A11103 Ofifi^mE

NAFL INST OF STANDARDS & TECH R.I.C.

A1 11 03088942

/Measurements and standards for recycled QC100 .U57 N0.488, 1977 C.2 NBS-PUB-C 19 NBS SPECIAL PUBLICATION 488

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

Measurements and

Standards for

\ Recycled Oil

AlllQB DflfiTME

NATL INST OF STANDARDS & TECH R.I.C.

A1 11 03088942

/Measurements and standards for recycled QC100 .US7 N0.488, 1977 C.2 NBS-PUB-C 19 NBS SPECIAL PUBLICATION 488

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

Measurements and
NATIONAL BUREAU OF STANDARDS

The National Bureau of Standards^ was established by an act of Congress March 3, 1901. The Bureau's overall goal is toj 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 pro-l mote public safety. The Bureau consists of the Institute for Basic Standards, the Institute for Materials Research, the Institute) for Applied Technology, the Institute for Computer Sciences and Technology, the Office for Information Programs, and thel Office of Experimental Technology Incentives Program. jM

THE INSTITUTE FOR BASIC STANDARDS provides the central basis within the United States of a complete and consist- ent system of physical measurement; coordinates that system with measurement systems of other nations; and furnishes essential services leading to accurate and uniform physical measurements throughout the Nation's scientific community, industry,

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' Located at Boulder, Colorado 80302.
mal Bureau of Standards SEP 1 2 WI

Measurements and Standards

u for Recycled Oil -i^ , ... u

Proceedings of o workshop held at the

National Bureau of Standards

Gaithersburg, Maryland,

November 22 and 23, 1976

Donald A. Becker, Editor

Recycled Oil Program

Institute for Materials Research

National Bureau of Standards

Washington, D.C. 20234

Sponsored by

Recycled Oil Program

Institute for Materials Research

National Bureau of Standards

Washington, D.C. 20234

U.S. DEPARTMENT OF COAAMERCE, Juanita M. Kreps, Secretary

Dr. Sidney Harmon, Under Secretary Jordan J. Baruch, Assistant Secretary for Science and Technology

,S , NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Acting Director

Issued August 1977
Library of Congress Catalog Card Number: 77-600032

National Bureau of Standards Special Publication 488

Nat. Bur. Stand. (U.S.), Spec. Publ. 488, 140 pages (Aug. 1977) CODEN: XNBSAV

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 1977

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

Price $3 Stock No. 003-003-01831-7
Foreword

The Recycled Oil Program of the Institute for Materials Research, National

Bureau of Standards (NBS) was formed in 1976 in direct response to the Energy

Policy and Conservation Act of 1975. The goal of this program, as described in

this legislation, is to develop test procedures for the determination of substantial equivalency of re-refined or otherwise processed used oil with new oil for

all end uses. This program is particularly suitable for NBS because it involves

both the development and evaluation of measurement methods and standards, and it

requires the independent third-party role for acceptance by all concerned parties

(virgin oil refining industry, oil re-refining industry, user industries, and

government regulators)

An important reason why recycled lubricating oil products have not met with

widespread consumer acceptance, both from the Federal Government as well as the

public, is the lack of reliable test procedures and standards on which realistic

performance criteria can be based. In the Energy Policy and Conservation Act

(Public Law 94-163), NBS is directed to develop such test procedures and standards.

The alternative to increased recycling of petroleum oils is the continued contamination of the environment and waste of our limited petroleum resources.

This volume contains the proceedings of a workshop on Measurements and

Standards for Recycled Oil, held at NBS on November 22 and 23, 1976. An important

objective of this meeting was to bring together interested persons from both the

public and private sectors to obtain their input and expert opinion on the current

status, needs, and problems relating to test methods and standards for the evaluation of recycled petroleum oil products. This publication should be of value to the many people who are interested in encouraging oil recycling.

John D. Hoffman

Director

Institute for Materials Research

National Bureau of Standards
Preface

On December 22, 1975, President Ford signed into law an act passed by the

Congress of the United States entitled "The Energy Policy and Conservation Act of

1975" (Public Law 94-163). Section 383 of this act states that the National

Bureau of Standards (NBS) shall develop test procedures "...for the determination

of substantial equivalency of re-refined or otherwise processed used oil... with

new oil for a particular end use." Further, NBS is to "...report such procedures

to the [Federal Trade] Commission..." as soon as practicable. The NBS workshop

held on November 22 and 23, 1976, is part of the NBS response to this legislation.

A major objective of the workshop was to obtain the input to NBS of those

people knowledgeable about measurements and standards for petroleum oils on the

current status, needs, and problems with existing test methods and standards for

the evaluation of recycled petroleum oil products. Since the accurate evaluation

of recycled oil quality is largely dependent upon the validity of virgin oil test

methods when applied to recycled oils, it is essential that the expertise and

experience of these experts be utilized wherever available. A second major

objective of this meeting was to help foster closer personal contact and communication among all those working on the testing of virgin and recycled petroleum

oil products

.

There was a total of 69 attendees at the meeting, with a breakdown as follows:

28 government representatives (Federal Trade Commission, Environmental Protection

Agency, Department of Defense, Energy Research and Development Administration,

General Services Administration, two State governments, and NBS); 32 representatives from private industries (engine manufacturers- - 10 , petroleum refiners and

additive manufacturers -- 13 , used oil re-refiners and processors -- 6 , and other heavy

Indus try- - 3) ; and 9 attendees who were consultants or who represented consulting

firms, testing laboratories, or non-profit organi zations

It was felt that the workshop participants made a very important contribution

to the knowledge and understanding of the current situation with regard to recycled

oil. We plan to hold another such meeting on recycled oil on November 29 and 30,

1977.

Donald A. Becker

Manager, Recycled Oil Program

iv
Abs tract

This publication is the formal report of the workshop on Measurements and

Standards for Recycled Oil, held at the National Bureau of Standards on November 22 and 23, 1976. There were seven sessions on specific subject areas at the meeting,

with a total of 26 formal presentations, plus extensive discussion periods. The

subject areas were as follows: (1) The NBS Responsibilities and Program, (II) Used

Oil Reused as Fuel, (III) Recycled Industrial and Hydraulic Oils, (IV and V) Recycled

Engine Oils, (VI) Barriers to the Utilization of Recycled Oils, and (VII) Problems

and Needs in Establishing Quality for Recycled Oil Products. Included in this volume

are the invited talks that were given and summaries of the extended discussions that

were held on each of these subject areas.

Key Words: Engine oil; fuel oil; hydraulic oil; industrial oil; lubricating oil; oil

specifications; petroleum standards; petroleum test methods; recycled oil; re-refined

oil; used oil; waste oil.

Disclaimer

:

In order to describe work in this field adequately, it has been necessary to identify

commercial materials and equipment in this book. In no case does such identification

imply recommendation or endorsement by the National Bureau of Standards, nor does it

imply that the material or equipment is necessarily the best available for the purpose

V
CONTENTS

Page

Foreword iii

Preface iv

Abstract v

WELCOMING REMARKS 1 E. Ambler

SESSION I. STATEMENT OF PURPOSE

THE NBS WORKSHOP OBJECTIVES AND THE NBS RECYCLED OIL PROGRAM 7 D. A. Becker

DISCUSSION 13

SESSION II. USED OIL REUSED AS FUEL

BURNING USED OIL AT A MILITARY INSTALLATION 17

C. F. Schwarz

FUEL OIL AND THE DEFENSE SUPPLY AGENCY 19

E. J. French

FUEL OIL SPECIFICATIONS 21

B. L. Weller

AUTOMOTIVE CRANKCASE DRAININGS USED FOR FUEL 27

B. R. Williams

DISCUSSION 33

SESSION III. RECYCLED INDUSTRIAL AND HYDRAULIC OILS

ASTM TEST METHODS FOR INDUSTRIAL OILS 37

L. B. Sargent, Jr. INDUSTRIAL OIL RECYCLING AT CHRYSLER 39

W. Katzenstein

INDUSTRIAL OILS: DESCRIPTIONS, ADDITIVES, AND TEST METHODS 41

J. W. Swain, Jr. THE USE OF RECYCLED INDUSTRIAL AND HYDRAULIC OILS AT FORD 45

J. W. Hunt

INDUSTRIAL LUBRICANTS, RECLAIMED OILS, AND TEST METHODS 47

C. J. Flake

DISCUSSION 51

vi
Page

SESSIONS IV AND V. RECYCLED ENGINE OILS

DOD EXPERIENCES IN TESTING LUBE OILS 55

T. C. Bowen

WASTE OIL RECYCLING- -AN IDEA WHOSE TIME HAS COME 57

C. J. Thompson and M. L. Whisman

COMMENTS ON ADDITIVE RESPONSE TO DIFFERENT BASE OILS 61

T. P. Sands

ACTIVITIES OF THE ASTM USED OIL TASK FORCE 63

W. W. Grouse, Jr.

ACTIVITIES OF THE API USED OIL TASK FORCE 65

B. W. Hutchings

CHEVRON RESEARCH'S EXPERIENCES WITH RE-REFINED OILS 69

F. Sam

ENGINE SEQUENCE TESTS FOR DETERMINATION OF LUBE OIL QUALITY 73

R. H. Kabel

SCREENING TESTS ON LUBE OILS 77

P. A. Asseff

LABORATORY TESTING ON RE-REFINED MOTOR OIL 79

B. R. Williams

DIESEL LUBE OIL TEST METHODS 89

J. A. MacLean

DISCUSSION 95

SESSION VI. BARRIERS TO UTILIZATION OF RECYCLED OILS

RECENT USED OIL LEGISLATION 101

H. B. Kaufman

THE LEAD PROBLEM ASSOCIATED WITH RECYCLED OIL 103

J. S. Cooper

FACTORS AFFECTING USED OIL RECOVERY/UTILIZATION AND EFFECTS OF PROPOSED

POLICY ALTERNATIVES 105

S. P. Maltezou

ENERGY CONSERVATION ASPECTS OF RE-REFINED OIL ." . 109

G. J. Mascetti

MARKETING BARRIERS FOR RECYCLED OIL 115

P. M. Cukor

DISCUSSION 123

SESSION VII. PROBLEMS AND NEEDS IN ESTABLISHING QUALITY

FOR RECYCLED OIL PRODUCTS

DISCUSSION 12 7

vii
Page

APPENDICES

APPENDIX I 131

APPENDIX II 135

viii
National Bureau of Standards Special Publication 488. Proceedings

a Workshop on Measurements and Standards for Recycled Oil held at Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August

WELCOMING REMARKS

Ernest Ambler

Acting Director

National Bureau of Standards

Washington, D.C. 20234

Good morning and welcome to the National Bureau of Standards (NBS) . It is a special pleasure for us to be sponsoring this workshop on Measurements and Standards

for Recycled Oil.

The intent of this workshop is to bring together interest groups from both the

public and private sectors to define the current status and needs and problems with

existing test methods and standards for the evaluation of recycled petroleum oil

products

.

About a month ago, the NBS Executive Board held a Long-Range Planning Conference.

Mr. Ted Gordon, the President of the Futures Group, spoke to us about "1985 and How

We Get There." In discussing materials use, and particularly energy-producing

materials, he said:

"The emerging raw material situation will stimulate not only the

development of marginal resources, but also the search for substitutes and acceptable recycling techniques and institutional

arrangements. The use of recycling materials as a strategy to respond to increasing materials costs and uncertain availability

is, of course, not new. What has changed are the equations by

which the economics of such activities are evaluated."

I think Mr. Gordon's statement is a fair assessment of our presence at this workshop. We have only to look around us to see some of these recent equations demonstrating both the economic and environmental import of activities like this workshop.

The Federal Energy Administration (FEA) estimates that reuse of wasted oil could

reduce oil imports by about 70,000 barrels per day, or about 7 percent of the Administration's energy conservation goal. Certainly, in these days of uncertain supply,

potential embargoes, and increased flow of money out of the U.S., reuse of wasted oil

is a much to be desired goal from both the economic standpoint and as a visible symbol

of this Nation's energy conservation accomplishments.

But economics is not the whole story. Last year more than 2.4 billion gallons of

lubricating oil were sold in the U.S. Nearly 20 percent of that total, or 500 million

gallons of oil, was released into the environment. Thus, this oil was not only an economic waste, it is now a pollutant endangering the citizens of this Nation.

How hazardous a pollutant? The Environmental Protection Agency (EPA) reports

that "...67 percent of all pollution in the waters of the world is caused by used

motor and industrial oil." And the National Cancer Institute states that 60 to 90

percent of all cancer is caused by environmental factors.

The problem, however, has not gone unnoticed. Indeed, efforts have been made by

many of you who are present today. In addition, several State and local groups have

been working on the problem. The City of San Diego has, for the past three years,

used re-refined oil in city vehicles. The S|;ates of Iowa and West Virginia have

similar pilot projects for State vehicles. At the Federal level, the Environmental

Protection Agency, the Energy Research and Development Administration (ERDA) , and the

Department of Defense (DOD) have programs to study these issues.

Among these Federal programs, I think this group. might have particular interest

in the ERDA work to examine variability of used engine oil composition and in the

cooperative EPA/DOD project to evaluate re-refined oils for military use. In fact,

there will be several speakers at this workshop detailing the activities of these

programs

.

1
But these efforts have also faced barriers. Perhaps the greatest of these barriers was defined by someone who will be speaking to you tomorrow. Mr. Peter Cukor

of Teknekron was the project manager of a study on used oil done for EPA in 1973.

That report to EPA stated, "Uncertainty as to the quality of re-refined lube oils is

the principal barrier to increased recycling of used lubricants."

And that barrier has now been recognized and addressed by the U.S. Congress.

Under the Energy Policy and Conservation Act of 1975, Congress has assigned to the

National Bureau of Standards certain responsibilities for establishing the quality of

recycled petroleum oil products. The purpose of Section 383 of this act is fourfold:

(1) to encourage the recycling of used oil, (2) to promote the use of recycled oil,

(3) to reduce the consumption of new oil, and (4) to reduce the environmental hazards

associated with disposal of used oils.

As to why Congress assigned the responsibilities to the National Bureau of , Standards, let me tell you briefly about our mission and activities. We were created ' by the Congress in 1901 as the central organization responsible for maintaining basic j standards, developing measurement techniques, and establishing dissemination procej dures. For three-quarters of a century, we have carried out a mission developed to i support and encourage the growth of commerce, industry, science, and technology.

j Over the years, NBS has provided the country with a scientific basis for accurate i measurements and sources of information on basic properties of materials determined by ! such measurements. In addition, our responsibilities to determine physical constants j and to solve almost any problem that arises in connection with standards have made the

scope of our research in the physical sciences almost unlimited.

If there is any single hallmark of the National Bureau of Standards, it is the

integrity and objectivity which are brought to bear on every project, thereby ensuring

accuracy and precision. And, it is this quality of objectivity which we feel is

crucial to our Recycled Oil Program. In response to Congressional mandate, we will be

investigating and evaluating the test procedures which can be used for the determination of substantial equivalency for various petroleum oil products.

We have formally established the Recycled Oil Program within the NBS Institute

for Materials Research. We have four line organizations, or institutes, at NBS

engaged in different types of research and development. The Institute for Materials

Research (IMR) conducts research to provide a better understanding of the basic

properties of matter and materials and develops standards for measuring their properties to help ensure their proper use by scientific, industrial, and commercial

communities

.

One of the major IMR activities, and one which some of you may be familiar with,

is the development, production, and distribution of Standard Reference Materials (SRM)

.

These SRM's provide the basis for calibration of instruments and equipment, comparison j of measurements on material, and aid in the control of , production processes. As to the impact of these SRM's, let me tell you that in this past fiscal year, more than

32,000 SRM's were sold to more than 16,000 different organizations.

Thus, we feel that IMR is an appropriate "home" for the recycled oil work. The

manager of this program is your workshop chairman, Mr. Donald Becker. Don and his

staff are now actively reviewing and evaluating the test procedures and standards to establish priorities and goals.

There are several actions, outside of NBS, which have been of considerable help

and interest to us, not the least of which is your very positive response to our announcement of and invitation to this workshop. The cooperation of the many interested groups in the public and private sectors has been quite helpful and encouraging to us. I would be remiss if I did not cite the assistance we have received from the

American Society for Testing and Materials (ASTM) Task Force on Used Oil and the total

membership of the ASTM Committee D-2 on Petroleum and Petroleum Products.

Finally, I would like to mention what we at NBS view as a very special action

taken by the Association for Petroleum Re-refiners. This group has voted to support

an industrial Research Associate to work in the NBS Recycled Oil Program during the

coming year. I know that Mr. Duane Ekedahl , the Executive Director of that association,

is with us this morning. Duane, I would like to say thank you for your vote of confidence in NBS. More importantly, I would like to commend your organization for taking

a step which we believe will serve to strengthen your own technical competence, as well

as to assist NBS and the Nation.

2
I would also like to invite any other organizations represented here today to seriously consider the Research Associate Program as a useful and effective method for

further development of mutually beneficial interactions in a particular area. The

Research Associate Program, which is an effort to increase understanding between

business and government, enables scientists and engineers from the private sector-

both domestic and foreign, as well as State and local governments -- to work on a fulltime basis for a specified period of time at NBS on projects of mutual interest.

Currently, we have 70 Research Associates at NBS representing 13 professional and

trade associations, 7 private firms, and 1 Federal agency. The criteria for participation are simple. The project:

must have non-proprietary objectives;

must be within the scope of NBS activities; and

must offer the prospect of publishable results of interest and

significance to the industrial and technical communities

represented and, thus, ultimately to the public.

For more information, may I refer you to this reprint from Commerce America

(Appendix I) which details the NBS Research Associate Program- -what it is and how it

works. When you are ready to talk it over with us, please feel free to contact our Industrial Liaison Officer--Mr. Peter de Bruyn, Mr. Donald Becker, or myself.

In closing, let me say again how strongly I support the efforts and intentions of

this workshop. And, I am very pleased that we are able to provide this important forum

for discussion and exchange of ideas and information on recycled oil.

Dr. Ernest Ambler, Acting Director of the National

Bureau of Standards, delivering the welcoming remarks.

3
Messrs. Peter de Bruyn, Industrial Liaison Officer of the National

Bureau of Standards (NBS) , and Duane Ekedahl, Executive Director

of the Association of Petroleum Re-refiners (APR) , discuss the

APR/NBS Industrial Research Associate Program while Dr. Ambler and

Mr. Michael Kerran, President of the APR, look on.
SESSION I STATEMENT OF PURPOSE

5

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

THE NBS WORKSHOP OBJECTIVES

AND THE NBS RECYCLED OIL PROGRAM

Donald A. Becker

Recycled Oil Program

Institute for Materials Research

National Bureau of Standards

Washington, D.C. 20234

I would first like to briefly discuss the overall objectives of the workshop.

The first and major objective is to obtain input to the National Bureau of Standards

(NBS) by the wide variety of experts present here in the areas of petroleum oils and

test methods on petroleum oils, and on the current status, needs, and problems with

existing specifications, with test procedures, and with standards for virgin petroleum

oil products when these are applied to recycled oil products. Since the accurate

evaluation of recycled oil quality is largely dependent upon the validity of these

test methods, the information that you have used in the past in your company, in your

organization, and in the American Society for Testing and Materials (ASTM) would be

extremely useful to NBS in order to eliminate unnecessary duplication of efforts.

This would greatly assist us to proceed as rapidly as possible in the responsibilities

assigned to us by the Congress, and to avoid at least some of the many pitfalls which

we realiz6 stand ahead in this program.

The second important objective is to help foster personal contact and communication between all the people who are working on test methods, both on recycled oil

tests and on virgin oil test methods. We think this communication will be very

important in order to get test procedures which are valid, and useful, and which can

be used to really determine the quality of the product.

The end uses which are considered here today, as shown in your program, are all

types of end uses including reuse as fuel; as hydraulic oils; as industrial oils,

including cutting oils, grinding oils, etc.; and as engine oils, both crankcase and

transmission oils. Both gasoline engine and diesel engine oils are included. Now, I want to make a short overview of the NBS program as we see it; and, at the end of this

I will have a number of questions which we have considered but, at present, for which

we have no answers. These are the types of questions we are going to have to answer. And so, I will be throwing them out to you to to consider and giving you some of our thoughts on them. I think they are serious questions- -questions which, to my knowledge,

have not been previously addressed. They are the type of questions that are going to have to be resolved in the NBS program.

Now I will briefly discuss the NBS responsibilities. On December 22, 1975,

President Ford signed an act passed by Congress entitled the "Energy Policy and Conservation Act of 1975," Public Law 94-163. In Section 383 of this act, it is stated

that the National Bureau of Standards "... shall develop test procedures for the

determination of substantial equivalency of re-refined or otherwise processed used

oil... with new oil for a particular end use." Further, it states that, NBS is to "...report such procedures to the [Federal Trade] Commission..." as soon as practicable.

As Dr. Ambler mentioned in his presentation, the purposes of Section 383 of this

law are fourfold: to encourage the recycling of used oil, to promote the use of

recycled oil, to reduce the consumption of new oil, and to reduce the environmental

hazards associated with the disposal of used oils. These purposes can be more simply

stated as energy conservation, resource conservation, and pollution control.

The NBS Recycled Oil Program therefore has as its primary objective to provide

these test procedures to the Federal Trade Commission (FTC) so that they can be used

to assure this substantial equivalence of recycled oil products with new oil products

for particular end uses. The initial NBS efforts were aimed toward gathering sufficient information about

the various industries and existing problems in order to formulate an effective

7
program. This was necessary because the last NBS project which was involved with

lubricating oils or petroleum oils, investigating such things as lubricity and test

methods, was terminated over 15 years ago. Therefore, when this law was passed, we had no program and we had to start from the ground up. The initial NBS efforts were concerned with contacting other organizations with interests in this area, i.e.,

the virgin oil refining industry, the used oil re-refining industry, the user industries, the automobile industries, various manufacturers, and the trade associations--the American Petroleum Institute, the National Petroleum Refiners Association, [ the Association of Petroleum Re-refiners, and the Society of Automotive Engineers. ' The standards organizations, especially ASTM, played an important part in our being

able to get information on the responsibilities and the test methods that would be i required for this type of work. Also, we interacted very strongly with the various

government agencies which had programs in recycled oil or in oils at all: the Energy f Research and Development Administration/Bartlesville was an important one, and you * will hear more about their work later on in the program; the Environmental Protection : Agency (EPA)/U.S. Army efforts for military specifications, like Dr. Ambler mentioned, ' and you will also hear more about that later on; the Federal Energy Administration, : which is mainly responsible for used oil collection programs; the Federal Trade f Commission (FTC), which will have the responsibility for the regulations as to label- j ing and enforcing these regulations; and EPA, from the environmental pollution point

of view. The information gathered was reviewed and evaluated, and the NBS Recycled j Oil Program was established.

j Before I get into the specific NBS program, let me briefly discuss two other

j subjects. The first one involves the volumes of used lubricating oil generated in the , States. Those of you who know much about used oils probably have seen these same | figures over and over. Everyone, I think, uses the same numbers because they were generated for an EPA study, the 1974 Report to Congress. My information now is that new oil consumption is up to about 2.5 billion gallons per year; but the important

thing that I want to point out is in the fate of used oil, the volume that is given

for used oils which are reused as fuel--480 million gallons per year in 1972. This is ' the largest end use of used oil at that particular time. The question of where the | unknown portion, which is the second largest, actually ends up is not known, but at i least some of this could well be used as fuel also.

j The second subject I want to mention is the applicability of Public Law 94-163.

After our information gathering effort and a study of the specific terminology used, i our interpretation is that the law includes all of the types of oils that were dis- | cussed earlier: engine oils, industrial lubricating oils, metal -working oils, hydraulic

oils, and oil which is reused as fuel- -any oil which can be recycled into an end pro- ! duct to which it can be substantially equivalent.

The NBS Recycled Oil Program is built around the knowledge that there presently

is a large number of existing petroleum oil test methods. These include ASTM tests,

Federal test methods and specifications, military test methods and specifications,

and so on. In general, the specifications and test methods in current use appear to be effective. Therefore, the NBS efforts will be, first, to establish the properties

which are both necessary and sufficient to establish substantial equivalency for any

particular oil, and these are not necessarily the same properties that a virgin oil

may have; and, second, to provide the FTC with a set of these test procedures which

are capable of verifying this equivalency. As I said, wherever possible existing test

procedures will be utilized.

The initial emphasis of the NBS program is on used oils which are recycled as fuel. This choice was made for a number of reasons. First, as I mentioned, the

current fate of used oils is primarily as fuel. Therefore, we feel it should have

the highest priority. Second, there are important environmental questions from un- controlled burning of used oils. And, third, this is a use which apparently can be

addressed rather quickly. As I mentioned when we started out, we had no program in

lubricating oils or in oil testing. Therefore, we are taking an easier problem first,

as long as it fits in with the other requirements; and we hope to gain the experience

with this subject in order to go on to the more difficult ones, like the automobile

engine oils. The other major uses will be addressed in turn. But, it is also

interesting to note that most of the procedures which will be examined for use with

recycled oil to be used as fuel are also the same test procedures which are used for

many of the other oils.

As Dr. Ambler mentioned in his talk, the Recycled Oil Program is in the Institute

for Materials Research, and I want to explain the internal structure a little bit to give you an idea how we will be working. In the Institute, which is composed of about

500 to 600 scientific and technical people, most of the technical people reside in the

8
6 technical divisions shown as squares on the bottom (figure 1) : Analytical Chemistry,

Polymers, Metallurgy, Inorganic Materials, Physical Chemistry, and Reactor Radiation.

The programs are in circles in the middle, the Recycled Oil Program being on the righthand side. The scientific expertise in the technical divisions, in all of the technical

divisions, is available to us to be drawn upon to evaluate and to look at the test procedures required for this program. In addition, there are several other Institutes

which will have information or basic expertise that will be available. For instance,

in the Analytical Chemistry Division, we will have scientists looking at methods for

sulfur analysis and for trace element analysis; in the Polymers Division, we have people

who will examine test methods for viscosity; in Metallurgy, people from the Corrosion ' Section will be looking at the copper strip corrosion test method and will evaluate

whether this method is a valid one when applied to recycled oil products; in Physical

Chemistry, there are a number of test methods to be examined such as distillation temperature, flash point, etc. In addition, in the Institute for Basic Standards we have

statistical support in the Applied Mathematics Division which will look at some of the

sampling methods which are required for certain specifications.

DIRECTOR

J.D. HOFFMAN

DEPUTY DIRECTOR

E. HOROWITZ

STANDARD

REFERENCE

MATERIALS

J.P. CALI

Program

Manager

ANALYTICAL POLYMERS METALLURGY INORGANIC REACTOR

RADIATION

J.J. RUSH

PHYSICAL CHEMISTRY

A.W. RUFF

MATERIALS CHEMISTRY

P.D. LaFLEUR R.K. EBY

Division Chief J.B. WACHTMAN, JR.Division Chief M.D. SCHEER

Division Chief Division Chief (Acting! Division Chief (Acting) Division Chief

Figure 1. National Bureau of Standards' Institute for Materials Research.

The overall program plan, therefore, is to collect existing test procedures and

to review them for applicability, whether they are necessary with a recycled oil product, and for validity, whether with some of the specific characteristics of a recycled oil product this test method is valid. Where required, laboratory programs

will be established to evaluate the applicability of existing test procedures or to develop new test procedures. Then, these test procedures will be delivered to the

Federal Trade Commission.

In our own evaluation of the testing situation, we separated the petroleum test

procedures into three groups. The first group consists of existing test procedure's

which are used to specify or qualify virgin petroleum oils and upon examination are found to be suitably valid for recycled oil products. In the second group are existing test procedures [e.g., ASTM) which are perhaps not presently required for virgin

petroleum oils but which may be required for recycled oil. For instance, an example

might be the ASTM procedure for neutralization number; it is not currently specified

for fuel oil, but for recycled oil it may be necessary. Group three consists of re- quired test procedures which do not presently exist for petroleum oils; these will

have to be developed.

! 9
I

Table 1 shows current fuel oil specifications. The middle column is the Federal

specification for burner fuel oil, VY-F-815C; the right-hand column is the ASTM D-396

specification for fuel oil; and on the left are a list of test methods. All of these

TABLE 1 FUEL OIL SPECIFICATIONS

FED. SPEC. ASTM D-396

V V - r - o ioL STAJ'IDARD

T'T TT"" T /~\ T T FUEL OIL, SPECIFICATION

BURNER FOR FUEL OIL

Flash Point D-93 or D-56 D-93 or D-56

Pour Point D-97 D-97

Water/ Sediment D-1796 (1,2,4) D-1796 (1,2,4,5)

Water D-95 (5,6) D-9S (6)

Sediment D-473 (5,5) D-473 (6)

Carbon Residue D-524 D-524

Asn D- 4 8 2 D-482

Distillation Temperature D-86 D-86

Viscosity, kinematic D-445 D-445 (1,2)

Viscosity, Saybolt D-2161 or D-88 D-88 (4,5,6)

Gravity, API D-287 D-287

Copper Strip Corrosion D-130 D-130

Sul fur D-1552, D-129 D-129, D-1551

D-1551 or D-2622 D-1552, D-2622

Aniline Point D-611

Container Sampling MIL-STD-105

Container Examination MIL-STD-290

Test Sampling D-270

Inspection FED. TEST 791-9601

various test methods are currently specified for virgin fuel oil: flash point, pour

point, water, sediment, carbon residue, ash, distillation, viscosity, etc. Most of

these would fit into group one test procedures. The types of things we will be

evaluating on each of these test methods include the effects of additives. This is

necessary since much of the recycled oil that is presently used as fuel is obtained

from what is called street drainings. This used oil has the additives from automobile

motor oils and, thus, contains oil soluble organometallics . How do these affect other

test methods? Viscosity improvers or pour-point depressants- -how do these affect perhaps the pour point measurement itself and also other test methods? Is this additive

going to make a particular test valid or invalid? The effect of contaminants on test

procedures must also be evaluated. For instance, the particle size distribution of wear debris par ticulates - -how does this affect the viscosity measurement? In many

of the cases where street drainings contain also drainings from automobile radiators--

ethylene glycol--how does this affect some of the test procedures? Will the test procedure still be a valid test if it has a contaminant in it, for example automobile

hydraulic fluids? How is this going to affect each of these tests? What about

synthetic motor oils? Obviously, if it is a polyester motor oil, it most likely will

make the saponification number invalid; but how is it going to affect other tests?

It is important to remember that, at least in some cases, these test methods that are going to be given to the Federal Trade Commission will be used on all quality oils.

