

Reference Materials: Calibrated Glass Standards for Fission Track Use, NBS Spec. Publ. 260-49 (November 1974). COM74-5I185

v
Hust, J. G., and Giarratano, P. J., Standard Refer- ence Materials: Thermal Conductivity and Electrical Resistivity Standard Reference Materials:

Electrolytic Iron, SRM's 734 and 797 from 4 to 1000 K, NBS Spec. Publ. 260-50 (June 1975). $1.00* SN0O3-OO3-0 1425-7 Mavrodineanu, R., and Baldwin, J. R., Standard

Reference Materials: Glass Filters As a Standard Reference Material for Spectrophotometry;

Selection; Preparation; Certification; Use-SRM

930, NBS Spec. Publ. 260-51 (November 1975). $1.90* SN003-003-0I48I-8

Hust, J. G., and Giarratano, P. J., Standard Refer- ence Materials: Thermal Conductivity and Electrical Resistivity Standard Reference Materials 730 and 799, from 4 to 3000 K, NBS Spec. Publ. 260-52 (September 1975). $1.05* SN003-003-

01464-8 Durst, R. A., Standard Reference Materials: Standardization of pH Measurements, NBS

Spec. Publ. 260-53 (December 1975, Revised). $1.05 SN003-003-OI55I-2

Burke, R. W., and Mavrodineanu, R., Standard

Reference Materials: Certification and Use of Acidic Potassium Dichromate Solutions as an

Ultraviolet Absorbance Standard, NBS Spec.

Publ. 260-54 (August 1977). $3.00* SN003-003-

01828-7

Ditmars, D. A., Cezairliyan, A., Ishihara, S., and

Douglas, T. B., Standard Reference Materials: Enthalpy and Heat Capacity; Molybdenum SRM 781, from 273 to 2800 K, NBS Spec. Publ. 260-55 (September 1977). $2.20* SN003-003-

01836-8

Powell, R. L., Sparks, L. L., and Hust, J. G., Standard Reference Materials: Standard

Thermocouple Materials, Pt.67: SRM 1967, NBS

Spec. Publ. 260-56 (February 1978). $2.20* SN003-003-0 18864

Cali, J. P. and Plebanski, T., Guide to United

States Reference Materials, NBS Spec. Publ. 260-57 (February 1978). $2.20* PB 277173

Barnes, J. D., and Martin, G. M., Standard Refer- ence Materials: Polyester Film for Oxygen Gas

Transmission Measurements SRM 1470, NBS

Spec. Publ. 260-58 (June 1979) $2.00* SN003-

003-02077 Chang, T., and Kahn, A. H. Standard Reference

Materials: Electron Paramagnetic Resonance

Intensity Standard; SRM 2601, NBS Spec.

Publ. 260-59 (August 1978) $2.30* SN003-

003-01975-5 Velapoldi, R. A., Paule, R. C, Schaffer, R., Mandel, J., and Moody, J. R., Standard Refer- ence Materials: A Reference Method for the Determination of Sodium in Serum, NBS Spec.

Publ. 260-60 (August 1978). $3.00* SN003-003

01978-0

Verdier, P. H., and Wagner. H. L., Standard Refer- ence Materials: The Characterization of Linear Polyethylene (SRM 1482, 1483, 1484), NBS

Spec. Publ. 260-61 (December 1978). $1.70* SN003-003-02006-I

Soulen, R. J., and Dove, R. B., Standard Reference

Materials: Temperature Reference Standard

for Use Below 0.5 K (SRM 768). NBS Spec.

Publ. 260-62 (April 1979). $2.30* SN003-003-

02047-8 Velapoldi, R. A., Paule, R. C, Schaffer, R. Mandel, J., Machlan, L. A., and Gramlich, J. W., Standard Reference Materials: A Reference Method for the Determination of Potassium in Serum. NBS Spec. Publ. 260-63 (May 1979). $3.75* SN003-003-02068

Velapoldi, R. A., and Mielenz, K. D., Standard

Reference Materials: A Fluorescence Standard

Reference Material Quinine Sulfate Dihydrate (SRM 936), NBS Spec. Publ. 260-64 (January

1980). $4.25* SN003-O03-O2I48-2 Marinenko, R. B., Heinrich, K. F. J., and Ruegg,

F. C, Standard Reference Materials: Micro- Homogeneity Studies of NBS Standard Reference

Materials, NBS Research Materials, and Other Related Samples. NBS Spec. Publ. 260-65

(September 1979). $3.50* SN003-003-021 14-1 Venable, W. H., Jr., and Eckerle, K. L., Standard

Reference Materials: Didymium Glass Filters for Calibrating the Wavelength Scale of Spectro- photometers (SRM 2009, 2010, 2013). NBS Spec.

Publ. 260-66 (October 1979). $3.50* SN003-003-

02127-0

Velapoldi, R. A., Paule, R. C, Schaffer, R., Mandel,

J., Murphy, T. J., and Gramlich, J. W., Standard

Reference Materials: A Reference Method for the Determination of Chloride in Serum, NBS Spec.

Publ. 260-67 (November 1979). $3.75* SN003-

003-02136-9 Mavrodineanu, R. and Baldwin, J. R., Standard

Reference Materials: Metal-On-Quartz Filters as a Standard Reference Material for Spectrophoto- metry-SRM 2031, NBS Spec. Publ. 260-68

(April 1980). $4.25* SN003-003-02I67-9

Velapoldi, R. A., Paule, R. C, Schaffer, R., Mandel, J., Machlan, L. A., Garner, E. L., and

Rains, T. C, Standard Reference Materials: A

Reference Method for the Determination of Lithium in Serum, NBS Spec. Publ. 260-69 (July)

1980). $4.25* SN003-003-02214-4 Marinenko, R. B., Biancaniello, F., Boyer, P. A., Ruff, A. W., DeRobertis, L., Standard Reference

Materials: Preparation and Characterization of an Iron-Chromium-Nickel Alloy for Microanalysis, NBS Spec. Publ. 260-70 (May 1981). $2.50* SN003-003-02328-I Seward, R. W., and Mavrodineanu, R., Standard

Reference Materials: Summary of the Clinical Laboratory Standards Issued by the National Bureau of Standards, NBS Spec. Publ. 260-71 (November 1981). $6.50* SNO03-O03-0238I-7

Reeder, D.J., Coxon, B., Enagonio, D., Christensen,

R. G., Schaffer, R., Howell, B. F., Paule, R. C,

Mandel, J., Standard Reference Materials: SRM

900, Antiepilepsy Drug Level Assay Standard, NBS Spec. Publ. 260-72 (June 1981). $4.25* SN003-003-02329-9

vi
Interrante, C. G.and Hicho, G. E., Standard Refer- ence Materials: A Standard Reference Material Containing Nominally Fifteen Percent Austenite (SRM 486), NBS Spec. Publ. 260-73 (January

1982). $2.75* SN003-003-O2386-8 Marinenko, R. B., Standard Reference Materials: Preparation and Characterization of K-411 and

K-414 Mineral Glasses for Microanalysis: SRM

470. NBS Spec. Publ. 260-74 (April 1982). $3.50 SN003-O03-O23-95-7

Weidner, V. R., and Hsia, J. J., Standard Reference

Materials: Preparation and Calibration of First Surface Aluminum Mirror Specular Reflectance Standards (SRM 2003a), NBS Spec. Publ. 260-75 (May 1982). $3.75 SN003-003-023-99-0

Hicho, G. E. and Eaton, E. E., Standard Reference Materials: A Standard Reference Material

Containing Nominally Five Percent Austenite (SRM 485a), NBS Spec. Publ. 260-76 (August

1982). $3.50 SN003-O03-O24-33-3 Furukawa, G. T., Riddle, J. L., Bigge, W. G., and

Pfieffer, E. R., Standard Reference Materials- Application of Some Metal SRM's as Thermometric Fixed Points, NBS Spec. Publ. 260-77 (August 1982). $6.00 SN003-003-024-34-1

Hicho, G. E. and Eaton, E. E., Standard Reference

Materials: Standard Reference Material Containing Nominally Thirty Percent Austenite (SRM

487), NBS Spec. Publ. 260-78 (September 1982). $3.75* SN003-003-024-35-0 Richmond, J. C, Hsia, J. J. Weidner, V. R., and

Wilmering, D. B., Standard Reference Materials:

. Second Surface Mirror Standards of Specular

Spectral Reflectance (SRM's 2023, 2024, 2025), NBS Spec. Publ. 260-79 (October 1982). $4.50* SN003-O03-O24-47-3

Schaffer, R., Mandel, J., Sun, T., Cohen, A., and

Hertz, H. S., Standard Reference Materials: Evaluation by an ID/ MS Method of the AACC

Reference Method for Serum Glucose, NBS

Spec. Publ. 260-80 (October 1982). $4.75* SN003-

003-024-43-1 Burke, R. W., and Mavrodineanu, R. (NBS retired), Standard Reference Materials: Accuracy in Analytical Spectrophotometry, NBS Spec. Publ. 260-81 (April 1983). $6.00* SN003-003-024-8

Weidner, V. R., Standard Reference Materials: White Opal Glass Diffuse Spectral Reflectance Standards for the Visible Spectrum (SRM's 2015 and 2016). NBS Spec. Publ. 260-82 (April 1983). $3.75* SN003-003-024-89-9**

Bowers, G. N., Jr., Alvarez, R., Cali, J. P. (NBS

retired), Eberhardt, K. R., Reeder, D. J., Schaffer, R., Uriano. G. A., Standard Reference

Materials: The Measurement of the Catalytic

(Activity) Concentration of Seven Enzymes in NBS Human Serum SRM 909, NBS Spec.

Publ. 260-83 (June 1983). $4.50* SN003-003-024-

99-6

Gills, T. E., Seward, R. W., Collins, R. J., and

Webster, W. C, Standard Reference Materials: Sampling, Materials Handling, Processing, and

Packaging of NBS Sulfur in Coal Standard

Reference Materials, 2682, 2683, 2684, and 2685, NBS Spec. Publ. 260-84 (August 1983). $4.50* SN003-003-025-20-8

Swyt, D. A., Standard Reference Materials: A Look

at Techniques for the Dimensional Calibration of Standard Microscopic Particles, NBS Spec. Publ. 260-85 (September 1983). $5.50* SN003-003-

025-21-6 Hicho, G. E. and Eaton, E. E., Standard Reference Materials: A Standard Reference Material

Containing Two and One-Half Percent Austenite, SRM 488, NBS Spec. Publ. 260-86 (December

1983). $1.75* SN003-003-025-41-1 Mangum, B. W., Standard Reference Materials: SRM 1969: Rubidium Triple-Point - A Temperature Reference Standard Near 39.30 °C, NBS

Spec. Publ. 260-87 (December 1983). $2.25* SN003-003-025-44-5 Gladney, E. S., Burns, C. E., Perrin, D. R., Roelandts, I., and Gills, T. E., Standard Reference Materials: 1982 Compilation of Elemental

Concentration Data for NBS Biological, Geological, and Environmental Standard Reference

Materials. Spec. Publ. 260-88 (March 1984). $7.00* SN003-003-O2565-8

Hust, J. G., Standard Reference Materials: A Fine- G rained, Isotropic Graphite for Use as NBS

Thermophysical Property RM's from 5 to 2500 K, NBS Spec. Publ. 260-89 (September 1984). $4.50* SN0O3-OO3-O2608-5 Hust, J. G., and Lankford, A. B., Standard Reference Materials: Update of Thermal

Conductivity and Electrical Resistivity'of

Electrolytic Iron, Tungsten, and Stainless Steel, NBS Spec. Publ. 260-90 (September 1984). $3.00* SN003-O03-O26O9-3

Goodrich, L. F., Vecchia, D. F., Pittman, E. S., Ekin, J. W., and Clark, A. F., Standard Reference

Materials: Critical Current Measurements on an NbTi Superconducting Wire Standard Reference

Material, NBS Spec. Publ. 260-91 (September

1984). $2.75* SNO03-O03-O2614-O

Carpenter, B. S., Standard Reference Materials: Calibrated Glass Standards for Fission Track Use (Supplement to NBS Spec. 260-49). NBS

Spec. Publ.. 260-92 (September 1984). $1.50* SN003-003-O26I0-7

Ehrstein, J., Preparation and Certification of Standard Reference Materials for Calibration of Spreading Resistance Probes, NBS Spec. Publ. 260-93 (January 1985).

Gills, T. E., Koch, W. F. Stolz, J. W., Kelly, W. R., Paulsen, P. J., Colbert, J. C. Kirklin, D. R., Pei, P.T.S., Weeks, S., Lindstrom, R. M.

Fleming, R. F., Greenberg, R. R., and

Paule, R. C, Methods and Procedures Used at the National Bureau of Standards to Certify Sulfur

in Coal SRM's for Sulfur Content, Calorific Value, Ash Content, NBS Spec. Publ. 260-94 (December 1984). Mulholland, G. W., Hartman, A. W., Hembree,

G. O, Marx, E., and Lettieri, T. R., Standard

Reference Materials: Development of a I m

Diameter Particle Size Standard, SRM 1690, NBS Spec. Publ. 260-95 (May 1985).

vii
Carpenter, B. S., Gramlich, J. W., Greenberg, R. R., and Machlan, L. A., Standard Reference

Materials: Uranium-235 Isotopic Abundance Standard Reference Materials for Gamma

Spectrometry Measurements, NBS Spec. Publ. 260-96 (In Press). Mavrodineanu, R. and Gills, T. E., Standard

Reference Materials: Summary of the Coal, Ore,

Mineral, Rock, and Refractory Standards Issued by the National Bureau of Standards, NBS Spec.

Publ. 260-97 (In Press). Hust, J. G., Standard Reference Materials: Glass Fiberboard SRM for Thermal Resistance, NBS

Spec. Publ. 260-98 (In Press). Callanan, J. E., Sullivan, S. A., and Vecchia, D. F., Standard Reference Materials: Feasibility Study

for the Development of Standards Using

Differential Scanning Calorimetry, NBS Spec.

Publ. 260-99 (In Press). Taylor, J. K., Standard Reference Materials: Handbook for SRM Users, NBS Spec. Publ. 260-100

(In Press).

* Send order with remittance to Superintendent

of Documents, US Government Printing Office Washington, DC 20402. Remittance from

foreign countries should include an additional one-fourth of the purchase price for postage. ** May be ordered from: National Technical Information Services (NTIS). Springfield

Virginia 22161.

viii
TABLE OF CONTENTS

Page Preface iii Abstract x Introduction X Table 1. Category Index of Standards available from the National Bureau

of Standards 2 Coal, Ore, Mineral, Rock, and Refractory Standards 4 Table 2. Summary of Coal, Ore, Mineral, Rock, and Refractory Standards .... 6 A. Coals 5 B. Rocks, Minerals, and Refractories 8 C. Ores 14 Table 3. Composition of SRM's Prepared from Ores, Minerals, Rocks, and Refractories 22 Table 4. NBS Publications in the "260 Series" Related to Coal, Ore, Mineral, Rock, and Refractory Standards 26 Acknowledgment 26 Appendix I. Alphabetical Index by Standard Reference Material Name 27 Appendix II. Certificates for Coal, Ore, Mineral, Rock, and Refractory

Standards (listed in numerical order) 40

ix
Abstract

This publication is a summary of the coal, ore, mineral, rock, and refractory standards issued by NBS as Standard Reference Materials (SRM's). The material, com- position, certification, use, and remarks concerning each

of the SRM's described are presented in tabular form. Copies of the certificates of these SRM's are contained in the appendix for more detailed information. Key Words: Chemical composition; coals; ores; refractories

rocks; Standard Reference Materials.
Introduction

Since its inauguration in 1901, the National Bureau of Standards (NBS) has issued nearly 2000 different Standard Reference Materials (SRM's). Many of these have been renewed several times, many

have been replaced or discontinued as technology changed. Today, over 900 SRM's are available, together with a large number of scientific publications related to the fundamental and applied characteristics of these materials. Each material is certified for chemical composition, chemical properties, or its physical or mechanical characteristics. Each SRM is provided with a Certificate

or Certificate of Analysis that contains the essential data concerning its properties or characteristics. The SRM's currently available cover a wide range of chemical, physical, and mechanical properties, and a corresponding wide range of measurement interests in practically all aspects of fundamental and applied science. These SRM's constitute a unique and invaluable means of transferring to the user accurate data obtained at NBS, and provide essential tools that can be used

to improve accuracy in practically all areas where measurements are performed.

In addition to SRM's, the National Bureau of Standards issues a variety of Research Materials

(RM's) having various properties described in individual "Reports of Investigation." They are intended primarily to further the scientific or technical research on that particular material. Other materials, called Special Reference Materials (GM's), are also available from NBS. These are materials produced and certified by other Government agencies, standard organizations, or other nonprofit organizations, that are considered useful to the public and for which no alternate method

of national distribution exists.

The various categories of materials available from NBS are given in Table 1. This table lists these materials according to their chemical composition, physical properties, or engineering characteristics. A more detailed alphabetic enumeration of these materials is given in Appendix I. Table 1 and Appendix I were taken from NBS Special Publication 260, NBS Standard Reference Materials

Catalog, 1984-85 Edition . This publication lists every material available from the NBS Office of Standard Reference Materials. Further information on the reference materials available from NBS may be obtained from the Office of Standard Reference Materials, National Bureau of Standards, Gaithersburg , MD 20899. Information on other NBS services may be obtained from the Technical Information and Publications

Division, National Bureau of Standards, Gaithersburg, MD 20899.

In addition to these types of materials, NBS provides many additional services. These include: Measurement Assurance Programs, Calibration and Related Measurement Services, Proficiency Sample Programs, a National Voluntary Laboratory Accreditation Program, Standards Information Services, Standard Reference Data, and Technical Information and Publications.

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington,

DC 20402, under Stock No. 003-003-02558-5 (Price $5.50, add 25 percent for foreign orders.)
Table L. Categories of Standard Reference Materials available from the National Bureau

of Standards.

CERTIFIED CHEMICAL COMPOSITION STANDARDS

Steels (chip form) Plain carbon Low alloy High alloy Stainless

Tool

Steels (granular form) Steels (solid form) Ingot iron and low alloy Special ingot irons and low alloy Stainless

Spe cialty High-temperature alloys Tool Steelmaking Alloys

Cast Irons (chip form) Cast Steels, White Cast Irons, Ductile

Irons, and Blast Furnace Irons

(solid form) Nonferrous Alloys (chip form) Aluminum "Benchmarks"

Cobalt Copper Copper "Benchmarks"

Lead Magnesium

Nickel

Nickel Superalloy, Trace Elements

Nickel oxide Selenium Tin Titanium

Zinc Zirconium

Nonferrous Alloys (solid form) Aluminum "Benchmarks"

Cop per Copper "Benchmarks" Lead

Nickel Titanium

Zinc Zirconium

Gases in Metals High-Purity Metals Electron Probe Microanalyt ical Standards

Primary, Working, and Secondary

Standard Chemicals Microchemical Standards

Clinical Laboratory Standards Biological Standards Environmental Standards Analyzed gases Analyzed liquids and solids Permeation tubes Industrial Hygiene Standards Forensic Standards Hydrocarbon Blends Metallo-Organic Compounds Fertilizers

Ores Minerals, Refractories, Glasses, and Carbides

Cement Trace Element Standards Nuclear Materials

Special nuclear materials Plutonium assay Plutonium isotopic Uranium assay Uranium isotopic Neutron density standards Fission track glass standards Isotopic Reference Standards

2
Table 1. continued.

CERTIFIED PHYSICAL PROPERTY STANDARDS

Ion Activity Standards

pH standards

pD standards

Ion selective electrodes

Optical Standards Spectrophotometric

Thermal emittance

Refractive index Mechanical and Metrology Standards Magnification

Coating thickness Glass Elasticity

Density Polymer

Rheology

Heat Standards Superconductive thermoraetric fixed point devices Freezing Points Defining fixed points Determined reference points Melting points Calorimetric Combustion

Solution

Heat source Enthalpy and heat capacity Vapor pressure Thermal expansion Thermocouple materials Thermal resistance Magnetic Standards Magnetic susceptibility Magnetic moment Paramagnetic resonance

Radioactivity Standards Alpha-particle standards Beta-particle and gamma-ray gas standards Alpha-particle, beta-particle,

gamma-ray, and electron-capture

solution standards Contemporary standard for carbon-14 dating laboratories Environmental standards Low energy photon sources Gamma-ray "point-source" standards Radium gamma-ray solution standards Radium solution standards for random analysis Radioactivity standard reference materials currently not in stock Metallurgical Mossbauer

X-ray Diffraction

Gas Transmission

Permittivity

Reference Fuels Resistivity

ENGINEERING TYPE STANDARDS

Standard Rubber and Rubber- Compounding Materials Reference Magnetic Tapes Centerline Drawings, OCR-B

Sizing Standards Glass spheres for particle size Turbidimetric and fineness (cement)

X-ray and Photographic Standards

Surface Flammability Standards

Smoke Density Chamber Standards Water Vapor Permeance

Tape Adhesion Testing Standards

Color Standards

RESEARCH MATERIALS SPECIAL REFERENCE MATERIALS

3
Coal, Ore, Mineral, Rock, and Refractory Standards

The accurate determination of major and minor constituents in coals, ores, minerals, rocks, and refractories is important to our nation's scientific and industrial community as well as to commerce

and trade. In many industries, traceabllity of quality control to the national measurement system

is achieved through the use of Standard Reference Materials (SRM's). This publication is an attempt

to describe, in general terms, the composition, certification, and use of such SRM's. Essential information concerning the material composition, the certification parameters, and use is given in Table 2. Under "Remarks," additional data are provided. All the data and information contained in this table were extracted from the Certificates or Certificates of Analysis

issued for the included SRM's. An examination of the table gives the reader a general view of these SRM's. For more detailed information, the individual Certificates reproduced in Appendix II should

be consulted as well as any references cited in each certificate. The composition of the same SRM's, excepting the coals, by chemical elements are listed in Table 3. In the tables, similar

types of SRM's are grouped together to facilitate comparisons of their properties. The Certificates

in Appendix II, however, are arranged in numerical order. The SRM's listed in the tables include all of the coal, ore, mineral, rock, and refractory standards that were in stock as of January 1, 1984. These SRM's are the result of the concerted efforts of a number of scientists from the NBS National Measurement Laboratory, Center for Analytical Chemistry, and from industry. Each Certificate lists the individuals and laboratories who contributed to the preparation and certification of the SRM.

In addition to the SRM's and their Certificates, NBS issues a series of Special Publications

(SP), call the "260 Series," that relate directly to Standard Reference Materials as stated in the preface. The list of available publications in the "260 Series" is given at the beginning of this publication.

Table 4 lists several NBS SP 260 publications directly related to the SRM's described in this work. They should be of value to the user of these particular materials. Also, NBS SP 260-54 contains in its appendices three reprints on: "Standard Quartz Cuvettes for High-Accuracy

Spectrophotometry" (Appendix III); "Testing of Glass Volumetric Apparatus, 1959" (Appendix V); and

"The Calibration of Small Volumetric Laboratory Glassware, 1974" (Appendix VI). The last two publications have been out of print for several years. Other NBS publications, not in the "260 Series," and a number of NBS staff authored papers have been published that deal with specific SRM's or measurement techniques used in analytical chemistry.

Some of these are: SP 148, The Role of Standard Reference Materials in Measurement Systems; SP 378, Accuracy in Spectrophotometry and Luminescence Measurements (255 pp., 1973); and SP 466, Standardization in Spectrophotometry and Luminescence Measurments (150 pp., 1977). NBS Monograph

100, Trace Characterization, Chemical and Physical (580 pp., 1967); SP 422, Accuracy in Trace Analysis, Sampling, Sample Handling, Analysis, Vol. 1 and 2 (1304 pp., 1976); and SP 464, Proceedings of the Eighth Materials Research Symposium, Methods and Standards for Environmental Measurements (691 pp., 1977), provide further information on methodology for the analysis of a variety of materials and the determination of numerous constituents. They all should be of particular interest to the analytical chemist.

NOTE: The use of proprietary designations in Table 2 is for information only, and should not be construed as an endorsement of the product by either the Department of Commerce or the National Bureau of Standards. Table 3 was taken from an article by S. D. Rasberry published in Amer

Lab. , 15 (5), 96 (1983).

)'For complete bibliographic reference and ordering information, see "Other NBS Publications in This Series," pp. iv.

4
5
Table 2. Summary of Coal, Ore, Mineral, Rock, and Refractory Standards

A. Coals

Composition

1632b Trace Elements in Coal (Bituminous)

Obtained from Humphrey No. 7 mine and coal preparation plant

of the Consolidation Coal Co., Christopher Coal Co. Div., Osage, W.V. The coal was reduced in size to -60 mesh and sieved prior to blending. The

coal was then blended in a stainless steel coal blender.

Material should be vacuum

dried at ambient temperature

for 24 hours prior to use. Values based on a minimum

sample size of 250 mg.

C (total) 78.11; H 5.07;

N 1.56; S 1.89; Volatile

matter 35.4; Al 0.855; Ca .204; Fe .759; Mg .0383; K .0748; Na .0515; Ti .0454; values % by wt. As 3.72; Ba 67.5; Cd 0.0573; Co 2.29; Cu 6.28; Pb 3.67; Mn 12.4; Ni 6.10; Rb 5.05; Se 1 .29; Th 1.342; U 0.436; Zn 11.89; values yg/g. Not certified:

17 additional constituents

(see certificate).

1633a Trace Elements in Coal Fly Ash

Supplied by a coal fired power

plant and is a product of Pennsylvania and West Virginia

coals. Material was sieved through a #170 sieve and blended

in a Vee blender.

Material should be dried to a constant weight before use. Values based on a 250-mg or more sample size. Ca 1.11; Fe 9.40; K 1.88; Mg 0.455; Na 0.17; Si 22.8, values % by wt. As 145; Cd 1.0; Cr 196; Cu 118; Hg 0.16; Ni 127; Pb 72.4; Rb 131; Se 10.3; Sr 830; Th 24.7; Tl 5.7;

U 10.2; Zn 220, values yg/g.

Not certified: 15 additional

constituents (see certificate)

1635 Trace Elements in Coal

( Sub-bituminous)

Provided by the Eagle Mine of the Imperial Coal Company,

Erie, Colorado. Ground and sieved through a 230 m sieve

by the Colorado School of Mines Research Institute.

Material should be dried without heat to constant weight

before use. Values based on 250-mg or more sample size. As 0.42; Cd 0.03; Cr 2.5; Cu 3.6; Pb 1.9; Mg 21.4; Ni 1 .74; Se 0.9; Th 0.62;

U 0.24; V 5.2; Zn 4.7, values yg/g. Fe 0.239; S 0.33, values % by wt. Not certified

10 additional constitutents

(see certificate).

2682 Sulfur in Coal (Sub-bituminous)

Obtained from Bell Ayr Mine, Gillette, Wyoming The coal was reduced in size to -60 mesh and screened prior to blending. The -60 mesh coal was then blended in a stainless

steel cone blender.

Sample vacuum dried at ambient temperature for 24 hours or oven drying for 24 hours at 105 °C. Values based on 250- mg or more sample size. Sulfur (wt. %) 0.47; Furnace Ash (wt. %) 6.37; Calorific

Content 27.45 MJ .Kg . Not certified: 32 inorganic con- stituents (see certificate).

*National Bureau of Standards, Center for Analytical Chemistry. °American Society for Testing and Materials.

6
Certification Use Remarks

Analyses performed in the NBS CAC* Estimated uncertainty

0.0008 TO 2.1 depending on con- stituent.

For the calibration of apparatus and the evaluation of techniques employed in the analysis of coal or similar materialsShould be kept in its original

bottle. Should not be exposed

to intense sources of radiation, including ultraviolet

lamps or sunlight.

Analyses performed in the NBS For the calibration of appa- Should be kept in a tightly

CAC. Estimated uncertainty ratus and methods used in sealed bottle. 0.010 to 30 depending on con- analyses of coal fly ash and stituent. other materials with similar matrices for trace elements.

Analyses performed in the NBS Same as SRM 1632a. Same as SRM 1632a. CAC. Estimated uncertainty

0.15 to 1.5 depending on con- stituent.

Analyses performed in the Inorganic Analytical Research Division and Chemical Thermodynaics Division of NBS. Calorific values were deter- mined by procedures recommended

in standard ASTM° methods.

For the determination of sulfur

in coal

The Sulfur in Coal SRM's are sold individually rather than

in sets; however, only one Certificate of Analysis is provided. Therefore, the user must be careful to use the data specific to the SRM being used. Material should

be stored in a tightly sealed bottle away from sunlight and intense sources of radiation.

7
Table 2. A. Coals - continued.

SRM Material Composition

2683 Sulfur In Coal

( Bituminous)

Obtained from Humphrey Mine, Osage, West Virginia.

Processing same as SRM 2682.

Same as SRM 2682 except: Sulfur (wt. %) 1.85; Furnace

Ash (wt. %) 6.85; Calorific Content 32.70 MJ .Kg .

2684 Sulfur in Coal

( Bituminous)

Obtained from Delta Mine, Marion, Illinois. Processing

same as SRM 2682.

Same as SRM 2682 except: Sulfur (wt. %) 3.00; Furnace

Ash (wt. %) 11.09; Calorific Content 29.68 MJ.Kg

-1

.

2685 Sulfur in Coal (Bituminous)

Obtained from McElroy Mine, Captina, West Virgnia. Processing same as SRM 2682.

Same as SRM 2682 except: Sulfur (wt. %) 4.62; Furnace

Ash (wt. %) 16.53; Calorific

Content 28.15 MJ.Kg .

Rocks, Minerals, and Refractories

1 c Provided by Lone Star Ind., Limestone, ground, sieved, Argillaceous Limestone Inc., Cement and Construction blended. Analyses performed Materials Group, Houston, on 0.5-g or more sample. Texas. Dried 2 hours at 110 °C. SiO 6.84; Fe 0, 0.55; Al 6 1.30; TiO, 0.07;

P 6

5 0.04; MnO 6.025; CaO 50.3; SrO 0.030; MgO 0.42; Na 0 0.02; K-0 0.28; loss on ignition 39.9; all values % by wt

.

70a Feldspar

Feldspar, sample dried 2 hours

at 105 °C. SiO 67.1; Feo 0, 0.07:

Al.,0, 17.9; Cah 3.11; BaO 0:02; Na

2 0 2.5; K

2 0 11.8; Rb-O 0.06; loss on ignition 0.40; all values % by wt

.

76a Burnt Refractory

Provided by Harbison-Walker

Refractories Co., Garber

Research Center, Pittsburgh, Pennsylvania. Dobies were air dried at 120 °C, then fired at

1427 °C for 10 hours. The ground material was converted

to a fine powder (95%, 325 mesh) and was thoroughly mixed.

SiO 54.9; Al 0, 38.7; Fe„0- 1.6; TiO 2.0; Zr0„

0.15; MgO 0.52; CaO 0.22; K„0 1.33; Na0 0 0.07; P„0

L 2 loss on ignition 0.34; values % by wt

.

11

77a

Burnt Refractory

Same as SRM 76a. Si0„ 35.0; A1

2 03 60.2; Fe

2 03 1.0; TiO 2.6; Zr02 0.21; MgO 0.38; CaO 0.05; K 0 0.09; Na o 0.037; P-Oj 0.092; Li

2 0 0.02; SrO 0.009; loss on ignition 0.22; all values % by wt

.
Certification

Same as SRM 2682. Same as SRM 2682, Same as SRM 2682.

Same as SRM 2682. Same as SRM 2682. Same as SRM 2682.

Same as SRM 2682. Same as SRM 2682, Same as SRM 2682.

Chemical analysis performed by eight cooperating laboratories

including NBS-CAC. The esti- mated uncertainty: 0.005 to 0.3 depending on constituent.

For calibration and standardi- zation of analytical methods

and instrumentation.

Issued in cooperation with

ASTM.

Revision of Certificate dated 3-26-65.

Chemical analyses performed by three cooperating laboratories

including NBS-CAC. The values

are not expected to deviate from

the accurate value by more than

+1 in the last significant

figure reported.

For verifying the chemical and instrumental methods of analysis.The loss on ignition is not a certified value but is given

for information only. Issued

in cooperation with ASTM.

Same as SRM 76a. Same as SRM 76a. Same as SRM 76a.

9
Table 2. B. Rocks, Minerals, and Refractories - continued.

SRM Material Composition

Same as SRM 76a.

irnt Refractory

SiO 19.4; Al-O, 71.7;

Fe 6- 1.2; TIG, 3.2; ZrO, 0.31; MgO 0.70; CaO 0.11;

1.22; Na 0 0.078; P 0 1.3 Li

2 0 0.12; SrO 0.25; loss on ignition 0.42; all vaues % by wt

.

Ground glass sand powder 95% less than 106 ym. Blended and dried at 105 °C for 2 hours before use.Al 0. 0.66; Fe 0 0.082; Ti6

2

J 0.12; ZrO^ 0.034; all

values % by wt. Cr o°3 ^6 yg/g.

88a Dolomitic Limestone

Sample dried 2 hours at

110 °C. SiO 1.20; A1„0

0.19; Fe

2 0 6.28; TiO 0.02; MnO 0.03; CaO 30.1; SrO 0.01; MgO 21.3; Na 0 0.01; K-0 0.12;

P

2 0 0.01; C0

2 46.6; loss on ignition 46.7; all values expressed as percent.

97a Provided by A. P. Green Fire Sample dried 2 hours at Flint Clay Brick Co., Mexico, Missouri. 140 °C. Si0

2 43.67; Al o 0 38.79; Fe 0, 0.45; Ti0

2 1.90;

P 0 0.36; Lo 0.50; Na

2 0 0.0V; Li O 6.11; BaO 0.07; MgO 0.15; CaO 0.11; SrO 0.18; Cr 0, 0.03; loss on ignition

13.32; all values are % by wt.

98a Same as SRM 97a. Sample dried for 2 hours at Plastic Clay 140 °C. SiO 48.94; A1„0

33.19; Fe

2 0 1.34; TiO Z 1.61;

P 0 0.11; K

2 0 1.04; Na 0 0.082; Li 0 6.070; BaO 6.03; MgO 0.42; CaO 0.31; SrO 0.039; Cr 0. 0.03; loss on ignition 12.44; all values % by wt

.

99a Sample dried at 105 °C for 2 Feldspar hours. SiO, 65.2; A1

? 0 20.5; Fe„0

3 0.06; TKC 0.007; CaO 2.14; BaO 0.26; MgO 0.02; Na 0 6.2; K^O 5.2; P^

0.62; loss on ignition 0.26; all values are % by wt.

10
Certification Use Remarks

Same as SRM 76a. Same as SRM 76a.

Chemical analyses performed by Same as SRM 76a. The recommended data is the eight cooperating laboratories best estimate of the true including NBS-CAC. value based on data from the cooperators and NBS. Issued in cooperation with ASTM.

Revision of Certificate dated 1-31-67.

Chemical analyses performed by Same as SRM 76a. ZrO^ was determined by only three cooperating laboratories one of the cooperating labora- including NBS-CAC. tories and found to be 0.063

% by wt.

Chemical analyses performed by Same as SRM 76a. ZrO^ was determined by only three laboratories including one of the cooperating labora- NBS-CAC. tories and found to be 0.042

% by wt.

Revision of Certificate dated 3-26-65.