If someone represents a straight used oil as some type of product, the test has to be

valid for a straight used oil, as well as a high-quality re-refined oil. At the least,

there has to be some way to differentiate between these types of products in order to say it is or is not a valid test, or can or cannot be used on this type of product.

In the group two test procedures, the neutralization number is something that may i be required for certain recycled oil products, or perhaps a precipitation number. f There are existing tests for these, and they may very well be applicable directly to \ the recycled oil products. Trace element content is certain to be important for a num-, ber of end products. Elements such as lead, calcium, barium, zinc, etc., are of con- | cern for environmental pollution as well as for effects on certain types of performance,

I have also recently found out that virgin fuel oil has some types of additives. For

example, ferrocene is apparently added in low concentrations to improve burning and i reduce smoke of virgin fuel oil. How does this affect the range of trace element , concentrations for the existing virgin petroleum oils that are currently on the market?;

10 \

I

j' ^1
Group three test procedures- -fortunately, there are not too many of these, and

, perhaps they are not as much of a problem as they first appeared. Lead concentration

I is one possibility. We are going to have a speaker tomorrow who will talk about some of the problems EPA has with the lead pollution. Perhaps a test procedure for lead in

recycled oil will be found necessary. There are two existing ones, or at least two: D-1262 for lead in greases, and D-2788 for lead in gas turbine fuel. We do not know

at the present time whether one of these will be applicable to general recycled oil

products.

The ash content is also very interesting. Current virgin fuel oil specifications

include ash content. However, the ash method which is specified for use specifically

states that it is not valid in the presence of lead or in the presence of organometallics. Recycled petroleum oil that is to be burned may very well have either or both of; those. You can then use the sulfated ash procedure, which is valid for organometallics; but, here again, the procedure itself states that it is not valid in the

presence of lead. The question of whether this could be adapted or modified with very

little change is not really obvious at the present time. I think ash is an important

characteristic of recycled fuel oil that needs to be defined, but how best should it

be done in order to obtain an accurate value?

I The last potential test I will discuss is the polynuclear aromatics. It was

' published in the open literature about a year ago that used oil has significantly

higher polynuclear aromatic contents than virgin lubricating oil. For fuel use, that

is not quite the question; but rather the question is whether used oil has a higher

polynuclear aromatic content than virgin fuel oils. As far as we know at the present

time, there is not enough information to determine whether that is true or not. So,

in this case, we need more information. In industrial oils, it may be that the recent

information which has come to light on nitrosamines might be significant for certain

types of recycled industrial oils.

In summary, the detailed program plan is: (1) to identify the required test procedures for each particular end-use product; (2) to conduct a non - laboratory program

to collect existing test procedures and establish a review protocol, including outside

advice; (3) to review the test procedures for applicability and validity, all the

while maintaining coordination with outside government and private -sector groups--

where there are problems, we will have to go to the laboratory, verify the validity or applicability of existing test procedures, or develop new test procedures; and, finally,

(4) to establish the adequacy of the total package to define substantial equivalency

and then transmit these to the FTC. It is obvious that we will provide advice and

consultation to the FTC on these tests wherever required.

As I am sure most of you already know, there will be problems in carrying out the

requirements of this law. We are aware of some of these problems; others will certainly surface as we get further into the program itself. From what we know now, in

principal, recycled lubricating oil products are potentially able to qualify for all

end uses, i.e., the basic hydrocarbon structure is apparently not altered during use. However, at present we do not know whether existing qualifications or performance

standards are capable of establishing the substantial equivalency of all recycled oil

products for their end uses. In addition, the interlaboratory comparability of some

of the existing tests, i.e., the accuracy and reproducibility, are not fully known.

This is especially true for some of the non-ASTM tests for industrial oils and specialpurpose oils where I have seen in the test procedure the statement, "Reproducibility

is not established," or "Accuracy is not known."

Finally, we realize that the consequences of poor or inadequate standards could

be large. One of the ways that NBS is attempting to obtain input from all interested

parties is this workshop. We hope that you also will find the meeting both informative

and stimulating; and we invite your continued cooperation and input into the NBS program in the future. I look forward to hearing the following speakers, and I especially

look forward to the discussions to follow the speakers. I hope that all of you will

want to participate in these discussions and will frankly and openly present your views

and your experiences with these test methods and with recycled oil.

11

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. CIssued August 1977)

DISCUSSION

SESSION I. STATEMENT OF PURPOSE

The discussion on this first session centered around a number of different areas. Initial interestwas expressed in the time schedule for the National Bureau of

Standards' (NBS) program. The estimate was given by NBS of approximately one year for

the test procedures for recycled oil to be used as fuel. Completion of the other end

uses that will be addressed cannot be reliably estimated at present due to the large

number of unevaluated technical questions which still remain. It was pointed out,

however, that many of the tests which are being evaluated for use with the first end

use will also be the same tests as for other end-use products (e.g., viscosity, flash,

sulfated ash, copper strip corrosion). It was also noted that this current schedule

calls for the transmission of a set of tests for each end-use product as soon as completed, rather than waiting until all end uses have been completed.

The second area of discussion centered around NBS' cooperation with other groups

interested in oil recycling, especially with the Environmental Protection Agency (EPA),

concerning Public Law 94-163 as well as the more recent Public Law 94-580, the

Resource Conservation and Recovery Act of 1976, which gives EPA broad responsibilities

in resource conservation and hazardous waste management. In addition, NBS is interacting and cooperating with the Energy Research and Development Administration/

Bartlesville Energy Research Center in their program for the evaluation of new re-refining technology. It was also pointed out that the oil recycling system in

Europe is far ahead of the U.S. and that perhaps it would be profitable for the U.S.

to use available information from European governments and industries. The response

indicated that interaction with the European governments is taking place and that this

interaction will increase in the future. However, it was also pointed out that little

Or no information is currently available from Europe or elsewhere on the evaluation of

virgin oil test procedures for recycled oil products or specifically addressing the

basic question of determining quality in recycled oil products.

Another area of discussion was concern about the possibility of the government

setting industrywide test methods and specifications. Specific questions which were

brought up by industrial participants included what potential liability the government

would accept when a consumer product meets a government specification or test but is

later found not to be suitable for the end use described. In addition, concern was expressed about the ability of the appropriate government organization (i.e., NBS and/

or the Federal Trade Commission [FTC]) in keeping the promulgated test methods up to date in a rapidly changing field, as well as concern about the possibility of having

different tests or specifications for virgin and recycled petroleum oil products.

These concerns were thought to be serious ones by participants and were felt to require

additional discussion at a later time.

One question concerned the meaning of the term "substantial equivalence," as used in Public Law 94-163, concerning the NBS responsibilities. In response, it was pointed out that the legislative requirement of Public Law 94-163 is that the NBS provide the FTC with test procedures which can be used to determine whether a recycled

oil product is substantially equivalent to a~irgin oil product. There is no requirement that the recycled oils have to be able to pass these tests, only that if it does

it be substantially equivalent for that particular end use. It is also obvIFus that

the law is strongly supportive of oil recycling, so the implication certainly is that

these tests must be reasonable and usable for their intended purpose--and that purpose

is to establish reliable quality control for recycled oil products.

Another area of concern expressed by participants was whether new American

Petroleum Institute (API) engine oil classification (s) or equivalent would be developed

in order to meet the requirements of recycled oils. In the ensuing discussion, it was stated that there was no intent nor should there be a need to develop new classifications for recycled lubricating oils. It was felt important that industry and government work together to develop adequate criteria for defining appropriate service

levels for recycled oil products within the existing classification system. That

could mean that engine sequence tests would be required in order to establish the

additive response or various quality levels of a particular re-refined oil, for

example, or that enough data be accumulated in order to assure that a particular

13
I

I

additive package together with a certain base oil would provide an appropriate service

level. Engine manufacturers then stated that engine sequence tests by themselves are not satisfactory to adequately define effective field performance, but that the

correlation between satisfactory field use and engine sequence tests was required in

order to originally establish the usefulness of sequence tests. It was further felt

that field data for recycled oils should also be available in order to establish

similar types of correlation with the tests to be used.

During the discussi'on, one suggestion was made that perhaps the possibility shoulc

be evaluated of using all of the recycled and/or re-refined oil either as industrial

oils, or as fuel oil, in order to eliminate the difficult technical problems involved

with motor oils. However, it was pointed out that, even other considerations aside,

with the free enterprise system that exists in the U.S. it would be difficult or impossible to restrict the uses of a particular oil as long as it met the required

quality criteria.

Finally, the session ended with a statement by the NBS moderator concerning the

NBS program. It was stated initially that the NBS program does not wish to affect the

established specifications and testing system any more than necessary in oider to carry out the requirements of the various laws that have been enacted. It was also

pointed out that NBS has these requirements to provide various test procedures to establish substantial equivalency, and these requirements will be carried out. It is

not known at the present time exactly how these requirements are going to impinge on the existing system. However, it was emphasized that cooperation and collaborative

work with both government and industry together, through the American Society for

Testing and Materials and through other means, would be to everybody's advantage,

especially the consumers and users in the U.S.

1

14
SESSION II USED OIL REUSED AS FUEL

15

National Bureau of Standards Special Publication 488. Proceedings o£

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

BURNING USED OIL AT A MILITARY INSTALLATION

Charles F. Schwarz

Martel Laboratories, Inc. 1025 Cromwell Bridge Road

Baltimore, Maryland 21204

What I would like to talk about today is a project that was initiated back in

1968 at the Aberdeen Proving Grounds. Much of the work took place while I was still

head of the Fuel and Lubricants Division in the Coatings and Chemical Laboratory.

The actual work was done by Messrs. Maurice E. LePera and Gerald DeBono of the Fuel

and Lubricants Division. (This was before the subsequent reorganization and move to Fort Belvoir, where the report was compiled and completed.) The entire U.S. Army

report (MERDC R-2127) is included as Appendix II, so my remarks today will be quite

brief. However, I felt that the excellent and comprehensive work by Messrs. LePera

and DeBono should be brought to your attention.

At that time (1968) Aberdeen was disposing of waste oil by blending it into

No. 6 fuel oil, Federal Specification VV-F-815C. Approximately 40,000 gallons of

waste oil were consumed each year in this manner at Aberdeen. Since No. 6 fuel oil

is a relatively viscous product, no problems were encountered with the waste oil

disposal system. But in August 1972 when, due to sulfur restrictions, Aberdeen

changed from No. 6 fuel oil to No. 2 fuel oil, it was felt that a little more work

should be done to evaluate the blending of used oil with this distillate fuel oil.

Because of the obvious differences of properties between No. 2 and No. 6 fuel oil,

Aberdeen became concerned over the continuance of the waste oil disposal program.

Some of the questions to be considered included: Could stratification and/or

sedimentation problems due to the difference in gravity lead to a potential malfunctioning of the burner nozzles, since waste oil is considerably heavier than

No. 2 fuel oil? Also, would burning used oil create excessive stack emissions

exceeding the air pollution standards, due either to improper combustion or from the

composition or concentration of the waste oil product itself?

In April 1973, Aberdeen conducted an initial waste oil incineration program at

the main power house. Stack emissions were monitored by the U.S. Army Environmental

Hygiene Agency, the emission specialists for the Army, and they took measurements

while the No. 2 fuel oil, and the No. 2 fuel oil containing approximately one percent

waste oil, were burned. As described in the report, it was obvious from the results

that the one percent of waste oil burning in the No.' 2 fuel oil did not cause any

problems. This would be fine for us; but could other army installations that do not

have a large power house blend larger amounts? We then selected a small boiler system

at one of the Aberdeen Proving Ground (APG) messhalls for a second emission test program. This program was considered to be, a simple and accurate method for investigating different waste oil/fuel oil blends.

The burning system consisted of three five-tube high-pressure boilers, and

three oil-fired, low-pressure rotary cup KEWANEE burners. The system was originally

designed to burn a No. 4 or No. 5 fuel oil and was rated at 86.3 hp, 30,808 pounds

steam/hour, and 4,500,720 Btu.

In the initial program that was conducted in the power house, all the waste

products that w^ere generated at the Post were used. At that time, they were disposing of a lot of jet fuel from defueling aircraft, and so the fuel burned in the big

power house was quite light.

For the second program, it was decided to get a typical crankcase draining, or waste oil, for evaluation. Therefore, all of the drainings from the Post Exchange

Service Station were collected, and these were from commercial vehicles. No doubt,

this waste material had trace amounts of antifreeze and hydraulic brake fluid and

some transmission fluids. In addition, some water contamination occurred from the

improper drum coverings and/or closure procedures since the drums were stored outside. This water, after settling, was pumped out prior to the combustion-emission

17
tests to insure that water contamination did not influence the resultant stack emission studies. A 1,200 gallon tank truck containing 200 gallons of waste oil and 800

gallons of No. 2 fuel oil served as a temporary mixing reservoir. A final mixture

of about 27 percent waste oil was used for the three two-hour test runs. The mixture

was pumped directly from the fuel oil truck into our burners, so there was pretty

good control over what was burning. The truck tank was also sampled at three levels--

top, middle, and bottom--to see if stratification occurred. We therefore had a pretty

good handle on the actual product that was being burned.

As I mentioned earlier, the complete results of these tests can be found in the

U.S. Army Report 2127, Investigating Waste Oil Disposal By Direct Incineration , by

Messrs. M. E. LePera and G . DeBono [Appendix Ilj"!

In summary, it was determined that a 27 percent mixture of waste oil in No. 2 fuel oil was too high. From the results of these tests, a directive was issued to allow up to five percent of waste oil to be added to any No. 2 fuel oil in any other

Army installation without actual tests of air emissions.

18
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

FUEL OIL AND THE DEFENSE SUPPLY AGENCY

Edward J. French

Defense Fuel Supply Center

Cameron Station

Alexandria, Virginia 22314

In my talk this morning, I would like to tell you a little about Federal procurement of petroleum products. The Defense Fuel Supply Center procures most of the fuel,

lubricants, hydraulic fluids, etc., for the Federal Government, including the civilian

agencies. Primarily, we buy what the agencies ask for. They come to us and give us a set of requirements, along with specifications. Many civilian agencies, though, just

say, "We want fuel oil." So, based on what the Environmental Protection Agency's

restrictions are for the various locations that we buy for in the U.S., we procure an

oil which will give them the acceptable atmospheric emissions; or, in some cases, the

control is on the sulfur level in the fuel.

We are presently on the street trying to purchase two million gallons of a re- cycled oil for use as fuel. In this particular case, what we did is put in the regular W-F-815C requirements, except the requirement that it not contain recycled

materials was waived. We expect to have more of these types of purchases in the future.

All of the existing specifications, including sulfur level, sediment, etc., still apply.

In the past, we have encountered some problems in procuring fuel oil in the midwest where we know that recycled oil is going into it. The primary problem we found

with that oil was the sediment content. The supplier that is intending to bid on this

two million gallons of recycled oil that we requested, as I understand it, simply

settles the used oil and blends it in with virgin oil to make an acceptable blend.

The only way that we have determined in the past that our fuel oil was being

blended with used oil was the higher metals content and other components that normally

come only from used lubricating oil. It may be that one of the reasons that a lot of

the Federal activities do not want to buy fuel oil that already has been blended with

used lubricating or recycled oils is because they wish to add their own used oils that

they have generated into the fuel oil burner instead. The U.S. Army has published a report on a program to determine to what extent and how much used lubricating oil you

can put into fuel oil. In my opinion, one of the important limiting factors is the

environmental considerations involved. You will hear more about this Army study by

another speaker today.

1

19

National Bureau of Standards Special Publication 488. Proceedings o£

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

FUEL OIL SPECIFICATIONS

Burton L. Weller

National Oil Jobbers Council

1750 New York Avenue, N.W.

Washington, D.C. 20006

Before I start discussing fuel oil specifications, let me tell you a little

about why I am so interested in fuel oil. The National Oil Jobbers Council represents

the 12,000 independent petroleum marketers who market heating oil, gasoline, diesel

fuel, and related petroleum products, as well as the manufacturers of oil-burning

equipment. In addition, I am chairman of the American Society for Testing and

Materials (ASTM) Committee D-2's Panel on D-396, Standard Specification for Fuel Oils.

The primary function of this panel is to consider recommended changes to this specification. This specification provides the minimum criteria for different grades of fuel

oil intended for use in various types of fuel-burning equipraent under a variety of

climatic and operating conditions. It is used by purchasing agencies in formulating

contracts for the purchase of fuel oil, and for the guidance of consumers and engineers

in selecting the grades most suitable for their needs. Most fuel oils marketed are produced to meet this standard.

In this presentation I would first like to review the six grades of fuel oil.

Secondly, I would like to provide an insight into some of the testing requirements

that are outlined for these grades of fuel oil. There are ten testing criteria, along

with a number of testing techniques. We will not cover all the testing techniques,

but for a complete listing of them I would refer you to the specification itself

(table 1) . Finally, we will mention some of the new items that are currently being

considered by the D-396 Panel.

As I previously mentioned, there are six grades of fuel oil at the present time.

These may be broken into two categories: distillates are primarily used for residential heating, while residuals are mainly for commercial and industrial use.

• No. 1 - A distillate oil intended for vaporizing pot type burners

and other burners requiring this grade of fuel. )• No. 2 - A distillate oil for general purpose heating for use in

burners not requiring No. 1 fuel oil.

• No . 4 - Usually a residual oil and preheating is not required for

handling or burning.

• No . 5 Light - A residual oil and preheating may be required,

depending on climate and equipment.

• No . 5 Heavy - Also a residual oil, and preheating may be required

for burning and, in cold climates, may be required for

handling.

1 • No . 6 (Bunker C) - A heavy residual fuel oil for which preheating

is required for burning and handling.

Turning now to the 10 testing requirements, these are each briefly discussed

I below.

Flash Point . - When fuel oils are heated, a vapor is produced. At a certain

temperature"] the vapor will ignite by an external flame. This temperature is called

the flash point temperature.

! ASTM D-396 provides for flash point testing by: (1) the Pensky-Martens Closed

[Tester, and (2) the Tag Closed Tester. The specific testing' procedures D-56 and D-93

jare available in the ASTM Handbook. In both cases, the sample is placed in the cup

|0f the tester and, with the lid closed, heated at a specified constant rate. A small

flame of a specified size is directed into the cup at regular intervals. The flash

21

if
3

cn

Max Q.5

or

legal 0,5 or

legal legal legal legal legal

Copper strip

corro- sion No,

3

No,

3

gravity 60/60

°F

(deg

API)

Max

oi '2' <si c ^ e e > » ' ' 03 00 I 1 • ' • LO • O

o to o to

Kinematic

Viscosity,

cSt

u ^o a.0 o

Max

1 1 » 1 00

i 1 1 1 00 to

J 1 1 1 ^ vD

LO (SJ <SJ P rH

<; w Min

/—

) 1 ) I tsi C-J

1 1 1 1 ai

1 1 1 1 ^

U ^O Ph0

00

Max OJ vO S" ' r » LO CTl 1 fS] to VD O rH 1

At3

(100

Min o 00 •

1 . . \0 LO 1 rH CSI LO 1

Saybolt

Viscosity,

s

Furol

at

50

°C

(122

°F)

(40)

(300)

Min 1 /—

/-y LO

1 1 1 1 to

1 1 1 1 N

1 1 1 1 w w

IMiversal

at

30

°C

(100

"F)

Max --- (37.9) (125) (300) (900)

(9000)

Min

1

(32.6) (45) (

125) (

300) (

900)

Distillation

Temperatures

°C(°F)

90%

point 1

Max 1

228 (550) 338 (640)

--- 282 (540)

10% point Max 215 (400)

--- 0.10 0.10 0.10

Carbon

residue

on

101

bottoms Max

0.15 0.35

Water and

sedi- ment

yolume 0.05 0.05 0.50 1.00 1.00 2.00

D U Hh o o o oMax 00 o" vO O 1

1 rH ^ (^ <N1 1

1

1 1

'—' 1 >—' 1 1

-5 u (IT

r-l O 0 O

Min 38

or

legal (100) 38

or

legal (100) 55

or

legal (130) 55

or

legal (130) 55

or

legal (130) 60 (140)

Grade of

fuel oil

No.

1

No.

2

No.

4

No.

5

light No.

5

heavy No.

6

</)!

I u

22
point is taken as the lowest temperature at which application of the test flame causes

the vapor above the sample to ignite.

NOTES: (1) If the oil contains water, it should be removed by heating the oil

in a water bath. The test sample should then be taken from the top portion of the oil

sample. (2) Sometimes erroneous results are obtained by heating the sample too fast.

(3) Occasionally, one may contaminate the test sample with the cup-cleaning agent.

(4) When specifying flash points, the type of instrument used should be named and, more specifically, the method of test should be specified. These and otlier precautions

are taken in the testing procedures, as outlined in ASTM D-396 and the reference testing procedures.

Examples of typical flash points seen for the various fuel oil grades are found

in table 2.

TABLE 2 COMPARISON OF FLASH POINTS

Fuel Oil Grade Typical Flash Points ^

No. 1 No. 2 No. 4 No. 5 No. 6

130, 134, 140

160, 126, 176, 144, 204, 240

170, 182

245, 142, 100, 210

190, 224, 250, 330

^ in °F., Pensky-Martens closed cup

The type of equipment, location of storage tanks, the amount of preheating, and

the condition of equipment all have an impact on the flash point requirements of an

oil.

Pour Point . - Let us turn now to the second testing requirement, the pour point.

If temperatures between 80°F to 90°F were experienced the year round, consumers,

refiners, and suppliers in some instances would be happy. A feature of most oils is

their ability to congeal into a semi-fluid or a solid as the temperature drops. When

cold weather occurs, one can imagine what happens inside of tanks, lines, and pumps.

To protect the user and refiner, the pour point test was developed. The temperature

at which an oil will just flow under standardized conditions is known as the pour

point. The standard method of test for pour point of petroleum products is outlined

in ASTM standard D-97. After a preliminary heating, the sample is cooled at a specified rate and examined at intervals of 5°F for flow characteristics. The pour

point is set at 5°F above the temperature at which the oil becomes solid.

Pour points are a fair indication of what happens under actual conditions. The

type of oil and the condition to which the oil has been subjected immediately before

the test have a direct bearing on the results of the test. Therefore, the standardized test procedure specifies the conditions and handling of the oil before the test.

Some of the troubles that are attributed to improper pour points in cold weather

I include clogged strainers, unpumpable oil, clogged lines, erratic combustion, spitting,

I and smoke and carbon from poor atomization due to the heaviness of the oil. Generally,

the fuel oil supplier watches the pour point of his oil, especially those which are

not heated in his storage tanks because he, as well as his customer, must be able to

pump when cold weather sets in.

Water and Sediment . - The third testing requirement is for water and sediment.

A great source of trouble in all grades of fuel oils is the water and sediment that

are sometimes present in oil. Difficulties include: (1) complete stoppage of operation and combustion, (2) erratic and unsteady combustion, (3) sparking and spitting of

the flame, (4) flashback of the flame, (5) blocking of passage ways, (6) loss of heat,

j and (7) erosion of mechanical parts. The water and sediment in grades Nos. 1, 2, 4,

j and 5 are tested in accordance with ASTM D-1796, and grade No. 6 is tested by ASTM

j D-95 test procedures. The first is the test by centrifuge. The test is conducted by

I mixing the oil with a solvent, in a glass tube, and then whirling it in a centrifuge.

I The centrifugal force throws any water and sediment to the bottom of the tube, which

is calibrated, and a reading of the contaminants can then be taken. A second test

23
method is the water distillation test. In this method, the oil is mixed with gasoline

and distilled. The vapors are condensed and the liquids drop into a calibrated tube.

The water, being heavier than the gasoline, is then measurable. The third method is ' sediment by extraction which will not be covered here. i There are a number of causes for bottom sediment and water. They include:

(1) contamination by leaky tanks, (2) chemical reactions in the oil, (3) excessive

tank heating, (4) condensation, and (5) improper mixing, which may cause separation.

Carbon Residue . - There are four different types of carbon that may be present in

oil or may be produced by testing it. They are: (1) fixed carbon, which is the car- bon of the chemical compounds in the oil; [2) free carbon, which is the carbon that

has precipitated or has been loosened from the chemical hydrocarbon; (3) carbon formedi3|si on the burner tip due to incomplete combustion; and (4) carbon formed during the

carbon residue test. The test procedure is outlined in D-524, Test for Ramsbottom

Carbon Residue of Petroleum Products. The sample, after being weighed in a special

glass bulb, is placed in' a metal furnace maintained at approximately 1,000°F. The

sample is quickly heated to the point at which all the volatile matter is evaporated

out of the bulb. After a cooling period, the bulb is weighed and the residue is calculated as percentage of the original sample. The carbon residue serves as a rough

approximation of the tendency of the fuel to form deposits. Some examples of the

troubles encountered due to too high carbon residue are: (1) some burners will just

not handle too high a carbon residue, and (2) small combustion chanbers can build up a carbon residue on their walls.

Ash . - There are certain impurities or foreign materials present in most fuel oil

that are not apparent or noticible. These organic and inorganic substances are often

non-combustible and, after the combustion of the fuel oil, they form a residue called

ash. The laboratory procedure to determine the presence of ash is to heat the oil in

the presence of air. The vapors are then ignited and burned; then the temperature is

increased to burn the carbonaceous materials, leaving only the non-combustible ash,

which is weighed.

There are a number of problems that can arise as a result of ash. They are:

(1) manufactured objects in direct contact with combustion reactions may be affected

by the ash; (2) in low pressure boilers, it may result in a heat - transfer problem due

to the build-up of ash; and (3) in high-temperature steam boilers, it may cause the

surface of the metal to rust or corrode.

111

Distillation Temperature . - An oil is made up of a series of petroleum fractions,

each boiling at a higher temperature than the previous one. This is the basis of the

distillation tests. It furnishes the distillation range of the oil under test. To run the distillation test, oils are heated and vaporized in a glass flask, and the . vapors are then passed through a water-cooled condenser and into a graduated flask ^ [\ (ASTM D-86) . The temperatures are rated in 10-percent increments. The initial boil

ing point (IBP) is the temperature at which the first drop of condensed vapor appears ^fi: in a distillation test. The next temperature above the initial boiling point is the

10-percent point. This is the temperature at which 10 percent of the total volume of i the sample of oil will distill off. The spread between the IBP and the 10-percent

point should be small so once ignition takes place the oil will continue to burn. Thel distillation points of 20 through 80 are very seldom used, except to check the spread

of fractions. The closer they are together, the better it is since it is better to have a greater percentage of the distillation range on the lighter or lower side of

50 percent to facilitate the burning of the heavier ends of the fuel oil. In specify-|]

ing the 90-percent endpoint for a No . 2 oil with a minimum of 540°F to a maximum of

640°F, we have protected against a high endpoint. The maximum is specified as j protection against contamination by heavy oils which may be difficult to burn. '

Viscosity . - The viscosity of oil has been defined as its resistance to flow. In the U.S . , the Saybolt viscometer is usually used, the two types of which are the J Universal and the Furol. The difference between the two i.s the size of the opening a" the bottom of the outlet tube through which the oil that is being measured flows.

Another instrument used is the kinematic viscometer. The major difference between theb kinematic and Saybolt test is in the testing technique. While running the test, the c kinematic viscometer has a constant head which exerts a continuous downward pressure. ) The Saybolt viscometer has a fixed volume of liquid exerting the downward pressure

Grades 1 and 2 fuel oil are run using the kinematic tester, and grades 4, 5, and 6 are' run using the Saybolt viscometer. It is absolutely necessary when quoting a viscosity? [jj reading that the type of instrument, as well as the temperature, be given. To illus- ) trate, a viscosity may be shown as 500 SUS at 100, meaning 500 Saybolt Universal Secoh

at 100°F. . !

I 24
Viscosity would have to be considered the one most important single specific

I characteristic of a fuel oil. This is especially true of grades 5 and 6 oils, where

j the viscosity has to be known in order to adjust the pumping temperatures, the atomizing temperatures, and the pump pressures. The difficulties which may occur when an

oil has too high a viscosity are: (1) pumping problems, (2) insufficient oil at

burner, (3) flashbacks, (4) trouble with initial starting, (5) poor combustion, and

(6) a high carbon residue. An oil which is too light will: (1) cause too much oil to

be pumped, and (2) result in loss of economy.

j Gravity . - The oil industry employs the API gravity scale, devised jointly by the

American Petroleum Institute and the National Bureau of Standards. The relationship

between API gravity and the specific gravity is an arbitrary one: 1° API gravity

i equals 141.5 divided by the specific gravity at 60°F, minus 131.5. Where the term

I "gravity" is used by the oil industry, the term means API gravity. The test method is

, to float a hydrometer scaled to API units in the oil and take the API gravity readings

along with the temperature of the oil. As the gravity varies with temperature, the

' reading taken is corrected to API gravity at 60°F.

The gravity will tell you: (1) the lower the API gravity, the heavier the oil in

viscosity or consistency, the higher the carbon residue, and the heavier the weight;

the opposite is true for the higher API gravity; (2) the higher the gravity, the

greater the heat of combustion; (3) the higher the API gravity, the lower the unit

II weight of the oil; (4) the type of refining process; (5) the grade of the oil; and

j (6) as the API gravity decreases, the rate of combustion decreases.

] Copper Strip Corrosion . - ASTM D-130, Standard Method for Detection of Copper

I Strip Corrosion, provides for the immersion of a polished copper strip in a sample of

the fuel oil at a given temperature and for a given period of time. At the end of the

test, the copper strip discoloration is compared with the ASTM copper corrosion standard. The purpose of the test is to detect the corrosiveness of the fuel oil to

copper and is largely a measure of the active sulfur content of the oil.

jj Sulfur . - Sulfur is the third most important element present in oil. Compared

j with carbon and hydrogen, the percentage of sulfur is very small (up to 2 percent),

I but it consists of a large number of individual sulfur compounds. There are four

methods of test for sulfur that can be used. They are: (1) D-129, Oxygen Bomb

Combustion Method for Sulfur in Petroleum Products; (2) D-1551, Quartz Tube Method for

Sulfur in Petroleum Oils; (3) D-1552, High Temperature Method for Sulfur in Petroleum

Products, and (4) D-2622, X-Ray Spectrographic Method for Sulfur in Petroleum Products.