11
Table 2. B. Rocks, Minerals, and Refractories - continued.

SRM Material Composition

103a Sample dried at 110 °C for 2 Chrome Refractory hours. Cr 0 32.06; Al 0. 29.96; Fe0Z 12.43; MnO 0711; MgO 18.54; CaO 0.69; SiO 4.63; TiO 0.22; ZrO 0.01;

P 0 0.01; all values are STby wt.

154b Prepared by Titanium Dioxide Industries, Development

Missouri

.

the National Lead Ti0

2 99.74% by wt . on samples Research and dried 2 hours at 110 °C. Dept., St. Louis,

165a Glass sand blended to insure A1 -> 0 -} 0- 059 ; Fe

? 0- 0.012; Glass Sand homogeneity. Should be dried Ti6

2 0.011; Zr0

2 0.006; all

for 2 hours at 105 °C. values are % by wt

.

198 Al 0 0.16; Fe 0 0.66; Silica Brick TiO 0.02; P 0 0.022; MnO

0.008; CaO 2.71; MgO 0.07; Na 0 0.012; K

2 0 0.017; Li 0 0.001; loss on ignition 0.21 all values % by wt

.

199 M2°3 °' 48; Fe 2°3 0,7A; Silica Brick TiO 0.06; P 0 0.015; MnO

0.007; CaO 2.41; MnO 0.13; Na 0 0.015, K

2 0 0.094; Li 0 0.002; loss on ignition 0.17; all values % by wt

.

278 Natural glass obtained from The material should be dried Obsidian Rock Clear lake, Newberry Crater, to constant weight at 350- Oregon, and processed by the 600 °C. Al 0 14.15; CaO Colorado School of Mines, 0.983; FeO T.36; Fe 0. 2.04; Golden, Colorado, to a powder K 0 4.16; MnO 0.052; Na

2 0 of <200 mesh. 4.84; P o

s 0.036; SiO, 73.05; TiO 0.245; all data wt %. Cu 5.9; Ni 3.6; Rb 127.5; Sr 63.5; Th 12.4; Tl 0.54;

U 4.58; Pb 16.4; data wt (pg/g)'

12
Certification Use Remarks

Chemical analyses performed by eight cooperating laboratories including NBS-CAC.

Certified primarily for use in

the analysis of ores and geological materials containing

chromium.

For additional information on methods used for analysis and certification of constituent

elements see certificate.

Analyses performed by three cooperating laboratories including NBS-CAC. TiO was determined by controlled- potential coulometry and by volumetry. The uncertainty is 0.05 and represented the 95% confidence interval of the mean

of all accepted values.

Certified primarily for appli- cation in the paint and ceramic industries

.

For additional information on

the material and its composition see Certificate.

Chemical analyses performed by eight cooperating laboratories including NBS-CAC.

The certified data is the best estimate of the true value

based on the measurements from

the cooperators and NBS. SRM 165a was issued in cooper- ation with ASTM.

Chemical analyses performed by twelve cooperating laboratories

including NBS-CAC. All results

are based on samples dried at 105-110 °C.

One cooperating laboratory has reported a content of less than 0.01 ZrO % by wt

.

Same as SRM. 198. One cooperating laboratory has reported a content of 0.01 0.01 ZrO, % by wt.

Chemical analyses performed by four cooperating laboratories

including NBS-CAC. Uncertainty

of measurements varies from +0.3 to 0.002 depending on element

.

For evaluation of the accuracy

of analytical methods and instrumentation used in the analysis of geological type materials

.

Additional 21 constituents given but not certified (see certificate).

13
Table 2. B. Rocks, Minerals, and Refractories - continued.

SRM Material Composition

688 Obtained from a Cenozoic basalt Sample dried at 105 °C for 24 Basalt Rock flow near Jackpot, Nevada, and hours. Al

9

°r> 17.36; FeO 7. 64 processed by the Colorado School Fe 9 0„ 10.35, K,0 0.187; MnO

of Mines Golden, Colorado. 0.16^; Na.O 2.15, P-0, 0.134; SiO 48.4; TiO 1.17, all % by

wt. Cr 332; RB 1.91; Sr 169.2 Th 0.33; Pb 3.3, all yg/g.

C. Ores

27f The iron ore was provided by the Total Fe 65.97; SiO. 4.17; Iron Ore (Sibley) U.S. Steel Corp., Pittsburgh, A1 2°3 0,82; P °' 041 > Pennsylvania. The ore was S 0.005; TiO? 0.019; MnO

crushed, dry ground, and sieved 0.011; CaO 0.039; MgO 0.019; at the Colorado School of Mine Na 0 0.012; K„0 0.008; Research Institute, Golden, all values % by wt

.

Colorado, to pass a 150 mesh

sieve with about 50% passing a 200 mesh sieve. Analytical

samples were dried 1 hour at 105 °C.

69b Provided by the Aluminum Company The bauxite powder (<0.08 mm) Bauxite (Arkansas) of America, Bauxite, Arkansas. was dried at 140 °C for 2 The material was processed at hours. Analytical sample of the Colorado School of Mine 1-g or more. Al-O^ ^8.8; Research Institute. Mineral- Fe o°-j 7.14; SiO 13.43; TiO

ogical composition: 30% 1.90; ZrO 0.29; P 0 0.118; kaolinite, 60% gibbsite, 10% V^,. 0.028; Cr,0, 0.011; CaO siderite (semiquantitative). 0.1' ZnO 0.0035; ICO 0.068; SO 0.63; loss of ignition 27.2 at 1050 °C; all values % by wt

.

Estimated uncertainty 0.0005

to 0.2 depending on element.

79a Provided by American Smelting CaF

2 97.39 + 0.06 % by wt Fluorspar and Refining Co., El Paso, Texas, and ground to pass an

80 mesh screen.

14
Certification Use Remarks

Analyses performed by three cooperating laboratories

including NBS-CAC. Uncertainties for % by wt. constituents: from 0.1 to 0.002; for yg/g constituents: 9 to 0.01.

For verifying the accuracy of chemical and instrumental methods

of analysis used in the analysis

of geological type materials.

Chemical analyses performed by For use in verifying chemical Issued in cooperation with seven cooperating laboratories methods of analysis and in ASTM. including NBS-CAC using the calibrating instrumental

methods described in Part 12, methods of analysis. Chemical Analysis of Metals and Metal Bearing Ores, Annual Book

of ASTM Standards.

Chemical analyses performed by eleven cooperating laboratories

including NBS-CAC.

For verification of chemicals

and instrumental methods of analysis

.

Additional composition (not certified): BaO (0.008);

Na 0 (0.025); Ce (0.024); Co (0.0001); Hf (0.0063);

Sc (0.0008). Issued in cooperation with ASTM.

Chemical analyses performed in cooperation with the U.S. Customs Laboratories, Division

of Technical Services, following a standard procedure described in detail in the Certificate.

To assay imported fluorspar for industrial applications. Additional percent composition

(not certified): Fe (0.05-0.1)

Al and Sr (0.01-0.1); Mg (0.01- 0.05); Na (0.001-0.01);

Ba (0.001-0.005); K (<0.005);

Cu, Li, Mn, Pb, and Ti

(<0.001); Si0

2 (0.67); all are % values. Revision of Certificate dated 12-6-71.

15
Table 2. C. Ores - continued.

SRM Material Composition

Provided by Cominco American

Inc., Spokane, Washington, and prepared at the Magmont Mines, Bixby, Missouri, in the form of powder (<0.15 mm).

Sample dried 1 hour at 105 °C. Zn 57.3; Co (0.11); Ni (0.07);

S 30.6; Cd 0.78; Cu 0.31;

Pb 2.80; Fe 2.08; CaO 1.1; MgO 0.75; SiO (1.54); Ag 0.046, all values are % by wt.

120b Phosphate Rock (Florida) Provided by American Cyanamid

Co. as a powder to pass 200 mesh sieve.

Sample dried 1 hour at 105 ° C.

P^O,- 34.57; CaO 49.40; SiO4t6g; F 3.84; Fe-O, 1.10; Al 0, 1.06; MgO 6.28; Na

? 0 0.35; MnO 0.032; ICO 0.12-

0.090; Ti0

2 0.15; C0? 2.79; CdO 0.002; all values are % by

wt. Uranium 128.4 yg/g.

180 Provided by Minera Frisco of CaF

2 98.80 + 0.03 % by wt. High-Grade Fluorspar San Francisco Del Oro, Chih., Mexico

.

181, 182, 183 Fine powder of spodumene (SRM Li 0 wt . % in SRM 181 - 6.3

q

; Lithium Ores 181), petalite (SRM 182), and SRM 182 - 4.3 ; and SRM 183 - lepidolite (SRM 183). 4.1..

277 Provided by GTE Sylvania, W0

3 - 67.4 wt. %, determined Tungsten Concentrate Towanda, Pennsylvania, as a on 1-g or more sample. powder sieved (<0.15 mm) and blended. It is a mixture of con- centrates from China, Thailand,

and USA.

329 Provided by Cominco American Sample dried 1 hour at 105 °C. Zinc Concentrate Inc., Spokane, Washington, and Zn 45.5; Pb 6.06; Fe 12.94; prepared at the Sullivan Mine, CaO 0.08; MgO 0.16; Cd 0.14; Trail, B.C., Canada, in the Cu 0.13; Co (0.009); Ni form of powder (<0.15 mm). (0.006); S (31.7); SiO (0.61) In 0.019; Ag 0.0089; all values are % by wt.

16
Certification Use Remarks

Chemical analyses performed by four cooperating laboratories including NBS-CAC. The data are not expected to deviate

from the true value by more than +1 in the last significant figures reported.

Intended for the verification

of chemical and instrumental

methods of analysis.

Figures in parentheses are not certified. Should be kept tightly closed except when in direct use. Store in a desiccator over desiccant.

Chemical analyses performed by For the verification of chemical For potassium values see six cooperating laboratories optical emission and x-ray spec- Certificate, including NBS-CAC. Uranium was trometric methods of analysis, determined at NBS by thermal ionization mass spectrometry.

Additional trace elements

detected but not certified:

Fe 0.1-1.0; Al, Ba, Mg, Pb, Si, and Sr 0.01-0.1; Cu, K, Mn, Na, Ti, and V 0.001-0.01; Ag and Li

less than 0.001; all values expressed in percent.

Issued primarily for geochemical

use

.

Detailed information on the method used for the determination of CaF is given in the Certificate.

The deviation from given values For verifying the accuracy of Revision of Certificate dated

is not expected to be more than assay methods. 2-24-58.

+5 subscript number.

Chemical analyses performed in To verify the accuracy of Issued in cooperation with cooperation with 13 labora- chemical and instrumental ASTM. tories including NBS-CAC. The methods of analysis, estimated uncertainty 0.3 wt.

%. Additional elements indicated but not certified are: Ca, Fe, Pb, Mn, Nb, P, Si, S, Sn, Ti, As, Mo, Bi, Ce, Cr, Cu, Gd, La, Nd, 0, Sc, Ta, Th, U, Y, and

Zr.

Chemical analyses performed by Intended for the verification Figures in parentheses are not four cooperating laboratories of chemical and instrumental certified. including NBS-CAC. The data methods of analysis. are not expected to deviate

from the true value by more than +1 in the last significant

figure reported.

17
Table 2. C. Ores - continued.

SRM Material Compos ition

330 Copper Ore, Mill Heads

Provided by Magma Copper Co., San Manuel, Arizona. It was sieved and blended at NBS.

Sample dried at 105 °C for 2 hours. Cu 0.8A; Mo 0.018; both values % by wt. Re 0.30 ppm by wt . Not certified: Au (0.093); Ag (1.51) ppm by wt

.

331 Copper Ore, Mill Tails Provided by Magma Copper Co., San Manuel, Arizona.

Cu 0.091; Mo 0.0022; both % by

wt. Re 0.04 ppm by wt . on samples dried at 105 °C for 2 hours. Not certified: Au (0.034); Ag (0.243) ppm by wt

.

332 Copper Concentrate

Provided by Magma Copper Co., San Manuel, Arizona.Cu 28.4; Mo 0.64 % by wt

.

Re 10.2 ppm by wt . on samples dried at 105 °C for 2 hours.

Not certified: Au (2.14); Ag (38.7) ppm by wt

.

333 Molybdenum Concentrate

Provided by Magma Copper Co., San Manuel, Arizona. Homo- geneity obtained by special blending and mixing procedures.Cu 1.038; Mo 55.3; Re 0.087; all % by wt . on samples "as received." Not certified:

Au (8.9); Ag (25.0) ppm by wt

.

690 Iron Ore Concentrate

( Canada

)

Provided by the Iron Ore Company of Canada, Labrador

City, Newfoundland, Canada, as

a powder (<0.1 mm).

Fe 66.85; SiO 3.71; Al-0,

0.18; P 0.011; S 0.003; TiO

? 0.022; MnO 0.23; CaO 0.20; MgO 0.18; Na

2o 0.003; K,0

0.0030, on samples dried at 105 °C for 1 hours. All values are % by wt.

691 Reduced Iron Oxide Provided by Allis-Chalmers

,

Reduction Systems Div., Milwaukee, Wisconsin, and processed as a powder (-200 mesh) at the Colorado School

of Mines Research Institute,

Golden, Colorado.

Values based on 0.5-g or more

sample size. Fe, total 90.8;

Fe, metallic 84.6; SiO 3.7;

Al 0 1.22; TiO 0.27; CaO

0.53; MnO 0.043; MgO 0.52; Na 0 0.186; Cu 0.032; Co 0.030

P 0.006; S 0.008; C 0.12; all values % by wt . Not certified

11 additional constituents

(see certificate).

692 Iron Ore (Labrador)

Prepared by the Bethlehem

Steel Corp., Bethlehem, Pennsylvania, as a fine powder

( 200 mesh).

Sample dried 1 hour at 105 °C, values based on 0.5-g or more

sample. Fe 59.58; SiO 10.14;

Al 0- 1.41; P 0.039; S 0.005; Ti6

2 0.045; MnO 0.46; CaO 0.023; MgO 0.035; Na 0 0.008; K

2 0 0.039, all values % by wt

.

18
Certification

Analyses performed by two coop- erating laboratories including

NBS-CAC. Estimated uncertainty

0.01 and 0.001 for Cu and Mo, and 0.06 for Re.

For verifying the accuracy of chemical and instrumental

methods of analysis, and for evaluation of the material

balance in copper mining and metallurgical industries.

Keep the material tightly

closed in a desiccator over desiccant. Revision of Certificate of 2-20-73.

Estimated uncertainty 0.001 for Same as SRM 330. Same as SRM 330.

Cu; 0.0002 for Mo; and 0.02 for

Re.

Estimated uncertainty 0.1 for Same as SRM 330. Same as SRM 330, except

Cu; 0.01 for Mo; and 0.2 for Re. revision of Certificate dated 2-20-73 and 1-20-77.

Analyses performed by two Same as SRM 330. Same as SRM 330. cooperating laboratories in- cluding NBS-CAC. Estimated uncertainty 0.010 for Cu; 0.1 for Mo; 0.001 for Re.

Analyses performed by six For verifying the chemical and Issued in cooperation with cooperating laboratories in- instrumental methods of ASTM. eluding NBS-CAC. Estimated analysis, uncertainty from 0.0005 to 0.01 depending on constituent.

Analyses performed by six cooperating laboratories in- cluding NBS-CAC. Estimated uncertainty 0.001 to 0.6 depending on constituent.

For the evaluation of chemical

and spectroscopic methods of analysis

.

Material packaged in dry nitrogen to prevent oxidation.

Should be stored in desiccator

over desiccant. Issued in cooperation with ASTM.

Analyses performed by six For verifying the chemical and Issued in cooperation with

cooperating laboratories in- instrumental methods of ASTM. eluding NBS-CAC. Estimated analysis, uncertainty 0.001 to 0.06 depending on constituent.

19
Table 2. C. Ores - continued.

SRM Material Composition

693 Prepared by the Bethlehem Sample dried 1 hour at 105 °C, Iron Ore Steel Corp., Bethlehem, values based on 0.5-g or more

(Nimba) Pennsylvania, as a fine powder sample. Fe 65.11; SiO 3.87; (200 mesh). Al 0. 1.02; P 0.056; S 0.005; TiO 0.035; MnO 0.091; CaO

0.016; MgO 0.013; Na O 0.0028; K 0 0.0028; all values % by wt

The bauxite powder (<0.08 mm) was dried at 140 °C for 2 hours. Analytical sample of 1-g or more. Al 0 54.5; Fe 0. 8.70; Si0„ 3.79; TiO

2.54; ZrO 0.14; P 0 0.050;

V 0 0.072; Cr„0 0.047; CaO

0.018; MgO 0.012; MnO 0.004; ZnO 0.0014; ICO 0.009; SO 0.21; loss on ignition 29.9 at 1050 °C; all values % by wt. Estimated uncertainty 0.0007

to 0.3 depending on element.

The bauxite powder (< 0.08 mm) was dried at 140 °C for 2 hours. Analytical sample of

1-g or more. A1„0„ 45.8;

Fe 0, 20.0; Si0„ 6.81; TiO

2.52; ZrO 0.065; P 0 0.97;

V 0 0.063; Cr 0 07100; CaO

0.71; MgO 0.18; MnO 0.41; ZnO

0.037; K

2 0 0.062; SO 0.13; loss on ignition 22.1 at 1050 °C. All values % by wt

.

Estimated uncertainty 0.2 to 0.003 depending on element.

698 Mined in Jamaica, provided by The bauxite powder (<0.08 mm) Bauxite Reynolds Metals Co., Bauxite, was dried at 140 °C for 2 (Jamaican) Arkansas, processed at the hours. Analytical sample of Colorado School of Mines 1-g or more. Al

? 0. 48.2; Research Institute. Mineral- Fe 0, 19.6; SiO 0.69; TiO ogical composition: 75% 2.38; ZrO 0.061; P-0 0.37; gibbsite, 20% hematite, 5% V 0 0.064; Cr 0 0.080; CaO anatase (semiquantitative). 0.62; MgO 0.058; MnO 0.38; ZnO 0.029; K 0 0.010; SO- 0.22; loss on ignition 27.3 at 1050 °C. All values % by wt. Estimated uncertainty 0.002 to 0.4 depending on element.

696 Same as SRM 69b. The material Bauxite was mined in Surina, South (Surinam) America. Mineralogical composition: 5% kaolinite, 80% gibbsite, 10% pyrite, 5% anatase (semiquantitative).

697 Same as SRM 69b. The material Bauxite was mined in the Dominican

(Dominican) Republic. Mineralogical compo- sition: 15% kaolinite, 50% gibbsite, 10% boehmite, 5% anatase; 20% hematite (semi- quantitative )

.

20
Certification Use Remarks

Analyses performed in coopera- Same as SRM 692. Same as SRM 692. tion with five laboratories

including NBS-CAC. Estimated uncertainty 0.0005 to 0.07 depending on constituent.

Same as SRM 69b. Same as SRM 69b. Additional composition (not certified): BaO (0.004); Na 0 (0.007); Ce (0.0041);

Co (0.00009); Hf (0.0032); Sc (0.0008). Issued in coop- eration with ASTM.

Same as SRM 69b. Same as SRM 69b. Additional composition (not certified): BaO (0.015); Na 0 (0.036); Ce (0.069); Co (0.0013); Hf (0.0014);

Sc (0.0058). Issued in coop- eration with ASTM.

Same as SRM 69b. Same as SRM 69b. Additional composition (not certified): BaO (0.008); Na 0 (0.015); Ce (0.030); Co (0.0045); Hf (0.0015); Sc (0.0051). Issued in coop- eration with ASTM.

21
Table 3. Composition of SRM's Prepared from Ores, Minerals, Rocks, and Refractories (listed by chemical constituents and category).

Constituents

AliO. BaO C (Total) CdCdO

CaO

Co

CO, Cu

Cr,0, F

27f

Iron ore, Sibley, 100 g

0.82

Composition of ore SRMs 3 SRM type, wt/unit

Canada,

150 g

0.18

reduced, 100 g

1.22

Labrador, 150 g

Iron ore, Nimba,

150 g

1.02 60 g48.8

(0.008)"

.13

(.0001)

HfFe (Total) FejO. PbCeMgO

MnO

P

NiP ; 05 KiO

SiOi Ag

Na,0

S

ScSO=

TiO> UV,0) wo,

ZnZnO

ZrO. Loss on

ignition Moisture

0.019

.011

.041

0.012

.005

0.18

.23 .011

.0030

3.71

0.003

.003

0.52

.043

.006

0.035

.46

0.008

.005

0.013

.091 .056

0.0028

.005

(.0063)

7.14

(0.024) .085

13.43

(0.025)

(.0008)

.63 1.90

.0035

.29 27.2

22
Constituents

Al,0, BaO C (Total) CdCdO

CaO

Co

CO, Cu

Cr,0,

696

Bauxite, Surinam, 60 g

54.5

(0.004)

Bauxite, Dominican,

45.8

(0.015)

.71 (.0013)

SRM type, wt/unit 120b Phosphate

rock, Fla., 90 g

1.06

.62 (.0045)

0.002

49.40

277 Tungsten cone,

100 g Ta (0.20)

Zinc ore 100 g'

1.1g

(0.11)

Zinc 100 g'

InHfFe (Total) Fe,0,

MgO

MnO

P

NiP,0, KiO

SiO, Ag

Na>0

S

ScSO,

TiO, U

V,0, WO,

ZnZnO

ZrO, Loss on

ignition Moisture

(.0032)

8.70

(0.0041) .012

.050

.009

3.79

(0.007)

(.0008)

.21 2.64

0.072

.0014

(.0014)

20.0

(0.069) .18

.062

6.81

(0.036)

(.0058) .13 2.52

0.063

.037

(0.030) .058

.38

.37 .010

.69

(.015)

(.0051) .22 2.38

0.064

.061 27.3

0.28

.032

34.57

0.12 4.68

(7.4)

(0.07)

Mn (10.0) (0.03)

O, (21.4) Ti (2.2) Mo (0.06) 67.4

2.80

0.75

(1-54) 0.0467

0.45

"Concentrations expressed in wt<7o unless noted otherwise. *Values in parentheses are not certified, but are given for information only.

23
Composition of rock, mineral, and refractory SRMsa SRM type, wuunlt

1C 88a 70a 99a 97a 98a 81a 165a Limestone, Limestone, Feldspar, I Feldspar, Clay, Clay, Glass sand,

argillaceous, 0lolomitlc, potash, soda, flint plastic Glass sand, (low Iron), Constituents 40 g 40 g 60 g 60g 75 g AI1O1 1.30 0.19 17.9 20.5 38.79 33.19 0.66 0.059 BaO 0.02 0.26 0.075

0.03 CaO 50.3 30.1 5

.11 2.14 .11 .31 .03 .03 46 nQlg b

(l.l) jig/g COj FeO

~~ 46.6 ~ ~

FeiOj 0.55 0.28 0.0750.0650.45 1.34 0.082 0.012

LiiO — .11 0.070 MgO 0.42 21.3 z .02 .15 .42 MnO .025 0.03 - -

PjO, .04 .01 — .02 .36 .11 —

KjO .28 .12 11.8 5.2 .50 1.04 —

RbiO - 0.06 —

SiOi 6.84 1.20 67.1 65.2 43.67 48.94 —

Na,0 0.02 0.01 2.556.2 0.037 0.082 —

SrO .030 .010 — .18 .039 TiOi .07 .02 0.10 0.007 1.90 1.61 .12 0 ' 1 ZrOi — — .034 .006 Loss on 39.9 46.7 .40 .26 13.32 12.44

ignition SRM type, wt/unit 1S4b 278 688 76a 77a 78a 103a 198 199 Burnt Burnt Burnt Titanium Obsidian Basalt refractory. refractory, refractory. Chrome Silica dioxide, rock, rock, (AI.O.—40%) (^1,0.-60%) (Al iOj— 70%) refractory, refractory, refractory, Constituents 90 g 35 g 60g 75 g 75 g 75 g 60 g 45 g 45 g AUO, 14.15 17.36 38.7 60.2 71.7 29.96 0.16 0.48 BaO CaO 0.983 0.22 0.05 0.11 0.69 2.71 2.41 Cr,Oj 32.06 CO, FeO 12.43 Fe,03 2.04 10.35 1.60

1.00

1.2 0.66 0.74 LbO 0.042 0.12 .001 .002 MgO .52 .38 .70 18.54 .07 .13 MnO 0.052 0.167 0.11 .008 .007 P,Os .036 .134 0.12Q

0.092 1.3 .01 .022 .015 K2O 4.16 .187 1.33 ,090

1.22 .017 .094 Rb.O

SiO= 73.05 48.4 54.9 35.0 19.4 4.63 Na,0 4.84 2.15 0.07 0.037 0.078 .012 .015 SrO .037 .009 .25 TiO: 99.74 0.245 1.17 2.O3 2.66

3.22

0.22 .02 .06 ZrO, 0.15 0.21 0.31 0.01 Loss on (0.34) (0.22) (0.42) .21 .17 ignition

"Concentrations expressed in wt<Co unless noted otherwise. 'Numbers in parentheses are not certified, but are given for information only.

24
Composition of ore standard reference materials'

SRM.Type, wUunit

79a 180 181 182 183 330 331 332 333

Fluorspar, Fluorspar, Lithium Molybhigh ore ore ore ore ore Copper

Constitu- grade, grade, (spodumene), (pelalite), (lepidolite). mill heads, mill tails, cone, conc,

enls 120 g 120 g 45 g 45 g 45 g 100 g 100 g 50g 35 g CaF, 97.39 98.80

Li.0 6.3g 4.3 4.1 Cu 0.84 0.091 284 1.038 Re .30ppm .04ppm 10.2 ppm .087 Mo .018 .0022 .64 55.3

(0.93) ppm" (.034) ppm (2.14) ppm (8.9) ppm

Ag (1.51)ppm (.243) ppm (38.7) ppm (25) ppm

"Concentrations expressed in wt percent unless noted otherwise. ^Values in parentheses are not certified, but are given for information only.

25
Table 4. NBS Publications in the "260 Series" Related to Coal, Ore, Mineral, Rock, and Refractory Standards

260-8 Analysis of Uranium Concentrates at the National Bureau of Standards

260-37 Methods of Analysis of NBS Clay Standards 97a, 98a 260-94 Methods and Procedures Used at the National 2682, 2683, 2684, 2685 Bureau of Standards to Certify Sulfur in Coal SRM's for Sulfur Content, Calorific Value, Ash Content

ACKNOWLEDGMENT

The authors gratefully acknowledge the contributions of Ms. Julie Frum who prepared this manuscript for publication.

26
Appendix I. Alphabetical Index by Standard Reference

Material Name

Name SRM Name SRM

Acetanilide 141c Aluminum, Freezing Point Standard 44f Acid Open-Hearth Steel, 0.2% Carbon 19G Aluminum, Magnetic Gram 763 Acid Potassium Phthalate 84j Susceptibility AISI 1045 Steel 20g Aluminum Oxide, Melting Point 742 AISI 4340 Steel 361 Aluminum Rod Ultra Purity RM 1R

AISI 4340 Steel 1261a Aluminum-26 Radioactivity Standard 4229 AISI 94B17 Steel (Modified) 362 Americium-241 Alpha-Particle 4904F

AISI 94B17 Steel (Modified) 1262a Standard Albacore Tuna RM 50 Americium-241 Gamma-ray Standard 4213

Alkali Lead Silicate Glass 712 Ammonium Dihydrogen Phosphate 194 Alpha Quartz 1878 Angiotensin I (Human) 998 Alumina (Reduction Grade) 699 Anisic Acid 142 Alumina Silicate Glass 714 Anticonvulsant Drug Level Assay 1599

Aluminosilicate Glass Standard Aluminum Alloy 85B Antiepilepsy Drug Level Assay 900 Aluminum Alloy 6011 (Modified) 858 Standard Aluminum Alloy 601 1 (Modified) 1258 Antimony-125-Tellurium-125m, 4275B Aluminum Alloy 7075 859 Europium- 154, Europium- 155 Mixed- Aluminum Alloy 7075 1259 Radionuclide Point-Source Standard Aluminum Block, Eddy Current 1860 Antimony- 1 25-Tellurium- 1 25m, 4276B

Conductivity Europium- 154, Europium- 155 Mixed- Aluminum Block, Eddy Current 1861 Radionuclide Solution Standard

Conductivity A.O.H., 0.4C Spectrographic Steel 413 Aluminum Block, Eddy Current 1862 Standard

Conductivity Argillaceous Limestone IC Aluminum Block, Eddy Current 1863 Arsenic Trioxide Reductometric 83d Conductivity Standard Aluminum Brass Standard for 1118 Assay-Isotopic Standard for Potassium 985

Optical Emission and X-ray Assay-Isotopic Standard for Rhenium 989

Spectroscopic Analysis Assay-Isotopic Standard for Silicon 990 Aluminum Brass Standard for CI 1 18 Assay-Isotopic Standard for Strontium 987

Optical Emission and X-ray 2% Austenite in Ferrite 488

Spectroscopic Analysis 5% Austenite in Ferrite 485a Aluminum Brass Standard for 1119 15% Austenite in Ferrite 486

Optical Emission and X-ray 30% Austenite in Ferrite 487

Spectroscopic Analysis Aluminum Brass Standard for CI 1 19 Optical Emission and X-ray

Spectroscopic Analysis Aluminum Casting Alloy 356 855 Aluminum Casting Alloy 380 856 Aluminum Cube Ultra Purity RM IC Aluminum 2-Ethylhexanoate 1075a

27
Name SRM

Austenitic Stainless Steel, Thermal 1460 Conductivity and Electrical

Resistivity Austenitic Stainless Steel, Thermal 1461 Conductivity and Electrical

Resistivity Austenitic Stainless Steel, Thermal 1462 Conductivity and Electrical

Resistivity Barium Crown Glass 713 Barium Cyclohexanebutyrate 1051b Barrium-133 Radioactivity Point-Source 4241B

Standard Barium-133 Radioactivity Standard 4251B

Basalt Rock 688

Base Oil 1083

Basic Electric Spectrographic Steel 404a

Standard

Basic Open-Hearth Steel, 0.1% Carbon 15g

Basic Open-Hearth Steel, 0.1% Carbon 335

Basic Open-Hearth Steel, 0. 1 % Carbon 1 228

Basic Open-Hearth Steel, 0.2% Carbon 1 lh Basic Open-Hearth Steel, 0.4% Carbon 12H

Basic Open-Hearth Steel, 0.5% Carbon 152A

Basic Open-Hearth Steel, 0.8% Carbon 14f Basic Open-Hearth Steel, 1% Carbon 1227

(Disk)

Basic Open-Hearth Steel, 1.1% Carbon 16f Basic Open-Hearth Steel, 1.1% Carbon 337 0.4C Basic Oxygen Furnace Steel 178 Bauxite (Arkansas) 69b

Bauxite (Dominican) 697

Bauxite (Jamaican) 698

Bauxite (Surinam) 696 Benzene in Nitrogen 1805 Benzene in Nitrogen 1806 Benzene Permeation Device 1911 Benzoic Acid 140b Benzoic Acid 350a Benzoic Acid Calorimetric Standard 39i Benzothiazyl Disulfide Rubber 373f Compound

Beryllium-Copper Standard 1122 Beryllium-Copper Standard CI 122 Beryllium-Copper Standard CI 123

Name SRM

Beryllium on Filter Media 2675 Bessemer Steel (Simulated) 8j 0.1% Carbon

Bilirubin 916

Bis(l -phenyl- 1, 3-butanediono) 1080a copper (II) Bis(l -phenyl- 1, 3-butanediono) 1052b oxovanadium (IV) Black Porcelain Enamel for Directional 2021 Hemispherical Reflectance Black Porcelain Enamel for Directional 2022 Hemispherical Reflectance

Blast Furnace Iron Standard 1143a

(Chill Cast White)

Blast Furnace Iron Standard 1144a

(Chill Cast White)

B.O.H., 0.4C Spectrographic Steel 417a

Standard

Boric Acid 951 Boron-Doped Silicon Slices for 1521

Resistivity Measurements

Borosilicate Glass 93a

Borosilicate Glass 623

Borosilicate Glass 717

Borosilicate Glass 1825

Borosilicate Glass, Thermal Expansion 731 Bovine Liver 1577a Bovine Serum Albumin 926 Bovine Serum Albumin (7% Solution) 927 Branched Polyethylene 1476 Brewers Yeast 1569

Bright Copper Microhardness 1894 Standard

Bright Nickel Microhardness Standard 1895 Bromobenzoic Acid 2142 Burnt Refractory 76a Burnt Refractory 77a Burnt Refractory 78a Cadmium Cyclohexanebutyrate 1053a Cadmium, Vapor Pressure 746 Calcium Carbonate 915 Calcium 2-Ethylhexanoate 1074a Calcium in Low-Alloy (Silicon) Steel 1254 Calcium Molybdate 71 Calibrated Glass Beads 1004

Calibrated Glass Beads 1017a

Calibrated Glass Beads 1018a

Calibrated Glass Spheres 1003a Carbon Dioxide in Air 1670 Carbon Dioxide in Air 1671 Carbon Dioxide in Air 1672 Carbon Dioxide in Nitrogen 1674b Carbon Dioxide in Nitrogen 1675b Carbon Dioxide in Nitrogen 2619a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2620a (Combustion Efficiency Gas Standard)

28
Name SRM

Carbon Dioxide in Nitrogen 2621a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2622a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2623a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2624a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2625a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen 2626a (Combustion Efficiency Gas Standard) Carbon Dioxide in Nitrogen (Mobile 2632 Source Emission Gas Standard) Carbon Dioxide in Nitrogen (Mobile 2633 Source Emission Gas Standard) Carbon Monoxide in Air (Ambient 2612a

Air Quality Gas Standard) Carbon Monoxide in Air (Ambient 2613a

Air Quality Gas Standard) Carbon Monoxide in Air (Ambient 2614a

Air Quality Gas Standard) Carbon Monoxide in Nitrogen 1677c Carbon Monoxide in Nitrogen 1678c Carbon Monoxide in Nitrogen 1679c Carbon Monoxide in Nitrogen 1680b Carbon Monoxide in Nitrogen 1681b Carbon Monoxide in Nitrogen (Mobile 2635 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2636

Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2637 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2638 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2639 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2640 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2641 Source Emission Gas Standard) Carbon Monoxide in Nitrogen (Mobile 2642 Source Emission Gas Standard) Carbon- 14 Radioactivity Standard 4245 Carbon-14 Radioactivity Standard 4246 Carbon Steel 1224 Carbon Steel, 0.6% i3g

Cast Iron 4^

Cast Iron 5L

Cast Iron 6g

Cast Iron 70

Cast Iron Car Wheel ]22h

Cast Steel 3 CI 173 Cast Steel Standard 1138a

Cast Steel Standard 1139a

Name SRM

Catalyst Package for Lubricant 1817 Oxidation

Centerline Drawings for Optical 1901 Character Recognition, B

Characters Centroid Color Chart 2106

Centroid Color Kit 2107 Cesium- 137, Barium- 137m Point-Source 4200B

Radioactivity Standard

Cesium-137, Barium-137m Point-Source 4207

Radioactivity Standard Cesium-137 Burn-Up Standard 4233B

Cesium- 134 Radioactivity Standard 4250B

Channel Black Rubber Compound 375g

Chlorine-36 Beta-ray Standard 4943

Chlorine-36 Radioactivity Standard 4422L

Chlorobenzoic Acid 2144 Chrome Refractory 103a Chromium-Molybdenum-Aluminum 106B

Steel Chromium-Molybdenum Steel 36b Chromium-Molybdenum Steel 133B Chromium-Nickel-Molybdenum Steel 139b Chromium-Nickel-Molybdenum Steel 1222 17Chromium-9 Nickel-0.2 Selenium Steel 339 Chromium-Nickel Spectrographic Steel 408a

Standard 15Chromium-7 Nickel Steel 344 16Chromium-4 Nickel Steel 345 Chromium-51 Radioactivity Standard 4400L-F Chromium Steel 163 Chromium-Tungsten Steel 155 Chromium-Vanadium Spectrographic 407a

Steel Standard

Cholesterol 911a

Chrysotile Asbestos Fibers 1876

Citrus Leaves 1572

Clinical Laboratory Thermometer 934

Cobalt Cyclohexanebutyrate 1055b Cobalt-Molybdenum-Tungsten Steel 153A

Cobalt-57 Radioactivity Standard 4408L-C

Cobalt 60 Radioactivity Standard 4915D

Commerical Bronze Standard for 1115 Optical Emission and X-ray

Spectroscopic Analysis Commercial Bronze Standard for CI 1 15 Optical Emission and X-ray

Spectroscopic Analysis Commercial Bronze Standard for 1116

Optical Emission and X-ray

Spectroscopic Analysis

29
Name

Commercial Bronze Standard for Optica] Emission and X-ray

Spectroscopic Analysis Commercial Bronze Standard for Optical Emission and X-ray

Spectroscopic Analysis Commercial Bronze Standard for Optical Emission and X-ray

Spectroscopic Analysis Common Lead Isotopic Standard Copper Concentrate Copper Heat Capacity Test Specimen

Copper-Nickel-Chromium Cast Iron Copper Ore, Mill Heads Copper Ore, Mill Tails Copper-Thermal Expansion

Copper, Secondary Freezing Point Standard

Cortisol (Hydrocortisone)

Creatinine Cr-Mo Low Alloy Steel Cr-Mo Steel (ASTM A-213) Cr-Mo (SAE 4140) Spectrographic

Steel Standard Cr-Mo (SAE 4150) Spectrographic

Steel Standard Cr-Mo (SAE X4130) Spectrographic

Steel Standard Cr-Ni-Mo Steel (AISI 8620) 18Cr-10Ni Steel (AISI 304L) Cr-V Steel (Modified) Cr-V Steel (Modified) Cr-V Steel (SAE 6150)

Crystalline Potassium Dichromate

Crystalline Potassium Iodide, Heterochromatic Stray Radiant Energy Standard

Crystalline (Ruby) Electron Paramagnetic Resonance

Absorption Intensity Standard Cupro-Nickel (CDA 706) Cupro-Nickel (CDA 715) Cupro-Nickel, 10% (CDA 706) Doped

SRM Name SRM

CI 1 16 Cupro-Nickel, 10% (CDA 706) High 874 c

P

|

ir ' ty 143c

1117 Dextr 41b D^lucose 917

Dibutyltin Bis(2-ethylhexanoate) 1057b CI 1 17 2009

the Wavelength Scale of Spectrophotometers

981 2010

332 the Wavelength Scale of Spectrophotometers n^A Disodium Hydrogen Phosphate 18611c 330 Disodium Hydrogen Phosphate 2186II

331 D-Mannitol 920

Dolomitic Limestone 88a Ish* Doped Platinum 681L1 Doped Platinum 681L2

341 914 Electrical Residual Resistivity Ratio 769

1270 Standard

291 365 414 Electrolytic Iron 1265a

Electrolytic Iron, Thermal 1463 427 Conductivity and Electrical

Resistivity a 1464 ^'cond'uctivi^and ^Electrical 293 Resistivity' ^ ^

101 f Electronic and Magnetic Alloy 1159 Standard ^Standard

3"'1 Magnet' C A"°y 1 160

f 3 935 Enriched Boric Acid 952 2032 Equal-Atorn Lead Isotopic Standard 982

Estuarine Sediment 1646 Europium- 152 Point-Source Standard 4218E

2601 Europium- 152 Radioactivity Standard 4370B

Extra Dense Lead Glass 709 Fe-Cr-Ni Alloy Microprobe Standard 479a

1275 Fe-3Si Alloy Microprobe Standard 483

1276 Feldspar 70a

875 Feldspar 99a Ferrochromium (Low Carbon) 196 Ferrochromium Silicon 689 Ferroniobium 340 Ferrophosphorus 90

Ferrosilicon 58a

Ferrosilicon 59a

Ferrosilicon (75% Si) 195

First Surface Aluminum Mirror for 2003a

Specular Reflectance

First Surface Mirror, Gold on Glass 2008a

30
Name SRM Name SRM

Fission Track Glass Standard 961 Gold-198 Radioactivity Standard 4405L-B

Fission Track Glass Standard 962a Gold-Silver Wires for Microprobe 481

Fission Track Glass Standard 963a Analysis

Fission Track Glass Standard 964 Gold, Vapor Pressure 745

Flint Clay 97a Gray Cast Iron 334 Fluorobenzoic Acid 2143 Halocarbons (in methanol) for Water 1639 Fluorspar 79a Analysis Free-Cutting Brass 1 103 High-Alloy Steel (A-743) C1288

Free-Cutting Brass C1104 High-Alloy Steel (AISI 310 Mod.) C1287

Freeze-Dried Urine 2670 High-Alloy Steel, (AISI 414 Mod.) C1289

Freeze-Dried Urine Certified 2671a High-Alloy White Cast 892

for Fluoride High-Alloy White Cast Iron 890

Freeze-Dried Urine Certified 2672a High-Alloy White Cast Iron 891

for Mercury High-Carbon Ferrochromium 64c

Fused-Silica Thermal Expansion 739 High-Carbon Ferromanganese 68c

( radolinium-148 Alpha-Particle 4907 High-Carbon Steel (Modified) 364 Standard High-Carbon Steel (Modified) 1264a Gallium Melting-Point Standard 1968 High-Grade Fluorspar 180 Gallium-67 Radioactivity Standard 4416L-D High-Nickel Steel 126c Gas Furnace Black Rubber Compound 382a High-Nickel Steel 1 158 Gasometric Set (1095-1099) 1089 High-Purity Gold 685 Gasometric Standard for Unalloyed 357 High-Purity Platinum 680L1A

Zirconium High-Purity Platinum 680L2A

Gasometric Standard for Unalloyed 358 High-Purity Platinum Thermoelement 1967 Zirconium High-Purity Zinc 682 Generator Columns for Polynuclear 1644 High-Silicon Steel 179 Aromatic Hydrocarbons High-Silicon Steel 1 134 Gilding Metal ' 2 High-Silicon Steel 1 135 Gilding Metal

li V

High-Silicon Steel (Calcium Bearing) 125b Gilding Metal High-Sulfur Steel 105 Gilding Metal r i 1 1 > High-Sulfur Steel 129c

11 14 High-Sulfur Steel 1 136 Gilding Metal ri 114 High Temperature Alloy A286 348

Glasses for Microchemical Analysis 1871 High Temperature Alloy M308

1872 SI 199 Glasses for Microchemical Analysis 1873 S816

Glasses for Microchemical Analysis 1874 High-Temperature Alloy 1206-2 Glasses for Microchemical Analysis 1875 High-Temperature Alloy 1207-1 Glass Fibers for Microanalysis RM 31 High-Temperature Alloy 1207-2 Glass Filter for Transmittance 2030 High-Temperature Alloy 1208-1 Measurement High-Temperature Alloy 1208-2 Glass Filters for Spectrophotometry 930D Homogeneous River Sediment for RM 45B

Glass Fluorescence Source 477 Radioactivity Measurements

Glass Sand 81a Human Liver, Environmental 4352

Glass Sand 165a Radioactivity Glass Spheres 1019a Human Lung, Environmental 4351 Gold Coating on Glass Sealing Alloy 1398a Radioactivity Gold Coating on Nickel 1379 Human Serum 909 Gold Coating on Nickel 1380 Gold Coating on Nickel 1399b Gold-Copper Wires for Microprobe 482

Analysis Gold-195 Radioactivity Standard 4421L

31
Name

Hydrogen in Unalloyed Titanium Hydrogen in Unalloyed Titanium Hydrogen in Unalloyed Titanium Hydrogen in Unalloyed Titanium Hydrogen-3 Radioactivity Standard Hydrogen-3 Radioactivity Standard Hydrogen-3 Toluene Radioactivity Standard 4-Hydroxy-3 methoxy-DL-mandelic

Acid (VMA)

ICTA High Temperature Set

Differential Thermal Analysis ICTA Low Temperature Set Differential Thermal Analysis ICTA Mod Temperature Set Differential Thermal Analysis ICTA Mid Temperature Set Differential Thermal Analysis ICTA Polystyrene Differential Thermal Analysis ICTA Thermogravimetry Set Incoloy, 901 and Hastelloy X

Inconels, Alloy 600 (Chips)

Inconels, Alloy 600 (Solid) Inconels, Alloy 625 (Chips)

Inconels, Alloy 625 (Solid) Incoloy, Alloy 800 (Chips)

Incoloy, Alloy 800 (Solid) Incoloy, Alloy 825 (Chips)

Incoloy, Alloy 825 (Solid) Indium-Ill Radioactivity Standard

Ingot Iron Spectrographic Steel Standard

Intermediate Purity Selenium

Intermediate-Purity Zinc

Iodine- 123 Radioactivity Standard

Iodine- 125 Radiactivity Standard

Iodine- 129 Radioactivity Standard

Iodine-131 Radioactivity Standard

Iron Foil Mossbauer Standard

Iron-55 Low-Energy Photon Standard

Iron Metal (Clinical Standard)

Iron Ore (Labrador)

Iron Ore (Nimba)

SRM Name SRM

352b Iron Ore (Sibley) 27f 1086 Iron Ore Concentrate (Canada) 690

1087 Iron-59 Radioactivity Standard 441 1L- 1088 Isobutylene-Isoprene (Butyl) Rubber 1495 4361 Isobutylene-Isoprene (Butyl) Rubber 388L 4926C Isotopic Standard for Bromine 977 4947 Isotopic Standard for Chlorine 975

Isotopic Standard for Chromium 979

925 Isotopic Standard for Copper 976

Isotopic Standard for Magnesium 980 GM 760 Isotopic Standard for Silver 978 Krypton-85 Gaseous Radioactivity 4308C GM 757 Standard Krypton-85 Radioactivity Standard 4235 GM 759 Krypton-85 Radioactivity Standard 4935C

Lead-Barium Glass 89 GM 758 Lead-Base Bearing Metal 53e Lead-Base Bearing Metal 1 132 GM 754 Lead Cyclohexanebutyrate 1059c Lead in Reference Fuel 1636a GM 761 Lead in Reference Fuel 1637a SI 198 Lead in Reference Fuel 1638a 864 Lead Nitrate 928

1244 Lead on Filter Media 2674

865 Lead-203 Radioactivity Standard 4420L

1245 Lead, Secondary Freezing Point 49e 866 Standard

1246 Lead-Silica Glass

867 Lead-Silica Glass (Viscosity) 711 1247 Lead-Silica Glass for dc Volume 624 4417L-C Resistivity 420a Lead-Silica Glass for Dielectric 774

Constant 726 Lead 206 Spike Assay and Isotopic QOI 991 728 Solution Standard 4414L-C Leaded-Tin Bronze Alloy 4407L-H Light-Sensitive Paper

4949

B

Light-Sensitive Paper 701H

4401 L-I Light-Sensitive Plastic Chip 7m

1541 Linear Polyethylene

Ws-> 4260C Linear Polyethylene

937 Linear Polyethylene 1483 1484 693 Linerboard, Standard for Tape 1810 Adhesion Testing Liquid Absorbance Standard for 931c

Ultraviolet and Visible Spectrophotometry

Lithium Carbonate 924

Lithium Ore 181 Lithium Ore 182 Lithium Ore 183 Low-Alloy Steel, (AISI 4130) 1225 Low Alloy Steel 1226 Low Alloy Steel (A242 Mod.) C1285 Low-Alloy Steel, AISI 4130 72g Low Alloy Steel (AISI 1526, Modified) 1269 Low-Alloy Steel (Hy 80) 1286

32
Name SRM

Low-Alloy Steel Set (661-665) S668 Low-Carbon Silicon Steel 131c Low-Carbon Silicon Steel 1036 Low-Carbon Stainless Steel (AISI 166c 316L) Magnesium-base Alloy 171 Magnesium Cyclohexanebutyrate 1061c Magnesium Gluconate Dihydrate 929 Magnetic Coating on Magnetic 1365a

Substrate (Nickel on Steel) Magnetic Coating on Magnetic 1366a

Substrate (Nickel on Steel) Magnetic Coating on Non-Magnetic 1367a

Substrate (Nickel and Chromium

on brass Magnetic Tape, High Density 6250 Manganese Fluoride, Magnetic Gram 766

Susceptibility Manganese Ore 25d Manganese-54 Point-Source 4997E

Radioactivity Standard Manganese-54 Radioactivity Standard 4257 Manganese Steel 100B Manganous Cyclohexanebutyrate 1062b Maraging Steel 1 156 Metal on Quartz Filters for 203

1

Spectrophotometry

Metals on Filter Media 2676b Methane in Air 1658a Methane in Air 1659a Methane in Air 1660a Medium Manganese Spectrographic 405a

Steel Standard Mercaptobenzothiazole 383a Mercury, Freezing Point 743 Mercury-203 Radioactivity Standard 441 8L

Mercury in Water, u.g/mL 1641b Mercury in Water, ng/mL 1642b Microcopy Resolution Test Chart 1010a Microprobe Standard - Cartridge Brass 478

Mineral Glasses for Microanalysis 470 Molybdenum Concentrate 333 Molybdenum, Heat Capacity 781 Molybdenum-99 Radioactivity 4412L-H

Standard Molybdenum-Tungsten-Chromium- 1 34A

Vanadium Steel Naval Brass Standards for Optical 1 106 Emission and Spectroscopic

Analysis Naval Brass Standards for Optical CI 106 Emission and Spectroscopic

Analysis Naval Brass Standards for Optical 1 107 Emission and Spectroscopic

Analysis Naval Brass Standards for Optical CI 107 Emission and Spectroscopic

Analysis

Name SRM

Naval Brass Standards for Optical 1 108 Emission and Spectroscopic

Analysis Naval Brass Standards for Optical CI 108 Emission and Spectroscopic

Analysis Neutral Glass 716 Neutron Density Monitor Wire 953 Nickel-Chromium Cast Iron 82b Nickel-Chromium-Molybdenum Cast Iron 107C Nickel-Chromium Steel 32E

Nickel-Copper Alloy 882

Nickel Cyclohexanebutyrate 1065b

Nickel Oxide, No. 1 671 Nickel Oxide, No. 2 672

Nickel Oxide, No. 3 673

Nickel-63 Radioactivity Standard 4226

Nickel Silver (CDA 762) 879

Nickel Siver (CDA 770) 880

Nickel Spectrographic Steel Standard 409b

Nickel Sphere, Magnetic Moment 772

Nickel Steel 33d Ni-Cr-Mo-V Steel 1173

Nicotinic Acid 148 Niobium-94 Gamma-ray Standard 4201

B

Nitric Oxide in Nitrogen 1683b

Nitric Oxide in Nitrogen 1684b

Nitric Oxide in Nitrogen 1685b

Nitric Oxide in Nitrogen 1686b

Nitric Oxide in Nitrogen 1687b

Nitric Oxide in Nitrogen (Mobile 2627 Source Emission Gas Standard)

Nitric Oxide in Nitrogen (Mobile 2628 Source Emission Gas Standard)

Nitric Oxide in Nitrogen (Mobile 2629 Source Emission Gas Standard)

Nitric Oxide in Nitrogen (Mobile 2630 Source Emission Gas Standard)

Nitric Oxide in Nitrogen (Mobile 2631 Source Emission Gas Standard) Nitrogen Dioxide in Air (Stationary 2653 Source Emission Gas Standard) Nitrogen Dioxide in Air (Stationary 2654 Source Emission Gas Standard) Nitrogen Dioxide in Air (Stationary 2655 Source Emission Gas Standard) Nitrogen Dioxide in Air (Stationary 2656 Source Emission Gas Standard) Nitrogen Dioxide Permeation Device 1629a 4-Nitrophenol 938

33
Name SRM

Nodular Cast Iron 342a Nomina] One Micrometer Polystyrene 1690 Spheres Non-Fat Powdered Milk 1549 Nonmagnetic Coating on Magnetic 1359

Substrate (Copper and Chromium

on Steel) Nonmagnetic Coating on Magnetic 1360

Substrate (Copper and Chromium

on Steel) Nonmagnetic Coating on Magnetic 1361b

Substrate (Copper and Chromium

on Steel) Nonmagnetic Coating on Magnetic 1362a

Substrate (Copper and Chromium

on Steel) Nonmagnetic Coating on Magnetic 1363a

Substrate (Copper and Chromium

on Steel) Nonmagnetic Coating on Magnetic 1364a

Substrate (Copper and Chromium

on Steel) NPL GM Alpha Alumina 8005 NPL GM Alpha Alumina 8006 NPL GM Alpha Alumina 8007 NPL GM Alpha Alumina 8008 NPL GM Graphitized Carbon Black 8001 NPL GM Graphitized Carbon Black 8002 NPL GM Melting Point Set 8000 NPL GM Non-porous Silica 8003 NPL GM Non-porous Silica 8004

N-tertiary-Butyl-2-benzothiazolesulfen- 384d amide Rubber Compound

Obsidian Rock 278

Octaphenylcyclotetrasiloxane 1066a

Oil Furnace Black Rubber Compound 378b Opal Glass Powder 91 Optical Emission and X-ray 1 102 Spectroscopic Analysis

Optical Microscope Linewidth 474 Measurement Standard

Optical Microscope Linewidth 475 Measurement Standard

Optical Microscope Linewidth 476 Measurement Standard

Name SRM

Organics in Shale Oil 1580

Oxalic Acid 4990C Oxygen in Ferrous Materials 1090 Ingot Iron Oxygen in Ferrous Materials 1091

(Stainless Steel AISI 431) Oxygen in Ferrous Materials Vacuum 1092 Melted Steel Oxygen in Maraging Steel 1094 Oxygen in Nitrogen (Gas Standard) 2657 Oxygen in Nitrogen (Gas Standard) 2658 Oxygen in Nitrogen (Gas Standard) 2659 Oxygen in Titanium-Base Materials 355 Oxygen in Valve Steel 1093 Oyster Tissue 1566

Palladium, Magnetic Gram 765

Susceptibility Penetrant Test Block 1850 Peruvian Soil, Environmental 4355

Radioactivity Petroleum Crude Oil 1582 Phosphate Rock (Florida) 120b Phosphor Bronze (CDA 521) 871 Phosphor Bronze (CDA 544) 872 Phosphorized Copper, Cu VIII C1251

Phosphorized Copper, Cu IX C1252

Phosphorized Copper, Cu X C1253

Phosphorus-32 Radioactivity Standard 4406L-G

Photographic Step Tablet 1008 Pine Needles 1575

Plastic Clay 98a

Platinum, Magnetic Gram 764

Susceptibility Plutonium-238 Alpha-Particle Standard 4906B

Plutonium-240 Alpha-Particle Emission- 4338

Rate Solution Standard Plutonium-239 Alpha-Particle Solution 4331 Standard Plutonium-242 Alpha-Particle Solution 4334B

Standard Plutonium Isotopic Standard 946 Plutonium Isotopic Standard 947 Plutonium Isotopic Standard 948 Plutonium Metal 949f Plutonium Metal (Standard Matrix 945

Material) Plutonium-244 Spike Assay and 996

Isotopic Standard

Polychlorinated Biphenyls in Oil 1581 Polycrystalline Alumina Elasticity 718 Standard

Polyester Plastic Film for Oxygen 1470 Gas Transmission

Polyisobutylene Solution in Cetane 1490 Polystyrene 1478 Polystyrene 1479 Polystyrene (Broad Molecular Weight) 706

Polystyrene (Narrow Molecular 705 Weight)

Polystyrene Spheres 1691 Portland Cement (Black) 1880

34
Name SRM

Portland Cement (Blue) 635

Portland Cement (Clear) 639

Portland Cement (Gold) 634

Portland Cement (Green) 638

Portland Cement (Pink) 637

Portland Cement (Red) 633

Portland Cement (White) 1881 Portland Cement (Yellow) 636

Portland Cement Fineness Standard 114n Potassium Chloride 2202

Potassium Chloride (Clinical Standard) 918

Potassium Chloride (Primary 999 Chemical)

Potassium Chloride for Solution 1655 Calorimetry

Potassium Dichromate 136d Potassium Dihydrogen Phosphate 200

Potassium Dihydrogen Phosphate 1861c Potassium Dihydrogen Phosphate 21861 Potassium Erucate 1076 Potassium Feldspar 607 Potassium Fluoride 2203

Potassium Hydrogen Phthalate 185e Potassium Hydrogen Tartrate 188 Potassium Iodide with Attenuator 2033 Potassium Nitrate 193 Potassium Tetroxalate 189 Powdered Lead Based Paint 1579

Priority Pollutant Polynuclear 1647 Aromatic Hydrocarbons (in Acetonitrile) Propane in Air 1665b Propane in Air 1666b Propane in Air 1667b Propane in Air 1668b Propane in Air 1669b Propane in Nitrogen (Mobile Source 2643 Emission Gas Standard) Propane in Nitrogen (Mobile Source 2644

Emission Gas Standard) Propane in Nitrogen (Mobile Source 2645 Emission Gas Standard) Propane in Nitrogen (Mobile Source 2646

Emission Gas Standard) Propane in Nitrogen (Mobile Source 2647 Emission Gas Standard) Propane in Nitrogen (Mobile Source 2648 Emission Gas Standard) Propane in Nitrogen (Mobile Source 2649 Emission Gas Standard) Propane in Nitrogen (Mobile Source 2650

Emission Gas Standard) Propane in Nitrogen and Oxygen 2651 (Mobile Source Emission Gas

Standard) Propane in Nitrogen and Oxygen 2652

(Mobile Source Emission Gas

Standard) Quartz Cuvette for Spectrophotometry 932 Quartz for Hydrofluoric Acid 1654

Solution Calorimetry

Name SRM

Quartz on Filter Media 2679a Quinine Sulfate Dihydrate 936

Radiogenic Lead Isotopic Standard 983 Radium-226 Gamma-ray Standard 4956 Radium-226 Gamma-ray Standard 4957 Radium-226 Gamma-ray Standard 4958 Radium-226 Gamma-ray Standard 4959 Radium-226 Gamma-ray Standard 4960 Radium-226 Gamma-ray Standard 4961 Radium-226 Gamma-ray Standard 4962 Radium-226 Gamma-ray Standard 4963 Radium-226 Gamma-ray Standard 4964B Radium Standard (Blank Solution) 4952B

Radon-226 for Radon Analysis 4953C Red Brass 1109 Red Brass CI 109 Red Brass 1110 Red Brass CI 1 10 Red Brass Red Brass Cllll Reduced Iron Oxide 691 Reference Fuel Isooctane 1816a Reference Fuel n-Heptane 1815a

Reflection Step Tablet 2061

Refractive Index Glass 1820

Refractive Index Silicone Liquids 1823

Refractive Index, Soda-Lime Glass 1822

Relative Stress-Optical Coefficient 708 Resulfurized-Rephosphorized Steel CI221

Rice Flour 1568 River Sediment 1645 River Sediment, Environmental 4350B

Radioactivity Rocky Flats Soil Number 1, 4353 Environmental Radioactivity Rubidium Melting Point 1969

Rutile Ore 670 Scanning Electron Microscope 484c

Magnification Standard Scanning Electron Microscope 2069 Performance Standard Secondary Standard Flexible Disk 3210

Cartridge (Computer Amplitude

Reference) Secondary Standard Magnetic Tape 3200 Secondary Standard Magnetic Tape 1600

Cassette Secondary Standard Magnetic Tape 3216

Cartridge (Computer Amplitude

Reference) Second Surface Aluminum Mirror for 2023

Specular Reflectance

35
Name SRM Name SRM

Second Surface Aluminum Mirror for 2024 Soda-Lime Sheet Glass 1831 Specular Reflectance Soda-Lime Silica Glass 622 Second Surface Aluminum Mirror with 2025 Soda-Lime Silica Glass 710 Wedge for Specular Reflectance Soda-Lime Silica Glass for Liquidus 773

Selenium-Bearing Steel 1 170b Temperature

Selenium-75 Radioactivity Standard 4409L-D Sodium Bicarbonate 191a Sheet Brass 37E Sodium Bicarbonate 2191

Silica Brick 198 Sodium Carbonate 192a

Silica Brick 199 Sodium Carbonate 2192 Silicon-Aluminum Alloy 87a Sodium Chloride 2201

Silicon Bronze 158A Sodium Chloride (Clinical Standard) 919

Silicon Density Standard 1840 Sodium Cyclohexanebutyrate 1069b

Silicon Density Standard 1841 Sodium Oxalate Reductometric 40h

Silicon Metal 57a Standard

Silicon Powder, Spacing Standard 640a Sodium Pyruvate 910

for X-ray Diffraction Sodium Tetraborate Decahydrate 1 87b

Silicon Power Device Level 1522 (Borax)

Resistivity Standard Solder 127b

Silicon Resistivity Standard for Eddy 1523 Solder 1131 Current Testers Special Nuclear Container DOT 6M, 9940

Silver 2-Ethylhexanoate 1077a 15 gal. Silver-Gold Thermocouple Wire 733 Special Nuclear Container, 55 gal. 9941

Silver, Vapor Pressure 748 Special Nuclear Container Type A, 9942

Sintered and Arc-Cast Tungsten, 1465 10 gal. Thermal Conductivity and Special Nuclear Container, Type A, 9943

Electrical Resistivity 55 gal. Sintered and Arc-Cast Tungsten, 1466 Special Nuclear Material Package 9910 Thermal Conductivity and Spectrographic Ingot Iron and 461

Electrical Resistivity Low-Alloy Steel Standard (Rod)

Sintered and Arc-Cast Tungsten, 1467 Spectrographic Ingot Iron and 462 Thermal Conductivity and Low-Alloy Steel Standard (Rod)

Electrical Resistivity Spectrographic Ingot Iron and 463

Sintered and Arc-Cast Tungsten, 1468 Low-Alloy Steel Standard (Rod) Thermal Conductivity and Spectrographic Ingot Iron and 464

Electrical Resistivity Low-Alloy Steel Standard (Rod) Smoke Density Chamber Standard 1007a Spectrographic Ingot Iron and 465 (Flaming Exposure Condition) Low-Alloy Steel Standard (Rod) Smoke Density Chamber Standard 1006b Spectrographic Ingot Iron and 466

(Non-flaming Exposure Condition) Low-Alloy Steel Standard (Rod) Soda-Lime Container Glass 621 Spectrographic Ingot Iron and 467 Soda-Lime Flat Glass 620 Low-Alloy Steel Standard (Rod)

468 Soda-Lime Glass 1826 Low-Alloy Steel Standard (Rod) Soda-Lime Glass Powder 92 Spectrograhic Ingot Iron and 1166 Low-Alloy Steel Standard

Spectrographic Stainless Steel 442 Standard

Spectrographic Stainless Steel 443 Standard

Spectrographic Stainless Steel 444

Standard

Spectrographic Stainless Steel D849

Standard (Disc) Spectrographic Stainless Steel D850

Standard (Disc) Spectrographic Stainless Steel 445 Standard (Group II)

36
Name SRM Name

Spectrographs Stainless Steel 446 S ectrosco ic Titanium Base Standard

Standard (Group II) S ectrosco ic Titanium Base Standard

Spectrographic Stainless Steel 447 S ectr sco ic Titam m Base Standard

Standard (Group II) pec^roscopic^ l^amum^ase an ar Spectrographic Stainless Steel 448 Spreading Resistance Calibration Standard (Group II) (100) n-Type Silicon Spectrographic Stainless Steel 449 Standard (Group II) (100) p-Type Silicon Spectrographic Stainless Steel 450 Spreading Resis' ance Ca'' brat' on

Standard (Group II) Spectrographic Stainless Steel 849 S r din R^ t' '^C l b t' Standard (Rod)

P(Tn) pVypTsthcon ^

'° n Spectrographic Stainless Steel 850 Stabilized Wine

Standard (Rod) Stainless Steel Spectrographic Steel Standard (Disc) D803a Stainless Steel Spectrographic Steel Standard (Disc) D807a Stainless Steel Spectrographic Steel Standard (Rod) 803a Stainless Steel (AISI 446) Spectrographic Steel Standard (Rod) 804a Stainless Steel (AISI 446) Spectrographic Steel Standard (Rod) 805a Stainless Steel, 13% Chromium

Spectrographic Steel Standard (Rod) 807a Stainless Steel, Cr-Ni

Spectrographic Steel Standard (Rod) 808a Stainless Steel, Cr-Ni

Spectrographic Steel Standard (Rod) 809a Stainless Steel Cr-Ni

Spectrographic Steel Standard (Rod) 817b Stainless Steel, Cr-Ni

Spectrographic Steel Standard (Rod) 820a Stainless Steel, Cr-Ni

Spectrographic Steel Standard (Rod) 821 Stainless Steel, Cr-Ni

Spectrographic Steel Standard (Rod) 827 Stainless Steel, Cr-Ni

Spectrographic Tool Steel Standard 436 Stainless Steel, Cr-Ni

Spectrographic Tool Steel Standard 437 Stainless Steel, Cr-Ni-Mo

Spectrographic Tool Steel Standard 438 Stainless Steel, Cr-Ni-Nb

Spectrographic Tool Steel Standard 439 Stainless Steel, Cr-Ni-Ti Spectrographic Tool Steel Standard 440 Stainless Steel for Pitting or Crevice

Spectrographic Tool Steel Standard 441 Corrosion

Spectrographic Tool Steel Standard 837 Stainless Steel Thermal Expansion

Spectrographic Tool Steel Standard 840 Stearic Acid Rubber Compound

Spectrographic Tool Steel Standard D837 Steel (AISI 1211) (Disc) Steel (Lead-Bearing) Spectrographic Tool Steel Standard D840 Strontium Cyclohexanebutyrate

(Disc) Strontium-85 Radioactivity Standard Spectrographic Tool Steel Standard D841 Strontium-89 Radioactivity Standard

(Disc) Styrene-butadiene Rubber (Type 1500) Spectrographic Zinc-Base Die-Casting 625 Succinonitrile Freezing Point Alloy A Sucrose

Spectrographic Zinc-Base Die-Casting 626 Sulfate and Nitrate on Filter Media

Alloy B Sulfur Dioxide in Nitrogen

Spectrographic Zinc-Base Die-Casting 627 Sulfur Dioxide in Nitrogen Alloy C Sulfur Dioxide in Nitrogen

Spectrographic Zinc-Base Die-Casting 628 Sulfur Dioxide in Nitrogen Alloy D Sulfur Dioxide in Nitrogen

Spectrographic Zinc-Base Die-Casting 629 Sulfur Dioxide in Nitrogen Alloy E

Spectrographic Zinc-Base Die-Casting 630

Alloy F

Spectrographic Zinc Spelter Standard 631 Spectroscopic Titanium-Base Standard 641 Spectroscopic Titanium-Base Standard 642

Spectroscopic Titanium-Base Standard 643

644

645 646

493

2529

1590 121d

123c 160b

367

1267 73c CI 151 1151a C1152

1152a C1153

1153a C1154

738 372h

368 1169b

1070a 4403L-I

4945 D

386h

1970

17c 2673

1661a 1662a

1663a

1664a

1693 1694

37
Name SRM Name SRM

S If D d N't T't R All Sulfur Dim'ide IVrin'Ji'hon T b 1627 Titanium Base Allo

Y

i anium ase ov m""!!"^) I na °ye ) 651 Uanium ase oy (Unalloyed) S If C "d

,U ^ P t T b 1626 154b "^"cm tube)

6 ermea '°n

"

6 Toluene1 '°X

' 6

21 lc Sulfur Dioxide Permeation Tube . ,„ Tomato Leaves

( 10 cm tube) Tool Steel (AISI M2) 132b

Sulfur in Coal 2682 Tool Steel (AISI M2) 1 157 Sulfur in Coal 2684 Tracealfoy (Nickel Base"

Sta"dard

897

? Sulfur in Coal 2685 High-Temperature Alloy) ^ThghTem^aTure^Allo ) 898

Sulfur in Residual Fuel Oil Sulfur in Residual Fuel Oil 1621b Tracealloy (Nickel Base 899 1622b High-Temperature Alloy)

S^lf"!- in R^id"

3

' F^l O'l 610

Sulfur in Residual Fuel Oil 1624a Trace Elements in a Glass Matrix 61

1

Sulfur Rubber Compound 371g Trace Elements in a Glass Matrix 612 Su ere nd tiv Th tr' F' d 767a Trace Elenk'nls in a Glass Matrix 613 P t D

Trace Elements in a Glass Matrix

614 Su ercon/uctive Thermometric Fixed 768 615 Toint°De

U

vice

e erm°me "C 1X6 Trace Elements in a Glass Matrix 616

Surface Flammabilit Standard 1002 Trace Elements in a Glass Matrix 617

Synthetic Sapphire 720

° 1632a Technetium-99 Radioactivity Standard 4288 Trace Elements in Coal (Sub- 1635 4410H-I ^Standard" "m Rad'°aCt' V' ty Trace Elements in Coal Fl Ash 1633a T hi th 1 N't 1808 Trace Elements in Fuel Oil Tham^mTrH Raihoaciivit Standard 4404L-F Trace Elements in Water 1643a Thermal Resistance Fibrous Glass 1451 1630

Batt

2^*2 4 Triraetlhri 'entane' 217c Thermal Resistan Fib Gl Tri almitin ^ 1595 Board ^ ' ^

Tris^Basimetric 723a Thorium-228, Thallium-208 Gamma-ray 4206C Tris, for Solution Calorimetry 724a 922

Tin-BaseSBearmg

t Meta'id 54D Tris(hydroxymethyl^ 923

Tin, Freezing Point 741 hydrochloride

Tin- 1 1 3-Indium- 1 1 3m Radioactivity 4402L-C Tris(l-phenyl-l, 3-butanediono) 1078b Chromium (III) Tin-121m Point-Source Gamma-ray 4264B Tris( 1-phenyl- 1 , 3-butanediono) 1079b

Emission-Rate Standard Iron (III) Tin, Secondary Freezing Point 42g Triphenyl Phosphate 1071b Standard Tungsten Carbide 276a Titanium Alloy 654a Tungsten-Chromium-Vanadium Steel 50c Titanium-Base Alloy 173b Tungsten Concentrate 277 Titanium-Base Alloy 176 782 Tungsten-20% Molybdenum Alloy 480

Electron Microprobe Standard Tungsten Thermal Expansion 737 Unalloyed Copper 1034 Unalloyed Copper, Cu "O" 393 Unalloyed Copper, Cu IV 457

Unalloyed Copper, Cu XI 454

Unalloyed Copper, Cu I (Chip) 394 Unalloyed Copper, Cu II (Chip) 395 Unalloyed Copper, Cu III (Chip) 396 Unalloyed Copper, Cu V (Chip) 398 Unalloyed Copper, Cu VI (Chip) 399 Unalloyed Copper, Cu VII (Chip) 400