, In addition. No. 1 fuel oil may be checked by method D-1266, the Lamp Method. Because

of the time element, I will not discuss the various testing techniques. Consistent

results on sulfur testing by different operators in different laboratories is not

always achieved. Naturally, this creates problems. Acceptable sulfur precision limits

frequently range from 0.1 percent to 0.01 percent. There appears to be two principal

reasons for this problem. The first reason is improper sampling. The supplier may

have a large storage tank of oil that has been blended to provide the proper sulfur

content. The sample is taken (correctly) from different levels in the tank, combining

the samples to a composite on which the sulfur test is run. The consumer may take

his sample from the truck which represents a certain strata of the supplier's tank.

3 Consequently, the analyses have not necessarily been run on the same sample. The

second reason is technique. At times, rather make -shift equipment has been used.

This factor has been found in a number of laboratories which have tried to use the same apparatus for checking sulfur in both steel and petroleum oils. Some refined

| products, such as gasoline and kerosine, have been treated for the reduction of sulfur.

I With the advent of the H-Oil Desulfurization process, the refining industry can now

make low sulfur residual fuel oils. The process can remove 60 percent of the sulfur,

bringing the content of a residual oil from 2.5 percent down to about 1.0 percent.

There are a number of troubles that can be attributed to sulfur. They are:

(1) corrosion by its combustion products (the most important problem) , and (2) many

manufactured articles are affected by the combustion products. In the glass industry,

a low-sulfur fuel is required (-0.25 percent S) . A high-sulfur material causes discoloration and pitting of the glass products. The largest users of fuel oil are the

open hearth furnaces of steel mills. For this industry, the absorption of sulfur

gases into the steel itself causes the metal to become brittle.

Finally, I have been asked to mention some changes that are currently being con- sidered for inclusion into ASTM D-396. There are' three potential changes that come

to mind at this time. They are:

25
1. Specification for a light No. 4 oil: The committee has been

requested to include a light No. 4 oil in the specification, with

recommended limits of: Flash - 130°F, or legal; Pour Point - 20°F

maximum; Water and Sediment - 50 percent maximum; Ash - 0.10 percent maximum; Viscosity - 5.8 kinematic centastokes maximum at

100°F or 45 Saybolt Universal Seconds maximum at 100°F; Gravity,

API - 30° maximum; and. Sulfur - legal.

2. Lubricity: The committee is currently conducting tests on some samples of fuel oil to determine if there is a lubricity problem.

3. There is a feeling that the higher aromatic fuels that come from

the catalytic cracking process may be causing a wear problem on the

seals in a fuel oil system. The committee is also looking at this

situation

Obviously, with over 20 million burners and systems in the field, serious con- sideration must be given to any change in the specification prior to adoption by the

panel

26
National Bureau o£ Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

AUTOMOTIVE CRANKCASE DRAININGS USED FOR FUEL

Belton R. Williams

Motor Oils Refining Company

7601 West 47th Street

McCook, Illinois 60534

Automotive crankcase drainings have long been an important source of feedstock

for re-refiners. The base oil derived from the used oil is used to compound motor

oils, hydraulic oils, and various kinds of industrial lubricants.

For reasons peculiar to the industry, primarily economic in scope, over the

years all of the available crankcase drainings have not been re-refined, and a significant volume was determined to be a pollutant of the environment. At the same

time, some crankcase drainings were being put into industrial fuel streams with varying degrees of success. Because of the environmental impact and various economic

considerations, much support has been given in recent years to burning the crankcase

drainings with little recommended processing and with major emphasis on diluting

with virgin fuel oil to meet ambient air quality standards and to minimize equipment

fouling.

Much data are available to sustain the argument over whether to burn or not to burn and how to burn or how not to burn. I would like to present data which pose

many of the considerations to be examined in the course of arriving at means of

determining substantial equivalency of products made from these materials. It should

be understood that the data do not draw any conclusions, they do not resolve the

controversy, and are presented for the informational value. Similar testing of other

samples may result in some variations, depending on technique of sample gathering and

exposure to extraneous contaminants.

The data presented in table 1 were from samples of automotive crankcase drainings

accumulated in our laboratory. The free water had already been drained from the

material, and the combined samples retained 5 percent water in the emulsion.

TABLE 1 CRANKCASE DRAININGS USED FOR FUEL

Raw Dehydrated Vacuum D-396

drainings drainings distilled No. 5 light

Flash, °F. 275 385 380 130

Fire, °F. 390 425 415

BS5W - vol. 12 % 5.2 % 0.01 % 1.0 % Ash - wt

.

1.95 \ 1.87 I 0.002 % 0.1 % SSU at 100 °F 372 340 211 150-300

V.I

.

123 124 97

Sulfur, % 0.5 % 0.5 % 0.2 2 % Legal

Btu - per lb. 18,351 18,880 19,341 18,500-19,400

The data for the raw drainings, dehydrated drainings, and the vacuum distilled

oil are presented to show the characteristics of crankcase drainings as they may be

entered into an industrial fuel stream with varying degrees of processing (decanting

to vacuum distillation), the latter removing substantially all of the contaminants.

For comparative purposes, the D-396 specification for #5 light industrial fuel is

presented.

In this case, the flash at any level of processing is above the D-396 minimum;

however, the water and sediment, in both the raw and dehydrated drainings are substantially above the maximum specified in D-396

27
The ash shown for raw drainings is typical and is improved minimally by dehydrating, but does conform if processed by adequate means.

Our experience indicates that most crankcase drainings are presented as #5 fuel

and, in this instance, come into spec only after having the extraneous materials

removed

The viscosity index is reasonably representative of both raw drainings and processed drainings, although the viscosity index is not a consideration in the D-39o

specification. This, incidentally, is not a finished base lube oil, but little

additional processing is required.

The sulfur, while generally' legal and typical of crankcase drainings, is improved

by vacuum distillation and does not conflict with most requirements established by

regul ation

On the assumption that BTU content would be interesting, we arranged to have the

analyses made on the drainings containing 5 percent water and those further processed.

As you see, there is not a significant variation from the usually designated range

for fuel oil (this is not an ASTM designation)

For the materials designated as raw drainings, dehydrated drainings, and vacuum distilled oil on the previous slide, we ran a spectrographic analysis on each and

also an analysis of a typical water sample drained from a waste oil collection truck

loaded with crankcase drainings. This latter material represents the free water which

is pumped out of the service station drain tank. These data are shown in table 2.

TABLE 2 CRANKCASE DRAININGS USED FOR FUEL

SPECTROGRAPHIC ANALYSIS - PPM

Raw Dehydrated Vacuum Typical

drainings drainings distilled water

Silver 0 0 0 0 Sodium 160 140 6 8,000

Zinc 1 ,100 1,000 2 1,300

Copper 50 40 6 18

Aluminum 33 28 2 74 Barium 200 160 4 230

Nicke

3 2 0 26

Chromium 27 23 0 10

Calcium 1,000 1 ,100 0 2,200

Iron 750 720 2 1,050

Silicon 47 40 4 100

Tin 20 17 0 340

Lead 7,800 6 ,900 13 550

Phosphorus 900 800 50 2,100

Boron 52 38 1 440

Magnesium 430 400 0 1,000

Vanadium . 5 4 3 20

Molybdenum 7 6 0 28

Manganese 42 39 3 65

Cadmium 2 0 0 37

Titanium 5 1 0 45

Mercury, ppb 0 . 88

It is interesting to note on the oil samples that dehydration of the raw drainings appears to lower, although minutely, some of the metallics. The most significant

numbers, of course, are lead, calcium, zinc, magnesium, and barium as they relate to accumulation and ashing. Vacuum distillation or other effective processing will re- move a substantial amount of the material.

Another comment about the water analysis. This phase is generally overlooked

when discussing the processing or non-processing of crankcase drainings for fuel; and,

since the water represented here is not bound up in an emulsion, it is easily decanted

either directly from the truck or from a settling tank.

28
j Table 3 shows the materials in the water as illustrated in table 2 and compares

i that with maximum limitations acceptable to the greater Chicago Metropolitan Sanitary

District (MSD) sewer system and also for discharge directly into streams under the

j jurisdiction of the MSD. The quantities are expressed in parts per million, except

for mercury near the bottom of the list which has a maximum acceptability of one-half

part per billion.

TABLE 3 MAXIMUM CONCENTRATIONS IN WATER ACCEPTABLE FOR

DISCHARGE - PPM^

Greater Chicago Metropolitan Sanitary District

Water from

drain oil Sewer Streams

Barium 230 2 2 Silver 4 0.1 0.1

Boron 440 1 Copper 18 3 1 Cadmium 37 2 0.15

Chromium -Total 10 25 23

Iron 1,050 50 2 Nickel 26 10 1 , Lead 550 0.5 0 .1/0.5°

Mercury - (PPB) 0 .88 0.5 0.5

Zinc 1 ,300 15 1 Manganese 65 1 Hexane Solubles 250 100 15

^ Except mercury, as noted

State streams limits

The parts per million found in water from drain oil may or may not appear significant when looked at individually. They do become very significant when compared with

the maximum levels of acceptability and must be taken into consideration in designing

an oil/water separation and water ^processing system for handling materials of this

type . Obviously, it is no longer acceptable to use a convenient ditch or empty lot to dispose of what I would term "process water;"

Earlier tables showed crankcase oils processed through a vacuum still and the

change in both properties and level of contamination. The data in table 4 show

typical properties of the still bottoms consisting of some hydrocarbons, and the

additive package remnants including V.I. improvers, pour-point depressants, and the

like. The material poses some rather interesting considerations, although the ash

level places it far outside the consideration of being used in a fuel product.

TABLE 4 VACUUM STILL BOTTOMS FROM CRANKCASE DRAININGS - TYPICAL PROPERTIES

Viscosity at 210 °F, SSU 5,000 + 500

Viscosity at 210 °F, Brookfield No. 2 Spindle rpm 1,100 CPS + 50

Pour point, °F. + 20

Flash COC, °F. 600 + Carbon residue, ASTM D-189 24%

Ash 141

Odor None

Sulfur 1.37

T.A.N. 4.0

. T.B.N. 0.9

PH 5.8

29
A spectrographic analysis of the still bottoms (table 5) indicates the high

concentration of the metallic components, particularly lead.

TABLE 5 VACUUM STILL BOTTOMS FROM CRANKCASE DRAININGS

SPECTROGRAPHIC ANALYSIS

Silver 0 Zinc 3 ,500

Copper 160

Aluminum 230

Barium 1,400

Nickel 10

Chromium 100

Calcium 7,000

Iron z , 000

Silicon 550

Tin 140

Lead 15,000

Phosphorus 2,000

Boron 10

Magnesium 1,300

Vanadium 0 Molybdenum 10

Manganese 70

Cadmium 0 Titanium 70

As a commentary, it is interesting to note that the lead level in crankcase I drainings is beginning to decline, although not dramatically as some are inclined to \ believe. My information shows that about three years ago the lead level in crankcase i drainings was about 1 percent by weight, and currently it has decreased to about i 0.8 percent, a change of approximately 20 percent.

| The data in table 6 are from a rather interesting situation where crankcase | drainings were offered at the height of the energy crunch as recycled, reclaimed lube | oil which correlated closely to a light #5 fuel. These data show the specifications I quoted, an analysis of a sample taken from the material being offered, and a compari- ! son with the ASTM D-396 specification. '

TABLE 6 FUEL OIL FROM CRANKCASE DRAININGS

(LIGHT NO. 5)

Quoted Actual ASTM D-396

API gravity at 60 °F 25.2 27.1

SSU viscosity at 100 "°F 240 148 150-300

Pour point °F. -5 -50

Flash, °F. (Pensky-Martins) 182 128 130

Sulfur, % 0 .35 0.36

Ash, % 0.48 1.44 0.1

Water and sediment, % 7 1
A comparison of viscosities, pour points, and flash showed a high degree of

dilution, which is not uncommon in either crankcase drainings or waste oils from

industrial operations. This, of course, dictates that necessary precautions be

observed to avoid endangering both employees and equipment.

The ash values are questionable, and the water and sediment level in the actual

sample is about typical for decanted drainings.

Finally, table 7 shows spectroanalysis on samples taken from boilers which had

been fired almost exclusively on waste oil fuel. The boilers were taken out of ser- vice for cleaning, due to the high concentration of deposits in the equipment. It

is interesting to note the high level of metals in the deposits and the variations

between types of waste oil used. As an example, in the second column, it is apparent

that a significant volume of crankcase drainings were used as fuel because of the

high lead concentration, lead being approximately 10 percent of the weight of the

deposits

.

TABLE 7 SPECTROANALYSIS ON' SAMPLES OF BOILER DEPOSITS (PPM)

(WASTE OIL FUEL)

1696 1872 1866 1868

Zinc 60,000 3,800 1,400

Copper 12,000 3,150 135 150

Nickel 2,500 2,000 105 90

Chromium 200 1,250 150 150

Calcium 84,000 8,850 114 ,000

Iron 12,000 10,500 18 ,000 2 , 850

Silicon 3,700 9,600 11 ,000 8,250

Lead 6,000 100,000 570 620

Phosphorus 160,000 33,000 18,800

Magnesium 15 ,000 530 950

Vanadium 3,700

Sodium 3,600

31

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

DISCUSSION

SESSION II. USED OIL REUSED AS FUEL

The first area of discussion in this second session was why burning used oil

should be considered as oil recycling. Most people agreed that burning was not the

optimum end use for this material. However, any time a waste material is used more

than once it is being recycled. The question of whether this type of recycling is

I the best use oT existing resources is an entirely different question and depends on

j a number of factors, including whether existing resources of virgin lubricating oils

are being used to the maximum or not. If current lubricating oil virgin stock is

' being reformed or cracked to form fuel oil or gasoline or something else, then the resource conservation aspect may not really be relevant here. Appropriate consideration must also be given to energy conservation and environmental pollution, however.

A second area of concern was expressed about the environmental aspects of

emissions from burning used lubricating oils, especially the lead emissions (automotive used oils currently average 0.8 percent to 1.0 percent by weight of lead],

along with other elements added as additives (zinc, phosphorus, calcium, magnesium,

barium, etc.). A more recent concern may be the element manganese, which is now

j replacing lead in certain types of gasoline. Since there are no trace element test

! methods currently required in existing virgin fuel oil specifications, this is an

; area which requires consideration for recycled oils used as fuel. Part of the problem

of lead and/or heavy-metal emissions is that the Environmental Protection Agency

(EPA) currently does not have ambient air quality standards, as will be described in

a paper in the conference. Therefore, even though some people were concerned about

the emissions while burning used oil, they did not actively consider this a restriction

since there were no existing regulations. It was pointed out by one speaker that the

Federal Government is currently going out on bid for a large quantity of fuel oil in

which the restrictive clause in the specification eliminating recycled oil has been

removed. It was indicated that these bids will be evaluated on an "as is" basis, as long as the product meets all other existing specifications. These specifications

would limit the amount of non-processed used oil' which could be blended with a No. 2 fuel oil, for instance, and still meet the American Society for Testing and Materials

(ASTM) specifications. However, apparently up to 30 percent or so of non-processed

used oil could be blended with a No. 6 fuel oil and still meet these existing ASTM

specifications. It was also mentioned that this type of procurement may result in

problems if a No. 2 fuel oil were purchased which has a used oil component if that

used oil were from a gasoline engine. This is so because in many cases at government

installations the diesel fuel oil is stored together with No. 2 fuel oil, and it is

known that lead from used gasoline crankcase oil is very damaging to diesel engines.

The discussion also centered around using a test method such as ash in order to evaluate the metals content of a fuel oil/used oil blend. There was a variety of

opinions on this matter, some of the persons feeling that the ash specification

should only cover those components of the fuel which actually create an ash in the

end-use situation, thereby evaluating material buildup in the burner situation. The

feeling was also expressed that the actual total ash content is of concern because

of the potential effect on different types of combustion systems, such as erosion in

I the burner itself, or because of the effect on some types of furnace materials, such

I as refractory bricks.

j In the ensuing discussion, the question was brought up as to whether the National

Bureau of Standards (NBS) will actually be setting specifications for these materials.

The opinion was expressed that the NBS responsibilities include developing test procedures and forwarding these test procedures to the Federal Trade Commission (FTC)

for implementation by the FTC. However, it was also acknowledged that this implies

providing technical expertise to the FTC in the evaluation of these test procedures

as applied to oils. It was felt by several NBS representatives that the ideal situation would result from the cooperation of ASTM specifications committees and/or the

I Federal specifications people in providing the necessary specifications providing for

I effective utilization of recycled oil products. To this end, conversations have

j already been initiated between NBS personnel and ASTM and the appropriate Federal

I specifications personnel.

33
One point of discussion that was brought up was whether NBS had the right to con-l

sider limiting factors for used oil reused as fuel in light of EPA not having set suchi

regulations. It was then pointed out that the enabling legislation under which the

NBS Recycled Oil Program is functioning states "substantial equivalency" to the virgin;

end product, and, therefore, tests are required which will provide a recycled oil pro-|

duce which is essentially the same as a virgin oil product. It was also discussed i that there were available EPA studies which indicated that when straight crankcase

j drainings were used with appropriate environmental controls (e.g., venturi scrubbers,

bag houses) the actual emissions were drastically reduced and apparently fell within

the range expected from virgin oil use. It would thus seem that under certain conditions this type of burning would be acceptable. A comment was also made that a court

decision exists which establishes that dilution of an environmental pollutant is not j a valid way to circumvent EPA emission regulations.

There was also considerable discussion about the increased maintenance that ] apparently results from combustion of used oils when such used oils have not been pro-|

cessed to remove debris and inorganic contaminants. Since the only current EPA | requirements are in the form of particulate emissions, the scrubbers mentioned pre- I viously apparently do an efficient job of removing these particulates and, thus, fall ' within the current environmental regulations. In addition, the use of used crankcase j oil for wetting down powdered coal in coal-fired power plants has received some , investigation. According to one report, this appears to be an acceptable way for | disposal of used oil due to the effective particulate and other environemntal , pollution controls on coal-fired power plants.

Finally, the discussion ended on the subject of whether the environmental con- siderations in disposal of the light ends and the heavy ends of the processed or re- refined oil (light ends including primarily the water removed from the used oil, heavy

ends being the sludge remaining after processing) did not result in a greater problem I than existed previous to the reprocessing of the used oil. Several participants spoke' on the success that they have had in eliminating or cleaning up these supposedly | environmentally very bad products. In particular, it was pointed out that since all \ of these by-products existed in the original material anyway, it was therefore

difficult to see how separating and concentrating these away from a useful material

resource would, in fact, be creating an additional problem that did not exist in the

first place. I

34
SESSION III RECYCLED INDUSTRIAL AND HYDRAULIC OILS

35

1 National Bureau of Standards Special Publication 488. Proceedings of

I a Workshop on Measurements and Standards for Recycled Oil held at NBS,

I Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

ASTM TEST METHODS FOR INDUSTRIAL OILS

Lowrie B. Sargent, Jr. Aluminum Company of America

Alcoa Technical Center

Alcoa Center, Pennsylvania 15069

j With all due apologies to Mr. Becker, I was not really certain what I was going

I to talk about this afternoon until this morning, so I wrote a speech. With your permission, I will try to wear two hats, too. I would like to tell you a little about

Alcoa's program, but I will speak principally about the American Society for Testing

and Materials (ASTM) and how it may interface with the Bureau's Recycled Oil Program.

Alcoa is very pleased to see the National Bureau of Standards' (NBS) program

getting underway. We have been committed to conservation of petroleum energy sources

for a long, long time. We think this is a necessity, we think we have to do it. We

have spent a lot of money in the last few years developing techniques and methods so that we could recycle used materials. Admittedly, most of the volume of used oils

I is recovered in-house. Our industry, not just Alcoa, since its beginning has had a

, program of recycling rolling oil as an indication of our interest. These are all

1 circulating systems; the materials are filtered, reclaimed, and reused continuously,

we hope for a long period of time. When we have to dispose of materials because of

some unforeseen circumstance, e.g., if we have something that has gotten out of hand,

we try to rectify this in-house, also. As a last resort, we go outside for information. We are doing a great deal of this.

I I might mention, because we were talking about burning fuels this morning, that

I we have adopted a policy at Alcoa that we will burn waste oil only as a last resort.

We would much rather use it for something more valuable than fuel oil. Much of the

oil that has to be reclaimed is intrinsically more valuable than fuel oil. We cannot

see the point of burning this used oil unless there is absolutely nothing else we can

do with it. So, we will be watching the NBS program as a corporate thing because we

are very much in favor of it, and we will cooperate in any way we can.

I looked around this morning, and it looked to me almost like we were reconvening

ASTM Committee D-2 because many in the audience are faithful D-2 workers.

For those of you not acquainted with D-2, I might explain our relationships. I was chairman of Committee D-2 for nine years until they got tired of me about a year

ago. I have been on the Board of Directors of ASTM for the last two years, so I can speak from both standpoints. As was mentioned several times this morning, by

Dr. Ambler and by others, there has been a very close relationship between NBS and

ASTM- -not just in Committee D-2, but ASTM in general. Mr. Becker's boss, Dr. John D. Hoffman, is on the Board of Directors of ASTM. I have sat with him on the board for

the last year-and-a-half or two. I know he is very much interested in ASTM activities.

We have had many NBS people in ASTM in the various committees, including D-2, and we hope that continues. We have an on-going program with the Federal agencies in all

j aspects of standardization. Some of you may know that a few years ago we had a

I president of ASTM who was a Federal employee, and he has been heading up an interagency

committee to do more about standardization; and, of course, we have been getting a lot

of input from him.

As many of you know, ASTM is committed to the development of test methods and

specifications. This is our business; we are in the business of standardization. As

you also know, many of the test methods used by yourselves and other people in this

whole field are ASTM methods; and, if you remember the table Mr. Becker used, I believe

the majority, if not almost all, of the methods listed were ASTM methods. We hope this

^ will continue.

' ASTM reacts from needs. We do not generate a need; hopefully, we react to needs

expressed by somebody else. I would hope that if there is need in this area, ASTM

I will react to that need. This means that you have to participate. One of the things

j that disturbs some of us is that we will have somebody or a group of people coming to

37
ASTM saying, "We need test methods in this area," and they expect ASTM to do it. I am'

not sure what they think ASTM is. They will come in and say they need something, then!

walk out and we do not see them again. Apparently, they think there is a corporate

body somewhere in the ASTM which works and does all this business for the government,

and that is not so. It is you people and other people who have the need who are goingto do the work. So, if you are not prepared to work toward the efforts, then do not ' come to ASTM because you are not going to find some anonymous group to do the work for

you

I was supposed to t'alk about industrial oils, but much of what I was going to say

has already been mentioned by the others who have already spoken. Therefore, I would

like to discuss some of the ways ASTM could interface with people involved with I recycled oil .

I We do not have a committee in D-2 specifically for recycled oil, and I do not

know whether we will. That is yet to be determined. D-2 is made up of a number of

committees and is generally broken into two general categories: the so-called product'

committees (committees on turbine oils, industrial oils, etc.), and the research and j development committees which are structured differently and which do what is commonly | called the scientific work in D-2. Several of these committees now have subgroups and i subcommittees which are working on recycled oil and recycled products. This is still • somewhat in its infancy, and I am sure it is going to grow. Just how it is going to I be structured eventually has yet to be determined.

I am certain that you will find that many of the existing test methods are going : to be able to be used, as they are, for recycled oil. I am sure we are going to find

we are going to have to change some of the others. We would hope that this will be

done within the confines of the ASTM.

I One of the things going for the ASTM is the fact that we develop these standards ' by the so-called consensus method. Hopefully, the producers, users, and consumers get!

together in all these matters and the final result is that they agree on acceptable

methods, tests, and specifications. We process the standardized tests to the American

National Standards Institute, as you know, to become the national standards and to the

International Standards Organization to become international standards. Consensus

methods are going to have considerable weight in the legal aspects of standardization.

I am quite sure that methods that are not developed by this method will not be looked

upon legally, eventually. ASTM regards this as kind of a home for you.

I might mention that the next meeting of ASTM Committee D-2 (if you will allow me

a bit of a plug) is going to be in New Orleans, so I hope it will be a little bit warmer than it is in Gaithersburg this morning. That will be the week in December

starting December 5. I am sure that the problem of recycled oil tests is going to come

up in those meetings, and I would like to see as many of you there as can possibly get

there. It is a nice place to go, particularly in. December.

38
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

I Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

ji

I INDUSTRIAL OIL RECYCLING AT CHRYSLER

William Katzenstein

Chrysler Corporation

Chemical Division

5437 West Jefferson Street

Trenton, Michigan 48183

I am very fortunate to have a lot of experts here today. I joined Chrysler about

10 years ago; and, long before I came aboard, Chrysler already was recycling oil.

Mr. Swain, who was involved in it initially, and Mr. Mullinger, who had been involved

in it long before I came aboard in the re-refining aspect, are both here. So, I am going to have a lot of people to help me today if I do not have the answers. Basically, when the energy crunch hit in 1973, although Chrysler had been doing a

j lot of reclaiming, they decided to take another look at this program. In October 1974,

I a committee met to draw up new ways of improving our recycling; and, after many meetings, a new program emerged. In February 1975, the Chemical Division of Chrysler

Corporation was given the job to manage tht total recycling program involving primarily

I waste oil sludges. Basically, the oil sludges were converted to oil by removing solids

and water; and this cleaned-up oil was returned either as various reclaimed basestocks

to meet original specifications, or else it was returned as a re-refined hydraulic

fluid. As shown on figure 1, the manufacturing plants represent either our stamping

plants or our general manufacturing plants. The waste influents are collected and go

to our environmental treatment facilities which are waste treatment facilities. The

j material is treated sufficiently in order to generate a good water that can be dis-

! posed of directly into the sewer. That is the primary reason why we have these

I facilities -- to generate a good water which meets required specifications. It just

turns out that today this by-product that we get, which is an oil - containing sludge,

has a value. The water goes to the sewer and the oil sludge is taken to a reclaimer

who will then break the sludge, through various proprietary processes, remove the

solids, remove the water, and will return the products to the Chrysler Corporation

where they are formulated into industrial lubricants, cutting oils, hydraulic oils,

etc. We now also utilize reclaimed oils for making water in oil emulsions and

hydraulic fluids. These products are returned to our plants for reuse. Excess re- claimed oil is diverted to a re-refiner. He, in turn, will then make re-refined

I hydraulic fluid from it and return it to Chrysler.

One of the important things we talk about is segregation. In our stamping plants,

for example, we generate a completely different type of fluid than we do in our general manufacturing plants. These press oils are very high in viscosity; and, since

the stamping plants usually do not have any environmental treatment facilities, they

basically have large tanks where the influent is collected. By heating and by

letting the material stand, the water is separated and drained off. This water is now hauled to a waste treatment plant for processing. The oil is taken to a reclaimer who,

in turn, will then break out the contaminants and blend it with other oils for reuse. What we are trying to do is keep it from being mixed in with other oils. At this time,

it is a difficult problem and we are not having very much success. Also shown in the figure is a return water from the reclaiming. The Chrysler

Corporation feels that as long as the water that is generated in waste oil sludge goes

to reclaimers, even though the reclaimer does not segregate from all the different

feedstocks, that those volumes equal to what he gets are returned. He will therefore

return water equal in volume to what he picks up.

A typical stamping plant reclaim oil that we get will run in the viscosity range

of as high as 600 SSU to 800 SSU. When we pump it out of pits, where it is just

purely from the presses, it is still a very good oil. We just received a sample in

last week that was running close to the viscosity of the virgin oils (1450 SSU) . If

somehow we could segregate this, clean it up through a simple filtration method, it

could be put right back into a plant and eliminate the 20-percent to 30-percent loss

factor currently obtained through re-refining.

39
CHRYSLER

MANUFACTURING

PLANT

WASTE

INFLUENTS

return water ENVIRONMENTAL

TREATMENT

FACILITIES

RECLAIMER (special viscosity oil)

SPECIALTY

PRODUCTS

CORPORATE USE

[SEGREGATED OIL)

water to sewe

SECONDARY

TREATMENT

FACILITY

RE-REFINER

CHEMICAL

DIVISION

BY-PRODUCTS

FROM

REFINING

HYDRAULIC

OIL

FORMULATED

SPECIALTY PRODUCTS

CORPORATE USE

CORPORATE USE

PUBLIC SALE

FORMULATED

SPECIALTY PRODUCTS

PUBLIC SALE

Figure 1. Industrial oil recycling process at Chrysler.

40
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

INDUSTRIAL OILS: DESCRIPTIONS, ADDITIVES, AND TEST METHODS

John W. Swain, Jr.

40 Denton Road

Wellesley, Massachusetts, 02181

First, since this is a workshop on oil recycling, I believe we should define the

processes used in oil recycling - -reclaiming , reprocessing, and re -refining- -which are used to recycled used engine oils and industrial oils.

Reclaiming is the process which removes large particles, sludge, and water using

heat, gravity settling, or simple filtration.

Reprocessing goes one step farther and employs chemical treatment (usually acid

or alkali), heating to 160°F to 200°F. This removes solids, water, and most of the

original additives and compounds formed during use. Re-refining has three steps: pretreatment to remove solids, water, most of the

original additives and compounds formed during use by chemical and/or solvent action;

distillation, usually with activated clay in-situ and steam, at temperatures ranging

from 500°F to 65G°F to remove light ends, color bodies, and other compounds not

I removed by pretreatment; and post treatment to remove the spent clay. This step may

also include further steam stripping and neutralization. Currently, there is work

being done using the hydrotreating process replacing clay.

I Most of the emphasis on oil recycling has been directed to used engine oils, with

j little attention being paid to industrial oils. The fact is that use of industrial

j oils has been increasing at a higher rate than automotive and aviation oils. For

example, the sales of these oils in 1967, 1973, and 1975 were: Million Gallons/Year

1967 1973 1975

Automotive and aviation oils 1,170 1,294 1,271

Industrial oils 1,450 1,883 1,586

The industrial oil sales for 1975 were down because of decreased industrial production.

The recoverability factor of industrial oils should be higher than automotive

since there i3 a smaller volatility loss and no do-it-yourselfers.

Those not familiar with oils seem to think that there is a great difference

between automotive lubricants and industrial oils. Actually, the major difference is

in the additive package rather than the basestocks. For example, an oil with a viscosity of 170 at 100°F SSU can be used to produce engine oils, hydraulic oils,

cutting oils, bearing oils, quench oils, gear oils, and many more. There are several fluids used in industry which properly are not oils. These include the synthetic machining and process fluids, as well as non-flammable hydraulic

fluids. However, the use of these is relatively small compared with use of other oils

by industry. '

It is generally thought that used industrial oils can be recycled more easily

than used engine oils since the oils are less contaminated and the use of the oil is

less critical. Neither of these propositions is necessarily true. Used industrial

oils segregated at source can be reprocessed or re-refined more easily than used

engine oils. However, the large volume sources of used industrial oils are the waste

I water treatment facilities of large manufacturing plants. These present problems

! which few re-refiners want to handle.