Unalloyed Copper, Cu I (Rod) 494

38
Unalloyed Copper, Cu II (Rod) 495 Unalloyed Copper, Cu III (Rod) 496 Unalloyed Copper, Cu V (Rod) 498 Unalloyed Copper, Cu VI (Rod) 499 Unalloyed Copper, Cu VII (Rod) 500 Unalloyed Titanium 354 Uranium Isotopic Standard (Nominally U-0002

depleted to 0.02%) Uranium Isotopic Standard U-005a Uranium Isotopic Standard U-010

(Nominally 1% Enriched) Uranium Isotopic Standard (Nominally 1.5% Enriched) Uranium Isotopic Standard Uranium Isotopic Standard u mn

Uranium Isotopic Standard 1 1*050 (Nominally 5% Enriched) Uranium Isotopic Standard inn (Nominally 10% Enriched) Uranium Isotopic Standard (Nominally 15% Enriched) Uranium Isotopic Standard U 200 (Nominally 20% Enriched) Uranium Isotopic Standard U-350

(Nominally 35% Enriched) Uranium Isotopic Standard (Nominally 50% Enriched) Uranium Isotopic Standard U 750 (Nominally 75% Enriched) ranium sotopic tan ar II 800 (Nominally 80% enriched) Uranium Isotopic Standard U-850 Uranium" sotopic 'standard U 900 (Nominally 90% Enriched) Uranium Isotopic Standard U-930

(Nominally 93% Enriched) Uranium Isotopic Standard U-970

(Nominally 97% Enriched) Uranium Metal 960 Uranium Oxide 950b Uranium Oxide 969 Uranium-233 Spike Assay and 995

Isotopic Solution Standard Uranium-235 Spike Assay and 993

Isotopic Solution Standard Urban Dust/Organics 1649 Urban Particulate Matter 1648 Urea 912a Urea 2141 Urea 2152

Uric Acid 913 Vanadium and Nickel in Residual 1618 Fuel Oil Vanadium in Curde Oil 8505 Vanadium-49 Low-Energy Photon 4266

Standard Waspaloy 349 Wear-Metals in Lubricating Oil 1084

Name SRM

Wear-Metals in Lubricating Oil 1085

(300 ppm) Wheat Flour 1567 White Cast Iron 338 White Cast Iron (Disc) 1 145 White Cast Iron (Disc) 1146 White Cast Iron (Disc) 1 1 50 White Ceramic Tile for Directional 2019b

Hemispherical Reflectance White Ceramic Tile for Directional 2020

Hemispherical Reflectance White Iron 3d White Opan Glass Diffuse Spectral 2015

Reflectance Standard for the Visible Spectrum

Xenon- 127 Gaseous Radioactivity 4309G

Standard Xenon- 133 Gaseous Radioactivity 43071 Standard Xenon- 1 33 Gaseous Radioactivity 441 5L-I Standard Xenon-133, Xenon-137, Krypton-85 4310B

Mixed Gaseous Radioactivity Standard X-ray Film Step Tablet 1001 X-ray Powder Diffraction Intensity 674 Standard

X-ray Powder Diffraction (Mica) 675 Low 2 Theta

Ytterbium-169 Radioactivity Standard 4419L-B

Zinc-Base Alloy (Die Casting) 94c Zinc Concentrates 113a Zinc Concentrates 329 Zinc Cyclohexanebutyrate 1073b

Zinc, Freezing Point 740

Zinc, Freezing Point Standard 43h

Zinc Metal 683 Zinc Oxide Rubber Compound 370e

Zircaloy-2 360a

Zircaloy-4 Metal 1237

Zircaloy-4 Metal 1238 Zircaloy-4 Metal 1239 Zirconium-Barium Chromate 1651 Formulation for Heat-Source Powder Calorimetry Zirconium-Barium Chromate 1652 Formulation for Heat-Source Powder Calorimetry Zirconium-Barium Chromate 1653 Formulation for Heat-Source Powder Calorimetry Zirconium Metal 1234 Zirconium Metal 1235 Zirconium Metal 1236

39
U.S. Department ot t'onin

.luapita M. Kreps

Secretary

Appendix II. Certificates for Coal, Ore, Mineral, Rock, and Refractory

Standards (listed in numerical order). Rational ^Bureau of Standards

(tteritftcatt of £itml\jsxz

Standard Reference Material lc

Argillaceous Limestone

(In Cooperation with the American Society for Testing and Materials)

(All analyses are based on samples dried 2 hours at 1 10°C)

SiOa Fe2 Oj A12 0) Ti02 P20S MnO CaO SrO MgO Na2 0 K2O

Loss on

Ignition

Certified' Value, % by wt. 6.84 0.55 1.30 0.07 0.04 0.025 50.3 0030 0.42 0.02 0.28 39.9 Estimated"

Uncertainty 0.08 003 0.03 0.005 0.3 0.005 0.04 0.01 0.01 0.1 X^^^MeOiod^

Atomic Atomic

Absorption 1 1

2 1

< <

Photometric Absorption

Atomic

Absorption Absorption Absorption Absorption

°

6.82 b

0.53 b

1-33

C 0 07

d

0.04 C0.03 ' 50.40 ' 0.45 9

0.03 90.28 39.93

h 6.77 ' 1.31

C 07 03e

.02 k

50.l9 ' .54 9

.29 39.80

C

6.82 m

6.77

h 6.80

.55 1.27 .06 .05 .02

.03

"S0.18 m

50.S6

' 50.20

0.03

.38 m

43 .02 m

.29 39.82 39.85

D 6.92 ' .55

' 1.30 °,066 d

.038 .022 50.18 030

9

.02 9

.30 39.90 E 692 .57 1.29 m

.066 d039 .021 50.57 .028 .27 39.87 F 6.76 .57 .08 .04 .027 50.52 .03 .42 .02 39.97 G

P

6 91 1.35 .07 d

04 .027 50.20 .42 .02 .28 39.89

H .022

9 50 58

.034 38 9

.025 9

.30

e "true" value based on results of the cooperative analytical program

2. The estimated uncertainty of the "true"value is based on judgment and represents an evaluation of the combined effects of method imprecision,

possible systematic errors among met hods, and material variability for samples of 0. 5 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination.)

3. Detailed descriptions of many of the methods of analysis employed in the certification program for this SRM may be found in Part 13, Annual Book of ASTM Standards. They are also available as separate reprints. C25 and C 1 1 4, from ASTM headquarters. ASTM Standard Technical

Publication No. 395 also describes methods of analysis used in this certification work.

Silicomolybdate photometric method.

Ferron (8 hydroxy7-iodo-5-quinolinesulfonic acid) photometric method.

' Tiron (disodium- 1 , 2 dihydroxybenzene-3, 5-dftulfonate) photometric method. Molybdenum blue photometric method.

Peroxydisulfale photometric method.

' EDTA titration.

8 Flame emission spectrometry. Dehydration with HCI. Washington, D.C. 20234 December 14, 1978

SnCb reduction-l^CnO? titration. By difference between total NH4OH group and oxides of

iron, phosphorus, and titanium. Calcium precipitated as oxalate and titrated with standard KMnCU.

Magnesium determined gravimetrically as MgjPiOv.

"X-ray fluorescence spectrometry.

1 Atomic absorption spectrometry.

' H2O2 photometric. 'Dehydration with HCIO4.

J. Paul Cali, Chief

Office of Standard Reference Materials

40
PLANNING, PREPARATION, TESTING, AND ANALYSIS:

The material for this SRM was provided by Lone Star Industries, Inc., Cement and Construction Materials Group, Houston, Texas, through the courtesy of C. W. Moore.

At NBS, the material was ground, sieved and thoroughly blended. Chemical analyses for certification were performed in the following laboratories: Atlantic Cement Co., Inc., Ravena, N.Y., F. J. Hogan and W. Twiss.

California Portland Cement Co., Colton, Calif., P. Hawkins and N. Norton.

Ideal Basic Industries, Cement Division, Ft. Collins, Colo., J. W. Yule. Lone Star Industries, Inc., Cement and Construction Materials Group, Houston, Texas, C. W. Moore, L. S. Scheline, and I. Z. Somcio.

Martin Marietta Laboratories, Baltimore, Md., E. H. Scott. National Bureau of Standards, Center for Analytical Chemistry, Washington, D.C., T. C. Rains, M. B. Blackburn, T. J. Brady, J. D. Messman, and T. A. Rush, and by R. K. Bell, Assistant Research Associate, ASTM-NBS Research Associate Program.

Portland Cement Association, Skokie, 111., W. F. Mivelaz, R. F. Crow, E. LaBonde, A. G. Mateos, C. P. Palmiano, and H. Seiler. Universal Atlas Cement, Division of United States Steel Corp., Gary, Ind., Z. T. Jugovic. The overall direction and coordination of the technical measurements leading to certification were performed by J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference

Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

41
Dj"1S|-rerce "National %yxxm\x of ji>tanttartta

lalionaj Bufw of Standards *>- Certificate of (Analgsi*

Standard Reference Material 27f

IRON ORE (Sibley)

(In Cooperation with the American Society for Testing and Materials) This material is in the form of fine powder, for use in checking chemical methods of analysis and in cali- bration with instrumental methods of analysis. (Results based on sample dried for one hour at 105 °C.) Constituent Total Fe Si02 AI2O3 P S Ti02 MnO CaO MgO Na2 0 K2O

Certified' Value,% by wt 65.97 4.17 0.82 0.041 0.005 0.019 0.011 0.039 0.019 0.012 ' 0.008 Estimated

2 Uncertainty

0.05 0.03 0.03 0.001 <0.001 0.002 0.002 0.003 0.004 0.003 0.002 \ Method

3

Labs \

q

u u HCIO4

Dehydration

Atomic

Absorption

Photometric CombustionTitration

Photometric

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

A 66.01 °4.12 0.78 b0.042 0.005 c0.020 0.009 0.042 0.02 d0.012 d0.006 B

C65.98 4.18 .83 .042 .006 f .018

.014 9

.012

.041 9

.042

.013 9

.015 d .0I2 8 .0I0 d .011 °.009 C 65.93 \..8 .87 '.84 .039 ] .0O5 k .019

1 .010

.011 d

.039 .018 d009 d.008 D 65.92 4.14 m 82 .041 .006 .02 .006 .036 .023 d.016 d

.008 E "65.96 4.17 .79 b

.040 j.005 °.021 p Oil .035 .021 .010 .009 F "66.04 b

.042 q .017 .011 .027 .015 .007 G °65.96 4.20

r 82

.81 .040 j.005 f .018

.011 '.013 .035 .018 .009 .007

1 . The certified value listed for a constituent is the present best estimate of the "true" value based on results of the cooperative analytical program for certification.

2. Estimated uncertainty includes method imprecision, bias among methods, and material variability for samples 0.5 g or more.

3. A detailed description of many of the methods of analysis employed in the certification program for this SRM may be found in Part 12, Chemical Analysis of Metals and Metal Bearing Ores, Annual Book of ASTM Standards. NOTE: Laboratory C reported a value of 0.002 percent Zr02 by the pyrocatechol photometric method.

Sample fused in Na202.

b Alkali-molybdate method.

X-ray spectrometric method. Flame emission spectrometry. H2S reduction-K^CnCh titration Chromotropic acid photometric. Spectrographic method. Sample dissolved in HCI. silica removed by double de- hydration with HCI. Ignited silica treated with H2SO4

and HF. Aluminum separated by anion-exchange and determined by chelometric titration using 1,2 diaminocyclohexanetetraacetic acid and back titration with standard zinc

solution. Washington, D.C. 20234 May 31, 1977

Combustion-chromatographic

Titanium separated by anion-exchange and determined

photometrically with diantipyrylmethane.

' Photometric m Aluminum separated by anion-exchange and determined

gravimetrically with phenylhydrazine.

" SnCb reduction - KMnOa titration. H2O2 photometric.

Peroxydisulfate-arsentte.

q Atomic absorption spectrometry.

' Mercury cathode-NH4 OH-CupfeiTOn-AlP04.

(Over)

J. Paul Cali, Chief

Office of Standard Reference Materials

42
PLANNING, PREPARATION, TESTING, ANALYSIS: The iron ore material for this SRM was provided

to NBS by the United States Steel Corporation, Pittsburgh, Pa., through the courtesy of R. H. Colin. The "as received" material was crushed, dry ground, and sieved under contract with the Colorado School of Mines Research Institute, Golden, Colorado, under direction of M. G. Pattengill and H. O. VanMale. The final product passed a 150 mesh (105/im) sieve, with about 50% passing a 200 mesh (74/xm) sieve. At NBS the material was sieved and thoroughly blended. Homogeneity testing of selected samples representative of the final lot was performed at NBS by R. K. Bell, Assistant Research Associate, ASTM/NBS Research

Associate Program. The observed range of values is as follows: Constituent Range, % No. of determinations Sample size, grams

Fe ±0.05 16 0.5 Si02 £±0.02 4 1.0 P £±0.001 4 0.5

It is concluded that the material variability is within the method imprecision. Chemical analyses for certification were performed in the following laboratories: Alan Wood Steel Company, Conshohocken, Pa., V. J. Mercaldo. Andrew S. McCreath and Son, Inc., Harrisburg, Pa., R. F. Lippi. Booth, Garrett and Blair, Inc., Ambler, Pa., J. H. Ormsbee. Ledoux and Company, Teaneck, N. J., S. Kallman.

National Bureau of Standards, Analytical Chemistry Division, Washington, D.C. by T. C. Rains and S. A. Wicks, and by R. K. Bell, ASTM Assistant Research Associate. United States Steel Corporation, Research Laboratory, Monroeville, Pa., by J. D. Selvaggio, D. G. Cunning- ham, J. DiNardi, J. B. Ferons, A. V. Fioravanti, J. E. Friedline, J. R. Lucas, II, K. G. Mikos, C. W. Ponsonby,

D. Shafferman, and R. J. Wargo.

Weirton Steel Division, Weirton. W. Va., R. L. Zickefoose. The overall direction and coordination of the technical measurements leading to certification were performed

jointly by R. E. Michaelis, Office of Standard Reference Materials, and by J. I. Shultz, Research Associate, ASTM/NBS Research Associate Program. The technical and support aspects involved in the preparation, certification and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

43
U.S. Department of Commerce

Juanita Kreps

Ernest Ambler. Directoi ^National ^mtm of j^tandants

(dtttxixtnit of ^nalgst*

Standard Reference Material 69b

Bauxite (Arkansas)

(In Cooperation with the American Society for Testing and Materials)

(All analyses are based on samples dried 2 hours at 140 °C)

This material is in the form of fine powder (<0.08 mm) for use in checking chemical and instrumental methods of

analyses.

Certified Value

1 Estimated

Constituent Percent, by weight Uncertainty AI2O3 48.8 0.2 FezOj 7.14 .12 Si02 13.43 .10 Ti02 1.90 .05 Zr02 0.29 .07 p2o5 .118 .004 V2O5 .028 .003 Cr203 .011 .002 CaO .13 .02 MgO .085 .008 MnO .110 .005 ZnO .0035 .0005 K2 0 .068 .009 S03 .63 .02 Loss on Ignition

3 27.2 .2

'The certified value listed for a constituent is the present best estimate of the "true" value. "The estimated uncertainty listed for a constituent is based on judgment and represents an evaluation of the combined effects of method

imprecision, possible systematic errors among methods, and material variability for samples 1 .0 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination of most constituents.) Determined by igniting to constant weight at 1050 °C. Washington, D.C. 20234 George A. Uriano, Chief August 24, 1979 Office of Standard Reference Materials

(over)

44
ADDITIONAL INFORMATION ON THE COMPOSITION

Elements other than those certified may be present in this material as indicated below. These are not certified but

are given as additional information on the composition.

Concentration, Concentration,

Constituent Percent by weight Constituent Percent by weight BaO (0.008) Co (0.0001) Na20 (0.025) Hf (0.0063) Ce (0.024) Sc (0.0008) The mineralogical composition of SRM 69b was determined by x-ray diffraction studies at the Geological

Survey, U.S. Department of the Interior, Reston, Va., (J.W. Hosterman)to be 30% kaolinite, 60%gibbsite, and 10% siderite. These results are semiquantitative (to the nearest 5%). PLANNING, PREPARATION, TESTING, ANALYSIS:

The mine run material for this SRM was provided by the Aluminum Company of America, Bauxite, Arkansas, through the courtesy of T.J. Forbes and by the Alcoa Technical Center, Pittsburgh, Pa., courtesy of H.B. Hartman. It was processed (crushed, ground, sieved, and mixed) at the Colorado School of Mines Research

Institute under a contract with the National Bureau of Standards. Homogeneity testing was performed at NBS by J.S. Maples and T.E. Gills. Cooperative analyses for certification were performed in the following laboratories: Aluminum Company of America, Alcoa Center, Pa., R. C. Obbink. Aluminum Company of Canada, Ltd., Arvida Research Center, Arvida, Quebec, Canada, L. Girolami. Andrew S. McCreath & Son, Inc., Harrisburg, Pa., F. A. Pennington, Jr., R. F. Eakin, and S. L. Miller. General Refractories Co., U.S. Refractories Division, Research Center, Baltimore, Md., S. Banerjee. Geological Survey, U.S. Department of the Interior, Reston, Va., H. J. Rose, Jr., and J. W. Hosterman.

Kaiser Aluminum and Chemical Corp., Center for Technology, Pleasanton, Calif., H. J. Seim, A. E. McLaughlin, D. F. G. Marten, A. Kermaninejad, R. C. Kinne, J. R. Skarset, J. Boruk, and U. Vogel. National Bureau of Standards, Washington, D.C., R. K. Bell, ASTM-NBS Assistant Research Associate. National-Southwire Aluminum Co., Hawesville, Ky., N. Robinson and E. Gotzy. Ormet Corp., Burnside, La., W. L. Brown and A. D. Lafleur. Reynolds Aluminum Co., Alumina Research Division, Bauxite, Ark., J. B. Ezell, Jr. University of Kentucky, Institute for Mining and Minerals Research, Center for Energy Research

Laboratory, Lexington, Ky., T. V. Rebagay. The overall coordination of the technical measurements leading to certification were performed under the

direction of J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and R. Alvarez.

45
NBS Standard Reference Materials BAUXITE SERIES

September 4, 1979

R. E. Michaelis and R. Alvarez, NBS Office of Standard Reference Materials and

J. I. Shultz, ASTM Research Associate The following table gives the values for four bauxite SRM's that are available in the form of fine powder (<0.08 mm) for use in chemical and instrumental methods of analysis. They are being issued as a culmination of a major Industry-ASTM-NBS cooperative program. SRM No. 69b 696 697 698

Designation Arkansas Surinam Dominican Jamaican

Constituent Percent by Weight

AI2O3 48.8 54.5 45.8 48.2 Fe203 7.14 8.70 20.0 19.6 Si02 13.43 3.79 6.81 0.69 Ti02 1.90 2.64 2.52 2.38 Z1O2 0.29 0.14 0.065 0.061 p2 o5 0.118 0.050 0.97 0.37 v2 o5 0.028 0.072 0.063 0.064 Cr2 03 0.011 0.047 0.100 0.080 CaO 0.13 0.018 0.71 0.62 MgO 0.085 0.012 0.18 0.058 MnO 0.110 0.004 0.41 0.38 ZnO 0.0035 0.0014 0.037 0.029 BaO (0.008)" (0.004) (0.015) (0.008) Na2 0 (0.025) (0.007) (0.036) (0.015) K2 0 0.068 0.009 0.062 0.010 SO3 0.63 0.21 0.13 0.22 Loss on Ign. 27.2 29.9 22.1 27.3 Ce (0.024) (0.0041) (0.069) (0.030) Co (0.0001) (0.00009) (0.0013) (0.0045) Hf (0.0063) (0.0032) (0.0014) (0.0015) Sc (0.0008) (0.0008) (0.0058) (0.0051) Total (100.0) (100.1) (100.1) (100.1)

"Values in parenthesis are not certified. The value listed for a certified constituent is the present best estimate of the "true" value based on the results of

the analytical program for certification (10-12 laboratories). The individual certificates of analysis list the "estimated uncertainties" associated with the certified values (also listed is a semiquantitative mineralogical composition (±5%) as determined by x-ray diffraction studies at the U.S. Geological Survey).

Inquiries regarding the Bauxite SRM's 69b, 696, 697, and 698, should be directed to the Office of Standard

Reference Materials, Chemistry Building, B311, National Bureau of Standards, Washington, D.C. 20234.

(301) 921-2045. George A. Uriano, Chief

Office of Standard Reference Materials

46
Certificate of Snalpsfe

Standard Reference Material 70a

Feldspar

(All Analyses are Based on Samples Dried 2 hours at 10S °C)

Percent

Silica (SiO: ) 67.1 Alumina (AUO,) 17.9 Iron (as Fe,0,) 0.07, Titania (TiO: ) .01 Calcium (as CaO) .11 Barium (as BaO) .02 Sodium (as Na=0) 2.5, Potassium (as K-O) 11.8 Rubidium (as Rb50) 0.06 Loss on Ignition .40

Washington, D.C. 20234 George A. Uriano, Chief August 10, 1981 Office of Standard Reference Materials

(Revision of Certificate dated

3-26-65)

47
UiinilH M Kreps

Rational £8uram of j&tandartte

Certificate of ^nalgsi*

Standard Reference Material 76a, 77a, and 78a

Burnt Refractories

(In Cooperation With the American Society for Testing & Materials)

These materials are in the form of fine powder (<0. 15 mm) and are intended for use in checking chemical methods of analysis and in calibration with instrumental methods of analysis. SRM No. 76a 77a 78a

Constituent P e rcent by Weight

SiO: 54.9 35.0 19.4 AbO, 38.7 60.2 71.7 Fe: 0, I.60 l.Oo 1.2 TiO; 2.0, 2.66 3.2, ZrO; 0.15- 0.21 0.31 MgO .52 .38 .70 CaO .22 .05 .11 K2 0 1.33 .090 1.22 Na20 0.07 .037 .078 P2O, .12o .092 1.3 Li : 0 .042 .02 5 0.12 SrO .037 .009 .25 Loss on ignition (.34)

b (.22) (.42) Total (100.0) (100.0) (100.0)

J Based on samples dried at 105 °C for one hour.

h A figure in parenthesis is not certified but is given for additional information on the composition. CERTIFICATION: The value listed for a certified constituent is the present best estimate of the "true" value based on the results of the analytical program. The value is not expected to deviate from the "true" value by more than ± I in the last significant figure reported. For a subscript figure, the deviation is not expected to be more than ± 5. Based on the results of the homogeneity testing, maximum variations within and among samples

are estimated to be less than the uncertainty figures given above. Washington, D.C. 20234 j. paul Cali, Chief

April 5, 1977 Office of Standard Reference Materials (Revision of certificate dated 6-23-76. Only change: SrO values from uncertified to certified.)

(Over)

48
PLANNING, PREPARATION, TESTING, AND ANALYSIS: These replacements for the original Burnt

Refractory SRM's were especially prepared and provided to NBS by Harbison- Walker Refractories Company,

Garber Research Center, Pittsburgh, Pa., through the efforts of Dr. R. K. Scott. Carefully selected raw materials were batched to form extruded dobies. The dobies were air dried, oven dried at 120 °C, and then fired at 1427 °C for ten hours in kilns. The fired dobies were crushed and ground and converted to the fine powder product by air classification (about 95 %-325 mesh). The final products were mixed in a blender. At NBS, each of the materials was reblended and resieved. Homogeneity testing by chemical analyses was performed at NBS by K. M. Sappenfield on selected samples

representative of each lot of material for the key constituents, SiOj and Fe.'Oi. Standard Deviation of a Single Determination (in wt. %), n = 7 Constituent 76a 77a 78a SiO. 0.09 0.06 0.08 Fe2 Oj .03, .034 038 Cooperative analyses for certification were performed in the analytical laboratories at Harbison-Walker

Refractories Company, Pittsburgh, Pa., R. K. Scott and J. Ryan; and at Pennsylvania State University, College

of Earth and Mineral Sciences, University Park, Pa., N. H. Suhr, J. C. Devine, and J. B. Bodkin. Analyses were performed in the NBS Analytical Chemistry Division by R. K.. Bell, O. Menis, T. C. Rains, T. A. Rush, K. M. Sappenfield, M. A. Waguespack, and S. A. Wicks. The overall responsibility for the technical measurements at NBS was under the direction of W. R. Shields, I. L. Barnes, and O. Menis. The final coordination of the technical measurements was under the direction of J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of these SRM's were

coordinated through the Office of Standard Reference Materials by R. E. Michaelis.

49
diurnal Bureau ot Sliimlnrdv Krnest Ambler. Director

Rational ^Bureau of j^tandartb

Certificate of ^nalgsis

Standard Reference Material 79a

Fluorspar

This Standard Reference Material is an acid-grade fluorspar concentrate, to be used primarily for the assay of imported fluorspar for industrial applications. The assay value certified is dependent on the U.S. Customs

Laboratory Method given in this Certificate; however, two options exist for the determination of soluble

fluoride calculated as calcium fluoride in the acetic acid leach solution. Either the spectrophotometry procedure

(Part B), which was used for the original certification of this material, or the ion electrode procedure (Part C), which is included on this Certificate, may be used. The results of the two procedures show excellent agreement.

a Mean value based on 32 determinations using the U S. Customs Laboratory Method of analysis (attached). The determinations were made

by two analysts at each of three Customs laboratories and one NBS laboratory. Standard deviation of a single determination. The following values, obtained by quantitative spectrochemical analysis, are givenfor information only and are not certified: Fe, 0.05-0.1%; Al and Sr, 0.01-0.1%; Mg, 0.01-0.05%; Na, 0.001-0.01%; Ba, 0.001-0.005%; K, <0.005%; and Cu, Li, Mn, Pb, and Ti, <0.001%. The chemically determined value for SiC>2 is 0.67%. The analytical work leading to certification was performed in the Division of Technical Services, U.S. Customs

Laboratories, and by J. R. Moody and K. M. Sappenfield of the NBS Center for Analytical Chemistry. The

spectrochemical determinations were made by M. Darr of the NBS Center for Analytical Chemistry. A comparison of the ion electrode procedure with the spectrophotometric procedure was performed by R. L. Zimmerman, Jr., and H. G. Bertrand of the U.S. Customs Laboratory, New Orleans, La., and by J. R. Moody

of the NBS Center for Analytical Chemistry. This material was supplied by the American Smelting and Refining Company of El Paso, Texas; it was ground

to pass a 177 ^m (80 mesh) screen. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by J. L. Hague, R. E. Michaelis, and C. L. Stanley. Washington, D.C. 20234 George A. Uriano, Chief January 8, 1980 Office of Standard Reference Materials

(Revision of Certificate dated 12-6-71) (over)

Constituent Percent by weight

97.39

a ± 0.06b CaF2

50
Method for the Determination of CaF2 in Fluorspar

A. Calcium Fluoride Determination: Transfer a 0.5 ± 0.01 g sample, previously dried at 100 to 105 °C, to a 60 mL Pt dish. Add 15 mL acetic acid ( 1 :9) and approximately 50 mg of dry, ashless filter pulp. Digest on a steam

bath for 30 minutes and stir with a small glass rod at 5-minute intervals. Stir and filter through an 1 1-cm close- texture filter paper (S&S No. 589 Red Ribbon, or equal) to which has been added approximately 4 mL filter pulp slurry (1 g ash-free pulp in 100 mL of water). Thoroughly wash crucible, stir rod, and paper with small portions of hot water (approximately 35 mL). The filtrate and washings should be collected in a polyethylene

bottle for the determination of dissolved fluoride by either the spectrophotometric method described in Part B

or the ion-selective electrode method described in Part C. Transfer paper and residue to original crucible, wipe

the funnel with a small piece of filter paper.and add the paper to the crucible to assure recovery of fine particles. Dry crucible and contents, ignite to a dull red heat (600 °C), and cool to room temperature. Transfer the residue, as completely as possible, from the crucible to a 400-mL beaker by gently tapping the

crucible. Add 5 to 1 0 mL HC 1 to the crucible and warm on a steam bath or a temperature-regulated sand bath. Transfer the HC 1 to the beaker containing the residue. Police and wash the crucible with a minimum amount of

hot water. Repeat adding HCI and washing 2 or 3 times using a total of 25 mL HC1. Add approximately 0.5 g of

crystalline boric acid to beaker, cover with a watch glass, and digest on the steam bath for 1 5 minutes. Remove

the beaker and cool to room temperature. Add 0.5 mL HNOj and slowly evaporate on the steam bath to approximately 10 mL. During evaporation, the cover glass should be gradually removed from the beaker. Wash down the sides of the beaker with a fine stream of water and adjust the volume to approximately 75 mL. Heat to 70 to 80 °C, remove from heat, and add 100 mL of precipitating solution [3.8 g ammonium oxalate, 1. 1 g oxalic

acid, and 0.05 g disodium ethylenediaminetetracetate (EDTA) in 100 mL of water]. If a white precipitate forms

at this point, add HCI dropwise until it dissolves. Heat to boiling and slowly add N H4OH ( 1 : 1 ) until a heavy white precipitate forms. Add I mL of bromocresol

green solution (0. 1 g soluble salt in 100 mL of water) and continue the addition until the color of the solution changes from yellowish-orange to grayish-green. Digest for 30 minutes on the steam bath, let stand for 60

minutes at room temperature, and filter by decantation through a prepared Gooch crucible (size 3, prepared

with 2.1 cm glass-fiber filter paper, H. Reeve Angel No. X-934AH, or equivalent). Wash 3 or 4 times with a cold wash solution (0.2 g ammonium oxalate and 0. 1 g oxalic add in 100 mL of water) and finally with 3 or 4 10-mL

portions of cold water. (The washed precipitate should be free of chloride, ammonium oxalate, or any other contaminant that might reduce the KMn04 solution.) Transfer the contents of the crucible to a 400-mL beaker, add 250 mL H2SO4 (1:19), and adjust the solution temperature to 27 ± 3 °C. While stirring, add approximately

90 percent of the 0.15 N KMn04 solution to be used for titration. This should be added at a rate of approximately 30 mL per minute from a buret. Allow to stand until the pink color disappears, e.g., approximately 45 seconds. (If pink color persists, too much KMnO.4 solution has been added and the determination must be repeated.) Heat to 57 ± 3 °C and complete the titration by slowly adding the last 0.5 to I mL KMn04 solution dropwise and allowing each drop to decolorize completely before adding the next drop. The end point is a pink color persisting for 30 seconds or more. See calculations.

B. Determination of Fluoride in Acetic Acid Leach Solution: Remove all ions from the solution that might

cause interference in the spectrophotometric determination of dissolved fluoride, by using either the ion- exchange method, or the fluorine-distillation method described in 2 and 3. Prepare a reagent blank, by

substituting 15 mL of acetic acid (1:9), diluted to approximately 55 mL with distilled water and analyze simultaneously with sample.

1. Preparation of calibration curve: Prepare a dilute fluoride standard ( I mL - 0. 1 mg CaFi) from a standard

solution (I mL = 1 mg CaF2 ) of 1.0755 g NaF diluted to one liter in a polypropylene volumetric flask with

distilled water. Take a series of aliquots of 1, 2, 4, 6, 8, II, 16 mL.etc, from the diluted fluoride standard and

transfer them to 60-mL polyethylene bottles. Add 1 5 mL of acetic acid ( 1 :9) and sufficient distilled water to bring

the final volume to approximately 55 mL. Proceed to the ion-exchange or fluorine-distillation method.

51
2. Ion-exchange method: Prepare an anion-exchange column by pouring a slurry of distilled water and Rexyn

201 (OH) resin, or equivalent, sufficient to give a total exchange capacity of 27 to 30 meq, into a 25 mL

polystyrene buret plugged with washed absorbent cotton (not glass wool) and drain off the excess water without

allowing the water level to fall below the top of the resin column at any time. Continue this procedure until the

resin is within about 5 mL of the top of the buret. Wash the resin with 20mL N NaOH, and finally with distilled water (approximately 100 mL), until the effluent is no longer alkaline. Adjust the stopcock to give a flow rate of approximately 100 drops per minute. The flow rate is an indicator of the state of the column. Backwash with

distilled water whenever the flow rate falls below 100 drops per minute. Resin must be covered with liquid at all times. Prepare a cation-exchange column in the same manner as the anion exchange column using a slurry of distilled water and Rexyn 101(H) resin, or equivalent, sufficient to give a total exchange capacity of 40 to 45 meq. Wash

the resin with 50 mL of 1 N HC 1

, and finally with distilled water (approximately 200 mL) until the effluent is free of chloride ion. Flow rate should be approximately 100 drops per minute. Each of the diluted aliquots, as well as the blank, is run separately as follows: After completing both columns,

pass the entire volume from the polyethylene bottle through the anion-exchange column, always maintaining

the liquid level slightly above the top of resin. Wash the polyethylene bottle with distilled water and pass washings through the column using a total of approximately 60 mL for each sample. Discard the effluent and

washings. Recover the fluoride, acetate, and other anions from the column by passing 20 mL of IN NaOH

through the column at a flow rate of approximately 100 drops per minute. Collect the effluent in the original polyethylene bottle. Wash the column with distilled water and collect washings in the same bottle to capacity (60 mL). Pour the contents of this bottle, and water used to rinse it, into the cation column and collect the effluent in a 100-mL volumetric flask. Wash the column with distilled water and collect just short of the mark in the same

flask. Bring the liquid to the mark with distilled water. Proceed to the spectrophotometric determination.

3. Distillation method : Have water in a steam generator actively boiling, but do not connect to the fluoride

distillation apparatus (Willard and Winter, or equivalent) at this time. Distill each of the diluted aliquots,as well

as the blank.separately as follows: Transfer the entire volume from the polyethylene bottle to the 500-mL Claisen

flask of the distillation apparatus using a minimum quantity of water for rinsing. Add 50 mL H2SO4 (1:1) and a few glass beads. Insert a stopper carrying the steam tube and thermometer, and heat the flask with a Bunsen

burner or an electric heater. Connect the condenser at once and place a 200-mL polypropylene volumetric flask

at the receiving end. Water soon begins to distill over and the temperature of the liquid rises as the H2SO4

concentration increases. When the temperature reaches 120 °C connect the flask to the steam generator by means of the rubber tube. The rate of steam generation and the rate at which the Claisen flask is being heated should be regulated so that the temperature of the liquid in the distilling flask is maintained at 135 to 145 °C.

Distill until the total volume in the receiver is approximately 185 mL (Note 1). Disconnect the condenser and

rinse with a small portion of water, catching the washings in the flask containing the distillate, and fill to mark

with distilled water. Proceed to the spectrophtometric determination.

4. Spectrophotometric determination : Pipette about one-tenth of the volume of the solution from steps B-2 or B-3 containing approximately 0.1 to 0.2 mg CaF2 (not more than 50 mL) into a 100-mL polypropylene

volumetric flask and add 1 5 mL 0. 1 N sodium acetate solution and 25 mL methyl cellosolve. Bring the solution

level in the flask almost to mark with distilled water and allow to cool to room temperature (mixing reaction is slightly exothermic) before making a final volume adjustment. (Resulting solution should have a pH of 3 to 5; optimum color development occurs in this range.) Pour the entire contents of the volumetric flask into a 1 25-mL stoppered erlenmeyer flask containing 0. 1 g of thorium chloranilate (Note 2). Stopper the flask and place on a shaking apparatus. Shake for 55 minutes, remove, and allow the contents of the flask to settle for 5 minutes. Filter through a close-texture filter paper, discarding the first 5 to 10 mL of filtrate. Read the absorbance of sample against the reagent blank using 1 cm absorption cells in a Beckman DU

spectrophotometer, or its equivalent, at a wavelength of 330 nm and a slit width of about 0.2 mm. Plot absorbance vs mg of CaFi. This should yield a straight line passing through the origin.

52
5. Analysis of acetic acid leach solution: Carry the entire filtrate from the acetic acid digestion through steps B-2

or B-3 and finally B-4. Determine mg of CaF2 by using the calibration curve and proceed with calculation. C. Determination of Fluoride in Acetic Acid Leach Solution with an Ion-Selective Electrode.

I. Apparatus, Reagents, and Solutions

a. Special Apparatus

1) Fluoride specific ion electrode

2) Single junction reference electrode

3) Expanded scale pH meter with millivolt capability

b. Reagents ACS Reagent grades of sodium fluoride, glacial acetic acid, sodium chloride, and sodium hydroxide, must be used. For ( 1 ,2 Cyclohexylenedinitrilo)- tetraacetic acid (CDTA), a practical grade available from

a commercial source may be used.

c. Solutions

1) T1SAB II - (Total Ionic Strength Adjustment Buffer) To 500 mL of distilled water in an 800 mL beaker, add 57 mL of glacial acetic acid, 58 g of sodium

chloride, and 4 g of CDTA. Place the beaker in a cold water bath, on a magnetic stirrer. Stir the mixture, while adding concentrated sodium hydroxide, to provide a pH between 5.0 and 5.5. Transfer

the contents of the beaker to a 1-liter flask, and dilute to the mark with distilled water. (TISAB II is used to provide a constant ionic strength background, decomplex the fluoride ions, and adjust and

buffer the pH of the solution.)

2) Standards

a) Stock Solution (1900 ppmF~) - Dissolve 4.199 g of sodium fluoride in a 1-liter polypropylene volumetric flask and dilute to volume with distilled water.

b) Working stock solution (19.00 ppmF .) - Transfer 10 mL of stock solution (a) to a 1-liter polyproplene volumetric flask and dilute to the mark with distilled water.

c) Working standards - Prepare standards according to Table I. TABLE I F Cone. (Mg/mL) Working Stock (mL) TISAB II (mL)

Distilled Water (mL)

9.50 50.0 50

4.75 25.0 50 25

2.85 15.0 50 35

1.90 10.0 50 40

0.95 5.00 50 45

0.38 2.00 50 48

If prepared in a 100 mL flask, dilute to mark with distilled water. Store working standards in polyethylene bottles and refrigerate until use.

2. Procedure

Transfer the contents of the polyethylene bottles containing the acetic acid wash (Section A) to 200 mL

polyethylene volumetric flasks and dilute to volume with distilled water. Transfer a 25 mL aliquot to a 50 mL

polyethylene volumetric flask and dilute to volume with TISAB II. Place in refrigerator until ready for use. In a polyethylene bottle, prepare a reagent blank consisting of 15 mL of acetic acid (1:9) and approximately

55 mL of distilled water.

53
Transfer the working standards, test solutions, and the reagent blank to l50mL polyethylene beakers and allow

to come to room temperature. Stir all solutions with magnetic stirrers. Adjust the pH meter to -1 50 mV by use of

the 19.00 ppm F working stock solution. Record the values of the solutions beginning with the least concentrated working standard. NOTE: For solutions containing low concentrations of fluoride, the pH meter may require approximately two minutes to stablize (cessation of drift). Rinse and dry the electrodes with tissue paper between readings. Record the values of the test solutions and the reagent blank immediately following the working standards.

Plot a curve from the values obtained for the working standards, and determine the concentration of the test solutions from the curve. Proceed with calculations. D. Calculations:

First, calculate the % CaF2 found in Part A. Then calculate the % CaF2 found in either Part B

(spectrophotometry procedure) or Part C (electrode procedure). Add the value calculated for either Part B orC

to that calculated for Part A, to determine the total % CaF2 in the sample. For Part A: % CaF2 _ 3.904 ViN Ws

where: V, = Volume of KMnO\j solution used (corrected for blank) N = Normality of KMn04 solution Ws = gram weight of sample

For Part B: % CaF2 = 0.1 WC F Ws

where: Wc = milligram weight of CaF2 in aliquot F = aliquot factor; Total volume from B-2 or B-3 volume used Ws = gram weight of sample

where: C = observed concentration in ppm F~ (/ig F~/mL) V2 = volume of test solution A = aliquot factor; total volume

volume used G = gravimetric factor; CaF2 2F Ws = gram weight of sample

54
For the conditions described in Part C, this formula may be simplified as follows: 200

1) The sample is diluted to 200 mL and a 25 mL aliquot is taken; thus the aliquot factor, A, is: A= -^- = 8.00

2) The volume of test solution V2 is always 50 mL; V2 = 50.0 mL

3) The gravimetric factor, G, is: G= £^ =

780768

e = 2.055 2F 37.9968 by substitution: % CaF2 _ C x 50.0 x 8.00 x 2.055 x |Q-4 Qr Ws %CaF2 = 0.0822C Ws Note 1. The volume of distillate necessary for complete recovery of fluoride will vary with the capacity of the

distillation apparatus. Calibrate the apparatus by distilling a known quantity of fluoride to various final volumes to determine the volume necessary for complete recovery. Note 2. Chloranilates are supplied as dry powders of high stability. However, long storage may reduce activity. Drying at 105 °C for at least 4 hours restores activity. Keep bottles tightly capped to prevent moisture

absorption, which reduces activity and hinders the color development.

55
U.S. Department of Commerce

Juanita M. Kreps

Secretary Rational bureau of j^tandarcta

Qlerttfttate of (Analgsb

Standard Reference Material 81a

Glass Sand

(In Cooperation with the American Society for Testing and Materials)

This SRM is issued in the form of a ground powder (95% less than 106 pm) blended to ensure homogeneity. It should be dried for 2 hours at 105 °C before use. Recommended Value

Constituent Percent by Weight Range _s_ A1203 0.66 0.62 - 0.69 0.011 Fe2 03 .082 .075- .089 .0024

Ti02 .12 .10 - .14 .0064 Zrih .034 .025- .042 .0026 Cr2 03 46/xg/g 33 58 3.9 Certification - The recommended value listed for each oxide is the best estimate of the true value based on the

analytical data from both cooperators and NBS. The range ofvalues listed is the tolerance interval, constructed such that it will cover at least 95% of the population with a probability of 0.99. It is computed as X ± Its: where s

is the standard deviation, K is a factor that depends on n (the number of samples measured), p, the proportion of

the total sample covered (95%), and 7, the probability level (99%). In all cases none of the n values used exceeded the range specified. Thus, it includes variability between laboratories and between samples. The overall direction and coordination of the round-robin analysis leading to certification were performed by Paul Close, Chairman of ASTM Subcommittee C-14.02 on Chemical Analysis of Glass and Glass Products. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

Washington, D C. 20234 J. Paul Cali, Chief

January, 1978 Office of Standard Reference Materials

(over)

56
Chemical analyses for certification were performed in the following laboratories: Anchor Hocking Corp., Lancaster, Ohio, R. E. Carr Brockway Glass Co., Inc., Brockway, Pa., E. L. McKinley. Corning Glass Works, Corning, N.Y., Y. S. Su. Ford Motor Co., Lincoln Park, Mich., T. O. LaFramboise.

National Bureau of Standards, Analytical Chemistry Division, E. J. Maienthal, J. D. Messman and T. C.

Rains. Kimble Div. Owens-Illinois, Vineland, N. J., H. S. Moser.

Owens-Illinois, Inc., Toledo, Ohio, P. Close. Penn State Univ., University Park, Pa., J. B. Bodkin.

57
Department of Commerce

Malcolm Baldrige

{Secretary

j

trncsi Ambler, Lfcrecior Certificate of Qmlpm

Standard Reference Material 88a

Dolomitic Limestone

(All analyses are based on samples dried two hours at 110 °C)

Percent

Silica (SiO,) 1.20 Alumina (AL03 ) 0.19 Total Iron (as Fe2 03 ) .28 Titania (Ti02 ) .02 Manganese (as MnO) .03 Calcium (as CaO) 30.1 s Strontium (as SrO) 0.01 Magnesium (as MgO) 21.3 Sodium (as Na2 0) 0.01 Potassium (as K,0) .12 Phosphorus (as P2 05 ) .01 Carbonate (as CO,) 46.6 Loss on ignition 46.7

Washington, D.C. 20234 George A. Uriano, Chief

July 22, 1982 Office oi Standard Reference Materials (Revision ol Certificate dated 1-31-67)

58
U. S. Departriien#! of Commerce MauriceJ;JBL. Stans

Secretar

Certificate of Slnalpsitsi

STANDARD REFERENCE MATERIAL 97 a Flint Clay

(Results based on sample dried for two hours at 140 °C)

Analyst Si02 Al 2 Oi Fe2 0., Ti02 P2 Os K 2 0 Na2 0 Li 20 Zr02 BaO MgO CaO SrO Cr2 02 Loss on

Igni- tion

iiij 43.74 38.65 «£} {IS} 0.34 0.53' 0.033' 0.12' 0.063' 0.078' 0.16* 0.11* 0.1 7« 0.028" 13.32 43.68 38.95 .45 1.95 .35 .51' .041' .10" .07 .14« .11« .18" .03 13.31 43.60 38.79 .43" 1.87d .38' .46' Average.. 43.67 38.79 0.45 1.90 0.36 0.50 0.037 0.11 0.07 5 0.15 0.11 0.18 0.03 13.32 References: [1 1 G.E.F. Lundell and J.I. Hoffman, NBS J. Res. 1, 91 (1928) RP5.

|21 L. C. Peck, Geological Survey Bulletin 1170, (1964). »o-phenanthroline photometric method.

b Iron reduced with SnCl 2 and titrated with standard potas- sium dichromate solution. 'Cupferron gravimetric method.

•'H 2 02 photometric method.

'Flame emission spectrometry method.

'Pyrocatechol violet photometric method. "Atomic absorption method.

''Diphenylcarbazide photometric method. Molybdenum-blue photometric method. List of Analysts

1. R. K. Bell, B. B. Bendigo, T. C. Rains, T. A. Rush,

E. R. Deardorff, J. R. Baldwin, R. A. Paulson, W. P. Schmidt, and S. D. Rasberry, Analytical Chemistry Division, Institute for Materials Research, National Bureau of Standards.

2. L. C. Peck, United States Geological Survey, Denver, Colorado.

3. L. M. Melnick, J. D. Selvaggio, and D. G. Cunningham, Applied Research Laboratory, United

States Steel Corporation, Pittsburgh, Pennsylvania. The material for the preparation of this standard was proyided by the A. P. Green Fire Brick Company,

Mexico, Missouri. The overall direction and coordination of the technical measurements leading to certification were performed under the chairmanships of O. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification and issuance of this Standard Reference Material were coordinated through the Office of Standard Reference Materials by J. L. Hague.

Washington, D. C. 20234

October 8, 1969

J. Paul Cali, Acting Chief

Office of Standard Reference Materials

59
U. S. Departiftent of Commerce

Maurice_lL_Stans

Secretary

National Bureau of Standards

L. M. Brariscpmb, Director

Certificate of Snalpsfe

STANDARD REFERENCE MATERIAL 98 a Plastic Clay

(Results based on sample dried for two hours at 140 °C)

Analyst SiO, AhO, Fe2 02 TiO; P2 Os K 2 0 Na2 0 Li 2 0 Zr02 BaO MgO CaO SrO Cr20,

Loss

Igni- tion 1P1 48.98 33.13 & BS? 0.11 1.07" 0.080' 0.075' 0.042' 0.031' 0.42« 0.31» 0.041« 0.030h 12.40

21*1 48.91 33.31 1.35 1.64 .10 1.08' .083' .064* .03 .43" .31" .037« .04 12.49 3___ 33.12 1.28* 1.61'' .11' 0.98' Average. . 48.94 33.19 1.34 1.61 0.11 1.04 0.082 0.070 0.03 0.42 0.31 0.039 0.03 12.44 References: [1] G.E.F. Lundell and J.I. Hoffman, NBS J. Res. 1, 91 (1928) RP5.

[2] L.C. Peck, Geological Survey Bulletin 1170, (1964). »o-phenanthroline photometric method.

bIron reduced with SnCl 2 and titrated sium dichromate solution. 'Cupferron gravimetric method.

d H202 photometric method.

'Flame emission spectrometry method.

'Pyrocatechol violet photometric method. "Atomic absorption method.

"Diphenylcarbazide photometric method. Molybdenum-blue photometric method. List of Analysts

1. R. K. Bell, B. B. Bendigo, T. C. Rains, T. A. Rush,

E. R. Deardorff, J. R. Baldwin, R. A. Paulson, W. P. Schmidt, and S. D. Rasberry, Analytical Chemistry Division, Institute for Materials Research, National Bureau of Standards.

2. L. C. Peck, United States Geological Survey, Denver, Colorado.

3. L. M. Melnick, J. D. Selvaggio, and D. G. Cunningham, Applied Research Laboratory, United

States Steel Corporation, Pittsburgh, Pennsylvania. The material for the preparation of this standard was provided by the A. P. Green Fire Brick Company,

Mexico, Missouri. The overall direction and coordination of the technical measurements leading to certification were performed under the chairmenship of O. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification and issuance of this Standard Ref- erence Material were coordinated through the Office of Standard Reference Materials by J. L. Hague.

Washington, D. C. 20234

October 8, 1969

J. Paul Cali, Acting Chief

Office of Standard Reference Materials

60
Certificate of Snalpsfe

Standard Reference Material 99a

Feldspar

(All Analyses are Based on Samples Dried 2 hours at 105 °C)

Percent

Silica (SiOi) 65.2 Alumina (A1,03 ) 20.5 Iron (as Fe,0,) 0.06. Titania (TiO,) .007 Calcium (as CaO) 2.14 Barium (as BaO) 0.26 Magnesium (as MgO) .02 Sodium (as Na,0) 6.2 Potassium (as K,0) 5.2 Phosphorus (as PjO.) 0.02 Loss on Ignition 0.26

Washington, D.C. 20234 George A. Uriano, Chief August 10, 1981 Office of Standard Reference Materials (Revision of Certificate dated

3-26-65)

61
UNITED STATES DEPARTMENT OF COMMERCE

Washington 25, D.C. JSattonal bureau of g>tanfoarti£

Certificate of :Hnalps.e£

Standard Sample No. 103 a Chrome Refractory

(All results are based c ample dried for 2 hours at 105 to 110° C)

Analyst Cr203 A12 03 Total

iron as FeO MnO MgO CaO Si02 Ti02 Zr02 P206

l 32.05

k 31.95 CSS}

"32.08

-32. 10 32.12 "''31.78

1-29.95

/

I 30. 10 1 \ » 30.01 f

f

' 30.02 1 1

- 29.95 J

30. 05

"12. 43 "12. 43

•12. 45

d 0. 12 .12

11 '.10

• 18. 57

18. 50

18.51 18.62

'0.70

.69

f '.68 \ 1 '-67 j >>'.60

•4.68

»4. 68 "4. 59 -4. 58

«4. 63 "4.64

•0.22

.21 «,22

•'. 20

' 0.01 '0. 007

.01 *<.004

•"'.017

2

34

5 "12.43 6

>' 29. 91 •'12.40

29.85

k' 29. 80

"'.09 .10

-'. 10

•18.45

18.49

»' 18.63

'. 72 .70 b\74

! '.21 .25

"'.23

i.01 i'.Ol 7

8 ._

>' 12.43 "4.60 / ">'.009 \

{ °'.009 /

Average... 32.06 29.96 12. 43 0.11 18. 54 0.69 4.63 0.22 0.01 0.01

1 Dissolved in perchloric

» Dissolved

thod. Coi

Perchloric acid dehydi

lation and po tensometric titration with

i sulfate. Correci.'fi (or van.iJium.

by extracting RiOj

th chloroform, pre- weighed as AljOj. -KiCrjOj.

chloric acid. Gr<

for Ca and Mn.

i magnesium, sep

^

' Used R,03 precipit

i Dissolved in perchl

* Average of footnot

fusion with water, filtt

° Leach sodium iviom.ic- t precipitate. SnU, hM..<>,

o Perchloric .Kul-suHunc j< p Reduced with excess fci permanganate.

o Reduced with excess fei dichromate. Corrected (or v 'Separated with ammonia

cipitated with ammonia. Co

res

jrCrjOj.

Corrected for Ti.Oj.

* Leached 6odium i>fr.m-i<--M..li,i;ii hydroxide fusion, precipitated with ammonia. SnClj KjCrjO.

° Leached sodium peroxide fusion and dissolved hydn

ides. Periodate colorimetric method.

* Used filtrate of ammonia precipitation (footnote "t

pn-i ipit.w^.l ,•. |.hM ,ph.ite, separated as sulfat * Fused with sodium peroxide

perchloric acid.

' SiOj removed. with NH«OH. Aci

ecipitated in filtrat with NH.OR Co,

c TuS"

i perchloric and sulfuri :ids, precipitated

ilcium with alco- thod.

Gravimetric as phospha'

°' Prepared solution as in footnote "m." Peroiic

netric method.

p' Dissolved in nnrii , liy.lr", hlonc and perchloi

.Itered, volatilized arsenic as bromide, and prei phosphorus as phosphomolybdate. Determined th< :nt molybdenum as lead molybdate.

Dissolved in perchloric acid, volatilized ar Totnide and determine phosphorus colorimetri

approximately 900° C

List of Analysts

1. Keith M. Sappenfield, National Bureau of Standards.

2. Paul J. Byler, Booth, Garrett & Blair, Philadelphia, Pa.

3. Andrew S. McCreath & Sons, Inc., Harrisburg, Pa.

4. John H. Montague, E. G. Lavino and Co., Norristown,

Pa.

5. George Oplinger, K. A. Lane, and M. S. Budd, Solvay

Process Division, Allied Chemical Corp., Syracuse, N.Y. Washington, D.C, September 28, 1962.

6. B. C. Ruprecht and R. P. Lucas, Harbi:

Refractories Co., Pittsburgh. Pa.

7. L. J. Trostel, General Refractories Co., Baltimore, Md.

8. C. E. A. Shanahan, Richard Thomas & Baldwins, Ltd., Whitchurch, Aylesbury, Bucks, England.

A. V. Astin, Director.

62
U.S. Departim|n£6f Commerce

Rogers Cj£ Morton,

National Bkirelu o) Standards

Ernest Axbler, 'Acting Director Rational %nttm of ^tmintds

(fltrmxtntt of (Attaint*

Standard Reference Materials 113a and 329

Zinc Concentrates

These Standard Reference Materials are in the form of fine powder (<.15 mm) and are intended

for use both in checking chemical methods of analysis and in calibration with instrumental methods

of analysis. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant. SRM No. 113a 329

Element Percent by Weight'

Zinc 57.3 45. 5 Lead 2.80 6.06 Iron 2.08 12.94 Calcium Oxide 1.1, 0.08 Magnesium Oxide 0.75 • 16 5 Cadmium .78 .14 Copper .31 .132 Cobalt (H)b (.009) Nickel (.07) (.006)

Sulfur (Total) 30.6 (31.7)

Silicon Dioxide (1.54) (0.61) Indium .019 . Silver 0.046 7 d .0089

d

* Based on samples dried at 105 C for one hour Moistuie loas: for SRM 113a 0.08%; for SRM 329 0.4.%.

Figures in parenthesis are not certified but are given for information only.

jj Not determined. d

Troy ounces per ton is I3.63

for SRM U3a and 2.6„ for SRM 329. NOTE: The total of constituents reported for SRM 113a is 97.6% and that for SRM 329 is 98.0%. The remainder is expected to consist mainly of oxygen, carbon, and water of crystallization. CERTIFICATION: The value listed for a certified element is the present best estimate of the "true"

value based on the results of the analytical program. The value listed is not expected to deviate from

the "true" value by more than ± 1 in the last significant figure reported. For a subscript figure, the

deviation is not expected to be more than ± 5. Based on the results of homogeneity testing, maximum variations within and among samples are estimated to be less than the uncertainty figures given above. Washington, D.C. 20234 J. Paul Cali, Chief December 29, 1975 Office of Standard Reference Materials (Revision of Certificate of May 6, 1974 for change in silver results)

(over)
The material for these standards was supplied by Cominco American Inc., Spokane, Wash. The

material for SRM 113a was prepared at the Magmont Mines, Bixby, Mo., and that forSRM 329 at the Sullivan Mine, Trail, B.C., Canada. Following sieving and blending operations at NBS, homogeneity testing was performed by S. D. Rasberry and J. McKay, (x-ray fluorescence analyses); by E. J. Maienthal, (polarographic analyses); and by R. K. Bell, (chemical analyses).

Selected samples representative of the lot were analyzed and no significant variability was

observed when using subsamples of 0.5 g or larger. (Moisture determinations usually were made on

larger samples--up to 10 g.) Cooperative analyses for certification were performed in the analytical laboratories of Cominco,

Sullivan Mine, Trail, B.C., Canada, C. J. Mitchell; Cominco American Inc., Magmont Mines, Bixby,

Mo., R. J. Gibson; and St. Joe Minerals Corp., Zinc Smelting Division, Monaca, Pa., J. J. Aldrich. Analyses were performed in the NBS Analytical Chemistry Division by R. K. Bell and E. J. Maienthal. The overall direction and coordination of the technical measurements at NBS leading to certifi- cation were performed under the direction of 0. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification, and issuance of

these SRM's were coordinated through the Office of Standard Reference Materials by R. E.

Michaelis.

64
U. S. Departl^ntfof Commerce

Peter (Sgeterson lip Rational ^Bureau of j^tandartte

Certificate of ^nalgsis

Standard Reference Material 120b

Phosphate Rock

(Florida)

This standard is a finely powdered material intended for use in checking chemical methods of analysis and in calibration with optical emission and x-ray spectrometric methods of analysis. See ADDENDUM* (Over) for Uranium (Radium and Thorium)

(All results are based on samples dried for 1 hour at 105 °C.) Percent by Weight

ANALYST* P2 05 CaO SiOj F

Soluble Fe2 03 Soluble AI2 Oj MgO Na 2 0 MnO K 2 0 Ti02 C02 (MO

1 34.51 s 49.42b 4.70c 3.82d1.10e 1.09f « 0.29h 0.33f 9.032' 0.12f

-i 0.1

5

k 0.0021

2 34.51 m 49.35m 4.73" 3.79 m 1.10h 1.07" .28h .36h

.03 l h

.12) 0.09° 2.76P .002h

3 34.66" 49.38m 4.671 3.83 1.09h 1.07h .30 ,36h .032h

.12) .098° .15 2.79 ,002h 4 34.67

' 49.47m 4.694 3.81 s l.)3h 1.04h

.28h .35h ,032>< .087° .15 k 2.78P .003h

5 34.57 49.32"1 4.631 3.86 1.06h 1.05h

.25h .34* .085° 6 34.48m 49.451"

3.92s 1.14m 1.07' Average 34.57 49.40 4.68 3.84 1.10 1.06 0.35 0.032 0.12 0.090 0.15 2.79 0.002

Phosphorus weighedprecipitated with magnesia mixture, ignited and Mg1 PJ 0,.

' Calcium precipitated as oxalate, ignited and weighed as CaO.

Sample fused with Na,C0 3

, silica precipitated with ZnO and de- hydrated with HCI. Traces of Si0 3 recovered by H 3 SO„ dehydraFluorine distilled into NaOH solution and precipitated as lead chlorofluoride. Chloride is precipitated with excess AgN0 3 and

excess AgNO, is titrated with standard KCNS solution.

: SnClj reduction - K 3 Cr 3 0, titration. Flame emission spectrometry with repetitive optical scanning.

' A value of 1.13 percent was obtained for total A1 3 0 3 by gravimetry.

1 Atomic absorption spectrometry. K104 spectrophotometric method.

' Sample digested with mixed acids for 1 hour. Determinatio

pleted by atomic absorption spectrometry.

k H 3 0 3 spectrophotometric method.

' Polarographic method.

""Volumetric method.

Sample digested with dilute HCI or aqua regia for 15

Determination completed by atomic absorption spectrometry. p C03 absorbed and weighed. 4 Dehydration with HC104 in presence of boric acid. Molybdovanadophosphatc spectrophotometric method.

6 Distillation - titration with standard thorium nitrate solution.

' Aluminum precipitated with 8 hydroxyquinoline and weighed.

Washington, D C. 20234 J. Paul Cali, Chief

July 31, 1972 Office of Standard Reference Materials ADDENDUM* (Over) July 31, 1979

(over)

65
The overall direction and coordination of the technical measurements leading to certification were performed under the chairmanship of 0. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and C. L. Stanley.

PREPARATION, TESTING, AND ANALYSIS: The material for this standard was prepared by the American Cyanamid Company. Eighty five percent of the lot was made to pass 200 mesh sieve and some blending was done at the plant. Final sieving and blending operations were accomplished at NBS.

Homogeneity testing was performed by S. D. Rasberry, C. E. Fiori, and J. McKay with x-ray fluor- escence analysis. Calcium and phosphorus determinations were made on 14 samples representative of the top and the bottom of seven containers. The size of the samples taken for analysis was approximately 35 mg. The maximum variations in concentration among samples were within 0.09 percent for CaO and

0. 12 percent for P2 Os. The laboratories and analysts cooperating in the analytical program for certification were:

1. K. K. Bell, E. R. Deardorff, E. J. Maienthal, T. C. Rains, T. A. Rush, and S. A. Wicks, Analytical Chemistry Division, Institute for Materials Research, National Bureau of Standards.

2. J. Padar, Agrico Chemical Co., Division of Continental Oil Company, Pierce, Florida.

3. D. B. Underhill, Borden Chemical Co., Plant City, Florida.

4. C. C. Thornton, Thornton Laboratories, Inc., Tampa, Florida.

5. W. W. Harwood, R. M. Lynch and H. N. Gomez, International Minerals and Chemical Corp., Bartow,

Florida.

6. J . A. Sielski, American Cyanamid Co., Brewster Plant, Bradley, Florida.

ADDENDUM

Uranium has been determined at NBS by thermal ionization mass spectrometry, E. L. Garner and L. A. Machlan, and the following certification is made:

Value, /jg/g Estimated Uncertainty

3 Uranium 128.4 ± 0.5 'The estimated uncertainty is based on judgment and represents an evaluation of method imprecision and

material variability. (NOTE: On similar phosphate rock materials, a value of 127 ^g/g for uranium was reported in Ref. 1; additionally, values of 17 /ug/g for thorium and 43 pCi 225 Ra/g for radium also were reported.) Ref. 1 Agr. Food Chem.,16,No. 2, 1968 (p232)

66
U. S. Department of Commerce

Frederick B. Dent

Secretary

^atinttal ^Sttram af j^tanttartl*

Certificate of (JVnalgsis

Standard Reference Material 154b

Titanium Dioxide

This standard is in the form of fine powder, certified primarily for application in the paint and

ceramic industries.

Titanium Dioxide (Ti02)

Percent by Weight' 99.74 b

1 Based on material dried at 110 °C for two hours.

1 The value Riven in this certificate is based on the following pertinent analytical data:

" The uncertainty figure represents the 95% confidence interval of the mean of all accepted values.

Uncertainty0 0.05

Method

Controlled-potential coulometric

(0.2g samples) Volumetric (0.35g samples)

Volumetric (Analyst A)

Volumetric (ASTM D1394)

NBS

Average

99.73

99.71 Cooperators

3

99.75

99.78

Standard

Deviation'

0.03

0.04

0.05

Number of Determinations

" Two discrepant results were omitted.

I Results from one cooperating laboratory were deemed significantly high and have been omitted.

Results from Analyst B at the same laboratory were deemed significantly low and have been omitted.

Washington, D. C. 20234 J. Paul Cali, Chief May 16, 1 973 Office of Standard Reference Materials

67
PLANNING, PREPARATION, TESTING, and ANALYSIS: The material for this SRM has been

carefully selected and prepared not only to reflect the present composition needs but also the

anticipated future requirements. A particular ilmcnite ore was chosen so that, after beneficiation, the material would provide the

desired high rutile to anatase ratio (rutile 97+%, anatase about 2%). Bleaching agents were not added; thus the material has the characteristically yellowish color of rutile. The lot was thoroughly blended in the laboratory and then screened through a 44/im (325 mesh) sieve. Preliminary testing on 6 samples, representative of the lot, showed no evidence of inhomogeneity. The planning, preparation and preliminary testing were under the supervision of John J. Libera, Research and Development Department, National Lead Industries, St. Louis, Missouri. Cooperative analyses for certification were performed in the analytical laboratories of E. I. Du Pont De Nemours & Co., Pigments Department, Wilmington, Delaware, T. D. McKinley; National Lead

Industries, Titanium Pigment Division, South Amboy, New Jersey, Benjamin S. Sanderson; and

Sherwin-Williams Research Center, Chicago, Illinois, R. W. Scott. Analyses were performed in the Analytical Chemistry Division of the National Bureau of Standards by J. R. Baldwin and G. Marinenko. The overall direction and coordination of the technical measurements at NBS leading to certifica- tion were performed under the direction of 0. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and C. L. Stanley. ADDITIONAL INFORMATION ON THE COMPOSITION:

Certification is made only for the TU>2 content. Investigations of this material at NBS and at cooperating laboratories provided some additional information that may be useful, but is not

certified: Constituent Weight Percent P2 0s (0.04) Si02 (0.01) Fe2 03 (0.006) Pb (0.003) CaO (M).01) V (M).001

Cr (M).0005) Cu CvO.0005) MgO (M).01)

Moisture ( 1 10 °C-2 hours) (0.02 to 0.05) Loss on Ignition (900 °C for one (0.06 to 0.07) hour under helium)

If in the use of this SRM, determinations are made for any of the uncertified minor and trace constituents, it would be appreciated if the results were forwarded to the Office of Standard

Reference Materials. When sufficient information has been received the Certificate will be revised.

68
Department of Commerce

Juanita M«. Kreps

Secretary-'

jtional Bureau of Standards Emesl Ambler. Director Rational ^vtvtm of Standards

Certificate of (Analgsi*

Standard Reference Material 165a

Glass Sand

(In Cooperation with the American Society for Testing and Materials)

This SRM has been blended to ensure homogeneity. It should be dried for 2 hours at 105 °C before use.

Constituent Percent by Weight Ran '£ _s_ AI2O3 0.059 0.051 -0.066 0.0024 Fe2 03 .012 .007 - .017 .0018 Ti02 .011 .0065- .015 .0016 ZrQ2 .006 .0005- .012 .002

Certification - The value listed for each oxide is the best estimate of the"true"value based on the analytical data from both cooperators and NBS. The range of values listed is the tolerance interval, constructed such that it will cover at least 95% of the population with a probability of 0.99. It is computed as X ± Ks: where s is the standard

deviation, K is a factor that depends on n (the number of samples measured), p, the proportion of the total samples covered (95%), and y, the probability level (99%). In all cases none of the n values used exceeded the range specified. Thus, it includes variability between laboratories and samples. The overall direction and coordination of the round-robin analysis leading to certification were performed by

Paul Close, Chairman of ASTM Subcommittee C- 14.02 on Chemical Analysis of Glass and Glass Products. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed. Washington, D.C. 20234 J. Paul Cali, Chief October 1 6, 1 978 Office of Standard Reference Materials

(over)

69
Additional Information A content of 1 jig/g for C^Ch is not certified but rather is provided for information only. Chemical analyses for certification were performed in the following laboratories: Anchor Hocking Corp., Lancaster, Ohio, R. E. Carr. Brockway Glass Co., Inc., Brockway, Pa., E. L. McKinley. Corning Glass Works, Coming, N.Y., Y. S. Su. Ford Motor Co., Lincoln Park, Mich., T. L. LaFramboise.

National Bureau of Standards, Analytical Chemistry Division, E. J. Maienthal, J. D. Messman and T. C.

Rains. Kimble Div. Owens-Illinois, Vineland, N.J., H. S. Moser.

Owens-Illinois, Inc., Toledo, Ohio, P. Close. Penn State Univ., University Park, Pa., J. B. Bodkin.

70
U. S. Department* of Commerce

MauriceiJa. Stans

L. M. Br£o§apnifr. Director

Standard Reference Material 180

High-Grade Fluorspar

This Standard Reference Material has a high calcium fluoride content and is issued primarily for the geological and geochemical scientific community. [NOTE: This material is not a substitute for the fluorspar standard, SRM 79, used primarily for the assay of fluorspar imported for industrial

use.] Constituent Percent, by weight CaF 2 98.80a ± 0.03b

fThe value certified is based entirely on the method given in this certificate and is the mean of eight determinations. "The standard deviation of a single determination. Trace elements: These were determined by a general qualitative spectrochemical method and are given for information only. Fe, 0.1 - 1.0%; Al, Ba, Mg, Pb, Si, and Sr, 0.01 - 0.1%; Cu, K, Mn, Na,

Ti, and V, 0.001 - 0.01%; and Ag and Li, less than 0.001%. Analyst - E. K. Hubbard. The analytical work leading to certification was performed by K. M. Sappenfield, Analytical Chemistry Division, National Bureau of Standards. This material was supplied by Minera Frisco of San Francisco Del Oro, Chih., Mexico. The technical and support aspects involved in the preparation, certification, and issuance of this standard reference material were coordinated through the Office of Standard Reference Materials by J. L. Hague, R. E. Michaelis, and C. L. Stanley.

Washington, D. C. 20234 J. Paul Cali, Chief March 31, 1971 Office of Standard Reference Materials

(over)

71
METHOD FOR THE DETERMINATION OF CaF2 IN FLUORSPAR

*Transfer 0.50 g of fluorspar, previously dried at 100 to 105 °C, to a tared, ignited platinum

crucible. Add 15 ml of acetic acid (1:9) containing 0.667 g of CaC03 per liter. Digest on a steam

bath for 30 minutes and stir at five minute intervals. Add about 0.04 g of ashless filter pulp and stir for an additional minute. Filter through a double 12.5 cm extra dense filter paper (S & S No. 589 Red Ribbon) to which has been added about 0.04 g ashless filter pulp. Thoroughly wash the

crucible, paper, and stirring rod with 5 ml portions of hot water (40 to 60 °C), using a total of about 35 ml. After washing, wipe the stirring rod with a small piece of wet filter paper and add the paper to the filter. Transfer the paper and residue to the crucible, dry in an oven at 80 °C, char slowly under an infrared lamp, and ignite in a muffle furnace at 600 °C. **Add 3 ml of HF to the residue in the crucible and evaporate to dryness. Add 1 to 2 ml of HC104 and evaporate to dryness under the hood. Cool, wash the inside of the crucible with 1 ml more of HC104 (to catch any undecomposed particles of calcium fluoride), and again evaporate to dryness. Cool the crucible and immerse in a beaker containing 150 ml of dilute HC1 (5:95). Warm the beaker

gently and remove the platinum crucible, being sure to remove adhering particles of Ca(C104 ) 2.