Re-refined oils are being used to produce hydraulic oils, cutting and grinding

oils, drawing oils and compounds, and forging oils and compounds. Often, all of these,

41
except hydraulic oils, can be made from effective reprocessing. I have set up seven categories of industrial oils and include some estimated sales for 1975.

jj Hydraulic and Circulating System Oils (314 million gallons) - Hydraulic oils^

have viscosities ranging from 150 to 900 at 100°F SSU. Today, most of the oils con- tain additives to prevent rust and oxidation, to decrease pump wear, to reduce leakage

to reduce foaming, and sometimes pour point depressants and viscosity index (V.I.)

improvers

Most of the tests specified for hydraulic oil are those using the American

Society for Testing and Materials (ASTM) procedures. These will include gravity, viscosity and viscosity index, flash and fire points, pour point, total acid and base

numbers, sulfated ash, copper cori:osion, emulsion number, oxidation rate, and corro- sion and foaming. While the ASTM D-943 is often used to test oxidation, many of the

larger com.panies use other simpler bench tests such as controlled heating and air

exposure of 300 ml to 600 ml of sample. The volatility loss, sludge generation, and

acid number increase are measured, as well as observation of "gum" on the beaker wall.

Many hydraulic oil specifications require pump-wear and seal-swell tests.

[ Circulating system oils are used to lubricate bearings and sometimes gears

Those lubricating bearings may contain rust and oxidation inhibitors, defoamers, V.I

improvers, and extreme pressure (EP) agents. Again, ASTM procedures are used for f determining viscosity; V.I.; flash, fire, and pour points; total acid and base numbers;'

sulfated ash; saponification number; foaming characteristics; rust and corrosion; and

copper corrosion, among others. Load and wear tests may also be specified. These may

use equipment as the Falex, Timken, or Shell Four Ball test equipment or others

devised by the user. •[

Metal Working Oils (145 million gallons) - Metal working oils include cut- f ting and grinding oils, drawing oils and compounds, forging oil and compounds, and

metal rolling and forming oil and compounds. Cutting, grinding, and drawing oils are divided into two categories: straight and emulsif iable

The straight oils contain sulfur, chlorine, and phosphorus compounds, fatty f oils and esters, and heavy metal soaps. The straight oils have a viscosity range of

as low as 45 at 100°F SSU for honing and lapping oils to several thousand seconds at

100°F for drawing oils. Most of the tests use ASTM procedures for viscosity; flash,

fire, and pour points; copper corrosion; sulfur; chlorine; phosphorus; and fatty oil,

ester, and heavy metal soap content. In some cases, sulfated ash determination is

required, as well as the saponification number. There may be user-modified tests of

the above, as well as bench machinability and load tests. Shop trials of these oils

are almost universally required.

Emulsifiable oils in use are mixed with water to provide a high rate of

cooling. These contain soaps and emulsifiers and varying degrees of EP and rustproofing additives and wetting agents to reduce surface and interfacial tension. Test

requirements include viscosity; flash, fire, and pour points; sulfur; chlorine;

phosphorus; fatty oil and soaps; and emulsifier content of the oil before mixing with

water. Bench tests are also made for emulsion stability, foaming, rust-proofing, wetting, hard-water stability, particle suspension, and tramp oil emulsifying. While

ASTM tests are widely used, there are more specific user laboratory tests than on hydraulic and circulating system oils. Occasionally, load tests are specified. i Drawing and Forging Compounds - These products range from compounded

straight oils , often with high viscosity, to oils containing solid lubricants, for \ example, molybdenum disulfide, graphite and mica, to compounds containing soaps and

oils and solid lubricants. Invert emulsions containing solid lubricants are also

used. The trend, however, is away from the high soap, pigmented compounds, and invert,

emulsion products to highly compounded oils. The additives usually employed are sulfur and chlorine compounds, fatty oils and esters, and heavy metal soaps.

Testing of these products requires the determination of viscosity, flash and

fire points, rust and corrosion, emulsion stability, water, solid lubricants, soap,

emulsifier, sulfur, fatty oil, and ester content. Tests for welding and metal - coating

compatibility, as well as load carrying ability, may also be required. While many of

these tests follow ASTM procedures, the diversity of uses and individual operational

requirements have established many specific in-house tests. I Rolling and Forming Oils and Compounds - Here again, there is a wide variety

of lubricants used. Metal rolling uses fatty oils, straight compounded petroleum oils,

and emulsifiable oils. Forming operations such as wire drawing require products ,

42
ranging from emulsif iable oils to such materials as aluminum stearate and solid

'lubricants. ASTM procedures are used where applicable, but many user-developed

j tests are employed.

Process Oils (402 million gallons) - Process oils include quenching oils,

" test fluids'^ transformer oils, oils which become part of the product, rust-proofing

oils, ink oils, and rubber and plastic oils.

These oils have special characteristics such as iodine number, KB value

(Kauri Butanol) , dialectic property, and tensile strength of rubber and plastic

products. The usual tests such as gravity, viscosity, and flash, fire, and pour

points are specified. Most of these are covered by ASTM procedures, although users

i usually have in-house analytical procedures.

I

I

i Specialized Lubricants - In this category I have arbitrarily placed

I spindle oils , gear lubricants, and slide and way lubricants.

I Spindle oils usually have a relatively low viscosity (70 to 150 at 100°F.

I SSU) and contain rust and oxidation inhibitors. Gear lubricants have a wider viscosity range and contain EP and anti-wear additives as well as rust- and oxidation-

' inhibitors, defoamers, and "tackiness" agents. Slide and way lubricants range in

.1 viscosity from 300 to 900 at 100°F. SSU. They contain EP and anti-wear additives as

'j well as "tackiness" agents.

I In addition to standard tests such as viscosity, flash and pour points,

I others such as panel retention and load and wear for slide and lubricants, wear tests

for spindle oils and load and wear tests for gear lubricants are usually required.

Again, many of these follow ASTM procedures but also employ in-house test procedures.

Test Oils - Many components of vehicles and other equipment are tested

after final assembly . These include automatic transmissions and power-steering

equipment. Usually these use the same oil as that specified for operation. These,

jthen, are subjected to the same tests as the operating lubricant. Some, such as the

j oil used to test the valve body of automotic transmissions, are modified to simulate

1 operational conditions, e.g., lower viscosity at operating temperatures.

These oils, with few exceptions, use standard ASTM test procedures.

Exceptions would be specialized loading, wear tests, and oxidation tests.

Since this workshop on recycled oils was organized to aid the National Bureau of

Standards in meeting the Congressional mandate to establish substantial equivalency,

I would like to address this aspect.

ASTM and industry test procedures appear to be adequate for determining the substantial equivalency of recycled oils. The buyer-beware principle is not as important

in the industrial area as in the consumer area since it can be argued that these users

are, or should be, aware of their lubrication requirements.

However, I am afraid that manufacturers of hydraulic equipment, gears, machine

tools, transformers, refrigeration units, compressors, and others will raise the same questions which have been raised by engine manufacturers. In some cases, such as hydraulic or compressor oils, the problem of establishing substantial equivalency may

require study. In others, such as cutting and grinding oils, there should be fewer

problems

.

1

43

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, NoVember 22 and 23, 1976. (Issued August 1977)

THE USE OF RECYCLED INDUSTRIAL AND HYDRAULIC OILS AT FORD

J. W. Hunt

Ford Motor Company

The American Road

Dearborn, Michigan 48121

During the energy crisis of 1973, recyclers with fantastic claims pounded on our

door, as I am sure they did everywhere. One major company even offered to set up a reclamation unit at one of our sites, to staff it, and to teach us how to operate it,

saying it could save us money since we could cut down on the purchase of new oil.

We were interested enough to proceed with a shop trial, when the reclaimer backed

off. We really do not know why; we believe they had second thoughts and they were

not quite ready. I also believe we are not quite ready. We are in the business of

making automobiles and do not really want to get into the oil reclamation business.

At Ford, our suppliers have been successful with recycling

Turbine oil.

Compressor oil,

Cutting fluids,

Hydraulic oil, and

Synthetic fire-resistant hydraulic oil.

The most notable successes are in reclaiming cutting fluids and hydraulic oil. For

one plant, 60 percent of all the cutting oil purchased is recycled; in another plant,

j 60 percent of all petroleum oil purchases end up being returned for recycling.

I think it is best to start out with how Ford does business. Ford has what is

called the "M-Numbered" system for "Maintenance" materials. Any maintenance material

that Ford buys in volume has a written specification furnished to Purchasing in order

to obtain competitive prices.

Ford has three specifications for hydraulic oils:

High viscosity index mineral oil with rust and oxidation inhibitors,

Antiwear paraffinic oil, and

Seal-swell oil with antiwear additive.

All approved sources have met the specifications; and, of course, recycled oil must

meet those same specifications. The primary test is one of wear, and all who seek

approval must pass a pump wear test conducted by our Manufacturing Process Laboratory.

The Ford Pump Test is run for 1,000 hours at 2,000 psi using a Vickers 104 pump,

and the maximum ring and vane wear cannot exceed 125 mg. Of five reclamation candidates, three passed with 70 mg to 80 mg of wear, one exceeded virgin material with

I only 37 mg of wear, and the last failed with wear of 256 mg at 100 hours. This con-

\ firmed that the recycling is practical and the use of recycled oil will, when done

properly, meet our needs.

The u^e or disposal of contaminated oil at Ford is accomplished by

Recycling: preferred, based on favorable economics and the conservation

of a natural resource; Burning as fuel: not preferred because of potential of contaminants

affecting stack emission levels and reducing the boiler efficiency;

Giving it away or paying to have it hauled away: not economically

sound, least preferred method, and only done when other practical

methods are not available.

The cost advantage lies in the recycling process which can produce an acceptable

product at five-sixths the cost of virgin oil. We believe that as more oil is re- claimed the cost advantage will increase. Under today's economics, it may not be cost

45
effective in some company's small plant, but in a larger Ford plant it usually is.

Last year, Ford suppliers recycled over 7,100,000 gallons of oil. However, several

open issues on recycled oil still exist.

Is the Ford specification the same as all other companies'? Will

Ford's oil be mixed with that of other companies and, if so, with

what adverse effects to Ford?

Do reclaimers have the capacity to handle segregated oil? What

are the minimum quantities required?

Is a national standard required? Or, does this drive out competitors?

We do not have all the answers, but we do know that

Reclamation is feasible,

Reclamation is cost effective, and

Reclamation is necessary to conserve a natural resource.

The reclamation (recycling) companies have the expertise, we have the "raw

material," and both of us can benefit through the recycling of waste oils. We do,

however, urge caution on reclaimers making exaggerated claims. For example, based

on one claim, we provided waste oil for reclamation and the returned product was

so bad it almost shut down the plant. This experience is remembered and could

hinder future applications of good systems and techniques.

46
National Bureau of Standards Special Publication 488. Proceedings o£

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

INDUSTRIAL LUBRICANTS, RECLAIMED OILS, AND TEST METHODS

Clark J. Flake

Armco Steel Corporation

703 Curtis Street

Middletown, • Ohio 45043

We have been asked to comment on test methods our company uses to evaluate

hydraulic oils. First, I might say that we are not expert in the field; we have been

working in this area for only a few years. We have developed a feel for performance

tests and evaluation techniques.

We started with fire resistant hydraulic fluids, and the tests shown in table 1 are those that we believe the fluids must pass to meet our service requirements. For

tight recirculating systems (low leakage) , oxidation tests are of considerable importance. Studying the literature on oxidation tests, we came up with 20 different

procedures in a very short time; obviously, there are more methods than agreement.

TABLE 1 PERFORMANCE TESTS USED TO EVALUATE HYDRAULIC FLUIDS^

• Viscosity - ASTM D-445

• Acid number - ASTM D-664 (Armco Modified Procedure)

• Low- temperature cycling (United States Steel Procedure)

• Oxidation resistance

- Inhibited oil oxidation - ASTM D-943

- Rotary bomb method - ASTM D-2273

- Oxidation stability (Federal Test Method 5308.6)

- Cigre method (IP 280)

• Pump test - ASTM D-2882

• Corrosion test

- Rust test - ASTM-665

- Copper strip corrosion - ASTM-130

• Thermal stability (United States Steel Procedure)

^Factory mutual approval required on fire resistant hydraulic

oils .

When we finally got things sorted out, we decided that a combination of the American

Society for Testing and Materials (ASTM) D-943, the Federal Test Method 5308.6, and

the Cigre procedure appeared to provide the most valuable information. We believe

our blend of the three tests works well, but we are collecting more data to evaluate

this. We have little interest in the ASTM test by itself because it requires so much

time to complete, 1,000 hours or more. This is too long.

We also have the rotary bomb oxidation equipment but find it effective only as long as you test fluids made from the same basestock and having the same additive

package. This test does allow you to measure variability within that system. HowI ever, in our experience it is not effective for comparing two products from different

\ suppliers. If you find that a hydraulic oil will pass this test, it is a good oil.

However, if the limits set for this test are too strict, you may find good oils failing it. So we use it for comparing oils of similar types, but not for comparison

I between various kinds of oils.

47
In our estimation, the most important test for hydraulic fluids is the pump test.

Although ASTM says the test should be conducted for 1,000 hours at 1,000 psi, most

people are actually using 2,000 psi at 100 hours, or something similar. It is some- what surprising to us that Ford is testing for 1,000 hours, as to my knowledge we have never had a test continue for anywhere near that length of time.

Other tests which we consider of value in qualifying hydraulics are the copper

strip corrosion test (D-130) and the rust test (D-665) . Generally, most fluids pass

these tests, which do not appear to be overly severe. However, by the same token, if

a failure should occur, it is likely that the use of this oil will lead to system

corrosion problems.

A large quantity of gear oil is used in our plants, and its quality is of extreme

importance because of the value of the equipment it protects. When we started testing

gear oil, the Environmental Protection Agency was requiring a change-over from leaded

products to sulfur-phosphorus compounds. A natural question was whether they would be

as good as the lead compounds previously used. Some of the tests used are shown in

table 2. We also used some of the tests shown in table 1 as well. Our testing program indicated the sulfur-phosphorus compounds to be better than the lead-base products

because of much better demulsibility characteristics.

TABLE 2 OTHER PERFORMANCE TESTS USED ON LUBRICANTS

• Falex wear ASTM D-2670

• Timken extreme pressure test ASTM D-2782

• Demulsibility characteristics ASTM-2711

• Foaming characteristics ASTM D-892

In addition to the previously discussed testing of hydraulic fluids and gear oils,,

the steel industry is faced with evaluation of many other lubricants including cutting I oil, rolling oils, grease, and the like. Further, major efforts have been made to collect and reclaim as much of our fluid losses as possible, and these pose a whole

series of additional problems. I would now like to discuss these briefly.

We are interested in reclaiming and even re-refining of our waste fluids. Our

terminology is a little different than usual, as we use the word "reclaiming" for what

other speakers frequently call "reprocessing." Our plants are scattered around the

country, and each of them has different needs. Our centralized research efforts are aimed at doing what we can to help each of them. For instance, one plant exchanges

its oil waste for re-refined oil, so it requires only a very crude clean-up system. ' One of our southern plants is not interested in recycling oils as fuel; they sell all

their oily wastes. Some other plants have small programs where they catch the leak , coming out of the machine, filter it, and put it back into the same system. We hope

to have more of this in the future. At this point, however, our major reuse of

reclaimed fluids has been for fuel.

Our two biggest plants have cold mills, and cold rolling oils contain about 50

percent fats. These are recirculating systems that are not only periodically dumped, ' but also leak. These oils are collected, along with products from other sources, and

result in about two million gallons per year. It has been a part of our work to [ up-grade these reclaimed oils to that we can reuse them as a more valuable product

than fuel. We have, in a few cases, been successful in these efforts. Our oil reclamation plant using heat, polymer additions, and vertical column clarification produces

a final product with very little water and sediment. Consequently, this reclaimed oil'

has, on occasion, been used for hydraulic oil: In one particular oil reclamation system which is not contaminated with rolling oil and therefore does not contain fats,

j the reclaimed product is a good oil. However, we sometimes get kerosene into this I system and suddenly we have 100 second hydraulic fluid with a flash point of 120°F. ! That is not acceptable at all. We also use reclaimed fluid for oiling coal in the

production of coke. However, our primary aim is to up-grade our reclaimed fluids for 1 use as hydraulic oils or gear oils.

Another possible use is for cutting oil, as we wind up with something like 10 ' percent fats in our final stream. Unfortunately, we cannot use that much cutting oil.i

48
It also appears to be potentially good stock for making greases. We have made a few

experimental batches, and it seems to be practical. Once again, however, we have not

got enough waste to provide grease for everybody, let alone ourselves.

There is one more thing I should mention. We did take a serious look at using

re-refiners. Unfortunately, there are no re-refiners near many of our plants. By the

time we consider the value of the reclaimed oil as fuel, transportation costs to and

from the re-refiner and his fee, it is not economical at this point in time. It appears that such processing is possible, but costs are too high.

49

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

DISCUSSION

SESSION III. RECYCLED INDUSTRIAL AND HYDRAULIC OILS

Session III had five presentations which covered descriptions and uses of test

methods for industrial oils and hydraulic oils, a survey of different types of

industrial oils and additives for industrial and hydraulic use, and descriptions of

I industrial and hydraulic oil recycling at the Chrysler Chemical Division and the

I Ford Motor Compan/. Discussion during this session produced estimates of the volumes

I of used oils generated from metal -working lubricants as approximately 500 million

I gallons per year (tlie largest industrial oil category) and of hydraulic fluids as

, approximately 240 million gallons per year.

I A statement mentioned repeatedly in the discussion concerned the greatest problem

in increasing the level of recycling for industrial and hydraulic oils, that of inplant segregation of the various oils. This is most difficult in older plants which

have not been designed to have separate internal waste screening and which use a

! variety of different types of oils (e.g., cutting oils and hydraulic oils) in highleak systems. Because of the recent increases in virgin oil costs, most new plants

I are including in the design facilities to help in the segregation of these oils.

I Since recycling of used oils is much more economical and reliable if the re-refiner or processor is able to start from a single type of oil, these decisions as to used oil

segregation are being justified on a cost-effectiveness basis.

Another area of discussion was in the final disposal of used oils which are not

segregated and which often, therefore, end up as a conglomerate mixture. Most dis- cussers acknowledged that when they had no other economic way to dispose of them

j these oils were burned for fuel to recover the energy content. Estimates as to the

i various percentages recovered for reuse as a lubricant ranged from approximately

I 20 percent to over 80 percent. A question was also asked as to whether there were

particular difficulties with using waste industrial oils for fuel, since some of them

1 contain fatty components, chlorinated compounds, or high-sulfur contents. The

I response indicated that for use in coal-burning power plants, either mixing with the

j coal or spraying on to the coal, this was no problem. Many types of oils can also be

' mixed directly into the virgin fuel oil and be burned in fuel oil burners. One person

discussed a problem that arose when used cutting oils containing metal fines tended to erode the burner nozzles and cause extensive buildup of deposits in the combustion

chambers

.

Several people reported using several types of industrial oils interchangeably in

order to eliminate contamination of one with the other. For example, in some construction equipment, an engine oil is used in the hydraulic system in order to have compatible oil systems. In another case, a recovered material which had only minor

reprocessing was blended with a virgin hydraulic oil and reused in a high-leakage

hydraulic system. Since the residence time in this particular hydraulic system was

rather short, it was felt that these oils were more than sufficient for that particular

I

service

.

j Several industrial companies which engaged the services of re-refiners to separate

and re-refine their industrial oils essentially tell the re-refiner what type of

! industrial oil they wish to have back. Since the re-refiner produced, in effect, a basestock material, it is primarily the additive package and the eventual use which

determine whether the product is satisfactory or not. Apparently, from the discussion,

I many plants are using internally reclaimed or externally reclaimed or re-refined

[industrial oils, either blending with virgin oils or in systems that have been

i evaluated with these types of oils.

There was a great deal of discussion on the oxidation stability tests used in

: evaluating both virgin and re-refined oils, and a great deal of antagonism surfaced

: towards the 1,000-hour American Society for Testing and Materials (ASTM) D-943, Test

!|for Oxidation Stability of Steam Turbine Oils. Most large companies have apparently

pdevised their own bench oxidation test and, thus, seldom use the D-943 method. It was

istated that many of these bench tests apparently correlate well with plant operation,

ii and obviously their actual operations requirements are the primary criteria which need

jlto be met. Some of the_ conditions that were varied in order to increase the severity

51
of oxidation tests include raising the temperature to 135°C (275°F) or 160°C (32S°F)

using oil soluble metal catalysts, or sometimes to bubble oxygen gas through the oil

instead of air or no gas. Particular measurements which are taken during or at the

end of the test include percent weight loss due to the volatility of light ends,

viscosity increase, sludge formation, etc. Everyone seemed to be agreed that an effective replacement for D-943 would be very welcome for evaluating industrial oils.

Another area of discussion was on the suitability of re-refined crankcase oils

for industrial uses. The consensus of the discussion seemed to be that a fully re- refined crankcase oil was essentially a high-quality base oil and could be formulated

to meet any number of high-quality industrial oil specifications, including hydraulic

oils, various lubricating oils, and cutting oils. It was also expressed that once

the higher-quality lube oils were contaminated with the lower-quality oils such as press oils and rolling oils they could still be reclaimed for primarily lower-quality

uses such as the metal -working oils.

The question was raised as to what effect the National Bureau of Standards' (NBS)

Recycled Oil Program and the Federal Trade Commission (FTC) would have on the closedloop recycling or re-refining. The reply was that the NBS program probably should not

affect in-plant processing or re-refining at all. Since these products, in effect, do

not reach the open market, it was felt that they would most likely not be considered

by the FTC under any trade regulation requirement developed in response to the NBS

test procedures.

In conclusion, comments by a speaker who was former chairman of the ASTM D-2

Committee on Petroleum Products and Lubricants (and is now a member of the ASTM Board

of Directors), as well as by other participants in the meeting, strongly encouraged

NBS to use ASTM to assist in helping develop needed test methods and specifications.

It was noted that almost all of the methods listed by previous speakers were ASTM test

methods, and it was hoped that this would continue in the area of recycled oils also.

The session discussion closed with a statement that the most important specification for industrial and hydraulic oils is that they must work well in the particular

system in which they are to be used.

52
SESSIONS IV AND V

RECYCLED ENGINE OILS

53

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

DOD EXPERIENCES IN TESTING LUBE OILS

Thomas C. Bowen

U.S. Army Mobility Equipment Research and Development Command

Ft. Belvoir, Virginia 22060

i Today I will review the Environmental Protection Agency (EPA) /Department of

' Defense (DOD) program on re-refined oils, make some general comments on military

I engine oil specifications, and discuss some limited experience the Army has had with

! re-refined oils. The major portion of the time I would like to spend on the EPA/DOD

j re-refined oil program.

1 Essentially, the program consists of looking at the quality of re-refined basestocks and their ability, once formulated, to meet specification requirements. This

will involve the following steps. First, samples of re-refined basestocks will be

• collected. These are the basestocks themselves, not fully formulated oils. Second,

! laboratory analyses, i.e., standard American Society for Testing and Materials (ASTM)

[procedures, will be used to look at various aspects of the basestocks such as physical

' characteristics, re-refining levels, and composition. Hopefully, from this we will

I be able to categorize the stocks. Initially, it was envisioned that three or four

. different categories (good to poor) could be obtained. This may or may not be possible. You could also end up with two categories: one category where oils would not

be considered for any further portion of the program, and another category where it

would be considered feasible to treat the oils with additives to produce a fully formulated engine oil.

In the third portion, we will blend the basestocks with additives and conduct

specification performance tests. These will be the laboratory engine tests, set

! forth by MIL-L-46152. Also, a portion of the program calls for evaluating the field

use of re-refined products. However, this does not involve the oil previously discussed. We have contacted the City of San Diego and are trying to work out a program

to examine vehicles they have operated for approximately two years on a re-refined

engine oil. This is intended to generate some field-performance and tear-down

; inspection data on vehicles operated on re-refined oils.

At the present time, we have 15 samples of basestocks. These have been forwarded

to the U.S. Army laboratory in San Antonio for chemical and physical analysis.

I now want to spend a little more time on the analyses. As I previously stated,

we will be looking at the physical properties, the re-refining levels, and the com- position of the oils. We will be using standard ASTM tests for this work. Tests will

include physical properties, i.e., viscosity, API gravity, color, pour point, flash

point, etc., of the oils. We are not going to address the validity of these tests for

re-refined oil. We will also be examining the re-refining level using tests such as

the neutralization number, carbon residue, total ash, and insolubles. The composition

will be evaluated using tests for aniline point, characteristic groups by clay-gel

absorption, boiling point distribution, and heavy metal content, both wear metals and

j additives

.

I From the Army's standpoint, we would like to demonstrate that you can re-refine

an oil, treat it with additives, and produce a product of acceptable performance.

Also, we would like to show that you can get some variation with re-refined products.

In plain words, two different basestocks treated with the same additive may not

necessarily give the same results. The Army believes strongly in the performance - type

specification which uses the sequence tests. In addition to these sequence tests, we

feel other items are required such as specifying a given viscosity class, compatibility

with other oils, pour requirement of the oil, etc. At the present time, we undoubtedly

are the "bad boys on the block" because our specifications state that re-refined oils

are not allowed. It is not that we do not believe the technology and the capability

are there to do the job. However, from past work we have seen less than satisfactory

performance from marketed re-refined oils.

In 1972, the Army purchased two re-refined products on the retail market and subjected them to the 1-G diesel performance test. I feel this shows the concern that we

55
had within the military towards re-refined oils. The photographs shown in figure 1 compare the typical pass results for our combat and tactical lubricating oil specification MIL-L-2104C with one of the re-refined oils that was tested. You can see

the re-refined product allows excessive deposits. We feel an oil of this quality

would create a serious problem if it were fielded in our equipment.

Figure 1. 1-G diesel performance test results \ comparing a re-refined oil with a MIL-L-2104C oil.

j

I The second re-refined oil tested was in essentially the same condition as the

first, but was not labeled as such. One product failed all tests, and the other pro-

' duct passed only the bearing corrosion test. Since the first product was labeled

j MIL-L-2104C in large letters and in smaller letters "CC-CD" and "SD-SE," as a consumer

I would gather this oil was fully compounded and satisfactory for use in highperformance diesel and gasoline engines. The test data do not substantiate this. It

is not known if these oils were representative of re-refined products in general, and,

therefore, one can only draw conclusions concerning the samples tested. i Where do we go after we finish the program? From our standpoint, we feel there

is still more work to be done. Even though we may demonstrate that an oil can be formulated and will give you satisfactory performance in the tests, there has to be a

' method for controlling the product from batch to batch. At the present time, to meet,

military specifications the base oil must come from the same source and the same refining treatment must be used. For a re-refined product, this would require testing

of every batch of oil produced, which from the re-refiners' standpoint is neither

satisfactory nor economically feasible. Therefore, you would have to try and work | data from this program and, hopefully, the data which the National Bureau of Standards

will be generating in its program into some type of alternate method to accept and

control re-refined oils.

56
National Bureau o£ Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

WASTE OIL RECYCLING- -AN IDEA WHOSE TIME HAS COME

C. J. Thompson and M. L. Whisman

Bartlesville Energy Research Center

P. 0. Box 1398

Bartlesville, Oklahoma 74003

A research project to investigate re-re£ining of used crankcase oil conducted for the U.S. Energy Research and Development

Administration at the Bartlesville Energy Research Center (BERC)

is described with past accomplishments and planned goals. Technology developed at BERC during the course of this investigation

restores used oil to original quality through a vacuum-distillation

procedure that depends upon a solvent pretreatment to reduce

thermally activated coking and fouling precursors. The process

produces high yields of high-quality oil with essentially neutral

by-products that should be easy to dispose of in an environmentally

acceptable manner. Engine-performance data have been obtained on

two oils reclaimed with BERC-developed technology and a commercially re-refined oil with largely successful results. Studies are described that define the hydrocarbon composition of typical re- refinery feedstocks for evaluation of geographical and seasonal

differences. The major hydrocarbon composition of each of 30 feedstocks strongly suggests that the feed to a re-refinery is

sufficiently uniform to produce consistent products with reasonable

quality-control measures.

Plans are presented for future composition studies, increased

in-house processing capability, and the production of 1,000 gallons

of reclaimed oil from the BERC process. Fleet tests, currently in

progress in the State of Iowa, to evaluate the quality of the oil

and the potential savings represented by the use of re-refined

lubricating oil in State-operated motor vehicles are outlined.

Introduction

For years, most commercial, industrial, and governmental agencies considered the

dirty, black oil drained from automobile engines as a waste product and a nuisance, to be disposed of. Now, however, with the increasing realization that the Nation's

supplies of petroleum are limited and dwindling, used oil is being looked upon not as

a waste product, but as a valuable resource which can and should be recycled and

reused

.

In order to determine the significance of this resource, an estimate of the

volume and type of used lube oil that is potentially available is needed. Since there

is no systematic inventory of used lubricating oil in this country, the volume of

available used oil must be estimated from the quantity of new oil that is sold.

More than two billion gallons of new lubricating oils of all types are sold

annually in the U.S. According to recent U.S. Bureau of Mines data, the total lubricating oil demand in 1974 was 2.4 billion gallons. Of that total amount, 49 percent

is sold for automotive use, 1.7 percent is purchased by the government, and the

remaining approximately 49 percent is divided among industrial, electrical, railroad,

aviation, and like oils.

Scarcely any quantitative information is available as to the ultimate fate of

this lubricating oil. However, reasonable estimates suggest that about 1.2 billion

gallons of used oil are generated annually in the U.S. About half of the lube oil

sold is lost or consumed during use, and 1.2 billion gallons salvaged, 60 percent from

auto waste and 40 percent from industrial waste.

How significant is 1.2 billion gallons per year of used oil? It might be easier

to make comparisons if we convert gallons to barrels, the unit commonly used in the

57
petroleum industry. This quantity, 1.2 billion gallons, equals 28.5 million barrels.