Boil the contents of the beaker for 10 minutes. If any insoluble matter remains; filter, wash, and

ignite it in platinum. Treat the ignited residue with a few drops of HF and HC104 and heat to expel

the acids. Add 1 to 2 ml of HC1 and digest on a steam bath. Transfer the contents to the main

filtrate. Pass H2 S into the clear filtrate for several minutes and then make the solution ammoniacal. Continue with H 2 S for 10 minutes and allow the precipitate to settle for 20 to 30 minutes. Filter and wash with NH4 C1—(NH4 ) 2 S solution. (Prepare by passing a moderate stream of H2 S for 5 minutes

through a solution containing 5 ml of NH4 OH and 10 g of NH4 C1 per liter.) Neutralize the filtrate and washings with HC1, and add an additional 20 ml of HCL. Boil for 2 to 3 minutes to expel most of the H2 S. Add KBr-Br2 solution (20% solution of KBr saturated with Br2 ) until the solution remains yellow. Boil until the finely divided sulfur has been oxidized and the bromine has been expelled. If the sulfur or sulfides are not removed by the bromine treatment,

filter, wash the paper well and discard the residue. Dilute the filtrate to about 200 ml. Precipitate the calcium by adding 2 g of (NH4 ) 2 C2 04 -H 2 0 and, while stirring, slowly add NH4 OH until the

solution is slightly ammoniacal. Heat on a steam bath for one-half to one hour, stirring occasionally. Cool to room temperature. Filter on a close textured paper. Wash with a cold 0.1 percent solution of (NH4 ) 2 C2 04 -H 2 0. Ignite to constant weight. Calculate the percent CaF2 from the weight of the CaO.

References: *Removal of soluble calcium in acetic acid. Interlaboratory study of soluble calcium. ^Method: Calcium in fluorspar The Analysis of Fluorspar by G. E. F. Lundell and J. I. Hoffman, J. Res. Nat. Bur. Stand. (U.S.), 2

(1929) R.P. 51.

72
U. S. Department of Commerce

Malcolm Baldrige

^>ecreiary7

National Burwu 6r$tandards

Ernest Ambter. director

(Certificate of ^tralgsi*

STANDARD REFERENCE MATERIALS

181, 182, and 183

Lithium Ores

These SRM's are intended for use in checking the accuracy of assay methods. They are certified for their constituent of economic interest. Additional data for information only appears on page 2. These SRM's are supplied in the form of fine powder.

SRM 181 SRM 182 SRM 183 (Spodumene) (Petalite) (Lepidolite)

Wo Wo %

Li 20 6.3g 4.34

The value listed for Li20 in the three SRM's is the best estimate of the "true" value. The deviation is not expected to be more than ± 5 in the subscript number.

Washington, D.C. 20234 October 1, 1981 (Revision of Certificate dated 2/24/58 and Reprinted 8/20/70)

George A. Uriano, Chief

Office of Standard Reference Materials

(over)

73
The following values are approximate, and are listed only for information. Constituent Wt. % Wt. % Wt. %

Na2 0 (0.8) (0.4) (0.2) K2 0 ( .3) ( .1) (8. ) Rb2 0 --- ( .03) (3.5) Cs2 0 --- --- ( .3)

74
UNITED STATES DEPARTMENT OF COMMERCE

WASHINGTON 25, D.C. Rational Pureau of is>tanbarti£

Certificate of &nalp£e£

Standard Sample 198

Silica Brick

(All results are based on samples dried at 105° to 110° C.)

Analyst Al,0, Total iron as FejO, TiOs Zr02 PaOt MnO CaO MgO KaaO KsO Li,0 'Loss on

ignition

1

f "0.17

\

••".15

k. 19

•0.6S\

'«.67/

k.64

0.02 <0.01 1 0. 022 '0.006 2.72 0.07 i0. 007 > 0. 016 i 0.001 0.21

2.. k.01 k .012 "2.74 k.06 k .009 k .010 k .001 .32

3.... { V,5

-.671

".65/

'.69

.01

.02

".011 2.75 .06 -.02 ".03 .22

4 o. 17 ".026 2.73 '.008 k .016 k <.007

i. 002

.15

5

b.17 66

.68

.01 '.025 2. 72 .07 i.005 i. 012 .23

6. .03 .026 2.72 .07 .23 i.005 !. 001

7

b. 16 '. 68 .03 .025 <.005 .09 i.02 i.02 '.001 .22

8 16 '.66 .02

.02 K019 2.70 .08 .20

9.... k . IS '.66

{ :-.°o224}

'.008 2.74 .07 «<.01 .14

10 >>. 16 '.66 .01 nil 2.67 .06 .20

».». 16 '. 68 .01 .02

'.024 -.01 .0082.67 .09

12 «. 16 '.67 '.024 2. 71 .08 i.02 i. 018

Average.... 0.16 0.66 0.02 0.022 0.008 2. 71 0.07 0.012 0.017 0.001 0.21

:ibfe > Weighed

FejOj. TiOl,

» 1 g heated at 90t)° to 1,000° C. ill a covered platinum

"itedTM m£oH precipitate corrected for dPaOj.

separated from iron, i ii.mniiii, etc., with dium hydroxide, precipitated, nnd weighed as A1PO*.

d Same value obtained by the Aluminon photomctru: "Thiocyanate photometric method.

' SnCli-KaCnO method.

c Same value obtamed gravimetricaily as FejOi.

method.

Iron ueparated from aluminum : xchange, precipitated t

' ' reighed asFeiOi.

» Gravimetric. Weighed as MgiPiOt.

» Titration with AgNOi. following ion

ion of sodium and potassium chlorides.

roxyquinolinc precipitation. Bromate-thiosuliatc

See Trans. British Ceramic Society 51. No.

lethod.

' Weighed as A1PO..

' Orthophenanthroline photometric method.

1 by erioehromecyanine-R phoi w Same value t

List <

1. K. M. Sappenfield and R. A. Paulson, National Bureau of Standards.

2. G. R. Eusner, U. S. Steel Corp., Monroeville, Pa.

3. B. E. Gummo, W. O. Osborn, and R. N. Smith, Cres- cent Division, North American Refractories Co., Curwensville, Pa.

4. M. P. Bennett and Falba Whitney, Gladding, McBean & Co., Los Angeles, Calif.

5. B. C. Ruprecht, Harbison-Walker Refractories Co., Pittsburgh, Pa. Washington 25, D.C, January 6, 1960.

Analysts

6. A. R. Lesar, A. P. Green Fire Brick Co., Mexico, Mo.

7. L. J. Trostel, General Refractories Co., Baltimore, Md.

8. D. J. Hallisey, Jones & Laughlin Steel Corp., Pitts- burgh, Pa.

9. J. J. Hazel, Republic Steel Corp., Cleveland, Ohio.

10. Paul Smith, The Refractories Institute, Mellon Insti- tute, Pittsburgh, Pa.

11. J. B. Armstrong, Sparrows Point Plant, Bethlehem

Steel Co., Sparrows Point, Md.

12. W. F. Zollinger, Bethlehem Steel Co., Bethlehem, Pa.

A. V. Astin, Director.

75
UNITED STATES DEPARTMENT OF COMMERCE

WASHINGTON 25, D.C. jSational Pureau ot ^tanbarbs.

Certificate of .analyses.

Standard Sample 199

Silica Brick

(All results are based on samples dried at 105° to 110° C.)

Analyst A!2 U,

Total iron

as FeA TiOa Zr02 P20, MnO CaO MgO NaaO K,0 Li20

* Loss on

ignition

1 J

l»0.47 \ °.48

J 0. 761 -.74} 0.07 0.01 ' 0. 010 -0.005 2.41 0.13 '•0.015 1-0.09 >* 0.001 0.14

2 '.49 '.70 '.05 '.016 ' 2.45 '. 14 1.010 i.07

'.11

'. 002 .23

3 '.48 7S .05 2.42 . 12 '.02 .16

4 -.48 J.73 .06

.06

".026 2.38 .14 «. 014 KU i<.007 .002

.12

5 >>.51 ».74 ".012 2.39 .13 '•.010 i'. 088 . 16 .07 .015 .008 2.46 .14 '•.004 .12

>'.02

h. 10 \ 001

7 *>. 50 '.75 .07 .025 <.005 2.43 .10 >>.09 '•.002 .16

'.48 ".76 .07 '. 005 2. 38 .14 .13

9 : 72 .06 -.013 «. 007 '. 14 i<.01 .30

10 '•.49

'• '.48

75 .06 nil .03 2.37 .13 .17

11 74 .06 a. 008 ". 01 2.38 .14 '.097

12 '.48 d.74 .06 o.OlO 007 2. 39 .14 \03 >'. 087

Average.... 0.48 0.74 0.06 0.015 0. 007 2.41 0.13 0.015 0.094 0. 002 0. 17

900° C to 1,000° C. in I

b WciRhed ignited NH^OH prccipit

I'erOj, TiOi. and P1O1.

• Aluminum separated from iron, ti ../ cupferron, pirap

welshed .18 AhO, ,,n.l , .rrr 1 v„n Kit rJh mrlh.. I. •WViKh-J as FeiOi.

I Molybdenum-blue phot

« Periodate photometric

1 for PlOi.

rill.. l,i(.lllU !.

ed for ZrOi.

b Flame-photometric method.

1 Spectrographs determination,

i Same value obtained by separating

il l iiumtim by ion exchange, and we ^^X-KMnOi method.

1 Titration with ArNOi, f. .11. ...... :it.; ion of sodium and potassium chloride

10 8-Hydroxyquino"

!te titration. See 1

. 438 (1952).

» Titrated with TaCSOt),

i Phosphomolybdatc-alltal

• Weighed as AlPO..

jOrthophenanthroline^pht

etric method.

° Persulfate-arsenite method

MgiPiOt.

method,

eriochromecyaninc

NH.C1-

R photoCaCOi.

List of Analysts

1. K. M. Sappenfield and R. A. Paulson, National Bureau of Standards.

2. G. R. Eusner, U.S. Steel Corp., Monroeville, Pa.

3. B. E. Gummo, W. O. Osborn, and R. N. Smith, Cres- cent Division, North American Refractories Co., Curwensville, Pa.

4. M. P. Bennett and Falba Whitney, Gladding, McBean & Co., Los Angeles, Calif.

5. B. C. Ruprecht, Harbison-Walker Refractories Co., Pittsburgh, Pa. Washington 25, D.C, January 6, 1960.

6. A. R. Lesar, A. P. Green Fire Brick Co., Mexico, Mo.

7. L. J. Trostel, General Refractories Co., Baltimore, Md.

8. D. J. Hallisey, Jones & Laughlin Steel Corp., Pitts- burgh, Pa.

9. J. J. Hazel, Republic Steel Corp., Cleveland, Ohio.

10. Paul Smith, The Refractories Institute, Mellon Insti- tute, Pittsburgh, Pa.

11. J. B. Armstrong, Sparrows Point Plant, Bethlehem

Steel Co., Sparrows Point, Md.

12. W. F. Zollinger, Bethlehem Steel Co., Bethlehem, Pa. A. V. Astin, Director.

76
Rational $mt*n of ^tandanls

Certificate of ^nalgsts

Standard Reference Material 277

Tungsten Concentrate

(In cooperation with the American Society for Testing and Materials)

This material is in the form of powder (<0. 15 mm) intended for use in checking chemical methods of analysis and in calibration with instrumental methods of analysis. Constituent Certified Value' (wt%) Estimated Uncertainty

2 (wt%) WOj 67.4 0.3 (Results are based on samples dried at 1 10 °C for one hour) The certified value is the present best estimate of the "true" value based on the results of the cooperative program for certification.

2 The estimated uncertainty is based on judgment and represents an evaluation of the combined

effects of method imprecision,possible systematic errors among methods, and material variability for samples of 1 g or more (No attempt was made to derive exact statistical measures of

imprecision because several methods were involved in the determination.) CAUTION: The material for this SRM primarily was derived from wolframite ores. It is, however, a mixture

of concentrates from China, Thailand, and USA that contains titanium, niobium, tantalum, and tin in amounts not normally encountered in most wolframite concentrates. These constituents may interfere in the

"classic" chemical procedures and may necessitate appropriate changes in methodology. Also, x-ray fluoresc- ence methods of analysis that use SRM 277 to make relative measurements of "pure" wolframite (or scheelite) concentrates may exhibit systematic errors because of the unusual constituents contained in this concentrate. The overall coordination of the technical measurements leading to certification were performed under the

direction of J. I. Shultz, Research Associate, NBS-ASTM Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis. Washington, D.C. 20234 J. Paul Cali, Chief October 24, 1978 Office of Standard Reference Materials

(over)

77
PLANNING, PREPARATION, TESTING, ANALYSIS: The material for SRM 277 was carefully selected and provided to NBS by GTE Sylvania, Towanda, Pennsylvania, courtesy of J. Demangone. At Sylvania, the material was crushed and ground to a fine powder. At NBS the material was sieved (<0. IS mm) and thoroughly

blended. Homogeneity testing of selected samples representative of the lot of SRM 277 was performed by an x-ray fluorescence technique by R. E. Michaelis. The material variability was determined to be within ± 0. 1 (wt%) of wo3 . Cooperative analyses for certification were performed in the following analytical laboratories: Alfred H. Knight International, Ltd., Cheshire, U.K. - J. F. L. Knight. Benedict Kitto and Sons, London, U.K. - R. Peck. General Electric Company, Cleveland, Ohio - J. Rynasiewicz and J. W. Fulton. GTE Sylvania, Towanda, Pa. - R. Dyck; and Waltham, Mass. - J. F. Cosgrove. Hermann C. Starck, Berlin, Germany - O. Hilmer. Ledoux & Company, Teaneck, N. J. - S. Kallmann.

National Bureau of Standards, Washington, D.C. - E. R. Deardorff. Sandvik, A. B., Stockholm, Sweden - K. Kaarik; and Sandvik Asia Ltd. - N. R. Sanjana. Spectro Chem Labs , Inc., Franklin Lakes, N. J. - E. W. Hobart.

Treibacher Chemische Werke, Treibach, Austria - Z. Otto. Westinghouse Electric Corporation, Bloomfield, N. J. - P. J. Walitsky. Union Carbide Corporation, Bishop, Calif. - E. C. Gibbs and K. M. Wilder; and Niagara Falls, N. Y. - P. Greenberg. VEW Ternitz, Austria - A. J. Leeb. NOTE: Details regarding the methodology employed in the analysis of this SRM, along with other pertinent information, will appear in a separate publication. ADDITIONAL INFORMATION OF THE COMPOSITION: Certification is made only for the WOi

content; however, SRM 277 contains additional constituents of interest as indicated below. These are not

certified and are provided for information only. Table 1 lists those constitutents for which data were received from two or more laboratories that were in good agreement. (Most of these are expected to be proposed for

certification at a later date and, therefore, an indication of the uncertainty also is given.) Table 2 lists those constituents for which data were received from a single laboratory (or discrepant data from two or more laboratories).

78
NOT CERTIFIED

Table 1 Constituent Approximate Value (wt%) Approximate Uncer Calcium (0.37) (0.02) Iron (7.4) (.1) Lead (0.07) (01) Manganese (10.0) (.2) Molybdenum (0.06) (.01) Niobium (1.00) (.03) Phosphorus (0.03) (01)

Silicon (.85) (.05) Sulfur (25) (.03) Tin (.54) (-07) Titanium (2.2) (.2) NOT CERTIFIED

Table 2 Information Information

Constituent Value (wt%) Constituent Value (wt%)

Arsenic (0.015) Oxygen (21.4) Bismuth (.07) Scandium (0.05) Cerium (.03) Tantalum (.20) Chromium (.04) Thorium (.08) Copper (.02) Uranium (.13) Gadolinium (.01) Yttrium (.03) Lanthanum (.02) Zirconium (.01) Neodymium (.03) In addition to the above, trace concentrations were reported (ppm bywt.) for the following as an indication of the relative amounts observed: Antimony (3), Barium (20), Boron (20), Dysprosium (30), Erbium (20), Europium (10), Holmium (5), Hafnium (20), Indium (20), Lutetium (5), Praseodymium (50), Samarium (40), Tellurium (2), Terbium (10), Thallium (2), Thulium (10), Vanadium (70), Ytterbium (50) and Zinc (20). NOTE: Although SRM 277, Tungsten Concentrate, is expected to be stable under normal storage conditions, prudent cautions in the laboratory should be observed. The bottle should be kept tightly capped except when in direct use. Store in a desiccator over desiccant.

79
Rational ^Buram of js>tatttlartb

Certificate

Standard Reference Material 278

Obsidian Rock

This Standard Reference Material (SRM) is intended for use in evaluating the accuracy of analytical methods and

instruments used in the analysis of geological type materials. SRM 278 is a finely powdered obsidian rock, which was

obtained from Clear Lake, Newberry Crater, Oregon.

Certified Values of Constituents The concentrations of the constituents were determined by methods that are widely used in the field of geological analysis and have a demonstrated accuracy. The values given are "certified" values, i.e., those values that were determined by

either a definitive method, reference method, or by two or more independent methods, and "information" values that were determined by single or non-reference methods. The certified values are given in Table I. Table 1. Certified Values of Constituents

Constituent Contem- pt %) Constituent' Content

2 Wt(Mg/g) AI2O3

d 14.15 ±0.15 Cu e 5.9 ±0.2 CaO' 0.983 ± 0.002 Ni

e 3.6 ±0.3 FeO

' 1.36 ±0.02 Rb a,c 127.5 ±0.3

Fe2 03

l,f (Total Fe as Fe2 Oi)

2.04 ±0.02 Sr

e 63.5 ±0.1 K 2 0

a ' d,e 4.16 ±0.02 Th e,f 12.4 ±0.3 MnO b,f 0.052 ± 0.002 Tl

e 0.54 ± 0.04 Na2 0

a,J '' 4.84 ±0.05 u

e 4.58 ± 0.04 P2O5

b ' d 0.036 ± 0.003 Pb

c 16.4 ±0.2

sio2 u 73.05 ±0.13 TiQ2 h ' 8 0.245 ± 0.007

Methods ol Analysis:

' Atomic Absorplioi

Spectrometry

etry 'isotope Dilution Mass Spectrometry

he estimated uncertainties of the certified values are

tlects ol method imprecision, possible systematic err No attempt was made to derive exact statist lelerminalion ol most constituents.)

Neutron Activation Analysis Prompt-gamma Activation Analysis

Specific Ion Electrode Potentiometry

'Titrimetry

J Volumetry

1 judgment and represent an evaluation of the combined

ng methods and material variability of 250 mg or more,

^precision because several methods were involved in the

The overall direction and coordination of the technical measurements leading to certification were performed in the Inorganic Analytical Research Division, E. L. Garner, Chief. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference

Material were coordinated through the Office of Standard Reference Materials by T. E. Gills. Washington, D C. 20234 August 19, 1981 George A. Uriano, Chief

Office of Standard Reference Materials

80
Supplemental Information

Preparation The material was processed by the Colorado School of Mines, Golden, Colorado. Approximately 350 lbs of obsidian rock were crushed, ground, and sieved to <200 mesh. The material was mixed in a cone blender to ensure homogeneity. For homogeneity testing and certification samples were randomly chosen and analyzed for both major and minor

constituents. The inhomogeneity of this material is considered to be <2% relative. Analysis SRM 278, a natural glass, is hygroscopic and contains water that cannot be driven off by drying at low temperatures. This material will pick up additional water on exposure to the atmosphere. Thus, exposure time should be kept to a minimum. Furthermore, the sample should be ignited to a constant weight in a muffle furnace or over a small flame at a temperature between 350-600 °C. This procedure will ensure the accurate and precise determination of SiCh, K2O,

Na20, AI2O3 and possibly other major constituents. The analysts and laboratories cooperating in the analytical program for certification were: M.J. Blackman, E. L. Garner, J. W. Gramlich, L. A. Machlan, L. J. Moore.and R. Zeislerofthe Inorganic Analytical Research Division, National Bureau of Standards.

J. B. Bodkin, J. C DeVine, and N. H. Suhr of the Mineral Constitution Laboratories, The Pennsylvania State

University, University Park, Pa.

S. S. Goldich of the Department of Geology, Northern Illinois University, DeKalb, III. M. D. Glascock, C. C. Graham, J. R. Vogt, University of Missouri, Columbia, Mo.

The constituents given in Table 2 are not certified but are included for information only. Table 2. Information Values

Constituent Content wt % Constituent Content wt (jigjg) C (Total Carbon)J (0.05) Ba

f (1140 ) C02

d (0.01) B

8

( 25 ) F " (0.05) Ce ' ( 62.2 ) MgO " (0.23) Co

f ( 1.5 ) Cr '

( 6.1 ) Cs ' ( 5.5 ) Eu

r ( 0.84) Gd g

( 5.3 ) Hf ' ( 8.4 ) Lu ' ( 0.73) Sb '

( 1.5 ) Sc ' ( 5.1 ) Sm 1,8

( 5.7 ) Ta ' ( 1.2 ) Tb ' ( 1.0 ) Yb ' ( 4.5 ) Zn f ( 55 )

81
U.S. Departntu^bf Commerce

Rogers t'jj. Morton,

sVcjjetar> National Hkirftl o) Standards

Ernest Ambler, Acting Director Rational IBureait of j^tantlanb

(ttertititat* of ^nalgst*

Standard Reference Materials 113a and 329

Zinc Concentrates

These Standard Reference Materials are in the form of fine powder (<.15 mm) and are intended

for use both in checking chemical methods of analysis and in calibration with instrumental methods

of analysis. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant. SRM No. 113a 329

Element Percent by Weight"

Zinc 57.3 45.5 Lead 2.80 6.06 Iron 2.08 12.94 Calcium Oxide l.la 0.08 Magnesium Oxide 0.75 .16S Cadmium .78 .14 Copper .31 .132 Cobalt (.11)* (.009) Nickel (07) (.006)

Sulfur (Total) 30.6 (31.7)

Silicon Dioxide (1.54) (0.61) Indium ...c .019 . Silver 0.046 7 6 .0089

d

' Based on samples dried at 105 °C for one hour. Moisture loss: for SRM 1 13a 0.08%; for SRM 329 0.4,%.

Figures in parenthesis are not certified but are given for information only.

c Not determined. d Troy ounces per ton is 13 t> 3

for SRM U3a and 2.6„ for SRM 329. NOTE: The total of constituents reported for SRM 113a is 97.6% and that for SRM 329 is 98.0%. The remainder is expected to consist mainly of oxygen, carbon, and water of crystallization. CERTIFICATION: The value listed for a certified element is the present best estimate of the "true"

value based on the results of the analytical program. The value listed is not expected to deviate from

the "true" value by more than ± 1 in the last significant figure reported. For a subscript figure, the

deviation is not expected to be more than ± 5. Based on the results of homogeneity testing, maximum variations within and among samples are estimated to be less than the uncertainty figures given above. Washington, D C. 20234 J. Paul Cali, Chief December 29, 1975 Office of Standard Reference Materials (Revision of Certificate of May 6, 1974 for change in silver results)

(over)

82
The material for these standards was supplied by Cominco American Inc., Spokane, Wash. The

material for SRM 113a was prepared at the Magmont Mines, Bixby, Mo., and that forSRM 329 at the Sullivan Mine, Trail, B.C., Canada. Following sieving and blending operations at NBS, homogeneity testing was performed by S. D. Rasberry and J. McKay, (x-ray fluorescence analyses); by E. J. Maienthal, (polarographic analyses); and by R. K. Bell, (chemical analyses).

Selected samples representative of the lot were analyzed and no significant variability was

observed when using subsamples of 0.5 g or larger. (Moisture determinations usually were made on

larger samples-up to 10 g.) Cooperative analyses for certification were performed in the analytical laboratories of Cominco,

Sullivan Mine, Trail, B.C., Canada, C. J. Mitchell; Cominco American Inc., Magmont Mines, Bixby, Mo., R. J. Gibson; and St. Joe Minerals Corp., Zinc Smelting Division, Monaca, Pa., J. J. Aldrich.

Analyses were performed in the NBS Analytical Chemistry Division by R. K. Bell and E. J. Maienthal. The overall direction and coordination of the technical measurements at NBS leading to certifi- cation were performed under the direction of O. Menis and J. I. Shultz. The technical and support aspects involved in the preparation, certification, and issuance of

.these SRM's were coordinated through the Office of Standard Reference Materials by R. E.

Michaelis.

83
U.S. Department of Commerce

Elliot L. Richardson,

Secretary Rational ^ureau of Standards

(Uerttftcate of (Analysts.

Standard Reference Material 330

Copper Ore, Mill Heads

This material is in the form of fine powder intended for use both in checking chemical methods of analysis and in calibration with instrumental methods of analysis. This SRM is one of a series of four SRM's issued primarily for use in evaluation of the critically important

"material balance" in the copper mining and metallurgical industries. The other three are: SRM 331, Copper

Ore, Mill Tails; SRM 332, Copper Concentrate; and SRM 333, Molybdenum Concentrate. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant.

Constituent Certified Value''

h Estimated

Uncertainty'

Total Copper Molybdenum

Rhenium

Percent b v Weieht

0.84 0.01 .018 .001 PPM bv Weieht

0.30 0.06

' Based on samples dried al 105 °C for two hours. Separate s

" The certified value is the hesi estimate of the "true" value.

' Estimated uncertainty includes both method imprecision and

more) for molybdenum, and 2 5 g (or more) for rhenium The following values indicate the results of the analytical tests made at NBS and the Magma Copper Company.

e used for rhenium and calcu

ariability with samples 0.5 g (c

) a dry-weight basis.

) for total copper, I Og <

Constituent / Method

I oial Copper

Isotopic dilution mass spectrometry

(0.5 g samples) Polarographic (0.5 g samples) Iodometric (2.5 g samples)

4 Molybdenum

Isotopic dilution mass spectrometry

( I g samples)

Isotopic dilution mass spectrometry

(2.5 g samples)

Standard

Deviation"

Percent by Weight

0.007

01

01 Range

0 0001 PPM by Weight Range

0.054

Number of Determinations

Details of the methods used, including drying and dissolution procedures, are given i

' Of single determinations for total Cu; range given for Mo and Re.

' This method has been studied extensively and the data are considered free from syste

4 Results from Magma Copper Company Washington, D. C. 20234 January 20, 1977

(Revision of Provisional

Certificate of 2-20-73) (Over)

J. Paul Cali, Chief

Office of Standard Reference Materials

84
PLANNING, PREPARATION, TESTING, ANALYSIS: The material for this SRM (330) was carefully

selected and provided to NBS by Magma Copper Company, San Manuel, Arizona, through the courtesy of

T. L. Young. At NBS this material was sieved and thoroughly blended, which involved several independent procedures [1]. Homogeneity testing of selected samples representative of the lot of SRM 330 was performed simultaneously

with the analytical program for certification. At NBS, 0.5 g samples showed the maximum variability for total copper to be ±0.010 percent. At Magma, 2.5 g samples showed the maximum variability to be ±0.01 percent. Cooperative analyses were performed at the Magma Copper Company, San Manuel, Arizona, by B. Cripe, R. L. Culder, A. B. Hall, D. A. Shah, J. T. Tadano, and M. Toelkes. Analyses were performed in the NBS Analytical Chemistry Division by E. L. Garner, J. W. Gramlich, L. A. Machlan, E. J. Maienthal, J. R. Moody, and T. J. Murphy. The overall direction and coordination of the technical measurements at NBS leading to certification were performed under the direction of W. R. Shields and I. L. Barnes. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis. ADDITIONAL INFORMATION ON THE COMPOSITION: Certification is made only for total Cu, Mo,

and Re. Although NOT CERTIFIED, the following additional information on the composition may be of

interest. Gold and Silver

Fire assay determinations for Au and Ag were made at Magma Copper Company:

Fire assay

Gold Silver PPM by Weight

(0.093) *(1.51)

Revised 02/28/79 "Acid-Soluble" Copper The total copper content includes "recoverable" sulfide copper and "nonrecoverable" oxide copper. Industrial practice is to determine "acid-soluble" copper and to relate this result to the oxide copper content. Investigation

at NBS provided additional information on "acid-soluble" copper that may be useful, but is not certified:

Constituent/ Method Average Range Number of Determinations

"Acid-Soluble" Copper

Isotopic dilution mass

spectrometry (2.5 g samples)

Percent

(0.069)

t?y Weight

(0.063-0.081) 9

REFERENCES

[I] J. R. Moody, I. L. Barnes, and R. E. Michaelis, Standard Reference Materials: Copper Ore, Mill Heads

SRM 330: Copper Ore, Mill Tails - SRM 331; Copper Concentrate - SRM 332, and Molybdenum Concentrate - SRM 333; Nat. Bur. Stand. Spec. Publ. 260-xx (in press). [2] W. R. Shields, Editor, Nat. Bur. Stand. Tech. Note 546, (1970).

85
J.S. Department of Commerce

Elliot L. Richardson,

Certificate of (Analgsis

Standard Reference Material 331

Copper Ore, Mill Tails

This material is in the form of fine powder intended for use both in checking chemical methods of analysis and in calibration with instrumental methods of analysis. This SRM is one of a series of four SRM's issued primarily tor use in evaluation of the critically important

"material balance" in the copper mining and metallurgical industries. The other three are: SRM 330, Copper

Ore, Mill Heads; SRM 332, Copper Concentrate; and SRM 333, Molybdenum Concentrate. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant.

Constituent Certified Value a,b Estimated

Uncertainty'

Total Copper Molybdenum

Rhenium

Percent b y Weight

0 091

.0022 PPM bY

.04

0.001 .0002 Weight

.02

' Based on samples dried at 105 °C for two hours Separate samples are used for rhenium and calculated to a dry-weight basis.

h The certified value is the best estimate of the "true" value.

' Estimated uncertainty includes both method imprecision and material variability with samples 1 Og (or more) for total copper and molyb- denum, and 2.5 g (or more) for rhenium. The following values indicate the results of the analytical tests:

Standard Number of

Constituent / Method 1 Average Deviation2 Determinations

Total CoDDer Percent by Weight

Isotopic dilution mass spectrometry

1 0.0915 0.0005 15

(1.0 g samples) Polarographic .091 .001 4

(2.5 g samples) Molybdenum Range

Isotopic dilution mass spectrometry' .0022 0.0001 2

( 1.0 g samples) PPM bv Weight

Rhenium Range

Isotopic dilution mass spectrometry' 0.043 0.016 6

(2.5 g samples)

' Details of the methods used, including drying and dissolution procedures, are given in a separate publication [1].

' Of single determinations for total Cu, range given for Mo and Re.

1 This method has been studied extensively and the data are considered free from systematic errors [2]. Washington, D. C. 20234 J. paul Cali, Chief January 20, 1977 Office of Standard Reference Materials

(Revision of Provisional

Certificate of 2-20-73) (Over)

86
PLANNING, PREPARATION, TESTING, ANALYSIS: The material for this SRM (331) was carefully

selected and provided to NBS by Magma Copper Company, San Manuel, Arizona, through the courtesy of

T. L. Young.

At NBS, this material was sieved and thoroughly blended, which involved several independent procedures [1]. Homogeneity testing of selected samples representative of the lot of SRM 331 was performed simultaneously with the analytical program for certification. At NBS, the maximum variability for total copper was determined

to be ±0.0008 percent (15 determinations with 1 g samples). Analyses were performed in the NBS Analytical Chemistry Division by E. L. Garner, J. W. Gramlich, L. A. Machlan, E. J. Maienthal, J. R. Moody, L. J. Moore, and T. J. Murphy. The overall direction and coordination of the technical measurements at NBS leading to certification were per- formed under the direction of W. R. Shields and I. L. Barnes. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis. ADDITIONAL INFORMATION ON THE COMPOSITION: Certification is made only for total Cu, Mo,

and Re. Although NOT CERTIFIED, the following additional information on the composition may be of

interest. Gold and Silver

Fire assay determinations for Au and Ag were made at Magma Copper Company:

Fire assay

Gold Silver PPM by Weight

(0.034) *(0.243)

•Revised 02/28/79 "Acid-Soluble" Copper The total copper content includes "recoverable" sulfide copper and "nonrecoverable" oxide copper. Industrial practice is to determine "acid-soluble" copper and to relate this result to the oxide copper content. Investigation

at NBS provided additional information on "acid-soluble" copper that may be useful, but is not certified:

Constituent/ Method Average Range Number of Determinations

"Acid-Soluble" Copper Percent by Weight

Isotopic dilution mass 3 spectrometry (2.5 g samples)(0.051) (0.051-0.052)

REFERENCES

[I] J. R. Moody, I. L. Barnes, and R. E. Michaelis, Standard Reference Materials: Copper Ore, Mill Heads

SRM 330; Copper Ore, Mill Tails - SRM 331;Copper Concentrate - SRM 332, and Molybdenum Concentrate - SRM 333, Nat. Bur. Stand. Spec. publ. 260-xx (in press).

[2] W. R. Shields, Editor, Nat. Bur. Stand. Tech. Note 546, (1970).

87
U.S. Department of Commen

Juanita M. Kreps

Secretary

National Burepu • •{ M.inilurd-. Rational ^Bureau of Standards

(Certificate of JVrtalgsis

Standard Reference Material 332

Copper Concentrate

This material is in the form of fine powder intended for use both in checking chemical methods of analysis and in calibration with instrumental methods of analysis. This SRM is one of a series of four SRM's issued primarily for use in evaluation of the critically important

"material balance" in the copper mining and metallurgical industries. The other three are: SRM 330, Copper

Ore, Mill Heads; SRM 331, Copper Ore, Mill Tails; and SRM 333, Molybdenum Concentrate. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant.

Certified Value"

b Estimated

Uncertainty' Percent bv Weight

Total Copper Molybdenum

Rhenium

28.4 0.64 PPM by Weight

10.2 0.2

Based on samples dried at 105 °C for two hours. Separate samples are used for rhenium and calculated to a dry-weight basis. b The certified value is the best estimate of the "true" value.

c Estimated uncertainty includes both method imprecision and material variability with samples 0.5 g (or more) for total copper, 0.2 g (c more) for molybdenum and 2.5 g (or more) for rhenium. The following values indicate the results of the analytical tests: Standard Number of

Constituent/ Method 1 Average Deviation2 Determinations

Percent by Weight

Total Copper

Isotopic dilution 28.40 0.04 12 mass spectrometry

(0.5 g samples)

Electrogravimetry 28.39 .02 6

(2 g samples) Molvbdenum Range

Isotopic dilution 0.639 0.008 3 mass spectrometry

3 (0.2 g samples) PPM bv Weight Rhenium Range

Isotopic dilution mass spectrometry 10.20 0.20 3

(2.5 g samples)

Details of the methods used, including drying and dissolution procedures, are given in a separate publication [1]. Of single determinations for total Cu; range given for Mo and Re. This method has been studied extensively and the data are considered free from systematic errors. [2].

Washington, D.C. 20234 June 26. 1977 (Revision of Provisional Certificate of 2-20-73 and draft certificates of 7-4-76 and 1-20-77) (Over)

J. Paul Cali, Chief

Office of Standard Reference Materials

88
PLANNING, PREPARATION, TESTING, ANALYSIS: The material for this SRM (332) was carefully selected and provided to NBS by Magma Copper Company, San Manuel, Anzona.through the courtesy of

T. L. Young.

At NBS, the material was sieved and thoroughly blended, which involved several independent procedures [1]. Homogeneity testing of selected samples representative of the lot of SRM 332 was performed simultaneously

with the analytical program for certification. The maximum variability for total copper was determined to be ±0.06 percent (0.5 g samples). Analyses were performed in the NBS Analytical Chemistry Division by R. K. Bell, E. L. Garner, J. W. Gramlich,

L. A. Machlan, J. R. Moody, L. J. Moore, and T. J. Murphy. The overall direction and coordination of the technical measurements at NBS leading to certification were performed under the direction of W. R. Shields and I. L. Barnes. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis.

ADDITIONAL INFORMATION ON THE COMPOSITION: Certification is made only for total Cu, Mo,

and Re. Although NOT CERTIFIED, the following additional information on the composition may be of

interest. Gold and Silver

Fire assay determinations for Au and Ag were made at Magma Copper Company:

Gold Silver PPM by Weight

Fire assay *(2.I4) *(38.7)

•Revised 02/28/79

REFERENCES

[1] J. R. Moody, I. L. Barnes, and R. E. Michaelis, Standard Reference Materials: Copper Ore, Mill Heads - SRM 330; Copper Ore, Mill Tails - SRM 331; Copper Concentrate - SRM 332; and Molybdenum Concentrate - SRM 333, Nat. Bur. Stand. Spec. Publ. 260-xx (in press).

[2] W. R. Shields, Editor, Nat. Bur. Stand. Tech. Note 546, (1970).

89
U.S. Department of Commerce

Elliot L. Richardson, Rational ^uram of Standards

Certificate of JVnalgsis

Standard Reference Material 333

Molybdenum Concentrate

This material is in the form of fine powder intended for use both in checking chemical methods of analysis and in calibration with instrumental methods of analysis. This SRM is one of a series of four SRM's issued primarily for use in evaluation of the critically important

"material balance" in the copper mining and metallurgical industries. The other three are: SRM 330, Copper

Ore, Mill Heads; SRM 331, Copper Ore, Mill Tails; and SRM 332, Copper Concentrate. CAUTION: The bottle should be kept tightly closed except when in direct use. Store in a desiccator over

desiccant. Estimated

Constituent Certified Value ' b Uncertainty' Percent b y Weight

Total Copper 1.038 0.010 Molybdenum 55.3 Rhenium 0.087 .001

• Based on samples run "as received " CAUTION: The bottle should be kepi tightly closed except when in direct use

1 The certified value is the best estimate of the "true" value.

c Estimated uncertainty includes both method imprecision and material variability with samples 0 25 g (or more) for total copper, molybde- num, and rhenium The following values indicate the results of the analytical tests made at NBS and the Magma Copper Company.

Constituent/ Method' Average

Standard

Deviation 2 Number of Determinations Percent by Weight

Total Cooper

Isotopic dilution mass spectrometry' 1.038 0.007 11 (0.25 g samples) Polarographic 1.034 Oil 6

( 1.0 g samples) Atomic absorption spectrometry'

1 1.033 .002 3 (1.0 g samples)

10 Isotopic dilution mass spectrometry

3 55.31 .02 (0.25 g samples) a-Benzoinoxime gravimetric 5 55.43 .04 10

(0.25 g samples) Rhenium

Isotopic dilution mass spectrometry

3 0.0869 0.0003 17 (0.25 g samples) Thermal neutron activation analysis

6 .085 .002 9

(0. 15 g samples)

Details of the methods used are Of single determinations. This method has been studied extensively and the dal. Results from Magma Copper Company

Average of two independent analysts at NBS.

Determinations made relative to an industrial molybdenum cona

by a number of industrial laboratories and by isotopic dilution Washington, D. C. 20234 January 20, 1977

(Revision of Provisional

Certificate of 2-20-73)

separate publication [I].

considered free from systematic errors [2],

le reference material containing 0. 1 140 wt. %of Re, (as determined

spectrometry at NBS.)

J. Paul Cah, Chief

Office of Standard Reference Materials

(Over)

90
NOTE: Recommendation is made that this material be analyzed in the "as received" condition. SRM 333contains a small quantity (about 1%) of fuel oil introduced in the flotation process. Investigations at NBS indicate

that the analytical results made on the "as received" samples may be calculated to the dry-weight basis by use of an acetone stripping procedure (includes fuel oil and moisture)[l]. (For information only, a calculated MoS2 content thus would be 93.2±0.2%.) ADDITIONAL INFORMATION ON THE COMPOSITION: Although certification is made only for total Cu, Mo, and Re, recommended values for Au and Ag are given below:

Fire Assay, Magma

(14.58 g samples)

Au Ag ppm by weight

8.9 25.0

Neutron activation values at NBS on 0.2 g portions (final blended material) gave values of 12.5 ppm Au and 22.6 ppm Ag. Definite evidence of inhomogeneity was observed for Au on these 0.2 g portions. Recommendation

is made that sample sizes of 2.5 g (or more) be used to ensure homogeneity (<5% relative), regardless of the method used. PLANNING, PREPARATION, TESTING, ANALYSIS: The material for this SRM was carefully selected and provided to NBS by Magma Copper Company, San Manuel, Arizona, through the courtesy of T. L. Young. At NBS, highly specialized blending and mixing procedures were employed to obtain satisfactory homogeneity.

Extensive chemical analyses performed by Magma both for total copper and for molybdenum sulfide demonstrated that homogeneity was not achieved until the total blending and mixing procedures were performed three separate times [1]. Final homogeneity testing was performed at NBS simultaneously with the analytical program for certification. The maximum variability of the accepted lot was determined to be ±0.010 percent for total copper, ±0.0010

percent for rhenium; and ±0.06 percent for molybdenum (all using 0.25 g samples). Cooperative analyses were performed at the Magma Copper Company, San Manuel, Arizona, by Y. Arias,

B. Cripe, R. L. Culver, A. B. Hall, D. A. Shah, J. T. Tadano, and M. Toelkes.

'Analyses were performed in the NBS Analytical Chemistry Division by R. K. Bell, E. L. Garner, T. E. Gills,

J. W. Gramlich, P. D. LaFleur, L. A. Machlan, E. J. Maienthal, J. R. Moody, L. J. Moore, and T. J. Murphy. The overall direction and coordination of the technical measurements at NBS leading to certification were per- formed under the direction of W. R. Shields and I. L. Barnes. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis.

REFERENCES

[1] J. R. Moody, I. L. Barnes, and R. E. Michaelis, Standard Reference Materials: Copper Ore, Mill Heads

SRM 330; Copper Ore, Mill Tails - SRM 331 Copper Concentrate - SRM 332, and Molybdenum Concen

trate - SRM 333, Nat. Bur. Stand. Spec. Publ. 260-xx (in press).

[2] W. R. Shields, Editor, Nat. Bur. Stand. Tech. Note 546, (1970).

91
IVp.ul

Malt.

Rational ^mtnn of j^tanttartta

(Kerttftcate

Standard Reference Material 688

Basalt Rock

This Standard Reference Material (SRM) is intended for use in evaluating the accuracy of analytical methods and

instruments used in the analysis of geological type materials. SRM 688 is a finely powdered basalt rock that was obtained from a Cenozoic basalt flow near Jackpot, Nevada.

Certified Values of Constituents The concentrations of the constituents were determined by methods that are widely used in the field of geological analysis and have a demonstrated accuracy. The values given are "certified" values, i.e., those values that were determined by

either a definitive method, reference method, or by two or more independent methods, and "information" values that were determined by single or non-reference methods. The certified values are given in Table 1. Table 1 Certified Values of Constituents

Content 2 Content 2 Constituent wt (%) Constituent

Wt (Mg/g) AI2O3

c ' 8 17.36 ±0.09 Cr

b ' c 332 ±9

FeO 8 7.64 ±0.03 Rb d 1.91 ±0.01

Fe2 03 e,B 10.35 ±0.04 Sr

d 169.2 ±0.7

(Total Fe as Fe2 03 ) Th d 0.33 ± 0.02 K2O h,d 0.187 ±0.008 Pb

d 3.3 ±0.2 MnO d,h,e 0.167 ± 0.002 Na: 0

b,L,e 2.15 ±0.03

P2O5 0.134 ± 0.003 Si02

c 48.4 ± 0.

TiQ 2 a,b 1.17 ±0.01

electrode polentiometry

1. Methods of Analysis Colorimetry Neutron

Emission spectrometry Specific i< ^Gravimetry iTitrimetry

Isotope dilution mass spectrometry

2. The estimated uncertainties of the certified values are based on judgment and represent an evaluation of the combined effects of method imprecision,

possible systematic errors among methods and material variability of 250 mg or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination of most constituents.) The overall direction and coordination of the technical measurements leading to certification were performed in the Inorganic Analytical Research Division, E. L. Garner, Chief. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference

Material were coordinated through the Office of Standard Reference Materials by T. E. Gills. Washington, D.C. 20234 August 18, 1981 George A. Uriano, Chief

Office of Standard Reference Materials

92
SUPPLEMENTAL INFORMATION

Preparation The material was processed by the Colorado School of Mines, Golden, Colorado. Approximately 600 pounds of basalt rock were crushed, ground, and sieved to <200 mesh. The material was mixed in a cone blender to ensure homogeneity. The inhomogeneity was tested by taking random samples and analyzing for both major and minor constituents and was

found to be <_2% relative.

Analysis SRM 688 may pick up additional water on exposure to the atmosphere. Thus, exposure time should be kept to a minimum. Before analysis, it is recommended that the material be dried at 1 05 ° C for 24 hours. Typical weight loss upon

drying is approximately 0.2 percent. The analysts and laboratories cooperating in the analytical program for certification were:

I. L. Barnes, M. J. Blackman, E. L. Garner, J. W. Gramlich, L. A. Machlan,L. J. Moore, and R. Zeisler of the Inorganic Analytical Research Division, National Bureau of Standards.

J. B. Bodkin, J. C DeVine, and N. H. Suhr of the Mineral Constitution Laboratories, The Pennsylvania State

University, University Park, Pa.

S. S. Goldich of the Department of Geology, Northern Illinois University, Dekalb, 111. The constituents given in Table 2 are not certified, but are included for information only.

Table 2 Information Values

Constituent Content wt % Constituent 1 Content wt(/xg/g) CaO c (12.17) Ce

e (13.3) co2

f (0.05) Coe (49.7) F

f (0.02) Eue

( 1-07) MgO c (8.4 ) Hf

e

( 1.6) Lu

e

( 0.34) Sc

* (38.1) Ba

b (200) V

b (250) Cu

b (96) Ni

b (150) Sm e (2.79) Tb ' (0.448) u

d (0.37) Yb ' (2.09) Zn

e (58.0)

93
Rational ^Bureau of jltattttartte

(Hertifttate of ^nalgsb

Standard Reference Material 690

Iron Ore Concentrate (Canada)

(In Cooperation with the American Society for Testing and Materials)

This material is in the form of powder (<0. 1 mm) for use in checking chemical methods of analysis and in calibra- tion with instrumental methods of analysis. (Results based on samples dried for one hour at 105 °C.)

Constituent

Total Fe Si02 AI2O3 P S TiCh MnO CaO MgO Na2 0 K2 0

Certified' Value (wt. %) 66.85 3.71 0 18 0.0 II 0.003 0.022 0.23 0.20 0.18 0.003 0.0030 Estimated

2 Uncertainty 0.07 0.02 0.01 0.002 0.001 0.002 0.01 0.01 0.01 0.001 0.0005 \ Method 3

Labs\ u o d f, u -g I Q

Atomic

Absorptior

Photometr Combustio

Titration

Photometr Absorptior

Atomic

Absorptior

Atomic

Absorptior

Atomic

Absorptior

Atomic

Absorption

° 66.91 3.70 0.17 ' 0.009 <0.005 0.021 0.24 0.20 0.17 0.0026 0.0030 B 66.88 3.76 .17

C .013 .003

e 026 .23 .20 .19 004 .003 C

' 66.82 3.70 .19 Oil .006 .024

h .23 ' .19 .19

' .0023 .0034 D 66.85 3.73 .18 .021 .23 .21 .18 .0028

1 .0030 .0029

E 66.83 S.69

3.73 .20 .009 .002

9

.022 .24 .21 .18 .002 .003

1 . The certified value listed for a constituent is the present best estimate of the "true" value based on results of the cooperative analytical program for certification.

2. The estimated uncertainty is based on judgment and represents an evaluation of the combined effects of method imprecision, possible systematic errors among methods, and material variability for samples of 0.5 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determinations.)

3 A detailed description of many of the methods of analysis employed in the certification program for this SRM may be found in Part 1 2, Chemical Analysis of Metals and Metal Bearing Ores, Annual Book of ASTM Standards.

a H2S reduction b Sample fused in Na2 CC»3

c Alkali-molybdate method

d H2 02 photometric

g Chronotropic acid ph

h Photometric method

1 Spectroscopic method

j Flame

k Chromazurol S ph'

Washington, D C. 20234 October 24, 1978

J. Paul Cali, Chief

Office of Standard Reference Materials

94
PLANNING, PREPARATION, TESTING, ANALYSIS:

The iron ore powder concentrate material for this SRM was prepared in final powder form, minus 74 /xm (200

mesh), by the Iron Ore Company of Canada, Labrador City, Newfoundland, Canada, through the courtesy of

L. Rompre'

At NBS, the material was resieved and thoroughly blended. Homogeneity testing of selected samples representative of the final lot was performed at NBS by R. K. Bell, Assistant Research Associate, ASTM-NBS Research Associate Program. The results for iron indicate that the material variability (0.5 g samples) is < the method imprecision. Chemical analyses for certification were performed in the following laboratories: Bethlehem Steel Corporation, Homer Research Laboratories, Bethlehem, Pa., D. A. Flinchbaugh.

Inland Steel Company, Indiana Harbor Works, East Chicago, Indiana, J. E. Joyce. Ledoux and Company, Teaneck, New Jersey, S. Kallman and C. L. Maul.

National Bureau of Standards, Center for Analytical Chemistry, Washington, D.C., T. C. Rains, T. J. Brady,

J. D. Messman, and T. A. Rush and by R. K. Bell, ASTM Assistant Research Associate. STELCO, The Steel Company of Canada, Ltd., Hilton Works, Hamilton, Ontario, Canada, O. P. Bhargava. The overall direction and coordination of the technical measurements leading to certification were performed

jointly by R. E. Michaelis, Office of Standard Reference Materials and by J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

95
U. S. Department of Commerce

Malcolm Baldrige

Na

EmTM'l A

Um<bfcr0rm!^n

,o''rrdS Rational ^uram of j^tandartb

(tterttfttate of (Analysts

Standard Reference Material 691

Reduced Iron Oxide

(In cooperation with the American Society for Testing and Materials)

This Standard Reference Material (SRM) is intended for use in evaluating chemical methods and in calibrations associated with

optical emission and x-ray spectrometnc methods of analysis. SRM 691 is a finely powdered material (-200 mesh) and must be kept in a tightly sealed bottle when not in use. It is recommended that the material be stored in a desiccator over a suitable desiccant when not in use. Long term (>3 years) stability of this SRM has not been rigorously established. NBS will continue to monitor this material and any substantive changes will be reported to users. The certified values given below in Table 1 are based on samples of at least 0.5 g, the minimum amount to be used for analysis. Non-certified values which are given for information only, are listed in Table 2. Table I

Certified, Value,' Estimated Certified Value,' Estimated

Constituent % by wt. Uncertainty" Constituent Uncertainty

:

Iron (Total) 90.8 ± 0.5 Copper 0.032 ± 0.003 Iron (Metallic)' 84.6 .6 Cobalt .030 .007 SiO: 3.7 .2 Phosphorus .006 .001 Al;Oj 1.22 .07 Sulfur .008 .001 TiO: 0.27 .04 Carbon (Total) .03 CaO .63 .03 MnO .043 .002 MgO .52 .02 Na:0 .186 .002

I. The certified value listed for a constituent is the present best estimate ol the "true" value based on the results ol the cooperative program lor certification.

2. 1 he estimated uncertainty listed lor a constituent is based on judgment and represents an evaluation ol the combined effects ol method

imprecision, possible systematic errors among methods, and material variability for samples 0.5 g or more (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination ol most constituents.)

3. The metallic iron was determined by the ISO (Bromine-melhanol) method. The overall coordination of the technical measurements leading to certification was performed under the direction of J.I. Shultz. Research Associate,. ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference Material were coordinated through the Office of Standard Reference Materials by T.E. Gills.

Washington, D.C. 20234 George A. Uriano, Chid

April 12, 1982 Office of Standard Reference Mater

96
PLANNING, PREPARATION, TESTING, ANALYSIS:

The material for this SRM was provided by Allis-Chalmers, Reduction Systems Division, Milwaukee, Wis., courtesy of

L.J. Wrangell. It was processed (crushed, ground, sieved, and mixed) at the Colorado School of Mines Research Institute, Golden, Colorado, under a contract to the National Bureau of Standards. The final product (-200 mesh) was blended at NBS.

Homogeneity testing of selected samples representative of the final lot was performed at Allis-Chalmers, L.J. Wrangell; at Ledoux & Co., Teaneck, New Jersey, by S. Kallmann; and at NBS by E.R. Deardorff.

Siability tests conducted over a seven-month period at NBS, during which samples were exposed to relative humidities of 75 and

90 percent at room temperature, indicated sufficient stability of the material for use as an SRM.

1 his material was packaged in a dry nitrogen atmosphere to prevent oxidation. If signs of oxidation are detected, please transmit

this information to NBS for documentation into the monitoring program.

Cooperative analyses for certification were performed in the following laboratories: Andrew S. McCreath & Son, Inc., Harrisburg, Pa.; F.A Pennington. Jr., R.F. Eakin, G.L Dobbs, J.C. Forney, and

1 W Richards. Inland Steel Company, Indiana Harbor Works, East Chicago, Indiana; J.E. Joyce.

Institut de Recherches de la Siderurgie, Maizieres-les-Metz, France; G. Jecko. Ledoux and Company, Teaneck, New Jersey; S. Kallmann.

National Bureau of Standards, Inorganic Analytical Research Division, C.G. Blundell, T.A Butler, E.R. Deardorff. M.S. Epstein, R.M. Lindstrom, T.C. Rains, M. Sadjadi, and R.M. Stone. United States Steel Corp., Research Laboratory, Monroeville, Pa.; J.D. Selvaggio, D.S. Shafferman, A W. Fioravanti. D.G. Cunningham, K.G. Mikos, R.C. Cline, and H.S. Karp. The values shown below are not certified since they are not based on the results of at least two independent laboratories or methods. These values are included for information only. Table 2 Content Content

Wt. Percent Element M8/g Cr (0.03) As (14) Ni ( .3 ) Zn (40) K ( .06) Pb (<20) Cd (< 5) Mo (<20) Sn K10)

N (50) V (135)

97
iHjmrtmenl f>| Commerce

luanita M. Krep?

Secretary Rational ^mtnn of j^tantlartb

Certificate of (Analgst*

Standard Reference Material 692

Iron Ore (Labrador)

(In Cooperation with the American Society for Testing and Materials)

This material is in the form of powder (<0. 1 mm) for use in checking chemical methods of analysis and in calibra- tion with instrumental methods of analysis. (Results based on samples dried for one hour at 105 °C.)

Constituent Total Fe Si02 AI2O3 P S T1O2 MnO CaO MgO Na2 0 K2O

Certified' Value (wt. %) 59.58 10.14 0.039 0.005 0.045 0.46 0.023 0035 0.008 0.039 Estimated

2 Uncertainty 0.06 0.05 0.04 0.002 0 001 0.005 0.01 0.003 0 004 0.002 0.003 \ Method3

Labs \

1 O

HCIO4

Dehydration

Atomic

Absorption

Photometric

CombustionTitrationPhotometric

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

A

° 59.55 10.09 1.40 0.039 <0.005

d 0.041 0.47 0.022 0.034 0.008 0.040

59.58 10.26 1.48

' .035 .004 .05 .45 .02 .04 .005 .036

C

59.63

' 59.62 10.10 1.42 .040 .007

9

.048 .47 .025 .028 .008

J .040

' .039

D 59.60 10.16 1.40 .043 .47 .021 .033

1 .010

.009 .041

E 59.50 Vl2

10.05 .039 .004

9 050 .46 .01 .038 .008 .041

F 59.58 10.18

' 1.37

1.46 .040 .005 9.043 .46 .026 .035 .008 .035

1 . The certified value listed for a constituent is the present best estimate of the "true" value based on results of the cooperative analytical program for certification.

2. The estimated uncertainty is based on judgment and represents an evaluation of the combined effects of method imprecision, possible systematic errors among methods, and material variability for samples of 0.5 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determinations.)

3. A detailed description of many of the methods of analysis employed in the certification program for this SRM may be found in Part 12, Chemical Analysis of Metals and Metal Bearing Ores, Annual Book of ASTM Standards.

a H 2 S reduction

b Sample fused in Na2 CO;

c Alkali-molybdate i d H2O2 photometric

e Atomic absorption

f Silver reductor

hod

g Chromotropic acid photometric

h Photometric method

i Spectroscopic method

k Chromazurol S photometric

I Mercury cathode-NH 4 OH-Cupferron-AlP04 Washington, D.C. 20234 October 24, 1978

J. Paul Cali, Chief

Office of Standard Reference Materials

98
PLANNING, PREPARATION, TESTING, ANALYSIS:

The iron ore material for this SRM was prepared in final powder form, minus 74 jim (200 mesh), by the Bethlehem Steel Corporation, Bethlehem, Pa. through the courtesy of J. M. Karpinski. At NBS, the material was resieved and thoroughly blended. Homogeneity testing of selected samples representative of the final lot was performed at NBS by R. K. Bell, Assistant Research Associate, ASTM-NBS Research Associate Program. The results for iron indicate that the

material variability (0.5 g samples) is < the method imprecision. Chemical analyses for certification were performed in the following laboratories: Bethlehem Steel Corporation, Homer Research Laboratories, Bethlehem, Pa., D. A. Flinchbaugh.

Inland Steel Company, Indiana Harbor Works, East Chicago, Indiana, J. E. Joyce. Ledoux and Company, Teaneck, New Jersey, S. Kallman and C. L. Maul.

National Bureau of Standards, Center for Analytical Chemistry, Washington, D.C., T. C. Rains, T. J. Brady,

J. D. Messman, and T. A. Rush,and by R. K. Bell, ASTM Assistant Research Associate. STELCO, The Steel Company of Canada, Ltd., Hilton Works, Hamilton, Ontario, Canada, O. P. Bhargava.

United States Steel Corporation, Research Laboratory, Monroeville, Pa., L. M. Melnick, J. D. Selvaggio, R. W. Cline, D. G. Cunningham, A. V. Fioravanti, J. R. Lucas II, C. W. Ponsonby, L. E. Povirk, D. Shafferman and R. J. Wargo. The overall direction and coordination of the technical measurements leading to certification were performed

jointly by R. E. Michaelis, Office of Standard Reference Materials,and by J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

99
[H-imrlini'iU ol ( 'ommeri

luamla M. Krepa

Secretary Rational £ittreau of j^tanttartfe

Certificate of (Attalgsis

Standard Reference Material 693

Iron Ore (Nimba)

(In Cooperation with the American Society for Testing and Materials)

This material is in the form of powder (<0. 1 mm) for use in checking chemical methods of analysis and in calibra- tion with instrumental methods of analysis. (Results based on samples dried for one hour at 105 °C.)

Constituent

Total Fe SiOi AI2O3 P S TiCh MnO CaO MgO Na;0 K2O

Certified' Value (wt. %) 65.11 3.87 1.02 0056 0.005 0.035 0.091 0.016 0.013 0.0028 0.0028

Estimated

2 Uncertainty 0.07 0.02 0.04 0 001 0 001 0.003 0.004 0 004 0.002 0.0005 0.0006 \ Method

3

Labs \

1 O

HCIO4

Dehydration

Atomic

Absorption

Photometric CombustionTitrationPhotometric Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

Atomic

Absorption

A °65.1l

b

3.87 1 04

C 0.056 <0.005

d 0.034 0 094 0.016 0.013 0.0029 0.003

B

e 65 13 65.14 3.83 1.11 .055 005 .036 095 .020 Oil 0023 003

C 65.10 3.89 1 06 .032 .087 .015 .012 0030

.0033 .003 D 65.11

9 3.86

3.88 0.98 .056 005 .038 090 .01 .015 .003 .003

E 65.09 3.87 0.98

1.06 .056 .007 .033

9

.091 018 .015 002 002

1. The certified value listed for ; , the present hen estimate of the "true" value based on results of the cooperative analytical program for certification.

2. The estimated uncertainty is based on judgment and represents an evaluation of the combined effects of method imprecision, possible systematic errors among methods, and material variability for samples of 0.5 g or more (No attempt was made to derive exact statistical nprecision Iht.hisc sorr.il methods were involved in the determinations.)

3 A detailed description of many of the methods of analysis employed in the certification program for this SRM may be found in Part 12. Chemical Analysis of Metals and Metal Bearing Ores. Annual Book of ASTM Standards

a H2 S reduction b Sample fused in Na2CC>3

c Alkali-molybdate method

d H2O2 photometric

e Silver reductor

f Chromotropic acid photometric Washington, D.C. 20234 October 24, 1978

g Photometric method

h Spectroscopic method

i Flame emission

j Chromazurol S photometric

k Mercury cathode-NH4 OH-Cupferron-AIPOa

J. Paul Cali, Chief

Office of Standard Reference Materials

(over)

100
PLANNING, PREPARATION, TESTING, ANALYSIS:

The iron ore material for this SRM was prepared in final powder form, minus 74 /xm (200 mesh), by the Bethlehem Steel Corporation, Bethlehem, Pa. through the courtesy of J. M. Karpinski. At NBS, the material was resieved and thoroughly blended. Homogeneity testing of selected samples representative of the final lot was performed at NBS by R. K. Bell, Assistant Research Associate, ASTM-NBS Research Associate Program. The results for iron indicate that the material variability (0.5 g samples) is < the method imprecision. Chemical analyses for certification were performed in the following laboratories: Bethlehem Steel Corporation, Homer Research Laboratories, Bethlehem, Pa., D. A. Flinchbaugh. Ledoux and Company, Teaneck, New Jersey, S. Kallman and C. L. Maul.

National Bureau of Standards, Center for Analytical Chemistry, Washington, D.C., T. C. Rains, T. J. Brady,

J. D. Messman, and T. A. Rush,and by R. K. Bell, ASTM Assistant Research Associate. STELCO, The Steel Company of Canada, Ltd., Hilton Works, Hamilton, Ontario, Canada, O. P. Bhargava. United States Steel Corporation, Research Laboratory, Monroeville, Pa., L. M. Melnick, J. D. Selvaggio, R. W. Cline, D. G. Cunningham, A. V. Fioravanti, J. R. Lucas II, C. W. Ponsonby, L. E. Povirk, D. Shafferman and R. J. Wargo. The overall direction and coordination of the technical measurements leading to certification were performed

jointly by R. E. Michaelis, Office of Standard Reference Materials and by J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification,and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed.

101
Department of Commerce

.luanita Kreps

Secretary

itional Bureau of Standard*

Krnest Amblw. Director Rational ^ureau of Standards

Certificate of ^nalgsis

Standard Reference Material 696

Bauxite (Surinam)

(In Cooperation with the American Society for Testing and Materials)

(All analyses are based on samples dried 2 hours at 140 °C)

This material is in the form of fine powder (<0.08 mm) for use in checking chemical and instrumental methods of

analyses.

Constituent

Certified Value

1 Percent, by weight Estimated

Uncertainty AI2O3 54.5 0.3 Fe203 8.70 .10 S1O2 3.79 .10 Ti02 2.64 .05 Zr02 0.14 .02 p2o5 .050 .006 v2 o5 .072 .006 Cr2 03 .047 .003 CaO .018 .002 MgO .012 .003 MnO .004 .001 ZnO .0014 .0007 K2 0 .009 .003 SOj .21 .03 Loss on Ignition

3 29.9 .2 The certified value listed for a constituent is the present best estimate of the "true" value.

2The estimated uncertainty listed for a constituent is based on judgment and represents an evaluation of the combined effects of method

imprecision, possible systematic errors among methods, and material variability for samples 1 .0 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination of most constituents.) 'Determined by igniting to constant weight at 1050 °C. Washington, D.C. 20234 George A. Uriano, Chief August 24, 1979 Office of Standard Reference Materials

(over)

102
ADDITIONAL INFORMATION ON THE COMPOSITION

Elements other than those certified may be present in this material as indicated below. These are not certified but

are given as additional information on the composition.

Concentration, Concentration,

Constituent Percent by weight Constituent Percent by weight BaO (0.004) Co (0.00009) Na20 (0.007) Hf (0.0032) Ce (0.0041) Sc (0.0008) The mineralogical composition of SRM 696 was determined by x-ray diffraction studies at the Geological

Survey, U.S. Department of the Interior, Reston, Va., (J.W. Hosterman) to be 5% kaolinite, 80%gibbsite, 10%

pyrite, and 5% anatase. These results are semiquantitative (to the nearest 5%). PLANNING, PREPARATION, TESTING, ANALYSIS:

The material for this SRM was mined in Surinam, South America, and was provided by the Aluminum Company of America, Alcoa Technical Center, Pittsburgh, Pa., through the courtesy of H. B. Hartman. It was

processed (crushed, ground, sieved, and mixed) at the Colorado School of Mines Research Institute under a

contract with the National Bureau of Standards. Homogeneity testing was performed at NBS by J.S. Maples and T.E. Gills. Cooperative analyses for certification were performed in the following laboratories: Aluminum Company of America, Alcoa Center, Pa., R. C. Obbink. Aluminum Company of Canada, Ltd., Arvida Research Center, Arvida, Quebec, Canada, L. Girolami. Andrew S. McCreath & Son, Inc., Harrisburg, Pa., F. A. Pennington, Jr., R. F. Eakin, and S. L. Miller. General Refractories Co., U.S. Refractories Division, Research Center, Baltimore, Md., S. Banerjee. Geological Survey, U.S. Department of the Interior, Reston, Va., H. J. Rose, Jr., and J. W. Hosterman.

Kaiser Aluminum and Chemical Corp., Center for Technology, Pleasanton, Calif., H. J. Seim, A. E. McLaughlin, D. F. G. Marten, A. Kermaninejad, R. C. Kinne, J. R. Skarset, J. Boruk, and U. Vogel. National Bureau of Standards, Washington, D.C., R. K. Bell, ASTM-NBS Assistant Research Associate. National-Southwire Aluminum Co., Hawesville, Ky., N. Robinson and E. Gotzy. Ormet Corp., Burnside, La., W. L. Brown and A. D. Lafleur. Reynolds Aluminum Co., Alumina Research Division, Bauxite, Ark., J. B. Ezell, Jr. University of Kentucky, Institute for Mining and Minerals Research, Center for Energy Research

Laboratory, Lexington, Ky., T. V. Rebagay. The overall coordination of the technical measurements leading to certification were performed under the

direction of J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and R. Alvarez.

103
NBS Standard Reference Materials BAUXITE SERIES

September 4, 1979

R. E. Michaelis and R. Alvarez, NBS Office of Standard Reference Materials and

J. I. Shultz, ASTM Research Associate The following table gives the values for four bauxite SRM's that are available in the form of fine powder «0.08 mm) for use in chemical and instrumental methods of analysis. They are being issued as a culmination of a major Industry-ASTM-NBS cooperative program. SRM No. 696 697 698

Designation Arkansas Surinam Dominican Jamaican Percent b vy Weight w e 1 g n 1 A12 03 48.8 54.5 45.8 48.2 Fe: 03 7.14 8.70 20.0 19.6 S1O2 13.43 3.79 6.81 0.69 TiOj 1.90 2.64 2.52 2.38 Z1O2 0.29 0. 14 0.065 0.061 P2O5 0.118 0.050 0.97 0.37 V2O5 0.028 0.072 0.063 0.064 Cr203 0.01

0.047 0.100 0.080 CaO 0.13 0.018 0.71 0.62 MgO 0.085 0.012 0.18 0.058 MnO 0.110 0.004 0.41 0.38 ZnO 0.0035 0.0014 0.037 0.029 BaO (0.008)' (0.004) (0.015) (0.008) Na2 0 (0.025) (0.007) (0.036) (0.015) K2O 0.068 0.009 0.062 0.010 S03 0.63 0.21 0.13 0.22 Loss on Ign. 27.2 29.9 22.1 27.3 Ce (0.024) (0.0041) (0.069) (0.030) Co (0.0001) (0.00OO9) (0.0013) (0.0045) Hf (0.0063) (0.0032) (0.0014) (0.0015) Sc (0.0008) (0.0008) (0.0058) (0.0051) Total (100.0) (100.1) (100.1) (100.1)

"Values in parenthesis are not certified. The value listed for a certified constituent is the present best estimate of the 'true" value based on the results of

the analytical program for certification (10-12 laboratories). The individual certificates of analysis list the "estimated uncertainties" associated with the certified values (also listed is a semiquantitative mineralogical composition (±5%) as determined by x-ray diffraction studies at the U.S. Geological Survey).

Inquiries regarding the Bauxite SRM's 69b. 696, 697, and 698. should be directed to the Office of Standard

Reference Materials. Chemistry Building. B31I, National Bureau of Standards, Washington, D.C. 20234.

(301) 921-2045. George A. Uriano, Chief

Office of Standard Reference Materials

: -
U.S. Department of Commerce

Juanita Kreps

I S<

National Bureau of Standards

Ernest ^mbter, Director Rational ^Bureau of jitattdante

(Esrttftcate of (Attaint*

Standard Reference Material 697

Bauxite (Dominican)

(In Cooperation with the American Society for Testing and Materials)

(All analyses are based on samples dried 2 hours at 140 °C)

This material is in the form of fine powder (<0.08 mm) for use in checking chemical and instrumental methods of

analyses.

Certified Value

1 Estimated

Constituent Percent, by weight Uncertainty AI2O3 45.8 0.2 Fe2 03 20.0 .2 Si02 6.81 .07 Ti02 2.52 .05 Z1O2 0.065 .007 P2O5 .97 .06 V2O5 .063 .005 Cr2 03 .100 .005 CaO .71 .03 MgO .18 .02 MnO .41 .03 ZnO .037 .003 K2O .062 .007 SO3 .13 .03 Loss on Ignition

3 22.1 .2 The certified value listed for a constituent is the present best estimate of the "true" value.

2The estimated uncertainty listed for a constituent is based on judgment and represents an evaluation of the combined effects of method

imprecision, possible systematic errors among methods, and material variability for samples I 0g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination of most constituents.) 'Determined by igniting to constant weight at 1050 °C. Washington, D.C. 20234 George A. Uriano, Chief August 24, 1979 Office of Standard Reference Materials

(over)

105
ADDITIONAL INFORMATION ON THE COMPOSITION

Elements other than those certified may be present in this material as indicated below. These are not certified but

are given as additional information on the composition. Concentration, Concentration,

Constituent Percent by weight Constituent Percent by weight BaO (0.015) Co (0.0013) Na2 0 (0.036) Hf (0.0014) Ce (0.069) Sc (0.0058) The mineralogical composition of SRM 697 was determined by x-ray diffraction studies at the Geological

Survey, U.S. Department of the Interior, Reston, Va., (J.W. Hosterman) to be 15%kaolinite, 50%gibbsite, 10%

boehmite, 20% hematite, and 5% anatase. These results are semiquantitative (to the nearest 5%). PLANNING, PREPARATION, TESTING, ANALYSIS:

The material for this SRM was mined in the Dominican Republic and was provided by the Aluminum Company

of America, Alcoa Technical Center, Pittsburgh, Pa., through the courtesy of H. B. Hartman. It was processed

(crushed, ground, sieved, and mixed) at the Colorado School of Mines Research Institute under a contract with

the National Bureau of Standards. Homogeneity testing was performed at NBS by J.S. Maples and T.E. Gills. Cooperative analyses for certification were performed in the following laboratories: Aluminum Company of America, Alcoa Center, Pa., R. C. Obbink. Aluminum Company of Canada, Ltd., Arvida Research Center, Arvida, Quebec, Canada, L. Girolami. Andrew S. McCreath & Son, Inc., Harrisburg, Pa., F. A. Pennington, Jr., R. F. Eakin, and S. L. Miller. General Refractories Co., U.S. Refractories Division, Research Center, Baltimore, Md., S. Banerjee. Geological Survey, U.S. Department of the Interior, Reston, Va., H. J. Rose, Jr., and J. W. Hosterman.