This is enough oil to heat and cool 675,000 homes or operate 1,350,000 cars for a r year. Further, each barrel of used oil recycled saves a barrel of imported oil. l An often-stated, near-term conservation goal is to reduce oil consumption by one i million barrels per day within the next five years. If all used lube oils were re- | cycled and reused, that one effort would exceed five percent of the stated goal. i Perhaps of equal significance to the conservation aspects is the pollution i potential of the large quantity of used lube oil generated annually. Uncontrolled

disposal of used oil causes severe environmental damage. Used oil poses the greatest I potential damage to the environment through ground-water and stream contamination, [ but its heavy-metals content makes uncontrolled burning equally undesirable.

The fate of the 1.2 billion gallons of used oil can only be estimated. Approxi- I mately 43 percent is burned; 18 percent is used for road oil; 31 percent is unknown; \ and, unfortunately, less than 10 percent is being re-refined.

| The idea of re-refining used oil is certainly not new, and the re-refining j industry was quite active in the years following World War II. By 1960, there were about 160 re-refining companies in the U.S., with a combined annual capacity of about

300 million gallons.

Since that time, the re-refining industry has declined to fewer than 30 companies!

today. There are many reasons for this decline - -economic , technological, environmental!

and political. '

9 Prior to 1965, re-refiners enjoyed an excise tax rebate on sales of lubricating s oil for off -highway use, which is a major m.arket for re-refined oil. The tax rebate { was removed in 1965, and subsequent rulings by the Internal Revenue Service have [ changed what was formerly a tax advantage into what the re-refiners now consider a tax j( disadvantage. f Re -refiners claim that they have been placed at a further competitive disadvantagJ

by the 1964 Federal Trade Commission ruling that oils sold in interstate commerce i which are compounded in whole or in part of re-refined oil must be labeled as "Manu- o factured from Previously Used Oils." Re-refiners say that this label unfairly brands | all re-refined oils as inferior products.

i Most re-refiners have limited resources to develop improved process technology or

to construct new facilities. Also, because of increased environmental awareness, the

^ disposal of re-refining wastes has become more difficult and more costly. ij

|i Several approaches toward revitalizing the re-refining industry are now being \i pursued. Legislation has been introduced at both the national and State levels which |) is intended to encourage the re-refining of used oil. On the national level, i Representative Vanik of Ohio and Senator Domenici of New Mexico have introduced oil- ' recycling bills into their respective branches of Congress. Neither of these bills ; progressed very far through the Federal law-making process. However, the Energy Polic>

and Conservation Act, which was signed into law last December, contains a section on |i recycled oil which incorporates some of the provisions of the Vanik and Domenici bills 3 and does encourage the use of recycled oils. !

On the State level, oil -recycling bills have been introduced into several State 0 legislatures, including New York, California, Wisconsin, and Illinois, to name but a \ few.

\ Now, let us turn our attention from the legislative area to the research and t technology areas. Experimental !i

The Bartlesville Energy Research Center has been involved in a research project I: on re-refining of used crankcase oil for several years. One phase of this research ji has been the development of improved re-refining technology. A basic philosophy of f this research has been that the best method of reclaiming used oil is one that = effectively removes impurities but does not substantially change the hydrocarbon com- ^ position of the oil. The method which has been developed, and for which a patent is

pending, includes dehydration to remove water and gasolirie and solvent treatment with

a mixture of alcohols and ketones to precipitate coking precursors followed by vacuum '

58
distillation. Color and odor are improved by clay or hydrogen treatment. This process produces equal or greater recovery of re-refined oil and a smaller quantity of

by-products than the commonly used sulfuric acid-clay process. The by-products that

are produced are less hazardous and should be easier to find alternate uses for or

to dispose of than sulfuric acid sludge. Re-refined oil produced by the solvent

treatment -vacuum distillation method is equal if not superior in quality to that produced by the acid-clay process, and oils produced by this teclmology have shown some success in passing engine -performance tests (1).^ Although initial economic studies

look promising, they have not yet been fully Tnvestigated.

Another phase of the research has been to determine if there is a significant

and serious variation in the used oil feedstocks to re -refineries

.

A question that has concerned re-refiners for many years is whether or not there

is so much variation in the feedstock to a re-refinery that a consistent and quality

product cannot be produced. Some authorities claim that each truckload of used oil

delivered to a re-refinery presents a different feedstock, and, therefore, a potential

difference in the quality of the re-refined product. Others have suggested the

possibility of geographical and seasonal differences in used-oil feedstocks which

would affect the quality of the products. In order to investigate these questions,

30 samples of used automobile crankcase oil typical of re-refinery feedstocks were obtained from 25 different locations in the U.S. Duplicate samples were obtained

from five of the locations at different times of the year to check for seasonal

variations

.

The major hydrocarbon composition of each of the 30 used oils was determined by

separating each of the oils into four fractions by adsorption chromatography and

analyzing the fractions by mass spectrometry. Comparison of the composition data from

the 30 used oils indicated great similarity in the hydrocarbon composition regardless

of the regional or seasonal origin of the oil (2^) . This study strongly suggests that

the feed to a re-refinery is sufficiently uniform that consistent products can be

produced by re -refineries with reasonable quality-control measures in the plant.

A third phase of this research project compared commercially re-refined oils with

new oils in a number of laboratory bench tests, most of which were standard American

Society for Testing and Materials test methods. Some of the re-refined lubricating

oils purchased on the open market contained no additives and therefore could not pass

such tests as foam, corrosion, wear, and oxidation (3^). Other re-refined lubricating

oils provided by the re-refiners and formulated to me^et American Petroleum Institute

service classification SE could not be distinguished from new oils by these bench

tests; however, several failed one or more of the tests, indicating the need for

better quality control in the re-refinery (4^). Since the results of bench tests do

not always correlate with the results of engine -per formance tests, bench tests are not

completely definitive in measuring the quality of an automotive lubricant; therefore,

conclusions for equivalency based on bench tests await additional research.

Engine -per formance data have recently been obtained on three reclaimed lubricating

oils. Two oils reclaimed from used automotive crankcase drainings by BERC-developed

technology and one commercially re-refined oil were subjected to standard bench tests

and engine-test sequences to measure the quality of these oils (1) • A commercially

re-refined SAE 20 automotive lubricating oil successfully passed~the IIC, IIIC, and VC

engine-test evaluations that are required by automobile manufacturers to meet the

standards established for service SE and also the L-38 test required by the military

to meet the major requirements set forth in MIL-L-46152 specifications. One BERC-

.produced sample passed both IIIC and VC sequence tests and failed the IIC marginally.

Another BERC -produced oil successfully passed the IIC and IIIC test and failed the VC

marginally. Both oils passed the bench-scale L-38 test, which we understand correlates

quite well with the large scale L-38 test.

This study is believed to be the first documentation in the U.S. of successful

passing of engine - sequence tests by re-refined lubricating oils to meet standards

established for service SE and/or military specifications. Success in these tests

does not constitute qualification in these categories as this status is granted by an evaluation board and such qualification was not the purpose of this study. Rather,

these tests were run to establish the capability of producing quality products from

used lubricating oil feedstocks, and such capability now has been established.

^ Underlined numbers in parentheses refer to items in the list of references at the

end of this report.

59
In addition to these engine tests, fleet testing of recycled oil produced by [l BERC technology is being conducted in the State of Iowa. Vehicles operating with |^ virgin lube oil, commercially re-refined, and BERC-processed oil are in their 4th : month of a 24-month test program. Dip-stick samples are being taken and detailed

analyses completed on the used oil drained at selected intervals. At the end of this | 2-year, carefully monitored program, 10 engines will be disassembled to evaluate I, their condition and to determine any significant differences attributable to the oils j used. ! Proposed goals at BERC for fiscal year 1977 include a scaled-up pilot-plant

operation to produce about 1 ,000 gallons of reclaimed oil using BERC-'developed

technology. This product will be used in the evaluation of modified processing and | polishing procedures and to obtain further engine-test data. In this regard, some

j measure of in-house capability for processing is being achieved with the installation | of a full vacuum fractionation tower with a throughput capacity of about five gallons

per hour. This equipment plus reactors, appropriate tankage, and a solvent stripping

distillation unit should provide the in-house capability required to evaluate parameters associated with converting the BERC technology from a batch .process to a continuous process.

Another study being initiated is an extension of the composition studies which

have been performed and reported. This investigation is basically a composition

study on used automobile crankcase drainings generated in a closed-loop experiment.

Specifically, virgin stocks will be blended into a finished 10W30 lube oil and the

composition of the basestock determined. A fleet of automobiles will then be employedl

to accumulate about 4,000 miles using the blended oil. The drainings from this fleet

will be reclaimed using BERC technology and the composition study repeated on the ' reclaimed products. This cycle will be repeated once more to compare compositional

changes occurring in the oil resulting from both use in the automobile fleet, and also'

in processing after one and two complete cycles of use and reclamation. The benefits ' to be derived from this study are the assessment of compositional changes and the ! correlation of these changes with any marked improvement or detriment to oil quality ! that occur.

| Conclusions I

i It appears that the turn in the road has been reached for the reclamation of used!

lubricating oil. In spite of the decline over the past decade of the re-refining f industry, waste oil recycling is an idea whose time has come. Conservation of our !; petroleum resources is likely the strongest driving force in the turnabout for recycl-'

ing. The development of improved technology through both government and private ' research should have the end effect of stimulating a depressed industry. Higher ' prices of virgin crude oil make the economics of recycling more attractive, and with

higher profits will come increased activity in re-refining operation. And, too, I recent legislation which emphasizes increased use of recycled oil must be an important!

factor. Finally, environmental concern should soon reverse the trend toward burning j' and dumping used lubricating oils and channel more feedstock to the re-refiner. The

day might well come in the foreseeable future when much of the used lubricating oil

presently discarded, burned, poured upon rural roads, or otherwise wastefully disposedj

of will be reprocessed for continued use as a lubricating oil--not once or twice--but | many times. ; References i

[1] Reynolds, J. W. , Whisman, M. L. , and Thompson, C. J., Engine Sequence Testing of ! Re-refined Lubricating Oils, BERC/OP- 76/29 , October 8, 1976. ,

[2] Whisman, M. L., Cotton, F. 0., Goetzinger, J. W. , and Reynolds, J. W. , Waste ' Lubricating Oil Research: A Summary of Composition Variations Among 30 Used

Lubricating Oils Selected for Seasonal and Geographical Significance, Part 4, j' ERDA BERC/RI-76/4, 1976.

[3] Whisman, M. L. , Goetzinger, J. W., and Cotton, F. 0., Waste Lubricating Oil I Research: An Investigation of Several Re-refining Methods, BuMines RI 7884, 1974}

[4] Whisman, M. L., Goetzinger, J. W. , and Cotton, F. 0., V/aste Lubricating Oil !^ Research, A Comparison of Bench-Test Properties of Re-refined and Virgin ^ Lubricating Oils, BuMines RI 7973, 1974. ' i

60

!
lational Bureau o£ Standards Special Publication 488. Proceedings of

ji Workshop on Measurements and Standards for Recycled Oil held at NBS,

jiaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

i COMMENTS ON ADDITIVE RESPONSE TO DIFFERENT BASE OILS

T. P. Sands

Edwin Cooper, Inc. 1525 South Broadway

St. Louis, Missouri 63104

I The point that I would like to make in this short presentation is that I do not

jbelieve that anybody knowledgeable in the industry doubts the fact that an oil can be

Ire-refined and formulated to pass the engine sequence tests. I do not know of anybody

who doubts this. The data I want to present are not on re-refined oils; they are on virgin base oils. The four oils shown in table 1 are all from major oil companies;

TABLE 1 BASESTOCK RESPONSE

Oil company Sequence VC piston varnish

A 7.9

B 8.0, 8.0

C 7.9

D 6.7, 7.2

All major oil companies

All run with same dispersant- inhibitor

All virgin solvent refined basestocks

they are all solvent refined oils. From our capability after long years of experience,

we could not tell that any of those four oils were not the same as the others as far

as performance is concerned. But, you will notice the first three are passing and the

fourth one is a bad fail. We are not talking about test precision here; oil D is a bad fail. They all have the same dispersant- inhibitor in them.

Here is another case. In this case, there are only two oils (table 2). We do

have more data on them than the VC : however, notice the very drastic differences--

differences in all three tests. (I believe Mr. Kabel will agree that an 8.8 to a 6.0

TABLE 2 BASESTOCK RESPONSE

company

Sequence

VC

Sequence

lie

Sequence

IIIC

E 7.7 8.8 40 h

64 h

33 % 91 %

F 6.0 6.0 40 h

64 h

124 % solid

Both major oil company virgin solvent refined oils

Both run with same dispersant - inhibitor additive

jis a very great difference.) The difference between a solid oil at 64 hours and a l90-percent viscosity increase is significant. I just wanted to make the point here,

again, that passing the sequence test with 1, 2, 3, or 10 oils and a given additive

treatment does not prove that you are not going to get an outlier sometime; and I seriously doubt that there is any physical or chemical bench test that is able to pick out the differences between these kinds of oils with acceptable precision.

i 61
My only additional comment is that after 10 years experience at Gulf Oil Corpora-!

tion, from the oil company standpoint, and after 30 years experience in additives, we j have not found any way of characterizing a basestock to know what it will do from a ! performance standpoint. There have been a lot of people who have tried; you get a lot

of young engineers who believe that they can set up a bench test that would screen

them. We give them the opportunity to find out, and I do not know of any who have

been successful. We end up by putting them in an engine and running them. If they do|

not work, we reformulate, we increase the additive, we change the blend, we do some- ' thing. Believe me, speaking for this additive company- -and I was talking to Dr. Peter,

Asseff of Lubrizol at lunch and he agreed- -we would all like very much to have some I way of doing this to save the tremendously time-consuming and costly evaluations that

we have to go through. If I had been collecting information on this subject over thesi

40 years, I probably could have had several hundred examples like this. These that I ; gave today just happened to be two that we found within the last three months in our 1 work. !

i

62

1
National Bureau of Standards Special Publication 488. Proceedings of

i|a Workshop on Measurements and Standards for Recycled Oil held at NBS,

jiGaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

i|

I ACTIVITIES OF THE ASTM USED OIL TASK FORCE

J William W. Grouse, Jr. Sun Oil Company

P, 0, Box 1135

|i Marcus Hook, Pennsylvania 19061

; Today I plan to give a brief discussion that will cover (1) where the Task Force

fits in to the American Society for Testing and Materials (ASTM) organization,

(2) what is the objective of the Task Force, (3) what we have done to date, and (4) the

expertise we have currently on the Task Force to give you a feel of what we can do and

probably cannot do.

To start with, the title "ASTM Used Oil Task Force" is probably very misleading

because- it implies a much broader scope for our work than I feel we actually have.

I The location of the Used Oil Task Force is in the ASTM organization within Committee

jD-2 on Petroleum Products and Lubricants and, under that, in the Product Committee,

Technical Division B on Automotive Lubricants, and then further into Section 1 of the

Technical Committee B which is concerned only with gasoline engine oil. Therefore,

'our scope is essentially limited to the engine oil area.

j The objective of the Task Force is to provide technical expertise and assistance

in the engine oil area to the Environmental Protection Agency (EPA) and to the National

Bureau of Standards (NBS) to aid them in carrying out their respective charges. The reason the Task Force was created was from a request from the EPA, which at the time

jcame from Mr. Larry McEwen.

j To date, we have had two meetings. The first was with the EPA and the Department

of Defense to discuss their proposed program to characterize re-refined oils and evaluate them as fully formulated engine oils. This is the program that Mr. Thomas Bowen

just discussed. The second meeting was held with EPA and NBS to review these programs

that are currently being started. In the interim, the EPA program was transferred to Hazardous Waste Management under Mr. Hugh B. Kaufman as Project Manager.

Finally, the membership of the Task Force contains the following representation.

We have additive suppliers represented, car makers, re-refiners, engine builders,

petroleum refiners (including the American Petroleum Institute) , military approval

agencies, the Energy Research and Development Administration, the National Research

Council of Canada, consultants, the Defense Fuel Supply Center, and, of course, NBS and

EPA.

I

63

National Bureau o£ Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

ACTIVITIES OF THE API USED OIL TASK FORCE

Barry W. Hutchings

Exxon Company, U.S.A.

P. 0. Box 2180

Houston, Texas 77001

I appreciate the invitation to participate in this program. I think it is-a

good one. Any time a complicated subject like this can be discussed among various

interests with interchange o£ ideas, I think it is a step in the right direction.

My interest this afternoon can be stated very simply. I wish to relate to you

what the American Petroleum Institute (API) has been doing in the area of waste oil

for the past 10 years, or so; also, what it is doing now and what its general viewpoint is on the overall subject of used oil.

Let me move back in time about 10 years, to the late 1960's, and discuss a problem which we think is virtually non-existent today, i.e., that our member companies

were experiencing serious problems with their service stations in having drainings

picked up. I think if we look at the economics existing 10 years ago, we can see

why this was a problem. It is hard to realize now, but heavy fuel oil was selling

for $0.06 per gallon and commodity lubes were selling for less than $0.20 a gallon.

As a result, very few people, with the exception of the re-refiners, had very much

interest in used oil, and it was simply treated like garbage, at best. A lot of it

was getting into the waterways, which was an outrageous situation. It became so serious that the API took it upon itself to try to find a solution to the problem and

spent quite a bit of time doing so. One of the first things that the Institute did

was to determine how great the problem was and to find out where the oil was really

going--what disposal methods were being used. I do not have the time to go into all

the work that was done during these studies, but I think a few highlights are in order.

First of all, in looking at the extent of the problem, we did find that, in fact,

it was a big problem. Based on our own surveys and those of others, particularly the

Arthur D. Little study of 1969, we estimated about 40 percent of automotive used oil

was being disposed of in a questionable manner or in a downright harmful manner with

regard to the environment. Of course, this figure of 40 percent translated into

several hundred millions of gallons a year, which was an outrageous situation.

Secondly, the investigation showed that the other 60 percent of the oil was being

disposed of by burning, by being re-refined, or used as various forms of dust control.

For a number of reasons, some of which are still valid today, the re-refining industry

was judged to be unable to consume all of this used oil, even that from service stations alone. So, the API took upon itself to find alternative means of disposal.

Burning looked like a reasonable alternative simply because you could extract the very

high heating value that we talked about today. In an attempt to further clarify the

question of whether a used oil could be burned as a viable method of reuse, the API,

in 1974, planned and undertook a study at the Hawaiian Electric Company. Since this

represented one of the largest efforts of API in the area, I think it merits a few

minutes discussion.

By way of a little background, the Hawaiian Electric plant was an ideal test

vehicle because it had burned used oil for a number of years with no mechanical problems. They were used to handling it and had the proper facilities for handling it.

The unit itself, of course, was a boiler, normally firing No. 6 fuel oil, and it

generated 20 to 50 megawatts of power; so, it was a moderate-sized plant. No special

pollution control equipment was installed. The testing that the API undertook was

over a five-day period in January. The first day and the last day. No. 6 fuel oil

alone was burned to obtain baseline values; and, during the intervening thTee days,

various percentages of waste oil (primarily crankcase oil) were burned in the range

of 6 percent to 15 percent. Some of the major findings were: (1) about half of the

lead was determined to remain inside the boiler, and this has been, I think, the same

figure that other people have found, with only half of it being emitted into the

atmosphere; and (2) the estimates of atmospheric dispersion of the lead that was

65
I

emitted were calculated based on equations published by the Environmental Protection

Agency (EPA) , taking wind direction and normal averaging times into account. The

ground level lead concentrations were estimated to be below two micrograms per cubic

meter, which, at that time and I think probably still, is below the proposed ambient

air standard for lead. This was true even under soot-blowing conditions, when the

emissions were higher. I think it is important to note, again, that used oil was burned at the rate of 6 percent to 15 percent of the fuel. The reason I say that is

important is if you take all of the waste oil in the U.S. containing lead and blend

it with all of the No. 5 and No. 6 fuel oil consumed in the U.S., the ratio would be

only about 1-percent used oil. So, we feel that, although you cannot distribute all

the lead- containing used oil evenly, you probably can work on a practical basis of

perhaps 2 percent to 3 percent. We think, however, burning should take place only

where economics dictate that re-refining or some other alternative is just not the

better way to go.

All this preceding discussion dealt with what API has done in the past to look

for ways of keeping used oil, primarily crankcase oil, out of our waterways. The

other half of the problem is the industrial oil, which we have talked about considerably today. Metal-working fluids, hydraulic oil, and other lubricants -- these , of

course, eventually become used oil also. We think the answer to this situation is

fairly simple, and that is that economics are forcing a fair amount of these products

to be recycled now. One of our member companies did a study to dictate why this was happening. Although some of these economics I am going to discuss (table 1) will not

agree with some of the ones you have heard today, I think in the cases where the used

industrial oils are of low additive formulations, these are the economics at which we

are looking. We have looked at this over a period of years, going back in time to

TABLE 1

INDUSTRIAL CUSTOER'S INCENTIVES FOR RECLAIMING WASTE OIL

Industrial lube, average

FOB cost Cost of reclaiming from

survey

Incentive for reclaiming^ Low S HFO, average FOB cost Cost of cleanup or maintenance

Net value of waste oil as fuel

Delta savings in reclaiming over burning

cents/gallon

1972 1973 1974 1975 1976 1980

39 41 70 75 79 94

(20-30)

9-19

11

(20-30) 11-21

15

(20-30)

40-50

30

(20-30)

45-55

30

(20-30)

49-59

30

(20-30)

64-74

40

(1-5) (1-5) (1-5) (1-5) (1-5) (1-5)

6-10 10-14 25-29 25-29 25-29 35-39

(1)-13 (3) -11 11-25 16-30 20-34 25-39

*First year incentive. Sun, Keene, and others indicate waste oils can be reclaimed up to

10 times, depending on the type of waste oil.

1972, which, of course, was a pre-Arab embargo year (pre -escalating of the crude oil i price by the Oil Producing and Exporting Countries [OPEC]. You see that probably on average lubes were costing about $0.39 a gallon, while low-sulfur fuel oil was costing j, about $0.11 per gallon. The user who consumed both lubes and fuel, of course, had a choice of what to do with the material: reclaim it or consume it himself. We feel

that for some of the low-additive materials, with proper equipment, he could reclaim

it for $0.20 to $0.30 per gallon, which gave an incentive for reclaiming, for lube

use, of about $0.09 to $0.19 in 1972.

The other alternative was to burn it as fuel. Although in the case of Hawaiian | Electric and many other reported instances there were no problems with maintenance, a | reasonable debit for burning might have been $0.01 to^$0.05 per gallon, mostly to get

rid of the water. So, the value of the waste oil for fuel is the difference between I the cost of virgin fuel and the debit or $0.06 to $0.10. i

66
Faced with these two alternatives, the choice of which way to go is based on the

difference between total costs and total sales price. In 1972, this was anywhere

from -$0.01 to, perhaps, as high as +$0.13 per gallon. I do not know what the average

was . But look at 1976, this year. We are looking at a $0.79 average price for virgin

lube because of OPEC ' s escalation in crude price; we are looking at a much higher fuel

cost, perhaps $0.30 per gallon for a low-sulfur fuel oil. Following the same line of

economic argument, we see that the incentive for reclaiming industrial oil is now up

to about $0.49 to $0.59 a gallon versus a net fuel value of only $0.25 to $0.29. We

think this is the reason why many companies are reclaiming, particularly those that

are using low-additive lube oils. They are not burning them. We have heard some of

this spoken about today.

I do not think anybody is smart enough to know what 1980 is really going to look

like, but one scenario has it looking like this: again, an escalation on lube prices,

perhaps as high as $0.94 a gallon, fuel up perhaps as high as $0.40 a gallon. Here

we see an even higher incentive for reclaiming industrial lubes. So, we feel that

reclaiming is going to grow even faster, even with some probable increases in costs

for reclaiming.

This reclaiming is taking place both within the users' plants, as well as by outside reclaimers. Many of these outside reclaimers are re-refiners or ex-re-refiners.

There is one story about one such reclaimer, a very successful one, who is helping to recycle about 12 million gallons per year of industrial lubes. Even though it is in a house organ, you might be interested in reading about his story. (Editor's note:

"The Second Time Around," Wallover Oil Company, Exxon Oilways , No. 4, 1976.)

I think without too much of an over-simplification you can put used oil into

three distinct categories in discussing them in terms of today's environment. These

three are: (1) used industrial oils, (2) used commercial crankcase oils and service

station drainings, and, finally, (3) used oil removed from engines by do-ityourselfers. We think that in the majority of industrial lube applications economics

are going to force reclaiming to a maximum extent in the future- -not burning, but

reclaiming for lube use.

Some problems still remain with heavily compounded oil such as gear oils and

semiliquid greases, but we think most industrial lubricants can be reclaimed and money

can be made doing it. We also believe that, with a very few exceptions, used commercial crankcase oil and service station oil are being "recycled," either for lubes or fuel. The value is simply too great these days to throw it away by dumping it in the

environment

.

The third category, do-it-yourself drainers, remains a very serious problem.

Many attempts are being carried out right now; and I think there are just too many

people trying to work on the problem for it not to improve, including Federal agencies.

State governments, re-refiners, major oil companies, and civic groups. As chairman of

the API group most heavily involved in the used oil area, I hope to be able to propose

in the near future a program for API and its various member companies to undertake

that would help in overcoming this important problem.

This latter point brings me to the last part of my story --what API is doing now

and what its overall position is in regard to used oil. First of all, in addition to trying to work this problem of the do-it-yourself drainer, we feel that the API can be

of the most use in the overall area by contributing its expertise and counsel to those

who are charged with finding solutions to the problem. This means, of course, primarily working with government agencies which by mandate under the law have to find

some type of solution. We have been doing this to a certain extent in the past few

months. We hope to accelerate this and continue it in the future.

Our final statement is this. API has not yet taken a public, formal position on many aspects of used oil management. But, I think I can state without fear of contradiction that its irJembers subscribe to two basic concepts. One is that used oil represents a resource that should be conserved and should be recycled; but, we also feel

that any economic recycling method should be allowable as long as it is not dangerous

to the environment. We do not feel at the present time that burning is dangerous to the environment.

67

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

I CHEVRON RESEARCH'S (EXPERIENCES WITH RE-REFINED OILS

Floyd Sam

Chevron Research Company

5 76 Standard Avenue

Richmond, California 94802

Today I want to show you data generated about a year ago on a program that we at

Chevron Research carried out.

About a year-and-a-hal£ ago, we became very interested in the possibilities of

marketing a re-refined motor oil, initially at the service station level, which would

be an SE or SE/CC type oil. So, we began looking at different samples of lube oil

that came out of a re-refining company (Company A) with which we were working. These

results are found in table 1, and I think this will add a little more data to the

TABLE 1

TEST RESULTS ON RE-REFINED BASESTOCKS FRCM C(M>ANY A

Sample number

1 2 3 4 5 6 7 8 9

Gravity, °API 28.5

Flash, COC, °F 450 450 415 440 460 460 400 465 465 Viscosity at 100 "F, SUS Viscosity at 210 ^F, SUS 480 488 498 499 496 499 506 508 468 62.6 63.2 63.8 63. 8 63.8 63.8 64. 2 64. 2 61.8

Viscosity index 98 98 99 99 99 99 99 98 97

Color, ASTM D 1500 5.0 6.5 7.0 L 7. 5 L 7.5 7.0 L 6. 5 6. 0 L 7.0 Aniline point, '*F 228.5 Sulfated ash, wt 1 0.07 0.13 0.16 0. 16 0.16 0.16 0. 15 0. 15 0.17

Metals, ppm

Total 223 414 477 458 462 491 437 428 527 Calcium 175 366 440 430 432 445 410 404 459

Energy Research and Development Administration/Bartlesville information. You see over approximately one year, perhaps somewhat over a year, some physical analyses of

nine samples of basestock from the re-refiner. If you look at the values, there are

not many changes. It looks surprisingly uniform and consistent. You can see that the

viscosity at 210°F is about a 63 or 64; so, it is a reasonable starting material for

an SAE 30 motor oil.

A little more detailed analysis of these basestocks is shown in table 2. What I have done is added some of the metallics in detail. A couple of points I think you

I should keep an eye on are the oxygen content of one- -1,200 ppm-- and the chlorine,

which ranges from about 190 down to about 83. We will discuss this in more detail a little later.

The data given in table 3 are for comparison purposes. These results are from

another re-refined oil source we looked at (Company B) . You will notice its metallics level is very low. Again, though, the chlorine concentrations are pretty high--

390 ppm--and the oxygen level is at 570 ppm.

We pointed out the oxygen and chlorine levels to Company A and worked with it on

I the source of those particular elements in the finished base oil. Using its product,

I we started out on a first-step basis to formulate an SE/CC oil. I think, as Mr. Sands

I pointed out to you, we are all capable of making a satisfactory oil from almost anything that looks like a reasonable basestock. It is just a matter of money and time.

Some of the work we did is shown in table 4. We took an additive package that we have

been using with an SE/CC approval. The results shown for the virgin base oil are

69
TABLE 2 TABLE 3

ADDITIONAL RESULTS FOR SELECTED SAMPLES FRCM COMPANY A

PHYSICAL, CHEMICAL, AND BENCH TESTS ON

RE -REFINED OIL FRCM COIPANY B

Sample number

LCM

1782 1X 7S8 / oo F-29729

Gravity, °API 28 1 Flash, COC, °F yl AC A AZ Viscosity @ 100 °F, SUS AQQ rD 46o . 1

A Q7 4oZ U Viscosity @ 210 °F, SUS 63. 2 Di . 0 62 7 Viscosity index 98. 3 Q7 n y / . u 98 2 Color, ASTM D 1500 6

5 T 7 n 7 5 Oxygen, ppm 1200 Calcium, ppm 366 466 376 Chlorine, ppm 140 190 83 Magnesium, ppm 6 11 17 Silica, ppm 5 9 Aluminum, ppm 7 7 14 Nickel, ppm 5 5 5 Sodium, ppm 3 4 Iron, ppm 19 Zinc, ppm 15

TABLE 4

RE-REFINED BASE OIL - SE PROGRAM FOR

RE -REFINED OIL FROM COIPANY A

Wt % additive package

Test

SE limits

8.4" 8.4

Y^ 11.0

Zd

Sequence IIC

AER 8.4 8.5 8.1

7.9 8.1

8.4

Sequence I IIC, % A Vioo at 40 h 400 31 923 81

Sequence VC

PVAV

AS

7,9 8.0

8.5

7.6

8,0

9,4

8,3

8.5 9.3

L-38, BWL at

40 h, mg 40 18 26

"Has full SE/CC approvals in virgin base oil.

''X is a virgin base oil.

^Y is a re- refined base oil.

''z is a re-refined base oil.