Kaiser Aluminum and Chemical Corp., Center for Technology, Pleasanton, Calif., H. J. Seim, A. E. McLaughlin, D. F. G. Marten, A. Kermaninejad, R. C. Kinne, J. R. Skarset, J. Boruk, and U. Vogel. National Bureau of Standards, Washington, D.C., R. K. Bell, ASTM-NBS Assistant Research Associate. National-Southwire Aluminum Co., Hawesville, Ky., N. Robinson and E. Gotzy. Ormet Corp., Burnside, La., W. L. Brown and A. D. Lafleur. Reynolds Aluminum Co., Alumina Research Division, Bauxite, Ark., J. B. Ezell, Jr. University of Kentucky, Institute for Mining and Minerals Research, Center for Energy Research

Laboratory, Lexington, Ky., T. V. Rebagay. The overall coordination of the technical measurements leading to certification were performed under the

direction of J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and R. Alvarez.

106
NBS Standard Reference Materials BAUXITE SERIES

September 4, 1979

R. E. Michaelis and R. Alvarez, NBS Office of Standard Reference Materials and

J. I. Shultz, ASTM Research Associate The following table gives the values for four bauxite SRM's that are available in the form of fine powder (<0.08 mm) for use in chemical and instrumental methods of analysis. They are being issued as a culmination of a major Industry-ASTM-NBS cooperative program. SRM No. 69b 696 697 698

Designation Arkansas Surinam Dominican Jamaican

Constituent Percent by Weight

AI2O3 48.8 54.5 45.8 48.2 Fe2 03 7.14 8.70 20.0 19.6 Si02 13.43 3.79 6.81 0.69 Ti02 1.90 2 64 2 52 2.38 Zr02 0.29 0.14 0.065 0.061 p2 o5 0.118 0.050 0.97 0.37 v2 o5 0.028 0.072 0.063 0.064 Cr2 C>3 0.01

0.047 0.100 0.080 CaO 0.13 0.018 0.71 0.62 MgO 0.08S 0.012 0.18 0.058 MnO 0.110 0.004 0.41 0.38 ZnO 0.0035 0.0014 0.037 0.029 BaO (0.008)

a (0.004) (0.015) (0.008) Na2 0 (0.025) (0.007) (0.036) (0.015) K2 0 0.068 0.009 0.062 0.010 SO3 0.63 0.21 0.13 0.22 Loss on Ign. 27.2 29.9 22.1 27.3 Ce (0.024) (0.0041) (0.069) (0.030) Co (0.0001) (0.00009) (0.0013) (0.0045) Hf (0.0063) (0.0032) (0.0014) (0.0015) Sc (0.0008) (0.0008) (0.0058) (0.0051) Total (100.0) (100.1) (100.1) (100.1)

"Values in parenthesis are not certified. The value listed for a certified constituent is the present best estimate of the "true" value based on the results of

the analytical program for certification (10-12 laboratories). The individual certificates of analysis list the "estimated uncertainties" associated with the certified values (also listed is a semiquantitative mineralogical composition (±5%) as determined by x-ray diffraction studies at the U.S. Geological Survey).

Inquiries regarding the Bauxite SRM's 69b, 696, 697, and 698, should be directed to the Office of Standard

Reference Materials, Chemistry Building, B311, National Bureau of Standards, Washington, D.C. 20234.

(301) 921-2045. George A. Uriano, Chief

Office of Standard Reference Materials

107
I>t" irtment of ('(.inn Juanita jvK Kreps

Secretary Rational £5uram of j&tamtante

Certificate of (Analgsi*

Standard Reference Material 698

Bauxite (Jamaican)

(In Cooperation with the American Society for Testing and Materials)

(All analyses are based on samples dried 2 hours at 140 °C)

This material is in the form of fine powder (<0.08 mm) for use in checking chemical and instrumental methods of

analyses.

Constituent

Certified Value

1 Percent, by weight

Estimated

Uncertainty

2

AI2O3 48.2 0.4 Fe2 03 19.6 .2 Si02 0.69 .03 Ti02 2.38 .07 Zr02 0.061 .009 p2 o5 .37 .01 v2 o5 .064 .005 Cr2 03 .080 .006 CaO .62 .02 MgO .058 .008 MnO .38 .03 ZnO .029 .002 K2 0 .010 .002 SO3 .22 .03 Loss on Ignition

3 27.3 .2 The certified value listed for a constituent is the present best estimate of the "true" value.

2 The estimated uncertainty listed for a constituent is based on judgment and represents an evaluation of the combined effects of method

imprecision, possible systematic errors among methods, and material variability for samples 1 .0 g or more. (No attempt was made to derive exact statistical measures of imprecision because several methods were involved in the determination of most 1 Determined by igniting to constant weight at 1050 °C. Washington, D.C. 20234 August 24, 1979 George A. Uriano, Chief

Office of Standard Reference Materials

(over)

108
ADDITIONAL INFORMATION ON THE COMPOSITION

Elements other than those certified may be present in this material as indicated below. These are not certified but

are given as additional information on the composition.

Concentration, Concentration,

Constituent Percent by weight Constituent Percent by weight BaO (0.008) Co (0.0045) Na20 (0.015) Hf (0.0015) Ce (0.030) Sc (0.0051) The mineralogical composition of SRM 698 was determined by x-ray diffraction studies at the Geological Survey, U.S. Department of the Interior, Reston, Va., (J.W. Hosterman)tobe75%gibbsite, 20% hematite, and 5% anatase. These results are semiquantitative (to the nearest 5%). PLANNING, PREPARATION, TESTING, ANALYSIS:

The material for this SRM was mined in Jamaica, and was provided by the Reynolds Metals Company, Bauxite, Arkansas, through the courtesy of J. B. Ezell, Jr. It was processed (crushed, ground, sieved, and mixed) at the Colorado School of Mines Research Institute under a contract with the National Bureau of Standards. Homogeneity testing was performedi at NBS by J.S. Maples and T.E. Gills. Cooperative analyses for certification were performed in the following laboratories: Aluminum Company of America, Alcoa Center, Pa., R. C. Obbink. Aluminum Company of Canada, Ltd., Arvida Research Center, Arvida, Quebec, Canada, L. Girolami. Andrew S. McCreath & Son, Inc., Harrisburg, Pa., F. A. Pennington, Jr., R. F. Eakin, and S. L. Miller. General Refractories Co., U.S. Refractories Division, Research Center, Baltimore, Md., S. Banerjee. Geological Survey, U.S. Department of the Interior, Reston, Va., H. J. Rose, Jr., and J. W. Hosterman.

Kaiser Aluminum and Chemical Corp., Center for Technology, Pleasanton, Calif., H. J. Seim, A. E. McLaughlin, D. F. G. Marten, A. Kermaninejad, R. C. Kinne, J. R. Skarset, J. Boruk, and U. Vogel. National Bureau of Standards, Washington, D.C., R. K. Bell, ASTM-NBS Assistant Research Associate. National-Southwire Aluminum Co., Hawesville, Ky., N. Robinson and E. Gotzy. Ormet Corp., Burnside, La., W. L. Brown and A. D. Lafleur. Reynolds Aluminum Co., Alumina Research Division, Bauxite, Ark., J. B. Ezell, Jr. University of Kentucky, Institute for Mining and Minerals Research, Center for Energy Research

Laboratory, Lexington, Ky., T. V. Rebagay. The overall coordination of the technical measurements leading to certification were performed under the

direction of J. I. Shultz, Research Associate, ASTM-NBS Research Associate Program. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by R. E. Michaelis and R. Alvarez.

109
NBS Standard Reference Materials BAUXITE SERIES

September 4, 1979

R. E. Michaelis and R. Alvarez, NBS Office of Standard Reference Materials and

J. I. Shultz, ASTM Research Associate The following table gives the values for four bauxite SRM's that are available in the form of fine powder (<0.08 mm) for use in chemical and instrumental methods of analysis. They are being issued as a culmination of a major Industry-ASTM-NBS cooperative program. SRM No. 69b 696 697 698

Designation Arkansas Surinam Dominican Jamaican

Constituent Percent t y Weight

AI2O3 48.8 54.5 45.8 48.2 Fe2 03 7.14 8.70 20.0 19.6

SiC>2 TiOz 1.90 2.64 2.52 2.38 Zr02 0.29 0.14 0.065 0.061 p2 o5 0.118 0.050 0.97 0.37 V2O5

Cr2 03 0.011 0.047 0.100 0.080 CaO 0.13 0.018 0.71 0.62 MgO 0.085 0.012 0.18 0.058 MnO 0.110 0.004 0.41 0.38 ZnO 0.0035 0.0014 0.037 0.029 BaO (0.008)

a (0.004) (0.015) (0.008) Na2 0 (0.025) (0.007) (0.036) (0.015) K2 0 0.068 0.009 0.062 0.010 SO3 0.63 0.21 0.13 0.22 Loss on Ign. 27.2 29.9 22.1 27.3 Ce (0.024) (0.0041) (0.069) (0.030) Co (0.0001) (0.00009) (0.0013) (0.0045) Hf (0.0063) (0.0032) (0.0014) (0.0015) Sc (0.0008) (0.0008) (0.0058) (0.0051) Total (100.0) (100.1) (100.1) (100.1)

"Values in parenthesis are not certified. The value listed for a certified constituent is the present best estimate of the "true" value based on the results of

the analytical program for certification (10-12 laboratories). The individual certificates of analysis list the "estimated uncertainties" associated with the certified values (also listed is a semiquantitative mineralogical composition (±5%) as determined by x-ray diffraction studies at the U.S. Geological Survey).

Inquiries regarding the Bauxite SRM's 69b, 696, 697, and 698, should be directed to the Office of Standard

Reference Materials, Chemistry Building, B311, National Bureau of Standards, Washington, D.C. 20234.

(301) 921-2045. George A. Uriano, Chief

Office of Standard Reference Materials

110
trncsi Ambler, Krector Rational £8i*raw of j^tandartfe

Certificate of (Analysis

Standard Reference Material 1632b

Trace Elements in Coal

(Bituminous)

This Standard Reference Material (SRM) is intended for use in the calibration of apparatus and the evaluation of tech- niques employed in the analysis of coal or similar materials. SRM 1632b is a bituminous coal with a nominal sulfur content of 1.9%. It is in the form of a fine powder (-60 mesh).

Certified Values of Constituent Elements: The certified values for the constituent elements are given in Table 1 . The

certified values are based on measurements using proven techniques and methods. Noncertified values are given in Table 2 and are provided for information only. These values are based on measurements made using a single technique

or method. While no reason exists to suspect systematic bias in the information values, no attempt was made to deter- mine if such a bias exists that is attributable to the technique and/ or method used. A list of analytical techniques and methods used for the different analyses is given in Table 3. As part of its update certification program, NBS will periodically update many of these values to certification status.

Expiration of Certification: The certification of SRM 1632b will be valid up to 5 years from the purchase date. Should

any of the certified constituents become invalid prior to that date, purchasers will be notified by NBS.

Use: This material should be vacuum dried at ambient temperature for 24 hours prior to use. The certified concentrations are reported on a "dry-weight" basis, thus the concentration determined on undried samples should be adjusted for the moisture content of the sample. Typical moisture loss using the drying procedure stated above is 1.3%. A minimum sample size of 250 mg of the dried material is required for the certified values to be valid. This SRM should be kept in its original bottle. It should not be exposed to intense source of radiation, including ultra- violet lamps or sunlight. The statistical analysis of the certification data was performed by R.C. Paule of the National Measurement Laboratory. The technical and support aspects involved in the preparation, certification, and issuance of this Standard Reference

Material were coordinated through the Office of Standard Reference Materials by T.E. Gills.

Gaithersburg, MD 20899 Stanley D. Rasberry, Chief June 20, 1985 Office of Standard Reference Materials

(over)

111
Source and Preparation of Material: The coal for this SRM was obtained from the Humphrey No. 7 mine and coal preparation plant of the Consolidation Coal Company, Christopher Coal Company Division, Osage, West Virginia. This mine produces bituminous coal with a sulfur content of 1.8- 1.9 percent (dry basis). This coal was obtained from an underground mine that recovers coal from the Pittsburgh seam, which is considered the single most valuable and

extensive coal seam in the United States. Approximately 900 kg of the coal for SRM 1632b was oven dried prior to processing, in accordance with procedures

outlined in ASTM D20I3. The coal was reduced in size to —60 mesh and sieved prior to blending. The coal was then blended in a stainless steel cone blender (approximate capacity 0.85 cubic meter). After blending the coal was packaged

in polyethylene-lined aluminum cans and was subsequently repackaged in fifty gram units.

Analysis Major, Minor.and Trace Constituents: In general, the major, minor.and trace constituents were certified using two or more independent methods of analysis or two or more different laboratories. For those constituents that were deter- mined using a single method, technique, or laboratory, the values are given for information only. (Set Table 3).

Calorific Value: The calorific value was determined using measurements made In an Isoperibol calorimeter, an iso- thermal calorimeter, and an adiabatic calorimeter at two different laboratories.

Moisture, Ash, and Volatile Matter: The moisture, ash.and volatile matter values were determined on measurements made using the standard ASTM methods, D3 1 73, D3 1 74, and D3 1 75, respectively. In addition, commercial instruments commonly used for the determination of the parameters provided additional values.

Page 2 SRM 1632b

112
Table 1. Certified Values of Constituent Elements Major Constituents

Elements Carbon (Total) Hydrogen

Nitrogen

Sulfur

Volatile matter

Content

Wt. Percent

78.11 ±0.37*

5.07 ±0.06

1.56±0.07 1.89±0.06

35.4 ±1.1

Elements Aluminum

Calcium

Iron Magnesium

Potassium Sodium

Titanium

Content

Wt. Percent

0.855 ±0.019

0.204 ±0.006

0.759 ±0.045

0.0383 ± 0.0008

0.0748 ± 0.0028

0.0515 ± 0.001

0.0454 ± 0.0017 Trace Constituents

Element

Arsenic Barium Cadmium

Cobalt Copper

Lead

Content Mg/g

3.72 ±0.09

67.5 ±2.1

0.0573 ± 0.0027

2.29 ±0.17

6.28 ±0.30

3.67 ±0.26

Element Manganese

Nickel Rubidium

Selenium Thorium Uranium

Zinc

Content Mg/g

12.4 ±1.0

6.10 ±0.27

5.05 ±0.11

1.29 ±0.11

1.342 ±0.036

0.436 ±0.012

11.89 ±0.78

Calorific Value

14005 ± 35 Btu/lb (32.57 ± 0.08 MJ kg

-1

)

Ash, wt.%

6.79 ±0.16

The listed ± uncertainties for carbon, hydrogen, volatile matter, and calorific value are two

standard deviations of the certified value. The listed ± uncertainties for all other

constituents are two standard deviations for the certified values and include an allowance

for minor sample heterogeneity. The observed sample variability was generally less than two percent of the constituent value. The calorific value (MJ kg ) may decrease upon aging or normal oxidation of the coals. NBS will continue to monitor this value and report any substantive change in the certified calorific value to the purchaser. The reference date for the calorific value is May 1985.

c The calorific value is determined as HHV2 (Higher Heating Value- Moisture Free).

Table 2. Noncertified Values for Constituent Elements

Trace Constituents

Element Mg/g Element Mg/g Antimony (0.24) Lithium (10) Bromine (17) Molybdenum (0.9) Cerium (9) Samarium (0.87) Cesium (0.44) Scandium (19)

Chlorine (1260) Silicon, wt % (14) Chromium (11) Strontium (102) Europium (0.17) Tungsten (0.48) Hafnium (0.43) Vanadium (14) Lanthanum (5.1)

Page 3 SRM 1632b
Table 3. Analytical Techniques and Methods Used for (he Characterization of SRM 1632b

Method/

Element A B C D E F G H 1 j K L M — —

~m

Ash Content ^CO"lent

Brcr(To|a|) —> —

Ca

Cal Val \—^~

\

Cd

Ce

CICo

Cr

CsCu

Eu

FeH • 5 • • Hf

K • •

La

Li • Mg • Mn • Mo

N • 6 Na

Ni • Pb • Rb #

s

. Sb

ScSe

SiSm

SrTh

TiU

V

Volatile Matter • 3 W

Zn

Page 4 SRM 1632b

114
Analytical Methods

A. Atomic absorption spectrometry

B. Isotope dilution mass spectrometry

C. Instrumental neutron activation analysis D. Flame emission spectrometry

E. Flameless atomic absorption spectrometry

F. Ion chromatography

G. ASTM Methods: (1)D3173, (2)D3174, (3)D3I75, (4)D3I77,

(5)D3178, (6)D3179

H. Combustion coulometry L Commercial coal analyzers: moisture, ash, sulfur, Btu,

volatile matter, carbon, hydrogen, nitrogen

J. Commercial calorimeter K. Gas chromatography

L. X-ray fluorescence M. Inductively coupled plasma emission spectrometry

Analysts NBS

E.S. Beary W.A. Bowman

K.A. Brletic T.A. Butler J.D. Fassett J.W. Gramlich

R.R. Greenberg

, W.F. Koch

L.A. Machlan

A. Mario

w

D M. Mo

T.J. Murphy

P.J. Paulsen

P. Pella T.C. Rains

T.A. Rush

T.A. Sleater S.F. Stone

R. Zeisler

Laboratories

E. Huffman R. Peck Huffman Laboratories Dickerson Laboratory Wheat Ridge, Colorado 80034 El Paso, Texas 79912

J.B Bodkin

College Earth & Mineral Science The Pennsylvania State University

University Park, Pa. 16802

Page 5 SRM 1632b

115
U S. Department of CoiMl

Juanita Mk Kreps

Secretary

National Bureau of Standai

Ernest AnibliT. ijim t.ir Rational T&nttan of Standards

(tterttfttate of (Analyst*

Standard Reference Material 1633a

Trace Elements in Coal Fly Ash

This Standard Reference Material is intended for use in the calibration of apparatus and methods used in analyses of coal fly ash and other materials with similar matrices for trace elements. This material should be

dried to a constant weight before using. Recommended procedures for drying are: (1) drying for 24 hours at ambient temperature using a cold trap at or below -50 °C and a pressure not greater than 30 Pa (0.2 mm Hg);

(2) drying in a desiccator over P2O5 or Mg(C 104)2- When not in use, the material should be kept in a tightly sealed bottle. Long term (>3 years) stability of this SRM has not been rigorously established. NBS will continue to monitor this material and any substantive change will be reported to purchasers. The certified values given below are based on at least a 250-mg sample of the dried material, the minimum

amount that should be used for analysis.

Element' Content

2 Element Content %. Mg/g

Calcium 1.11 ± 0.01 Mercury

3 ,c 0.16 ± 0.01 Iron

3

' ,c 9.40 ± 0.10 Nickel

3 ' b,d ' e 127 ± 4 Potassium

3

' ,e 1.88 ± 0.06 Lead M' £ 72.4 ± 0.4 Magnesium ' 0.455 ± 0.010 Rubidium3

'

' c,e 131 ± 2 Sodium ' 0.17 ± 0.01 Selenium

3 ' 0 ' 8 10.3 ± 0.6

Silicon 22.8 ± 0.8 Strontium

3 ' e,f 830 ±30

Mg/g Thoriumb ' c 24.7 ± 0.3 Arsenic

,c 145 ± 15 Thalliumb,e 5.7 ± 0.2 Cadmium ,c

' ,g 1.0 ± 0.15 Uranium 10.2 ± 0.1 Chromium3

' ,c 196 ± 6 zinc

a,b,d,e,f 220 ± 10 Copper

3

' c 118 ± 3

Methods of Analysis:

a Atomic Absorption Spectrophotometry c Spectrometry

Isotope Dilution Mass Spectrometry

c Neutron Activation Polarography

Flame Emission X-ray Fluorescence Spectrometry

Inductively Coupled Plasma Emission Spectrometry

8 Isotope Dilution Spark Source Mass Spectrometry Gravimetry

2. The estimated uncertainty is based on judgment and represents an evaluation of the combined effects of method imprecision, possible systematic errors among methods, and material variability for samples

of 250-mg or more. (No attempt was made to derive exact statistical measures of imprecision because

several methods were involved in the determination of most constituents.) Washington, D.C. 20234

April 18, 1979 George A. Uriano, Chief

Office of Standard Reference Materials

116
The overall direction and coordination of the analytical measurements leading to certification were performed

in the Center for Analytical Chemistry under the chairmanship of L. A. Machlan. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed. PREPARATION, TESTING, AND ANALYSIS

This fly ash material was supplied by a coal fired power plant and is a product of Pennsylvania and West Virginia

coals. It was selected as a typical fly ash and is not intended as a fly ash from a specific coal or combustion process. The material was sieved through a # 170 sieve and blended for 2 hours in a Vee blender. The material was then removed and placed in a series of bulk containers from which specific samples were taken. Twelve bottles were selected for homogeneity tests. These samples were analyzed for cobalt, chromium,

europium, iron, scandium, and thorium by nondestructive neutron activation analysis. The observed standard

deviations for both 50 and 250 mg samples were consistent with counting statistics indicating that the fly ash is homogeneous within ± 5% (relative) based on these elements. The homogeneity analyses were performed in the NBS Center for Analytical Chemistry by R. R. Greenburg and J. S. Maples. Analyses for the various elements were made in the NBS Center for Analytical Chemistry by the following analysts: J. R. Baldwin, T. J. Brady,

E. R. Deardorff, M. G. Dias, L. P. Dunstan, M. S. Epstein, E. L. Garner, 1 E. Gills, C. A. Grabnegger, J. W.

Gramlich, R. R. Greenberg, S. Hanamura, S. H. Harrison, E. F. Heald, H. M. Kingston, E. C. Kuehner, L. A. Machlan, E. J. Maienthal, J. S. Maples, J. D. Messman, L. J. Moore, P. J. Paulsen, P. A. Pella, T. C. Rains,

K. J. R. Rosman, T. A. Rush, P. A. Sleeth, and R. L. Waters, Jr. The following values are not certified because they are based on a non-reference method, or were not determined by two or more independent methods. They are included for information only. Element Content Element Content Mg/g Aluminum

Barium

Titanium

140.15

0.8

Europium

Gallium Hafnium

4

58

7.6 Manganese 190

Cerium

Cobalt Cesium

Beryllium 12

I HO46

11

Antimony

Scandium Vanadium

Molybdenum 29

740

300

117
irl nu-nt "I < 'ommercf

mita M. Kreps

Secretary ^ ^National ^Bureau of js>tatttlartte

Certificate of (Analgst*

Standard Reference Material 1635

Trace Elements in Coal

(Subbituminous)

This Standard Reference Material is intended for use in the calibration of apparatus and the evaluation of

techniques employed in the trace element analysis of coal and similar materials. The material should be dried without heat to constant weight before use. The recommended procedures for drying are either vacuum drying at ambient temperature for 24 hours, or

freeze drying in which the drying chamber is kept at room temperature. The moisture content of this material is approximately 20%. Because of this moisture level, it is recommended that small individual samples be dried immediately before use. Drying of large samples may result in a violent discharge of water vapor and resultant

loss of sample. When not in use, the material should be kept in a tightly sealed bottle and stored in a cool, dark

place. Long-term (>1 year) stability of this SRM has not been rigorously established. NBS will continue to monitor this material and any substantive change will be reported to purchasers. The certified values given below are based on at least a 250-mg sample of the dried material, the minimum

amount that should be used for analysis. Element' Content, /ug/g

2 Element Content, ug/g2

Arsenic

3 b 0.42 ±0.15 Thorium0 ,e 0.62 ±0.04 Cadmiumc

' e 0.03 ± 0.01 Uranium0 0.24 ±0.02 Chromiumce

2.5 ±0.3 Vanadiume,g 5.2 ± 0.5 Copper

3 ' c ' e 3.6 ±0.3 Zinc ' 4.7 ± 0.5 Lead'" 1.9 ±0.2

Manganese ' 21.4 ± 1.5 Element Wt. %

2 Nickel

c,d 1.74 ± 0.10 lron

c

' e ' 0.239 ± 0.005 Selenium

3 ' e 0.9 ±0.3 Sulfurfh

0.33 ±0.03

Neutron Activation Spectrophotometry Flame Fmission Spectrometry

1. Methods of Analysis:

a. Atomic Absorption Spectrometry

b. Photon Activation

c. Isotope Dilution Mass Spectrometry

d. Polarography h. Gravimetry

2. The estimated uncertainty is based on judgment and represents an evaluation of the combined effects of method imprecision, possible systematic errors among methods, and material variability for samples

of 250-mg or more. (No attempt was made to derive exact statistical measures of imprecision because

several methods were involved in the determination of most constituents.) The overall direction and coordination of the analytical measurements leading to this certificate were performed

in the Analytical Chemistry Division under the chairmanship of L. J. Moore. The technical and support aspects involved in the preparation, certification, and issuance of this Standard

Reference Material were coordinated through the Office of Standard Reference Materials by W. P. Reed. Washington, D.C. 20234 George A. Uriano August 22, 1979 Office of Standard Reference Materials (Revision of Certificate (over) dated 1-23-78)

118
PREPARATION, TESTING, and ANALYSIS

This material was prepared from one lot of subbituminous coal from the Eagle Mine of The Imperial Coal Company, Erie, Colorado. The material was ground and sieved thru a No. 65 (230 /urn) sieve by the Colorado

School of Mines Research Institute. The material was then blended in a V-type blender. Samples for homogeneity testing were taken from the top, middle, and bottom of three bulk containers of coal, and analyzed by neutron activation analysis for sodium, scandium, chromium, iron, cobalt, lanthanum,

cerium, and thorium. Replicate analyses of 250-mg samples indicated a homogeneity for these elements of ± 2. 5% (relative) except for chromium, which was homogeneous within counting statistics of ± 6%. The homogeneity measurements were performed in the NBS Analytical Chemistry Division by R. R. Greenberg. Certifi- cation analyses for the various elements were made in the NBS Analytical Chemistry Division by T. J. Brady,

B. I. Diamondstone, L. P. Dunstan, M. S. Epstein, M. Gallorini, E. L. Garner, T. E. Gills, J. W. Gramlich,

R. R. Greenberg, S. H. Harrison, G. M. Hyde, G. J. Lutz, L. A. Machlan, E. J. Maienthal, J. D. Messman,

T. J. Murphy, and T. C. Rains. The following values are not certified because they were based on a non-reference method, or were not deter- mined by two or more independent methods. They are included for information only.

Element

Content

(Mg/g) Antimony (0.14) Cerium (3.6) Cobalt (0.65) Europium (0.06) Gallium (105) Hafnium (0.29) Scandium (0.63)

(wt. %) Aluminum (0.32) Sodium (0.24) Titanium (0.02)

119
U, S. Dcparlmem of Commerce

Malcolm Baldrigc Secretary

ErnesI Amblfcr. I .-. ^National ^Bureau of j^tattttartfe

Certificate of ^ttalgsi*

Standard Reference Materials

2682, 2683, 2684 and 2685

Sulfur in Coal

These Standard Reference Materials (SRM's) are intended primarily for use as analytical standards for the determination of sulfur in coal. In addition to sulfur they are certified for their calorific value (MJ- Kg ) and ash content. SRM's

2682-2685 each consists of a 50-g bottle of a different coal composition. Each material was ground to pass a 60-mesh

sieve and homogenized. The certification of the materials for sulfur is based on at least a 250-mg sample of the dried

material, the minimum amount that should be used for analysis (see drying instructions). The calorific values were

determined by procedures recommended in standard ASTM methods (see references in Table 1 ). The certification data

lor the four different coals are given in Table 1 along with methods used for certification. Noncertified values for major and minor elements are given in Table 2. These values are provided for information only. Notice to Users: These SRM's are sold individually rather than in sets; however, only one Certificate of Analysis is provided. Therefore, the user must be careful to use the data specific to the SRM being used. The uncertainty of a certified value is expressed as two times the standard error and includes observed variability within and between measurement methods and any observed material heterogeneity. For the certified heating values the uncertainty also includes additional allowances for possible limited sample degradation due to aging or normal

oxidation.

Certification analyses were performed by W.R. Kelly, W.F. Koch, P.J. Paulsen, and J.W. Stolz of the Inorganic

Analytical Research Division and J.C. Colbert and D.R. Kirklin of the Chemical Thermodynamics Division. Analyses for supplemental information were performed in the Inorganic Analytical Research Division by R. Fleming,

R. Greenberg, and R.M Lindstrom. The statistical analysis ol the certification data was performed by R.C. Paule of the National Measurement Laboratory. The overall direction and coordination of the technical measurements leading to certification were performed under the chairmanship of E.L. Garner, Chief of the Inorganic Analytical Research Division. The technical and support aspects involved in the preparation, certification, and issuance of these Standard Reference

Materials were coordinated through the Office of Standard Reference Materials by T.E. Gills.

Fcbruarv 7. 19X3 George A. Uriano, Chief

(Revision ol Certificate (over) Office of Standard Reference Materials d;ued I2-I4-X2)

120
Table 1 Certified Values for SRM's 2682, 2683, 2684, and 2685 SRM Coal Sulfur

1,2 ' 3 Furnace HHV25,6 No. Type Wt. % Ash Wt. % MJ Kg"' (BTU Ib

1 ) 2682 Sub-bituminous 0.47 ±0.03 6.37 ±0.18 27.45 ±0.56(1 1800± 240) 2683 Bituminous 1.85 ±0.06 6.85 ±0.02 32.70 ± 0. 14 ( 14060 ± 60) 2684 Bituminous 3.00 ±0.1

1 1.09 ±0.18 29.68 ±0.47 (12760 ± 200) 2685 Bituminous 4.62 ±0.1

16.53 ±0.15 28.15±0.42(I2100±180) ASTM D3I77 Standard Test Method for Total Sulfur in the Analysis Sample of Coal and Coke

2 Ion Chromatography with Bomb Combustion

Thermal Ionization Mass Spectrometry, Sealed Glass Tube Digestion

J ASTM D3I74, Standard Test Method for Ash in the Analysis Sample of Coal and Coke AS 1 M 1)2(11 5 Standard Test Method for Gross Calorific Value of Solid Fuel by the Adiabatic Bomb Calorimeter ASTM D3I80 Standard l est Method lor Calculating Coal and Coke Analyses from As-Determined to Different Bases HHV2-< Higher Heating Value - Moisture Free) Note: 1 he calorific values (MJ Kg ) may decrease upon the aging or normal oxidation of the coals. NBS will continue to monitor these calorific values and report any substantive change to the purchaser. The uncertainty of the heating value includes an additional allowance of 0. 1 2 MJ Kg for possible sample degradation. The reference dale for the calorific data is October 1982.

PREPARATION AND TESTING

Approximately one ton of coal was obtained from each of four different coal mine locations. All coals were oven dried

prior to processing in accordance with procedures outlined in ASTM D20 13. At least 1 000 pounds of each of the four

coals were reduced in size to -60 mesh and screened prior to blending. Each of the -60 mesh coals was blended in a stainless steel cone blender (approximate capacity 0.85 cubic meter). The coals were then packaged into individual 50-g

bottled units. Homogeneity testing was done on the bulk materials and 50-g bottled units. The homogeneity analyses were performed using x-ray fluorescence analysis. Replicate analyses indicated the material variability for sulfur to be

within ± 2% (relative) for all four SRM's. The homogeneity studies were performed by T.E. Gills and M. Watson of the Office of Standard Reference Materials and P. A. Pella of the Gas and Particulate Science Division.

121
ANALYSIS

Sulfur: The certified sulfur content is based upon the results of 3 independent methods of analysis: ion chromatography,

gravimetry, and thermal ionization mass spectrometry. Agreement with the certified values was found using 2 additional independent techniques, prompt-gamma activation analysis and a combustion IR technique.

Calorific Value (MJ-K.g~ )and Ash Content: The certified values for the calorific values and ash contents were

determined using measurements made in an adiabatic bomb calorimeter of the type used in commercial laboratories. This calorimeter is capable of reproducing determinations on benzoic acid to a precision of 0.07% (relative). This state- ment of precision was arrived at by averaging S calibrations made on the calorimeter using a benzoic acid standard that

is traceable to the NBS SRM 39i, Benzoic Acid. Major and Minor Elements: Analyses for major and minor elements were performed by thermal neutron activation

analysis and neutron capture gamma-ray activation analysis. These values are not certified but are to be used for information only. STABILITY

The long-term physical and chemical stability of these SRM's has not been rigorously established. However, NBS

recommends that the material be stored in the tightly sealed bottle away from sunlight and intense sources of radiation. NBS will continue to monitor these materials and any substantive change in their certification will be reported to the

purchaser. INSTRUCTIONS FOR DRYING

The certification of sulfur in these SRM's is based upon a properly dried sample. The recommended procedures for drying are vacuum drying at ambient temperature for 24 hours or oven drying for 24 hours at 105 °C. Typical moisture

loss using the recommended methods for drying are the following: SRM 2682, 18%; SRM 2683, 1.4%; SRM 2684, 3.6%; and SRM 2685, 1.8%. SUPPLEMENTAL INFORMATION

The values listed below are based on measurements made using a single method or technique and are given for information only. While no reason exists to suspect systematic bias in these numbers, no attempt was made to determine if such

bias attributable to the methods exists. The analyses of SRM's 2682-2685 for major and minor elements were made using NBS SRM's 1632a and 1635, Trace

Elements in Coal, as controls.

122
Table 2 Inorganic Constituents in SRM's 2682, 2683, 2684, and 2685 Mean Concentrations (jig/g) Unless Noted

Element/SRM 2682 2683 2684 2685 Al % 0.46 0.86 1.1 1.7 As 1.0 3.6 3.9 12 B 39 67 1 14 109 Ba 382 71 41 105 Br 3.7 17 1

5.6 C % 75 79 68 66 Ca % 1.1 0.20 0.44 0.52 Ce 10 9 12 18 Co 1.7 2.2 3.9 4.6 Cr 15 1

17 22 Cs <0.1 0.4 1.2 1.3 Eu 0. 17 0.18 0.23 0.36 Fe % 0.24 0.76 1.5 2.9 H % 4.7 5.0 4.8 4.6 Hf 0.60 0.42 0.57 0.91 K % 0.01 0.08 0.20 0.26 La 5.2 5.1 6.7 10 Mg % 0.2 0.05 0.08 0.

'Mn 26 13 36 41 N % 0.8 1.6 1.6 1.1 Na % 0.10 0.05 0.03 0.08 Rb <2 5.3 15 17 Sb 0.19 0.28 0.35 0.36 Sc 1.5 1.9 2.7 3.7 Se 0.91 1.2 1.9 1.9 Sm 0.78 0.86 1.7 Th 1.5 1.4 2.0 2.7 Ti % 0.05 0.04 0.06 0.09 U 0.52 0.42 0.90 0.95 V 15 14 22 31 w 1.8 0.48 0.56 1.2 Zn 8.6 9.5 110 17

123



Technical Publications

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information in the Federal Government regarding standards issued by NBS pursuant to the Federal Property and Administrative Services Act of 1949 as amended, Public Law 89-306 (79 Stat. 1127), and as implemented by Executive Order 11717 (38 FR 12315, dated May 11, 1973) and Part 6 of Title 15 CFR (Code of Federal

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