°F, cSt

°F, SUS

°F, cSt

°F, SUS

Gravity, °API Flash, COC, «*F Viscosity @ 100 Viscosity @ 100 Viscosity @ 210 Viscosity @ 210 Viscosity index

Pour, °F Color, ASTM D 1500 Aniline point, ®F Acid No. , mg KOH/g,

D-3242

Sulfur, wt % Ash, sulfated, wt % Nitrogen, ppm

Chlorine, total, ppm

Chloride, ion, ppm

Oxygen, ppm

Spectrographic § Atomic

Absorption Analysis

for Metals

Spectrographic

aliminum, boron,

barium, calcium,

chromium, copper, magnesium, silica,

tin

lead, zinc, iron,

nickel, phosphorus

Atomic absorption:

lead, zinc, iron,

nickel, ppm

Distillation, ASTM

D 1160 (atmospheric

pressure) , **F

St

5 10

20

3040

50

60

70

8090End point

Recovered, % In flask Cby

difference)

Results

Company B

28.8

Chevron

Research

Company

460 440

-- 82.27

373 376.7 9.402

57,13 57.1

102 99 +5 +10

4 4.5 224,6

0,04

0.19 Nil <0.005

42 390

23 570

Below limit

of

detection

Threshold of I detection I

>1

681

756

771 801

832

840 862

887 912

941 995

1024

93

70
actual data obtained at the time we were doing the re-re£ined oil formulation work, so those results are back-to-back with the re-refined base oil. You see that when we tested the same weight percent additive treatment, we had quite a bit of problem with

the sequence IIC test average engine rust. The Bartlesville people pointed out that

they, too, had some problems with the sequence IIC test. The IIIC was a failure, and

VC piston varnish was 7.6. The L-38 was fine.

We next tested an intermediate formula with about 10.0 weight percent additive

and had more IIC problems. Then we went to an 11.0 weight percent additive treatment,

which is about 30 percent overtreat, and about 1.2 percent to 1.3 percent sulfated ash.

At the normal treatment level, the package itself is close to 1 percent ash. You can

see that we did finally meet all the SE specification targets. However, we did not

obtain a 1-H pass on that oil needed for CC performance.

We did some further diesel testing with a different additive package to investigate the possibility of making a CD oil from this basestock. We again ran into

problems

.

I would like to show you the last step we took. We further processed the base

I oil using a proprietary extraction procedure and additional clay treating. This re- duced the metals to virtually nothing, chlorine down to less than 20 ppm (that is the

I detection limit) , and the oxygen down to about 730 ppm in this particular case (table

] 5) . Based on some additional in-house diesel engine screening work we did with a

j commercial CD package, we concluded that the base oil was satisfactory. We felt coni fident that we could, for example, pass a 1-G with it.

TABLE 5 TESTS ON RE-REFINED OIL AND

RE-REFINED, EXTRACTED, CLAY-TREATED OIL

FROM COMPANY A

Sample number

Tests F-29729 Extracted F-29729

(F-30183)

Gravity, °API

Flash, COC, °F

Viscosity at 100 "F, SUS

Viscosity at 210 °F. SUS

Viscosity index

Color, ASTM D-1500

Pour, °F

Sulfur, wt I Nitrogen, ppm

Chlorine, ppm

Oxygen, ppm

Calcium, ppm

Magnesium, ppm

Zinc, ppm

Iron, ppm

Aluminum

28.1

445

482.0

62. 7 98.2

7.5

+ 10

0.18

50

83

1200

376

17

15

19

14

28.4

450

465 . 3 62.0

99

4.5

0 .15

<20^

730

nil

nil

<10^

nil

nil

^Below detection level indicated.

We are not doing any

want to bring everyone up

and I thought it would be

more work on re-refined oils

to date. I know some of you

helpful to openly discuss it

at the present time, but I did

have been aware of this work,

today

.

71

. National Bureau of Standards Special Publication 488. Proceedings of

I a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

i ENGINE SEQUENCE TESTS FOR DETERMINATION OF LUBE OIL QUALITY

Richard H. Kabel

General Motors Research

GM Tech Center

Warren, Michigan 48090

For my presentation this morning I was asked to talk a little bit about sequence

tests and the history of the sequence tests. Back in 1952, the American Petroleum

1 Institute (API) service classification system had three different service categories:

I ML, MM, and MS. The more common one was used as the MS, or the "most severe," as it

became known. However, one of the problems was that these service classifications

' were not defined by performance tests. So, as one of my predecessors has said, it

I allowed an oil company to make an oil as well as they knew how- -which many did, or as

1 poorly as the public would let them- -which in some cases did happen. This service

j classification did result in field problems.

I In about 1954 and 1955, the automotive industry encountered many problems with

I some MS oils; and the MS definition included oils that were very good to oils that

I cause excessive problems in the field. So, they started collectively and individually

to develop sequence tests, and the American Society for Testing and Materials (ASTM)

got involved in 1956- -Section G-IV, Technical Division B of Committee D-2. They formed

a Section I at that point and gave it the responsibility to look at performance tests

which were being developed by the engine manufacturers. This was the formation of

Section I, Technical Division B, Committee D-2.

I The engine sequence tests were introduced in about 1958, and they became widely

! used in about 1960, as shown in table 1. The first publication of ASTM to include

! them in the STP form was STP 315, first published in 1962 and later periodically revised. It included the first five sequence tests. Sequences I, II, and III were ,

TABLE 1 ENGINE SEQUENCE TESTS

1958 Introduced

1962 ASTM STP 315

Sequence I Low- temperature , medium-speed

scuffing and wear

Sequence II Low- temperature deposits and

rusting

Sequence III High- temperature oxidation

Sequence IV High- temperature , high-speed

scuffing and wear

Sequence V Insolubles, sludging, screen clogging

developed by General Motors, IV by Chrysler, and V by Ford. As shown, the sequence I evaluated low-temperature and medium-speed scuffing; sequence II was rusting or lowtemperature deposits; sequence III was high- temperature oxidation; sequence IV evaluated high-temperature, high-speed scuffing and wear; and sequence V evaluated insolubles,

sludging, and screen clogging, or sludge from taxicab-type operations.

These sequence tests were introduced to evaluate specific parameters. They were

not intended to be all-proof type tests. Their intention was to distinguish between

acceptable and unacceptable performance in specific areas. They were not intended to replace field testing. They evaluated only these certain specific parameters, and oil

companies continued to field test their products before they were marketed.

Periodically, these sequence tests were revised, as shown in table 2. The MS

definition carried through to about 1971 and was followed by the SE classification

73
TABLE 2 ASTM STP 315 PUBLICATIONS

MS - 1962 - STP 315

MS - 1963 -- STP 315A

MS 1966 STP 315B

MS - 1967 - STP 315C

MS - 1968 STP 315D

SE - 1973 - STP 315F

SEQ. I, II, III, IV, V

SEQ. I, II, III, IV, V

SEQ. IIA, IIIA, IV, V

SEQ. IIA, IIIA, IV, VB

SEQ. IIB, IIIB, IV, VB

SEQ. lie, IIIC, VC

system. The first publication of STP 315 included the sequences I, II, III, IV, and

V. In 1963, STP 315A was published and contained updated or revised versions of

several of the procedures that improved the precision- -the same basic five procedures.

In 1966, STP 315B was published; sequence I was dropped and was combined with the

results obtained from sequences IIA and IIIA. In 1967, STP 315C was published and

sequence VB was introduced, replacing sequence V. In 1968, STP 315D was published,

and sequences IIA and IIIA were replaced by sequences IIB and IIIB. In 1973, STP 315F was published, and this was when we went to the SE classification system (actually, we went to it in 1971) . Sequence IIC replaced sequence IIB; sequence IIIC replaced IIIB; sequence IV was dropped, since oils that passed the sequence IIIC tests also passed

the sequence IV tests; and sequence VC replaced sequence VB

The SE performance classification system came into being about 1971 and is shown

in table 3. Category SA is still defined as motor light, or the most optimum type of |t service. There are no performance tests involved in defining SA other than some pour Ij and foam inhibition tendencies, as well as the viscosity. This may be one that we may

wish to consider for some re-refined oils if the equivalency can be established with

respect to foam and pour.

TABLE 3 ENGINE OIL PERFORMANCE CLASSIFICATION (1971)

SA ML

SB L-4, L-38, SEQ. IV

SC IIA, IIIA, IV, V, L-38, L-1

SD IIB, IIIB, IV, VB, L-38, L-1

SE IIB OR IIC, IIIC, VC, L-38

CA L-4, L-38, L-1

CB L-4, L-38

CC L-38, LTD, IIA or IIB, l-H

CD 1-D, 1-G, L-38

The SB classification was defined by the L-4 test, the L-38 test, and the

sequence IV test. As you can see, there are the various S categories down to the SE

which currently requires the IIC, IIIC, VC, and L-38 engine sequence tests. Original

ly, the SE had a IIB test requirement in it. The C category of oils for diesel

engines involves the L-4, L-38, and L-1 for the CA classification, CB requires the | L-4 and L-38; CC the L-38, LTD, IIA or IIB, and l-H; and the CD takes the 1-D, 1-G,

and L-38 tests. The CC and CD categories are still being used by engine manufacturers!

After discussing the history of the sequence tests overall, I would now like to take a moment to tell you a little bit about some of the problems that General Motors

| has had in developing some of these sequence tests. '

We have been working on sequence tests since about 1955, as shown in table 4.

j In our development of several of these, we have found it does take a considerable i amount of time and effort to establish correlation with field service. In table 5,

you can get an idea of the number of tests involved and of the length of time required

to develop test procedures that correlate with the field. We are talking about over

810 tests for development and about 10-1/2 years of time. This does not include iron-,

ing out problems such as hardware and fuel and things of that nature or the monitoring

74
TABLE 4 TABLE 5 HISTORY OF GENERAL MOTORS -DEVELOPED

SEQUENCE TESTS

1955 1960 Development stages

1960 - 1964 Sequences I'', II, and III 1964 1967 Sequences IIA - IIIA

1967 - 1970 Sequences IIB - IIIB

1970 - 1972 Sequences IIB and IIIC

1972 Sequences IIC and IIIC

TIME REQUIREMENTS FOR

SEQUENCE TEST DEVELOPMENTS

Qtarnipnrp No 0 f tes ts Time

I, II, and III 400 5 years

IIA - IIIA 165 2 -1/2 years

IIB - IIIB 100 14 months

IIIC 85 1 year

IIC 60 10 months

TOTAL STU" 10 -1/2 years

effort for reference oils. This only includes development time to correlate with

field service. Many types of field service have to be considered and have to be cor- related in order to have a test that is meaningful. Because of the various types of

service, you cannot develop everything into a sequence test. Thus, they are not allproof type tests. They only evaluate certain specific parameters. I guess we could

probably add a couple more years on here because we have been working on the wear

tests .The philosophy that we have used in developing tests is to control all parameters

which influence the test result except the quality of the lubricant. We try to make

that the only variable involved. Then we control the parameters at the levels which

result in good field correlation in the shortest possible time. All this means is

field tests plus the lab tests mean a lot of work and expense. We think it is necessary to define the performance requirements of engine oils.

75
iI

I'

!'

ii. I

St

llf
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

SCREENING TESTS ON LUBE OILS

Peter A. Asseff

The Lubrizol Corporation

29400 Lakeland Boulevard

Wickliffe, Ohio 44092

Perhaps the title should be lack of screening tests rather than screening tests.

There is a great incentive to develop laboratory bench-test procedures to correlate

with full-scale engine specification test requirements. Among the most obvious

incentives, of course, is the economic consideration and the time-saving potential of

such procedures. During my association with the additive industry, which spans an

interval of over 40 years, my company has continually investigated various methods

for accomplishing this objective. To date, we have not discovered satisfactory methods

to replace the engine tests; we wish we could. We have been able to use certain bench

tests to measure single properties of a lubricant such as oxidation stability, thermal

stability, rust protection, bearing corrosion protection, dispersivity characteristics,

high-temperature detergency, and others. One might then ask the question as to why

these tests cannot be combined to accurately predict the performance characteristics

of the lubricant in the various engine specification tests which were designed to measure pretty much the same parameters. We believe that the principal reason for our difficulties is the inability to duplicate the engine environment. One essential part

of this aspect is the effect of the fuel and the fuel - combus tion product on the performance of the lubricant. Many attempts have been made to introduce this fuel effect

into laboratory bench scale tests. But, to date, these efforts have not met with any

appreciable degree of success.

The lubricant screening tests which are employed in the investigation of additive

performance, at their best, merely improve one's chances of meeting the engine test

requirements . Among some of those which we have employed and which others have employed over the years are oxidation tests such as the Continental Oxidation Test, which is

a well-known aeration type test in the presence of a catalyst such as iron at temperatures in the range of 341°F. Others have used, and we have also, oxygen absorption

tests such as the Rotating Bomb Tests, which are currently in the American Society for

Testing and Materials procedure, running under pressure in a bomb or a circulation of

oxygen in a closed system at low pressures, measuring the amount of oxygen absorbed in

a unit time at elevated temperatures. Other types of tests are bearing corrosion tests

which measure the tendency of the lubricant to corrode bearings, principally copperlead bearings, under the conditions conducive to oxidation, and generally at temperatures around 300°F to 325°F. Among these are the Indiana Stir Oxidation Tests which

involve aeration by high-speed agitation in the presence of a copper-lead bearing; the

temperature in this case is 300°F. An old test from way back is the Underwood Oxidation Test, developed by Mr. Arthur Underwood, I believe of General Motors Research,

which involved circulation of an oil over an in-line electric heater, followed by

spraying the lubricant against bearing materials in a chamber in which air is simultaneously mixed with the lubricant. Bearing corrosion and oil deterioration are determined at various intervals during the test. The temperature in this case is 325°F.

There are tests which attempt to measure the combination bearing-corrosion and

lacquer-deposits tendencies of the lubricant, and these are oxidation tests run in the'

presence of a metal catalyst such as copper-lead bearing and steel surfaces which serve

as a surface for plating out varnish-forming materials which are the result of the

oxidation of lubricants. One of these is the SOHIO Oxidation Test, which is run at

325°F. A section of a copper-lead bearing is subjected to a high rate of shear in oil

surrounding the specimen in the presence of an excess of air. Catalysts are employed

to accelerate the rate of oil oxidation. Lacquer ratings are also determined on the

outer surface of the corrosion test unit.

Other tests have been designed to evaluate low- temperature sludge dispersency

characteristics. One laboratory-type test, which is used to evaluate this property,

is one which rates materials on the basis of their ability to suspend insolubles

derived from drain oils which have already been used dn the engine. The suspended

material is that which remains after a high-speed centrifugation of a mixture of the

sludge and oil, this said mixture having been prepared by either a sonic or a vigorous

mechanical agitation.

77
Other type tests have been used to measure the high- temperature deposition or

the detergency characteristics at high temperatures of the additive oil system. The

Panel-Coker Test, which many of you are familiar with, has been found to be a useful

screening device to evaluate the thermal stability and the detergency ability of the

lubricant oil additive system., In this test, the oil is flashed against a heated

steel panel, and the panel is then evaluated for deposits. Varying temperatures

ranging up to about 600°F are employed, depending on the objectives of the test. The

deposit level can also be varied by a variation in the time allowed for the oil to cook on the surface of the test specimen in the absence of splashing or renewing the

oil. Tests such as this may simulate the deposits produced in diesel-engine operation

One last comment I would like to make is about something called the "fuel factor.'

In general, as you know, the fuel does not burn completely. Various oxidation products- -acids , aldehydes, ketones, cracked hydrocarbons, unsaturates, oxides of

nitrogen, etc. --will get into the lubricant as blow-by. These materials then form a part of the lubricant. They are all mixed together in there, and you no longer can consider the pure clean lubricant. You must consider the effect of these materials

which are also a part of the lubricant. As these materials accumulate, they become

a greater part of the lubricant. The oxidation stability of these materials cannot

be satisfactorily determined, for example, by running a bench test on just the

lubricant by itself. If you attempted to combine all of these things together, you

might just as well put it in the engine, because that is where they exist in the first

place.

In conclusion, I did not attempt to cover all of the various tests which have

been used as screening tests or tests to predict the possible performance in the

various engine tests; however, these types I think are representative in general of

what has been employed. Again, let me emphasize that the only way to determine engine

performance is to run the oil in an engine.

78

5
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

LABORATORY TESTING ON RE-REFINED MOTOR OIL

Belton R. Williams

Motor Oils Refining Company

7601 West 47th Street

McCook, Illinois 60525

When the subject of used oil arises, it is usually discussed in terms of crankcase drainings from automobiles. Similarly, when re-refined oil becomes the subject

of discussion, it most frequently is thought of in terms of the same crankcase

drainings processed for reuse as motor oils. To broach either subject accordingly

is normal. Most of the attention given the subject of used oil and its recovery for reuse is expressed in terms of whether or not it can adequately lubricate an internal

combustion engine.

It, of course, has been noted that the subject neither begins nor ends with this

rather limited scope. The parameters of consideration are far broader, touching upon

many kinds of petroleum lubricants used in a multitude of applications and being

recovered for a variety of reuses. It does follow, however, that the recovery and

re-refining of automotive crankcase drainings for reuse in motor oils has a tremendous

importance to the acceptability of re-refining as a viable secondary industry. In a nut shell, it is because of the questionable quality connotation historically attributed to this concept of reuse.

In all candor, neither the proponents nor the opponents of motor oils made from

re-refined crankcase drainings have unequivocably proved their position. This is

mainly because one will not concede the validity of the other's arguments, and there

is insufficient data to prove one or the other totally wrong.

Neither my remarks nor the data I will present are intended to settle the controversy once and for all, but hopefully will demonstrate that an advocacy position is

acceptable within the frame of reason and practicality.

As discussed yesterday, the matter of feedstock variability has historically been

a primary point of contention. It has been charged that the re-refiner deals with a new feedstock every day; and, thus, his end product must also be variable. The

re-refiners have attempted to address this situation over the years.

In 1960, the Armour Research Foundation of Illinois Institute of Technology did

a study of re-refining for the Association of Petroleum Re-refiners and stated:

"There is an amazing uniformity in the chemical composition of the

oil drainings from the various parts of the country. It is more uniform than the composition of the crude oils from different sec- tions. This uniformity was established by infrared analysis and

determinations of the physical and chemical properties of the

distillate and residual material."

Yesterday, Mr. Charles J. Thompson related the work of the Bartlesville Energy

Research Center and their conclusions that feedstock to re-refiners is similar in

petroleum base composition regardless of seasonal or geographical location within

the U.S. Obviously, neither of these findings is absolute assurance that the feedstock will not be contaminated with oils of lesser quality, nor that it will be processed to meet the quality requirements of a base oil suitable for compounding highquality motor oils. It does, however, help to establish a credible base for

re-refiners to build upon in controlling their applied technology to produce products

of acceptable quality.

As is the case in any processing activity where the optimization of yields and

product quality is paramount, a re-refiner must utilize appropriate technology and

employ control systems throughout the process to achieve a consistently desirable

result. In short, control is mandatory.

79
Figure 1 is typical of the type o£ equipment used in collecting drain oil from

service stations. Upon arrival at the re-refinery, the free water is drained from

the truck into a primary water recovery system; and after being sampled and approved

for unloading, the truck is hooked up into an unloading manifold and the oil is

metered into the proper storage tanks.

Figure 1. Drain oil

collection truck.

Control for the re-refiner begins with the receipt and segregation of feedstocks

from which the base oils are to be extracted (figure 2) . Obviously, the re-refiner

depends on the waste oil collector to segregate or at least identify the types of oil

being delivered. It also behooves the re-refiner to establish safeguards to protect

the integrity of his feedstock.

Actually ,, crankcase drainings have peculiar characteristics readily identifiable

by experienced personnel who examine the material at the time the sample is drawn for

BS§W (bottom settling and water) analysis. Verification of quality can be rather

quickly accomplished by determining the viscosity, viscosity index, and flash, when

the oil appears to contain a diluent such as gasoline or solvent. If there is doubt

beyond this point, and in the absence of other means of determining the characteristics

of the material, the re-refiner can exercise the option of segregating the material

for processing into material for less critical use. A part of the control process

definitely includes careful segregation and storage of oils according to their

properties

Figure 2. Tankage for

feedstock segregation.

80

1

I
Various methods of re-refining are employed and include various combinations and

permutations of chemical treating, vacuum distillation, and atmospheric distillation

(figure 3). This is usually followed by clay contacting and filtration. Throughout

the process, it is absolutely essential that the re-refiner control temperatures,

steam pressure, pump pressure, and other factors which bear upon the quality of the

end product.

The plate and frame filter press, as shown in figure 4, is commonly used in re- refining. While not altogether necessary, it is considered a good idea to pass the

oil through a second filtration, or polish press, to be certain the finished oil

contains no ash materials which could have escaped the first filtration because of

broken filter pads. At this point in the process, a base mineral oil has been produced which is suitable for blending and compounding into motor oils or other products

for which they are appropriate.

Figure 3. Distillation

units

.

81
As mentioned earlier, control is extremely important, and the re-refiner must

either have in-house facilities or utilize the services of a commercial laboratory

to the extent necessary to insure quality (figure 5)

Figure 5. Quality control laboratory.

The laboratory depicted here is used for checking all incoming materials, such

as drain oil, blending oils, and additives. It is used for monitoring the re-refining

process for blending and for finished-product quality assurance. Samples are taken

from various stages of the process and are brought to the laboratory- control booth

where they are checked for viscosity, f ilterability , flash, etc, for process control.

All incoming blending materials, products in process, and finished products are checked at this point for viscosity at 100°F and 210°F. The Cleveland open cup method

is used for flash and fire tests. We also run sulfated ash tests on our motor oils.

Figure 6 shows the oxidation tester we use. This is an adaptation of the General

Motors E.M.D. silver corrosion tester and is used for making comparative oxidation

tests on base oils and finished products. Typical test results on motor oils will be

discussed later in this paper.

A Baird atomic emission spectrometer is used for determining the kinds and

quantities of metals in various oils being tested. It is very useful in identifying | characteristics of drain oil and additive level in finished products, as well as for

analysis of wear conditions in operating engines.

-

I A sulfur tester, analytical balance, ph meter, and bench vacuum distillation i equipment are used in the laboratory for performing various tes ts and analyses.

j In summary, the tests performed in our laboratory on motor oils include gravity,

flash and fire, viscosity at 100°F and 210°F, viscosity index, pentane insolubles,

total base number, total acid number, sulfated ash, spectrographic analysis of

additive, pour point, and others as deemed appropriate.

We continually test the virgin neutrals and bright stocks, as well as additives, , to determine their miscibility with re-refined base oils. This is accomplished by ,

82
making up blends and letting them stand for long periods of time to observe whether

there is any separation or stratification.

Figure 6, Oxidation

test equipment.

Results and Discussion

The data shown in table 1 represent approximately one million gallons of drain

oil and the finished base oil derived from it. You will note from the viscosity that

the oil is an SAE 20 and the changes in viscosity, viscosity index, and pour point

indicate the removal of diluents and polymers. From a re-refining standpoint, the

critical comparison is the ash, which is typical for automotive drain oil, and the

absence of ash in the finished oil, which is indicative of a proper re-refining job.

TABLE 1 TYPICAL PROPERTIES

BASE OIL RE-REFINED FROM AUTOMOTIVE DRAIN OIL

Drain Finished

oil oil

Viscosity at 100 ®F, SSU 357 366

Viscosity at 210 °F, SSU 61.45 57.27

Viscosity index 125 104

Ash, % 2.1 0.0

Pour point, °F -35 -20

83
Table 2 shows typical properties of a partial listing of motor oils utilizing

re-refined base oil, virgin blending oils, and appropriate additive packages. The

American Petroleum Institute service classifications indicate that the oils are com- pounded to the equivalent of SE grade or series 3.

TABLE 2 TYPICAL PROPERTIES

MOTOR OILS MADE FROM RE-REFINED OILS

Viscosity at Viscosity

Flash 100 °F 210 op index

SAE 20 - SA Grade 420 320 54 4 104

SAE 20W - SE Grade 420 320 55 0 104

SAE 30 - SE Grade 450 540 65 5 96

SAE 10W40 - SE Grade 395 322 74 0 153

SAE 30 - Series 3 450 540 65 5 96

The oxidation tester shown earlier is used for running comparative oxidation

tests. The test consists of heating 300 ml of oil to a selected temperature and

holding it consistently for 72 hours while stirring at 300 rpm with stainless -steel

stirrers. Both copper strips and steel strips are immersed in the oil during the

test

In the results shown in table 3, samples 5 and 6 are re-refined oils which

have been compounded to the equivalent of the SD and SE American Petroleum Institute

service classifications and are compared with four major brands, all of which are SE

oils :

• The percent weight loss of the four major brands ranged from

0.88 percent to 1.32 percent, while the re-refined oils were

at about the median of the range.

• The viscosity increase at 100°F ranged from 2.5 to 7.3 for

the first four and were 3.6 to 4.0 for the re-refined oils.

• At 210°F, the percent viscosity change for the re-refined oils was less than the major brands.

• The re-refined oil had less weight change on the steel strips

than the four major brands, while weight loss for the re-refined

oils on copper strips was about the median of the first four.

« The results of the pentane insolubles test show that all six

oils were good material and the variations in the final percentage are infinitesimally small.

Another test was recently run to test re-refined diesel lube oil. This is an E.M.D. two-cylinder silver bearing smear test. This test utilizes an E.M.D. 67 twocylinder engine and runs for 25 hours. The test results are based on a demerit

rating of the four central grooves in the silver bearing and the rating scale for

excellent, good, fair, bad, and very bad. The test conditions, the product being

tested, and the results are shown in table 4.

84
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o

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0) T-l •p +-> CO (/)

eno

o

to

• H in & q

0

u

CO ' CO

u

u

O C

I ^-1 •I—1 ^

eg

u t3 2 ^

O

r—t CO 2

•H

85
TABLE 4

E.M.D, TWO-CYLINDER SILVER BEARING SMEAR TEST

1. 25-hour, two-cylinder

engine test - EMD 567 engine

2. Test results - EMD de- merit rating of four

central grooves

3. Rating based on silver

smear and groove

deposits

4. Rating scale (demerits):

0 to 10

10 to 20

20 to 50 50 to 100 100 to 200

Excellent

Good

Fair

Bad

Very bad

Re-refined oil, compounded with

high dispersant additive

2 . Test oil properties

Tests

Viscosity at 100 °F Viscosity at 210 °F Viscosity index

TBN (D-2896)

Calcium (M-950)

Infrared trace

Results

982

79.2

749.32

0.32

Matches

1. Test oil:

2 . Bearing

demerits:

4 . Overall

rating

Re-refined

diesel lube

oil

7.3

3 . Bearing

appearance : Bright

Excellent

The material used was re-refined oil compounded with high dispersant additive

taken from a normal production run. The test oil properties are typical of that pro

duced for railway diesel engine service. At the conclusion of the test, the re-refi

diesel lube oil had bearing demerits of 7.3. The bearing appearance was bright, and

the overall rating was excellent. A photograph of the silver bearing at the conclus

of the test shows an absence of groove deposits and silver smear (figure 7)
Much has been said about engine tests, and we have our own proprietary engine

i test (figure 8). All joking aside, this figure shows a piston removed from an engine

' with over 105,000 miles, which was lubricated only with re-refined oil. Although

possibly of interest and comfort only to ourselves, it does indicate that re-refined

oil can be a quality product.

.HI

Figure 8. Piston after 105,000 miles and

lubricated only with re-refined oil.

There are many considerations involved in doing an acceptable job of re-refining.

jMuch, of course, depends on the adequacy of the technology; but the burden is ever

I upon the re-refiner to control his process and product quality through the medium of

] the same standards which are applied to the primary industry.

I

I There is no substitute for performance, and there is no substitute for control

i to maintain a standard of performance.

I'

i

j

87

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS

,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

DIESEL LUBE OIL TEST METHODS

James A. MacLean

f Caterpillar Tractor Company

Basic Engine Engineering

100 N.E. Adajris Street

Peoria, Illinois 61629

Caterpillar Tractor Company first experienced difficulty with lubricating oil

performance when we tried to put a diesel engine into a tractor back in the middle

1930 's. The trouble was the accumulation of residue from fuel and degraded oil which

forms deposits in the ring grooves of the pistons and on the lands and firmly locks

the rings in place so they cannot perform their normal function of sealing against

combustion pressure. As can be seen in figure 1, the face of the compression rings

is stained with lacquer, indicating the rings are stuck in the groove and, thus,

are not sealing. As this continues and gets worse, the second ring, which is now

not protected by the first compression ring, will begin to break up into small pieces.

This has already started in this figure. These pieces of piston ring will eventually

wallow away in the groove and seize against the liner; or, there might be scuffing

due to the increased temperature from improper heat flow out through the ring belt,

which will continue to the point that the engine will fail.

Figure 1. Diesel piston which has received inadequate lubrication.

There was a question at that time whether we could continue to offer a diesel

engine tractor because of this problem, but' our' friends in the oil industry worked

with us to develop oil additives which could reduce piston deposits and thus control

this problem. In figure 2 you can see the effect of oil additives on deposit control. These are pictures of the top part of the piston from a late model,^ 3406

Caterpillar diesel engine. From three different runs, one with a CC-class' oil, which

is not the recommended oil for this model engine, the second with a moderate performing CD-class oil (you can see the difference here in deposits on the piston lands),

and then the third with a superior CD oil. It is obvious that there is a significant

amount of difference in performance within the CD classification itself. This very

clearly demonstrates what oil additives are capable of contributing to the control of

piston deposits.

89
r ^^^^^^^^^^^^^^^

,

1 fe— -d . i

cc MODERATE CD SUPERIOR CD g|

I -J

1 -

m r~~ • • • • ""

Figure 2. The effect of oil additives on deposit control.

90
In these early days, we carried out oil tests in multicylinder engines. At first

we could not interest very many people in the oil industry in marketing the kind of

oil we needed, so we went into business for ourselves for a little while. As the

interest grew in the new oil formulations and oil companies became interested in

marketing these products, we developed a qualification system for oil and published a list of brand names of oil which we considered acceptable in Caterpillar engines. As

this oil qualification became a way of life, we developed the single-cylinder oil test

engine. This engine has had some significant modifications with time, but it is

essentially the same today (figure 3) as it was when originally designed.

TABLE 1 SUPERIOR LUBRICANTS (SERIES 3)

FOR CATERPILLAR DIESEL ENGINES

Caterpillar test no. 1-D 1-G

Duration, hours 480 480

Speed, rpm 1,200 1,800

Heat input (load) , Btu/min 5 ,600 5,850

Brake horsepower (approx.) 42 42

BMEP (approx.)

Temperatures, °F

134 141

Water from cylinder head 200 190

Oil to bearings 175 205

Air to engine 200 255

Pressures

Oil to bearing, psi 30 30

Air to engine, in.Hg.abs. 44-45 53

Fuel to injection pump, psi

Fuel sulfur, % wt

15-25 15-25

1.0 0.4

The engine test conditions that are currently used are shown in table 1, and are used for two reasons, one to assess the effects of high sulfur in fuel. This is

called the 1-D test. The sulfur in the fuel for the test must be 1 percent. In this

country, it is becoming a little unusual to find a fuel with 1-percent sulfur; however,

we market worldwide and in many areas of the world it is quite common to find fuels

with 1-percent sulfur or higher. That is why we continue to keep this test in our

system. The 1-G test is somewhat more severe in the sense that it is more highly

super-charged. Note that the BMEP level for the 1-G test is at 141, as compared to the 134 for the 1-D. If you are not familiar with the term BMEP, this is a way of

comparing the specific output of engines; 141 BMEP is a very typical output for heavyduty, turbocharged diesel engines. I think this would also be typical of our competitors - -Cummins , Mack, and so forth.

Caterpillar happened to be the first engine manufacturer to get into this oil

qualification business, probably because we were the first ones to put a diesel engine

in a tractor. Since we had started this, it became an industry-accepted specification.

It remains so today, even though in 1972 we abandoned our certification procedure and

now use other methods for describing our requirements to the field. One of these is

the military specification. It has become very common for diesel-engine builders to use the military specifications as a way of telling people in -the field what kind of

oil is recommended for a particular model of machine. You will notice that the tests

1-G and 1-D for the MIL-L-2104C are identical to those used in the Series 3 certification program (table 2) . The military qualification today is the only way that a company can get an outside organization to become involved with the approval of their

product. Many oil companies are interested in getting their product qualified by the

military so they can demonstrate to their customers that they have had an evaluation

by an independent body. But, if you qualify against the military specification, you

not only have to satisfy the diesel engine test requirement, you also have to satisfy

the gasoline engine tests also called for in that specification. This stimulated some interest in multipurpose oils, oils which were good performers in both gasoline- and

diesel-engine service. Many oil companies are interested in marketing an oil which

will satisfy the needs of both kinds of engines, gasoline and diesel.

91
The other common military specification used is MIL-L-46152, which includes one more gasoline engine test and a milder diesel engine test (table 3) . This one is used

by the military primarily for Federal gasoline -engine powered vehicles and for light

diesel trucks. However, many county, municipal, and other organizations establish

their specifications based on the military. So, again, there is a reason for people

who are supplying oil to want to go through the procedure of obtaining an approval of

their product by an independent body.

TABLE 2

MIL-L-2104C REQUIREMENTS

TABLE 3

MIL-L-46152 REQUIREMENTS

Tests and Performance Criteria Evaluated

Diesel engine performance tests:

Test No. 1-G: Ring sticking performance - high-speed 141 ME?

Test No. 1-D: Ring sticking performance - 1-percent sulfur fuel 135 H^P

Gasoline engine AMA test sequences:

lie Rust, scuffing, wear performance - low tenperature

VC Low-temperature deposition performance

L-38 Oxidation and bearing corrosion

Tests and Performance Criteria Evaluated

Diesel engine performance tests:

Test No. 1-H: Ring sticking performance - high-speed 110 EMEP

Gasoline engine AMA test sequences:

lie Rust, scuffing, wear performance - low temperature

VC Low- temperature deposition performance

L-38 Oxidation and bearing corrosion

IIIC Rust, scuffing, wear performance - high temperature

You have heard the American Petroleum Institute (API) classes mentioned, and j table 4 shows how the API service classes are related to the military specifications, j The ones for diesel engines of most interest today are the CD and the CC because most | diesel engines today use either one or the other of these specifications. Mack would i be the only exception, and they have their own qualification procedures and their own i engine tests. I Down through the years, from the middle 1930 's, there have been a number of

specification changes. As the Army upgraded their specifications, the API upgraded , theirs; and, Caterpillar upgraded theirs as the severity of the engine output was in- I creased. The chronological sequence is shown in table 5. The point I want to make i here is that this is an ongoing program. It is not going to stay at the current ! level; there are other specification changes which will come along and require addi- ; tional modifications.

j Caterpillar and some other engine manufacturers do not just use engine oil in

engines. They try to use engine oil in as many of the oil compartments of a vehicle | as possible. A few years ago we began to find that while some CD oils performed

satisfactorily in power-shift transmissions, others allowed slipping of the transmission clutch. Once the clutch slips enough, it will actually destroy itself.

Figure 4 shows segments of a failed clutch. The material in sintered bronze, and

some of the bronze material has been pulled out of position. The opposing plate is

steel, and the copper from the friction plate has smeared across the steel plate.

This is a sign of incipient failure. We find that certain CD oils will produce this

kind of failure and other CD oils will not. So, in our recommendations for transmissions these days, we have a requirement using an SAE-#2 Friction Test Machine to test the friction qualities of oils. This is called the TO-2 test. We call for a CD/TO-2 transmission oil. Becuase oil needs this extra quality for transmission

service, many oil companies will market only a CD/TO-2 oil in the constructionindustry area. So, in effect, we have added a requirement on to CD oil, the TO-2,

not for engine performance, but for transmission performance.

92
TABLE 4 TABLE 5

RELATIONSHIP BETWEEN API CLASSIFICATIONS AND MILITARY SPECIFICATIONS CHRONOLOGICAL SEQUENCE

OF SPECIFICATION CHANGES

API

service

class Military

specification

Old designations

Gonmercial API

CA MIL-L-2104A DG

CB MIL-L-2104A, Supp. 1 Supp. 1 EM

CC MIL-L-46152

MIL-L-2104B MIL-B DM

CD MIL-L-2104C

MIL-L-45199

Series 3, S-3 DS

Mack EO-H

1935 - Caterpillar Superior Lubricants

1938 - Detroit Diesel List

1941 - U.S. Army 2-104 1947 - API Engine Oil Classification (D Series)

1948 - Caterpillar Superior Lubricants (Series 2) 1950 - U.S. Army 2-104B Supp. 1 1950 - U.S. Army 2-104B Supp. 2 1952 - API Engine Oil Classification [D Series)

1954 - MIL-L-2104A

1956 - Caterpillar Superior Lubricants (Series 3) 1958 - MIL-L-45199

1961 - MIL-L-2104B

1970 - MIL-L-2104C

1970 - Mack EO-H

1970 - API Engine Oil Classification (C Series)

1971 - MIL-L-46152

Figure 4. Results of

inadequate lubrication

on a power -shift trans- mission clutch.
With all of this testing required, it can be very expensive to qualify an oil.

Table 6 lists typical costs for tests run by Southwest Reseatch Institute, one of the

independent laboratories doing this type of testing. Notice that in order to qualify

an oil for MIL-L-2104C the cost will run close to $15,000. If you add the TO-2 test,

where we require two runs minimum, it increases to $17,500. If a new additive system

is used, it is required that additional testing above and beyond just the singlecylinder test be done. We also require some kind of multicylinder engine test, so I have included the cost of an OL-1 test. So, for a new additive system for one grade

only, for both military specifications and the TO-2 and the Mack (this is the

minimum testing for a universal oil), total cost approaches $45,000. This assumes a passing result for each test run. If any test fails, rerunning of one or more of the

specified tests and possible reformulation of the oil will be necessary. We are talk

ing about a considerable sum of money to qualify an oil with these engine tests.

Everybody involved would welcome any kind of test, bench or otherwise, which would

allow us to do the job cheaper and still in a satisfactory fashion; but since 1935

we have not found a way to do it, not for oils with virgin basestocks -- not for

oils with recycled basestocks.

TABLE 6 TYPICAL DIESEL VEHICLE OIL QUALIFICATION COSTS

MIL--L-2104C MIL-L-46152

Test Cost Test Cost

1-G

1-D

lie

VC

L-38

$ 3,290

3,380

2,570

4,300

1,330

1-H

lie

IIIC

VC

L-38

$ 3,160

2,570

3,995

4,300

1,330

$14,870 $15,355

TO-2 $ 2,600 (2 Tests Minimum)

TOTAL $17,470

CD/TO-2 ADDITIONAL

1-G

1-D

L-38

TO-2

$ 3,290

3,380

1 .330

2 ,600

$10,600

OL-1

T-1

T-5

$ 7,150

6,560

13,830

New additive system, one TO-2 and Mack, October 1,

grade

1976

only, both military

- $45,000 minimum.

specifications plus assumes no reruns.

94
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

DISCUSSION

SESSIONS IV AND V. RECYCLED ENGINE OILS

There were two sessions on the subject o£ recycled oils, reflecting the current

interest and concern "with the re-re£ining o£ used engine oils back into high-quality

engine lubricants. These presentations can be separated into two groups: one on organizations with programs which are concerned with re-refined oils, and the other

on the test methods currently used on both virgin and re-refined engine oils. In the

I first group, presentations were made on the Environmental Protection Agency/U.S. Army

1 used oil program for evaluation of re-refined oils for use in military specifications;

the Energy Research and Development Administration recycled oil program, which includes

I establishing the variability of used oil composition throughout the country, develop-

! ing improved re-refining technology, and some testing of re-refined oils with engine

sequence tests; activities of the American Society for Testing and Materials (ASTM)

Used Oil Task Force; activities of the American Petroleum Institute Used Oil Management Task Force; and investigations of re-refined oils by a major oil company. The

I second group of presentations was made on the subjects of engine sequence tests for

j the determination of lubricating oil quality, screening tests used on lube oils,

I diesel lube oil test methods, and laboratory tests currently used on re-refined motor

j oils.

The discussions resulting from these sessions were long and varied, but centered

on a number of important points. There seemed to be no fundamental disagreement on whether a used crankcase oil could be re-refined into a high-quality product capable

of passing the very expensive and quality-defining engine sequence tests. The basic

problem, apparently, is that there are not enough test data on re-refined oils to

j enable these tests to be applied at a level which can produce sufficient economic

i return. A particular concern of re-refiners is that current military specifications

I specifically exclude re-refined oils, an exemption based on limited previous testing

experience with several oils. These oils apparently were not high-quality formulated

motor oils, and there was concern by a number of participants that these tests have

unjustifiably given re-refined oils a bad name. This is particularly important since

military specifications for administrative vehicle use (MIL-L-46152) are specifications that are widely used in Federal, State, and local government procurement, as well as in many industrial and company procurements for both gasoline and diesel

engine lubricating oils. Therefore, the exclusion of a particular type of oil from

these marketplaces could well have serious adverse effects, especially on consumer

acceptance. Several participants brought up the question of how these particular re- refined oils were selected for testing by the military, and it was acknowledged that

no special selection process ivas used to choose these re-refined oils, and it was also

acknowledged that the re-refined oils tested were probably not representative of the

general quality of re-refined oils. However, one of these oils was submitted to the

military for their consideration in purchase, and apparently both of the oils were

labeled as meeting certain high-quality criteria.

In several presentations, the engine sequence tests were described in some detail.

In these tests, the gasoline or diesel engine is on a test stand and is run for a prescribed period of time under very tightly controlled conditions. As many variables

i as possible are specified during the run, including the use of a standard fuel. For

example, one particular engine test runs for 196 hours. Then, the engine is dismantled

and inspected by certified "raters," who rate the engine as to the particular component

that is being tested: the Sequence IIC evaluates engine rusting and corrosion, the

Sequence IIIC primarily evaluates oil thickening and oxidation, the Sequence VC

evaluates sludge and varnish deposits, and L-38 evaluates bearing weight losses, and

the 1-H is a s inglie - cylinder test to evaluate diesel performance. The important point

was made that these engine sequence tests only evaluate selected parameters, problems

that were found to be important for virgin lubricating oils. It was suggested that

these same tests would not necessarily be able to judge whether a particular re- refined oil would be effective in actual usage or not, since the re-refined oils may

produce some problems which virgin oils do not have. For virgin oils, it was felt

extremely important that extensive correlation of these sequence tests have been made

with field data in order to establish whether or not there were problems not evaluated

by these existing tests. Apparently, such a problem had been recently discovered with

regard to a particular new additive component. This additive formulation in oil

95
apparently passed the sequence tests easily but caused excessive wear in field use. This problem was discovered in actual use, and that additive was quickly removed

from the marketplace for those uses in which there was a problem. Efforts are currently being made, particularly in the ASTM, to develop an additional engine

sequence test to help evaluate this type of wear problem.

In the current lubricating oil testing situation, the engine sequence tests

are a fairly recent development. They were first developed in the mid-1950's and

introduced in 1958. The current SA-SE classification system for motor oils was adopted in 1971. There was a great deal of discussion about the various tests for

these categories and about a perceived problem in that the SA category has no specified performance tests and the SB category has only limited available performance

requirements. Another problem is that the actual purchaser (consumer), e.g., the

do-it-yourselfer, seems to have very little understanding of what the entire classification system really means. The automobile manufacturers state in the instruction

manual that their warranties require an SE oil, and the manufacturer, by and large, seems to assume that the customer reads and remembers the instruction manual and

always uses an SE oil. It was pointed out to the assembled group that there presently

exist many non-additive oils for which rather excessive claims are made, often sounding like high-quality oils. These oils apparently sell in relatively large quantities

at inexpensive prices in retail outlets. It was also stated by several people that

approximately 50 percent of all engine lubricating oil is now sold over the counter to the do-it-yourselfers. Therefore, when individuals who do not completely understand

the service classification system purchase and change their own engine lubricating

oils, in some cases mistakes will be made and inappropriate oils used.

There was also a great deal of discussion on the question of the SE classification and under what conditions that classification is assigned to a particular oil.

During the discussion, a number of pertinent facts were brought out, including the

information that there is no formal SE qualification system. The oil is "required" to pass engine sequence tests, but this can be the opinion of the additive company or the

oil company; there is no formal approval system for SE service classification. In addition, it was brought out that in these engine sequence tests if an oil does not

pass the first time, it may be submitted for testing a second time or a third time

without prejudice. However, if a certain base oil and additive system does pass one

or more of the sequence tests, these tests do not have to be repeated in future submissions in order to fulfill all requirements for the SE classification. It is

apparently then up to the individual company to decide whether the SE quality is

obtained by that oil; each company has the responsibility to decide if that is true or not

These test results can become important, particularly in situations where a cus- tomer may make a claim against either the oil company or the automobile manufacturer,

e.g., during the warranty period of an automobile. If an oil that has an SE service

classification is used and a problem develops which entails litigation, the company

involved can substantiate that it did meet the SE performance criteria by showing the

test reports, etc., that absolve it from responsibility. It was also stated that it

would be very difficult to prove , in court or otherwise, that the oil was the primary

cause of a failure.

It was acknowledged in the discussion that it is certainly possible to put the

SE classification on a can of motor oil without running any engine sequence tests. It was felt that people in the oil companies or additive companies could put together an

SE additive package for a particular base oil and be confident that it will perform

adequately in the field without ever running sequence tests on that particular combination. Therefore, the discussion seemed to indicate that the SE service classification system is really a form of self approval; it is a way of providing a guarantee

to yourself and to other companies and of providing legal support needed in case of

claims made against you by any of your customers. The point was also brought up,

however, that the major refiners certainly have an extensive program of evaluating

their oils and additive packages, as do the additive companies; and, of course, the

engine manufacturers are also very interested in the quality of the product that will

be used in their vehicles. All of these organizations work together to try to better

define performance criteria for evaluating these oils, and, without question, many of

these companies are evaluating each other's products in order to determine whether

problems do exist. The statement was made that these sequence tests are methods

whereby the engine builders can convey to the oil industry the quality and perfor- mance required in lubricants for these modern engines.

96
There was also some discussion on the engine sequence tests and the precision

and reliability of these tests. Each of these tests was designed to evaluate specific

problems experienced in virgin oils and additive packages, and so there was some question about whether these tests would be adequate to evaluate recycled oil products

without extensive field experience with recycled products. The actual standard

deviation of the engine sequence is discussed in detail in the ASTM publication STP

315 ; however, the statement was also made that these deviations are not really that

great. And, without a particular piece of information which would indicate that some- thing has been changed or a very near miss in passing a sequence test, it would be a waste of money to just go |?ack and try again, hoping that the sequence test would be

passed

.

There was some discussion on the vari,ability of test results for the singlecylinder diesel tests. It was acknowledged that the single -cylinder diesel tests have

greater variability than the multicylinder tests for a number of reasons, including

having only one piston to evaluate, rather than multiple pistons. For this and other

reasons, the diesel tests are usually considered to be on the severe side, and sometimes a good oil will fail if the test happens to be a little more severe than normal.

In this case, people in their best judgment may want to re-run this test. It was pointed out that not only the test variability is included, but also the rating

variability. The various rating seminars have indicated, for example, that in the area of rust over half of the variability is attributable just to the rating technique

itself. Therefore, both of these factors need to be involved in the overall decision

on whether to re-run or not. However, there was general agreement that the proof of

the pudding is still performance in the field. If a lubricating oil is produced and

passes all the tests and if there are problems which start to come up in the field,

these tests certainly become questionable, not necessarily from the standpoint of the

test itself, but perhaps from the viewpoint of that particular product.

The final discussion in this session concerned expectations of the NBS efforts

with regard to test procedure development and evaluation for lubricating oils. Persons

very experienced and close to the engine lubricating oil field felt very strongly that

no bench test known can possibly replace the engine sequence tests. This was stated

to be due in part to what is called the "fuel effect," which is the effect due to con- tamination from the fuel particles, from gasoline dilution, and from the other effects

which actually occur in an engine and are virtually impossible to duplicate in any

other environment besides an engine. It was also stated that no bench tests or series

of bench tests can reliably predict how a lubricating oil basestock (before formulation with additives) will perform after formulation, or whether the formulated product

will be able to pass an engine sequence test. Finally, it was stated that, since the

proof of this system is in performance in the field and, at the present time, there

is very little data available which indicate that re-refined oils (even when formulated

to pass the engine sequence tests) can effectively function over long periods of time

in A variety of field service conditions, obtaining this type of field data was felt

to be crucial to any increased utilization of re-refined oils for motor use.

97
i

!

I

I

I,

1,
SESSION VI

BARRIERS TO UTILIZATION OF RECYCLED OILS

99

National Bureau o£ Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

RECENT USED OIL LEGISLATION

Hugh B. Kaufman

Environmental Protection AgencyHazardous Waste Management Division

Waterside Mall (AW-465)

Washington, B.C. 20460

Before I begin my short talk. I would like to give credit to a man named

Mr. Larry McEwen, who works at the Environmental Protection Agency (EPA) in the Solid

Waste Management Program. He really started a lot of our efforts, beginning about

three or four years ago. He is doing other things now, but he did a good job and

started the ball rolling. I only hope that we can continue on as well as Mr. McEwen

i did.

i Let me start by discussing a book I read about 10 or 15 years ago. It was written by a man named Mr. Robert Townsend; it was called Up the Organization . He

said that when you are in a management position or are looKing at specific issues sometimes it is good to be like a man from Mars - -pretend you are just walking in cold and

I try to figure out exactly what is going on. I did not know much about waste oil when

: I started, but I am trying to look at the subject right now as a man from Mars, as Mr. Townsend recommended. I would like to share with you some of the things that I see

.

The first thing I see is that many of you feel the best way to solve the problem

I is to form another American Society for Testing and Materials (ASTM) committee. I am not sure that is going to solve anything. Another thing I see is there is a tremendous

j preponderance of a "can't do" mentality. Let me illustrate what I mean. When we started a noise pollution program at EPA, we were talking about what we can do about

cutting down airport noise. The airport operators said, "We can't do anything; it's

the airlines." The airlines said, "We can't do anything; it's the airplanes we buy."

The engine manufacturers said, "We can't do anything; it's the guy who keeps running

his airport all day and all night." I noticed some of that going on here, too.

I have also copied down some "quotable quotes" that I have heard these past two

days. One of the things I heard was that the re-refining industry will not be able to make it; the transportation costs are going to be excessive. Mr. Belton Williams has

to go to New York and pick up some used oil and then cart it all the way back to Chicago. I also heard some comments that we can only do this in a real small urban

area because of the transportation issue. I understand that at the present time

Mr. Williams is going all the way from Chicago to West Virginia, picking up the used

oil, and then re-refining it and selling it back to the State at less total cost than

virgin oil, I also heard a statement that the engine sequence test is probably the

best way for us to know whether a lubricating oil is going to work or not. Yet, for

about three years the City of San Diego has been using recycled oil in their municipal

vehicles, and they have a lot of mileage on them by now. I do not know of any engine

sequence tests run on this re-refined oil, and I am not sure that the oil they are using could pass them if they were run.

I am saying these things not to say that what you are doing is, from my viewpoint,

wrong, or to try to cast aspersions. What I am saying is I do not think anybody here

but a few people really want the country to recycle their oil continuously. I could

be wrong, and I hope I am. In fact, it was interesting driving in today. I heard on . the radio that OPEC (Oil Producing and Exporting Countries) is going to meet again on December 15. They <are not arguing about whether they are going to raise the price or

not; they are arguing about how much they are going to raise it. I suspect the new President is going to be faced with, probably in the spring or summer, his first test

on the energy area; and they will probably have another kind of soiree and raise the

j price again.

' At the present time, a number of other countries in the world are recycling their

oil and making high-quality lubricating oil out of it. West Germany and South Africa,

for example. I would like to see us do that, too. Some people in the Congress would

like to see it also; and, I hope that Mr. Donald Becker's work and some of the

I technical people here helping Mr. Becker can help us get into that mode.

101
Before I start discussing the two pieces of legislation that are going to impact

on some of the issues we are discussing at this meeting, let me say that I would like

to see industry get their act together so the government does not always have to walk

in to help solve problems.

The first law passed involving oil recycling was the Energy Policy and Conservation Act that gave the National Bureau of Standards responsibility for developing test

procedures. The EPA has some authority in that law, too, with regard to labeling

containers of all new and used oil--more specifically, where to dispose of it and how

and to eliminate wasteful practices. "Wasteful practices" is a very interesting phrase

which we are having fun with at EPA.

The second act is the brand new Resource Conservation and Recovery Act of 1976,

which will lay down national standards for how to treat, dispose, or store hazardous

wastes. We are right now defining what a hazardous waste is, and one of the things

which might be a hazardous waste is used oil. We also have a section of that new act

which requires us to do certain things that would require the Department of Defense to spend a premium for a recycled product, compared with the price they spend for a virgin

product. There is another section which states that within two years we can take cer- tain actions to require all Federal facilities to procure recycled commodities, like

re-refined oil.

I guess most of you here have read those two acts. Some of you may not be as familiar with the second as the first. If you need further information, write me a note and I will be happy to send you copies of it, and we can also discuss them if you

are interested in doing so, especially since one of the main purposes of this meeting

was stated to be to get people talking to each other. Or, perhaps one of the problems

has been that some people have been talking to each other too long.

102
National Bureau of Standards Special Publication 488. Proceedings o£

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

THE LEAD PROBLEM ASSOCIATED WITH RECYCLED OIL

Jo S. Cooper

Environmental Protection Agency

Researqh Triangle Park, North Carolina 27711

The Environmental Protection Agency ' s - (EPA) current activities on lead as an air

pollutant are the result of recent litigation with the Natural Resources Defense

Council (NRDC) . On March 1 , 1976 , Judge Steward, Southern District of New York., ruled

in NRDC vs. Train that EPA must list lead under Section 108 of the Clean Air Act as a pollutant for which air quality criteria must be issued. Simultaneous with issuance

of air quality criteria, national ambient air quality standards will be proposed for

lead. Once an air quality standard is established, States must submit implementation

plans to EPA describing steps for achieving and maintaining such standards. Our

current schedule states that EPA will propose ambient standards for lead on August 10,

1977.

Because lead is used as a gasoline addition, it poses a problem as a contaminant

in used crankcase oil. In some cases, the used crankcase oil is burned as a supplemental fuel. The lead contained in the used oil is emitted when the oil is burned.

One of EPA's concerns regarding used crankcase oil stems from these potential emissions

of lead.

There are already two EPA regulations established to control the lead content of

gasoline. First, there is a regulation which requires the availability of an unleaded

grade of gasoline; unleaded gasoline is necessary for use in automobiles equipped with

catalytic converters. The second regulation requires the phase-down of lead content

in the total gasoline pool to 0.5 grams of lead per gallon of gasoline by October 1,

1979. Both regulations will significantly reduce lead emissions from mobile sources,

as well as the lead concentration in used crankcase oil.

Since 1971, ambient air quality levels of lead around the country have shown a decreasing trend, with most levels well below 5 yg/m^ for 90-day and 30-day averaging

periods. The decreases can be attributed primarily to the (1) introduction of automobiles with lower compression engines which require gasoline with lower octane and,

thus, lower lead content, and (2) the introduction of unleaded gasoline for use in

catalyst-equipped automobiles.

The EPA's activities relating to the establishment of an ambient air quality

standard are well underway. The draft air quality criteria have just been made available by EPA's Office of Research and Development for external review by the public.

This document addresses the scientific and technical information on lead and provides

a recommendation that an ambient level of 5.0 yg/m^ be considered as the point below

which adverse effects have not been observed. From this point, the Office of Air

Quality Planning and Standards will assess the data, determine an appropriate margin

of safety for the standard, and develop the recommendation for a proposed air quality

standard for lead. At present, our range of standard alternatives for assessment

range from 0.5 yg/m^ to 5.0 yg/m^ for a 90-day averaging period.

The burning of used crankcase oil could result in significant emissions of lead.

The majority of the studies currently available indicates that the burning of used

crankcase oil in power plants and other facilities results in ambient concentrations

below 5.0 yg/m^ for 24-hour periods. In most of these studies, the used oil is used

as a supplemental fuel and is mixed in small proportions with other fuel oils. It does not appear that burning of used crankcase oil would result in significantly high

air quality concentrations (greater than 5.0 ym/g^) unless the oil is used alone as

a fuel oil.

In support of the air quality standard, we are completing an analysis of the

total emissions of lead from the burning of used crankcase oil. Our emission calculations indicate that approximately 4,300 tons of lead per year come from the burning of

used crankcase oil. These calculations assume that 50 percent of the lead in the

crankcase oil is lost as an emission and that 300 million gallons of used oil are burned each year. The 4,300 tons of lead emissions per year from burning used oil can

103
be compared to the more than 200,000 tons of lead from automobiles each year. The

number of facilities which could burn waste oil is large, and the emission problem

could be widespread, although emissions at any one facility are probably small. At

present, we feel that the emissions of lead around major stationary sources such as primary nonferrous smelters will be our greatest problem with regard to lead, aside

from automotive emissions of lead.

The available studies regarding the burning of used crankcase oil and the analysis which we completed indicate that on the average lead emissions from sources burning used oil do not result in significantly high ambient concentrations of lead.

As phase-down of lead content in gasoline occurs and unleaded gasoline continues in

use, the lead content of used crankcase oil will decrease and the ambient lead con- centrations associated with burning of used crankcase oil will also decrease.

104
National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

FACTORS AFFECTING USED OIL RECOVERY/UTILIZATION AND

EFFECTS OF PROPOSED POLICY ALTERNATIVES

Sonia P. Maltezou

Senior Economist and Consultant

Mathematica , Inc. MathTech Division

Department of Economics

P. 0. Box 2392

Princeton, New Jersey 08540

In assessing the determinants of used oil allocation and recycling, we have

examined various facts pertaining to virgin and waste oil markets. Our analysis has

shown that there are several factors that influence the recovery of used oil and its

methods of utilization. Conveniently, we can group these factors into three classes:

1. Technical factors

2. Economic factors

3. Institutional factors

By technical factors we mean chemical and other contaminants in used oils that

prevent re -refiners from producing a final product with consistent characteristics.

Technical barriers result in higher production costs for re-refiners and affect the

overall marketability of re-refined products.

By economic factors we mean the supply-and-demand conditions in the virgin oil

markets and their influence on the supply-and-demand conditions in the used/re-refined

products markets. For example, when the price of virgin oils decreases, there is

less demand for used virgin oil, either as a fuel supplement or as a re-refining feedstock. This means less recovery in general and probatily more dumping. Beginning in

1973 with the Oil Producing and Exporting Countries' embargo and the resulting

increases in the price of virgin oils, used oil has become widely demanded and recovery

has increased substantially. However, strong profit incentives dictate that the bulk

of used oil supplies be used as fuel supplement rather than re-refined. Environmentalists view this trend with alarm because burning used oil as a fuel supplement without

control of emissions- -by far the most prevalent use recently- -results in serious air

pollution, and it creates potential fire hazards.

By institutional factors we mean government actions that directly and/or indirectly have influenced recovery, reuse, and re -refining of used oil. As we noted, the

1965 Reduction Excise Tax, by lowering the price of virgin lubricants to consumers,

resulted in approximately a 66 -percent reduction in re -refiners' output. The Federal

Trade Commission (FTC) labeling requirement (also instituted in 1965) , by emphasizing

rather the origin of the re-refined oil ("used oil") and not the characteristics and

quality properties acquired through re-refining, displaced re-refined products from

the retail market. Current regulation of the market price of virgin products also

militates against used oil recovery and re-refining.

With present policies failing to regulate the flow of used oil and, indeed, un- wittingly discouraging re-refining, many feel that there is need for some change in

current social policy toward used oil disposal and reuse methods. The general goal

of policy changes would be to encourage greater recovery of used oil (i.e., collection

of spent virgin oils) and to encourage more re-refining and less uncontrolled burning

of recovered used oil supplies.

To this effect, we have examined several proposed policy alternatives. These

alternatives fall into one of four groups:

1. Policies that aim to improve the quality of re-refined products:

Good-housekeeping regulations for generating sources

and collectors

lOS
Subsidies to re-refiners for technology improvements

j Quality tests for re-refined products 1

2. Policies that aim to change the economic incentives that burners

and collectors face, including:

j Taxes on burners

Taxes on collectors for sales to burners I Subsidies to collectors for deliveries to re-refiners ^ above normal levels of deliveries

Licensing of collectors

3. Policies that aim to lower institutional barriers to re-refined

products, including:

Taxes on virgin lubricants

Quotas for virgin oils

I Tax rebates for users of virgin and re-refined oils

j Regulating government procurement to include re -refined

j oils

Revising labeling requirements of the FTC

j 4. Policies that aim to change disposal habits and reuse methods j through educational and information programs addressed to: Used oil generating sources I Used oil direct users Buyers of virgin and re-refined oils

i The key to analyzing the effects of these policies for changing the current [ pattern of disposal and reuse to better reflect social costs and benefits is an under-|

standing of the determinants of prices and quantities in used oil markets. One can, of course, always appeal somewhat vaguely to the laws of supply and demand, but more , is required to develop an understanding that is useful for policy analysis.

| The evidence we have examined leads us to the conclusion that the used oil i collector- -the middleman between the generating sources and the intermediate or ' ultimate users of used oil - -operates as a discriminating monopolist serving two main

j sets of buyers: fuel dealers and re-refiners. These two markets have very different

demand elasticities, with fuel oil dealers' demand being far more inelastic than that ! of re-refiners'. From the resulting price discrimination model and our evidence on I demand elasticities, it followed that the supply to re-refiners is a residual and is i therefore very vulnerable to changes in conditions in virgin oil markets.

Using the discriminating monopolist model to explain price and quantity determination in used oil markets, we performed a qualitative analysis of the policy mea-

| sures listed above. In addition, whenever data were available we made quantitative | estimates of the effects of the proposed policies. From these analyses, the followingj.

conclusions were obtained. i,

1(a) Measures that improve the quality of used oil will result in an \ increase in both re-refiners' demand for feedstock and in burners'

demand for fuel supplement. They may also cause the collectors' | costs to change. The net effect of such measures on quantities j: of used oil recovered and re-refined is, thus, ambiguous. f

! 1(b) Measures that improve the real and perceived qualities of re- refined products will result, unambiguously, in an increase in I re-refiners' demand for feedstock and, hence, in an increase i

106
in recovery and re-refining. Unfortunately, it is difficult

to implement policies that improve output quality without

instituting those that improve input quality.

2(a) Measures that provide direct incentives for sales of used oil

to re-refiners (e.g., subsidies for sales to re -refi^ners)

and/or disincentives for sales to burners (e.g., taxes on such sales) will be effective in promoting re-refining and

discouraging burning. However, only those incentive measures

which have the effect of raising the marginal revenue from

sales to re-refiners (e.g., subsidies for such sales) will

result in more recovery. • If disincentive measures such as a tax on sales to burners are applied, care must be taken that

the tax is not so large as to cause collectors to exit the

industry and thereby reduce ultimately the quantity of waste

oil recovered.

2(b) Measures that require licensing of collectors and constrain

collectors to sell specified quantities to re-refiners will,

if enforced, result in increased re-refining. Whether or not

these measures will result in increased recovery and/or

decreased sales to uncontrolled burning will depend upon the

incremental cost of additional recovery relative to the

incremental loss of revenues of diverting sales from burners

to re-refiners. Constraint levels must be structured care- fully to avoid driving collectors out of the market altogether.

3(a) Measures that provide for taxes or returnable deposits on virgin lubricants will promote additional recovery and re- refining. However, the imposition of a tax introduces a distortion in the market for virgin lubricants if current

price and marginal social cost are approximately equal.

3(b) Measures that remove institutional barriers to the marketing

of re-refined products (e.g., government purchase specifications, labeling requirements), assuming that there are no valid reasons for such barriers, will increase the demand for

re-refined products and, hence, result in more re-refining,

more recovery, and less burning.

4 Measures that aim to educate the public on used oil handling

and reuse methods, as well as on the properties of re-refined

products, may contribute to higher recovery, less uncontrolled

burning, and higher demand for re-refined products.

Unfortunately, in this study as in so many other studies of environmental

resource policy, we have had to leave many questions unanswered. The most important

of these is: "Just how far should we go in encouraging recovery and re-refining and

in discouraging burning of used oils?" To provide a fully satisfactory answer to this question, we would need a great deal of quantitative information of the social

costs of the various methods of used oil reuse and disposal and information on the

social costs of implementing the various different policy measures that we have discussed. The problem of information unavailability clearly points to the need for

future work on the benefits of environmental protection. However, while the evidence

on benefits is being gathered, practical decisions will be made concerning target

levels for recovery, re-refining, and burning of used oils. Whatever target levels

are selected, we have shown that there are both effective and ineffective measures

for implementing these targets. Indeed, we have demonstrated that many of the

commonly proposed measures which we have examined will actually work in a direction

opposite to that intended. We concluded that used oil policy makers must conduct

economic analyses of the policy options under final consideration if serious mistakes

are to be avoided.

107

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

ENERGY CONSERVATION ASPECTS OF RE-REFINED OIL

Gene J. Mascetti

Environment and Energy Conservation Division

The Aerospace Corporation

2350 E. El Segundo Boulevard

El Segundo, California 90245

I I am going to discuss a study we have in progress related to the energy conservation aspects o£ re-refined oil. The scheduling of this meeting relative to the

I scheduling of our study is such that we are not far enough into the study to be able

I to present answers, but we can tell you something of what we are trying to do in this

j study.

! Most of the information is found in the tables, and I will just cover these

I rather briefly; I hope they are somewhat self explanatory. The title of our study is

i "The Energy Conservation Aspects of Re-refined Oil." I am in the Environment and

I Energy Conservation Division of The Aerospace Corporation. This study is being sponI sored by the Alternative Fuels Branch of the Division of Transportation Energy Conservation of the Energy Research and Development Administration (ERDA) . Mr. Eugene

Eckland is the Branch Chief.

A summary of the items covered in the briefing is found in table 1. As I said,

this is a presentation of what we are planning to do in the study, how we are planning

to do it, where we are, the factors we are going to consider, and some initial obserj vations we have made from looking into used lube oil re-refining and from talking to

1 people in the industry.

TABLE 1 TABLE 2 BRIEFING OUTLINE BACKGROUND AND OBJECTIVES

• Background and objectives

• Study approach

• Task description

• Study status and initial observations

• Re-refining energy and process

considerations

• Virgin lube oil energy requirements

Factors impacting production and usage

of re-refined oil

The background of our study, which was initiated in September 1976, is shown in

table 2. The study is concerned with the assessment of re-refining issues and does

not involve the development of new technology. The basic scenario that we will

address is designed to provide a more clear-cut answer to the question: "Is the use

of used oil re-refined back to lube oil the best use?" A second scenario assumes burning of used lube oil in furnaces.

• Study initiated in September 1976

- Projected completion date March 1977

• Assessment of energy conservation potential of re-refining lubricating oil

- Re-refining of used oil to lube oil

- Utilization of used oil as a fuel

• Required lube oil produced from

crude

• Study tasks

- Survey and evaluation of re-refining

process

- Economic and institutional aspects

of re-refining

- Cost/benefit analyses

- Recommendations for future ERDA

action

109
The study basically has four tasks, which are: survey of re-refining processes;

economic and institutional aspects of re-refining; cost/benefit analysis; and, finally,

recommendations to ERDA regarding future re-refining issues.

Our basic study approach (table 3) is to acquire and assess data. As I said

before, we are not attempting to develop technology; this is an assessment study. The

items we will be covering in the assessment range from process technology to the

TABLE 3 STUDY APPROACH

• Data acquisition procedure

- Review of literature related to re-refining of used oil

• Lube oils

• Hydrocarbon oils (not synthetic)

- Liaison with industry

• Re-refiners and refiners

• Government agencies and laboratories

• Universities and research organizations

• Additive manufacturers

• Data review and assessment summary

- Process technology

- Process economics

- Energy requirements

- Product utilization (marketing]

- Impact on crude oil usage

ability of the re-refining industry to remain healthy and viable and to re-refine used

oil successfully. The so-called "bottom line" is the impact of our two scenarios of

disposing of used oil, either by burning or re-refining, and the impact on crude oil

usage

Detailed objectives in the study plan are given in table 4. These correspond to the four original ones that I showed rather briefly before.

Task A, as we call it, is basically the compilation of data on re-refining.

Task B is an assessment of the data that we have acquired and assembled in a logical

order. This type of task is directed to the economic viability of the industry to re-refine oil. Task C is termed the cost/benefit analysis; this contains two scenarios

that we propose where the used oil is either re-refined back to lube oil or mixed with

fuel oil for subsequent combustion in a furnace or boiler.

In the scenario that looks at the burning of used oil, we would like to address

two aspects, one where used oil is just burned straight, and the other where it is

processed back to the equivalency of a fuel oil, which increases costs and its desirability as a fuel oil. The task output of this item is the assessment of energy i aspects of used oil utilization.

The final task is based on the previous work--to provide ERDA with recommendations

for their action. Potential items are shown in the table. ERDA, of course, will not

be providing legislative assistance, but perhaps they will be in a position to recommend certain legislative action. I The current s'tatus of the study is shown in Table 5. We are essentially completing the acquisition of data at this time. Some of the typical sources of information

j are shown. We did a patent search to see what kind of new processes or technologies i were potentially available and talked to people in the business.

| Some observations that we are finding as we go through data and talk to people ' are that the re-refineries that we have seen typically lack sophisticated instrumentation to keep track of process energy requirements. Some data we would like to have , for this study are not available; they are generally proprietary, and we cannot use

them. On the operation of refineries, we would like to address actual energy savings. '

110-
TABLE 4 TASK DESCRIPTION

Task A: Survey and Evaluation of Re-Refining Processes

• Lube oil re-refining processes

- Existing and new processes

- Process description

- Process equipment requirements

- Process energy requirements

-Product type and yield

-Environmental impact

• Task output

-Collation of data on process design, plant operation,

economics, etc. Task B: Economic and Institutional Aspects of Re-refining

• Process economics and energy evaluation

- Plant capacity

-Plant investment, operating costs, return on investment

- Feedstock collection and transportation

- Plant environmental considerations

-Expansion of capacity and conversion to new processes

- Assessment of process energy requirements

• Institutional impacts

- Specifications on lube oil quality

- Usage by governmental agencies

- Financial/ tax assistance to re-refiners

• Task output

- Assessment of technical and economic aspects of existing and new processes

Task C: Cost/Benefit Analysis

• All used oil re-refined back to lube oil

- Petroleum savings due to less virgin lube oil production

- Replacement of used oil currently used for road oil and fur- nace fuel by fuel oil or residual oil

• All used oil used as furnace fuel

- Increase in petroleum consumption to satisfy lube oil demanct

- Assessment of potential problems related to combustion of

waste oil (burner corrosion, burner operation, emission of

trace elements)

- Burning of untreated used oil versus processing of used oil

to comply with fuel oil standards

• Environmental considerations

• Economic impact

• Task output

- Assessment of the energy aspects of used oil utilization

Task D: Recommendations for Future ERDA Action

• Preparation of plan for future government-supported activities

in the area of used oil re-refining

- Technology research and development

- Demonstration of new processes

- Legislative assistance

- Environmental considerations

111
TABLE 5 STUDY STATUS AND INITIAL OBSERVATIONS

• Data acquisition phase nearly complete

- Government publications

- SAE publications

- Industry reports

- Journal articles

• Patent search completed

- Approximately 50 patents located

- Covers 1950 to 1975 time period

- U.S. and foreign patents

• Liaison with industry and ether organizations in progress

- Re-refiners, refiners, and additive manufacturers

- Government agencies, universities, and research

organi zations

• Literature and data review and assessment in progress

- Acid clay process widely used (sludge disposal; new processes)

- Many existing plants are small, individually owned,

and old

- Re-refinery plants run on self -generated fuels

- Heat recovery equipment not widely used

- Sophisticated process instrumentation lacking

- Computer modeling required to assess refinery

operations

- Some data considered proprietary

- Energy conservation may be secondary to environmental

and natural resource issues

If a mixed refinery product were produced at a different ratio of lube oil to fuel oil,

would there be savings in process energy? These data typically require a sophisticated

computer model of the refinery. We do not have practical information from industry on

this subject. It appears that perhaps the energy conservation potential may not be

the big driving force, but rather lube oil availability and/or conservation and the

environmental issues will be of primary concern. Table 6 shows what we are attempting to do in regard to re-refining, energy con- servation, and energy usage. We would like to consider the overall energy required in

the re-refining process, which includes the energy required to collect the oil, the i energy required to dispose of waste products, process energy, and the energy required ' to make chemicals or other treating agents used in the re-refining process. !

TABLE 6 RE-REFINING ENERGY AND PROCESS CONSIDERATIONS

• Process energy

• Process applicability to available feedstock

- Industrial oil

- Crankcase drainings

• Process suitability to scale of operation

• Process yield and characteristics of end product

• Credit for usable by-products

• Manufacture and transport of process chemicals

• Collection and transportation of used oil

• Waste product disposal

112
TABLE 7 TABLE 8 VIRGIN LUBE OIL ENERGY

REQUIREMENTS

FACTORS IMPACTING PRODUCTION AND

USAGE OF RE-REFINED OIL

• Current refinery practices and yield

of lube oil

• Change in refinery efficiency due to lube oil/fuel oil product shift

- Reduced virgin lube oil production

due to demand filled by re-refining

used oil

- Increased virgin lube oil production due to expansion of market

and no recycling of lube oil

• New lube oil production technology

- Hydrotreating in place of solvent

extraction

• Availability and difficulty of

extraction of lube oil from new sources of crude

Industry capacity

- Approximately 10 to 20 percent of

available used oil

- Number of re-refiners declining

~ Existing capacity not fully utilized

Capability for expansion

- Availability of feedstock

- Availability of capital

Product acceptance

- Question of quality

- Cost relative to virgin lube

- Widespread availability

- Label recognition

Legislative impacts

- Product standards and specification

- Controls on used oil disposal

- Environmental controls on re-refinery

operations

- Favorable tax legislation

- Mandatory utilization of re-refined

lube oil by governmental agencies

Table 7 is essentially a corollary to the preceding table. Here we are looking

at the total energy requirement to produce virgin lube oil using current refinery

practices. We would like to address the potential energy changes for varying product

mix, and maybe address new lube oil production techniques, such as hydrotreating, that

may make a lube oil from virgin crude less energy intensive. The final item shown is to try to predict future production of virgin lube oil from crude. It may not be as suitable or as easy to obtain as it is from current crude stocks.

Finally, in table 8 we delineate some of the factors we see that are impeding the

production and use of re-refined oils. Industry capacity has been declining in recent

years, and the typical re-refiner is a small businessman who generally lacks capital

to expand and who is also having difficulty increasing the availability of feedstock.

Of course, they will be in competition with the fuel oil people. The other serious

problem is related to product acceptance, quality, and costs relative to virgin lube

oil. Another somewhat institutional concern is the ability of a customer to recognize

the label. If he were buying a major brand, like Shell X-100, the label is recognized

from the east coast to the west coast; re-refiners tend to be small with brands which

are only distributed locally. Consumers are often reluctant to buy brands with which

they are not familiar. There are legislative impacts, which were previously discussed,

which can drastically influence the fate of re-refined oil. These include the development of product standards and specifications for re-refined oil, the amount of controls that are applied on used oil disposal, passage of favorable tax legislation, and

the use of re-refined oil by government agencies to provide an example for the marketplace .

113

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

MARKETING BARRIERS FOR RECYCLED OIL

Peter M. Cukor

Vice President

Teknekron, Incorporated

2118 Milvia Street

Berkeley, California 94704

I would like to discuss briefly some of the important conclusions of three of the

six parts of the recent studies we performed for the Environmental Protection Agency

(EPA) and how these relate to the problems of encouraging new investment in waste oil

recovery by re-refining [1, 2, 3].i This is important because the "bottom line," from

all the discussion we have had with re-refiners, oil companies, and private investors,

is: "Will anybody invest money in this business?" Money will be invested in re- refining only if an adequate return can be realized.

Rather than take a theoretical approach in trying to describe the economics of

re-refining, we conducted extensive interviews with industry representatives. Most of

the conclusions of our work are based on interviews with about 24 re-refiners which

were carried out in 1973, 1974, and 1975. It is interesting to find, however, that

firms in existence today differ from one another quite a bit; and those that went out

of business in the 1960's differ quite a bit from today's firms, as well.

Although some firms are larger than others, the major difference between firms is

the markets served. We found three different kinds of re-refiners. There is the re- refiner who, in the main, produces base oil for sale to jobbers or wholesalers. This

is an SA oil, perhaps an SAE-20, sold in the wholesale market. Such re-refiners compete with other lubricating oil wholesalers; they do not sell oil to final users. The

second kind of re-refiner sells to the final-user market, typically to commercial

customers such as operators of vehicle fleets, industrial firms, etc. In this case,

re-refined oil competes with established major brands of oil; the re-refiner sells

directly to the final user and at a price substantially greater than that charged the

wholesaler. The third kind is the custom "closed cycle" re-refiner who deals with

railroad or industrial oils. He is really providing a service, rather than a product.

This is an important distinction because the question then is not, "Is the quality of

re-refined oil as good as the quality of virgin oil," but rather, "How well have I segregated my product and how well is the re-refiner doing his cleaning." It is quite

a different situation.

Our conclusions from the survey were as follows. Firms which sell mostly in the

wholesale market had the worst economic performance, and I will describe the reasons

for that shortly. Most firms which sell in the commercial/ Indus trial market were able

to survive through the difficult times of the 1960 's and early 1970 's and are, by and

large, the most profitable. Therefore, one of the major recommendations of our study

was to examine marketing barriers to the sale of re-refined oil in the commercial/

industrial sector.

j Before discussing the different market sectors, let us take a look at figure 1,

j which shows the refinery gate price of a 300 neutral lube oil, f.o.b Houston, as a

I function of time

.

Many of you have heard the frequently cited statistics that there were about 150

j re-refiners in business in 1960 processing about 300 million gallons per year and that

currently there aije somewhere around 26 re-refiners processing under 100 million

gallons per year. Now, consider the refinery gate price for 300 neutral lube oil.

From 1960 to 1974, it remained essentially constant. Of course, the cost of re- refining did not remain constant during that period. As a consequence, you can see

[very clearly that if you had to sell re-refined oil in the wholesale market (at a price

I discount because in this market re-refined oil competes with the lower grades of virgin

oil, not this 300 neutral) you could probably sell it for about $0,23 or $0.22 per

gallon over this period of time. So, re-refiners during that time were caught in a

Figures in brackets indicate literature references at the end of this paper
53

60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 JFMAMJJASONDJFMAMJJASONDJFMAM

YEAR

Figure 1. Refinery gate price for 300 neutral lube oil 1960-1975 [4,5],

116
classic cost/price squeeze, and a lot of them went out of business. The cost of re- refining went up due to the higher cost of collection, increased use of acid to remove greater concentrations of additives, increased labor and material costs, etc. After

the Arab oil embargo, prices rose very sharply. Part of that very sharp rise was a consequence of price controls. Following the embargo, price controls on fuel oils were removed; however, controls on lube oil prices remained, creating a shortage of

these products. This enabled some re-refiners to penetrate markets they had never

served previously. It also tended to push up the price at which lube o,il was sold

after price controls were relaxed. Since that time, prices have softened somewhat,

and I believe they have now risen to where they were somewhere in early 1975.

The point of this discussion is that re-refiners serving the wholesale market

could not increase prices for about 15 years; now prices are higher, but so are costs.

If we again see a period of continued moderation in the price of oil at the same time

that other costs are escalating, we are likely to see a recurrence of this cost/price

squeeze. Therefore, the re-refiner who sells in the wholesale market, where profit

margins tend to be smaller than in the final-user market, is vulnerable to considerable

fluctuations in profitability.

The conclusion is as follows: How does a re-refiner penetrate the final-user

market? Again, we use some examples of what existing re-refiners have done. I would

like to talk about two final-user markets now and restrict my discussion to crankcase

oils . First, let us discuss the retail market. As part of the program for EPA,

Teknekron conducted a survey of lube oil consumers in Oakland, California [2]. We

I interviewed about 600 people who were buying lubricating oils at automotive supply

1 stores and discount houses. We had a number of objectives of this study. One was to investigate the possibility that purchasers of "over-the-counter" oil would return

their used oil for recycling. We also investigated some of the purchase habits of

retail consumers - -why they bought what they bought. Table 1 shows the API/SAE

(American Petroleum Institute/Society of Automotive Engineers) specifications of oils

bought by the interviewees. You can see that, in the main, top quality SD and SE oils

I were bought. Very few customers bought non-detergent oils. This may lead someone who

i is not familiar with oil marketing into thinking that the individual consumer is quite

I sophisticated. However, we found that most purchasers did not know what those letters

mean and probably could not care. Table 2 shows the factors that led to the oil purchase. We asked the people, "Why did you buy what you bought?" We recorded the

number of times, each factor was mentioned. As you can see, brand name was mentioned

approximately twice as often as lowest price. It is interesting that viscosity

received a higher frequency of response than the API classification. It shows that

the consumers may not be conscious of the difference between viscosity and performance

level. The conclusion here is, of course, that brand name is the major factor. It is

a surrogate for quality. Most consumers never want to see lubricating oil; they

certainly do not want to get it on their hands. There is no way they can tell how good

it is by looking at it. So, they buy on the basis of brand name.

TABLE 1 GRADE OF OIL PURCHASED [2]

Number of

respondents Percent

SC and SE 245 41.7

SD and SE 96 16.3

SC and SD-SE 69 11 . 7 SE 68 11.6

SA or ML 40 6.8

SC or MS 21 3.6

SB and SC 20 3.4

Others , rated 20 3.4

1 Others , not rated 9 1.5

100.0

TABLE 2 MOST IMPORTANT FACTOR

IN PURCHASE DECISION [2]

No . of times Relative

Factor mentioned frequency, % Brand name 349 65

Lowest price 114 21

Viscosity 34 6 API classification 8 2 Others 31 6 TM

117
TABLE 3 FACTORS IN OIL PURCHASE DECISIONS [2]

No. of times

mentioned

Relative

frequency, % Brand name 461 56 .

Lowest price 199 24 .

Vi s CO s i ty 69 8 .4 API classification 1 9 1 r 1 . 0 Recommendations of mechanic,

dealer, or manufacturer 13 1.6

Medium price 6 0.7

Recommendations of friends

or relatives 5 0.6

High price 5 0.6

Labeling^ 3 0.4

Other reasons 46 5.6

819 100 .0

Respondents were then asked to rank these factors in their order

of importance in deciding which oil to buy. Whereas brand name

was mentioned 2.3 times as often as lowest price, brand name was selected as the most important factor in the purchase decision

3.1 times as often as lowest price.

refers to phrases like "meets or exceeds all car manufacturers'

warranty requirements."

Table 3 indicates the frequency with which each of the factors listed in table 2 was mentioned as the most important factor. The previous table showed that brand name was mentioned twice as often as price. Here we see that in considering the most

important factor in the purchase decision, brand name was mentioned three times as often as price. A logical question is: "Is there any difference in consumer purchase

habits between those who buy only small amounts of oil and those who buy a lot of oil"; The answer is shown in the next table (table 4) where we did a cross tabulation.

Table 4 relates the most important factor in oil purchases to annual oil consumption. Again, we see that those who consume the most lube oil tend to make purchase

decisions on the basis of brand name rather than price or other factors.

What can we conclude from this information? It is clear that in the retail

market brand name is really the prime indicator of quality. We interpret this to meai

that customers view the brand name as a surrogate for quality. This implies that re- refined oils sold in the retail market under the label of an independent re-refining

company probably cannot compete with quality virgin oils produced by the major oil

companies. For this reason, some re-refiners who do produce quality oils tend to disj

courage or even prohibit their sale in discount houses or service stations. j

1

.1

118
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119
FEDERAL LABELING LAW

LOW QUALITY OF RE -REFINED

OILS WHICH ARE AVAILABLE

TO THE PUBLIC

LACK OF CONSUMER ACCEPTANCE

OF RE-REFINED OIL

RE-REFINED OIL AT

LOW PRICES IN COMPETITION WITH LOW

QUALITY VIRGIN

RETAIL SALES OF

LUBRICANTS

Figure 2. Barriers to public acceptance of re-refined oil [3]

In figure 2, we see an interesting phenomenon with regard to barriers to public

acceptance of re-re£ined oil. Keep in mind the situation in the retail market, and

let us consider some of the historical problems faced by the re-refining industry.

On the right side we have this lack of consumer acceptance. Re-refined oils never really have enjoyed a quality image. Although some re-refiners produce quality products, the re-refining industry has a history of opportunists and men of questionable

integrity whose actions have discredited the products of the quality-conscious firms.

Partially as a result of this situation, the Federal Trade Commission established

labeling regulations to protect the consumer from these shady operators. Because of

these regulations and because of the lack of consumer acceptance, we find that highquality re-refined oils are not sold in the retail market because retail customers

buy on the basis of brand name. This tends to reinforce the public's negative image

of re-refined oil. And what does re-refined oil compete with in the retail market?

They compete with the cheapest oils available, some of which have a negative viscosity

index (VI) or a very low VI. Some of the jobbers I have interviewed actually admitted

to buying negative VI base oil from virgin oil producers and blending it with re- refined oil to raise the VI. These products sell for $0,30 to $0.40 a quart or less.

There is no incentive for re-refiners to produce quality oils for the retail market

because retail consumers do not believe that they are of high quality and will not

pay the required price to make that sale attractive. So, we have this "vicious

circle .

The real question one wants to ask is: "How do you break that vicious circle?"

The only way I can think of is if the major oil companies were to sell re-refined

oil--not necessarily produce it, but sell it. Then re-refined oil might be accepted

in the retail market as a quality product. There is some evidence that over the

past couple of years at least one, and perhaps two or three, major oil companies have

actively investigated the feasibility of doing this. I think that the recession of

1974-1975 tended to dampen this activity quite a bit because lube oil supply became

relatively abundant. As far as the retail market is concerned, acceptance of re- refined oil will require the participation of those firms which have earned the con- fidence of quality-conscious consumers.

Let us talk briefly now about the commercial market. There are a couple of key

differences between the commercial and the retail market. Of course, the commercial

customer buys a lot more oil than an individual. The contact between the seller and

the consumer is direct, not through a middleman or a marketing outlet. The consumer

also tends to be able to evaluate the quality of the oil more objectively than the

individual purchaser in the retail market. He can look at the oil pressure guage on his vehicle; he frequently monitors the oil consumption. If he drives a dieselengine truck several hundred thousand miles, he is certainly very concerned about

frequency of maintenance. He is also very concerned about customer service. I understand that some of the major oil companies have been rationalizing their marketi,

120
operations so that they pay less attention to some o£ the more specialized, lower

volume accounts. This is an opportunity for re-refiners.

So, the factors for success in this commercial market are, of course, quality

assurance, a competitive price, and service.

How do we get this quality assurance? This is certainly a concetn for the

National Bureau of Standards. As the gentleman from Cummins said earlier, it is

very expensive to provide quality assurance. How have re-refiners been able to compete successfully in the commercial market? They have not succeeded because their

products have been qualified under specification MIL-L-2104C. Rather, re-refiners

have been able, over a number of years, to, establish "toe to toe, belly-to-belly"

relationships with quality-conscious commercial customers based on product quality

and reliable service.

One question that I think the government has to address now is how do you enable

a producer of re-refined oil to penetrate the commercial market without having to spend, say, 25 years in the business; you will not be able to attract new investment

in waste oil recovery unless investors can earn a reasonable return in a relatively

short period of time. Let me cite an interesting example. One of the firms we interviewed had historically sold almost all of its oil in the wholesale market, earning

about $0.01 per gallon on such sales. In the winter of 1974, when the Federal Energy

Administration had released price controls on fuels but not on lubes, the City of San

Diego received only one bid for its lube oil supply for the following year.- The only

bidder was the local re-refiner, who was awarded the contract. As a result of this

contract, he has been able to expand his commercial business on the basis of customer

satisfaction. The City of San Diego is, of course, a large quality-conscious customer

and a very visible one. Because of the favorable image of selling oil to the City,

this re-refiner has been able to compete in the commercial market. Now, more than

half of this re-refiner's sales are in the commercial sector, and he is making enough

money to expand his plant and facilities. So, I submit that if re-refiners want to expand sales to commercial consumers, they must get a foot in the door somehow. And,

if the government is interested in stimulating investments in re-refining, then perhaps some demonstration projects involving municipalities. State governments, or larger industrial or commercial firms which are willing to participate would go a long way towards showing that re-refined oils can be acceptable to the consumer. Once

this happens, the barriers in the commercial market will be much reduced, thereby

increasing incentives for investment in waste oil recycling.

References

[1] A Technical and Economic Study of Waste Oil Recovery, Part VI: A Review of

Re-refining Economics, Tekenkron, Inc., EPA Contract 68-01-2904, October 25,

1975 .

[2] A Technical and Economic Study of Waste Oil Recovery, Part II: An Investigation

of Dispersed Sources of Used Crankcase Oil, Teknekron, Inc., EPA Contract

68-01-1806, October 1973.

[3] A Technical and Economic Study of Waste Oil Recovery, Part III: Economic,

Technical and Institutional Barriers to Waste Oil Recovery, Teknekron, Inc.,

EPA Contract 68-01-1806, October 1973.

[4] Platts Oil Price Handbook and Oilmanac, 1960-1974.

[5] Platts Oilgram, January-May 1975.

121

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg , Maryland, November 22 and 23, 1976. (Issued August 1977)

DISCUSSION

SESSION VI. BARRIERS TO UTILIZATION OF RECYCLED OILS

There were five speakers in this session, and their presentations were on the

topics of the recent used oil legislation, the lead problem in recycled oils, economic

aspects of used oils, energy conservation aspects of oil recycling, and marketing

barriers for recycled oil. Besides the legislation under which the National Bureau of

Standards (NBS) is working, additional recent legislation affecting used oil includes

the Resource Conservation and Recovery Act of 1976 (Public Law 94-580) and, perhaps,

the Toxic Substances Control Act (Public Law 94-469) . This legislation affects both

the conservation of resources and the environmental and the toxicological problems

with disposing of certain types of waste products. The lead content of used oil has

been considered a serious environmental problem for many years, especially for uncontrolled burning or disposal. Recent court decisions have required the Environmental

Protection Agency (EPA) to set ambient air quality standards for lead, and the level

currently being discussed was reported to be about 5,0 yg/m^. These recommendations

were apparently based on data reported in the- literature; and, according to the

discussion, EPA has not made, burning tests to evaluate this problem first hand. Also,

it was reported that, to date, lead is the only trace element being evaluated for an ambient air standard.

Discussion on this question suggested that perhaps the total mass of lead from

used oil was rather small when compared to total lead emissions due to gasoline. The

rough estimate of contribution to lead emissions due to the burning of used oil was

about 2 percent, although the uncontrolled burning of used oil was indicated to be

the largest stationary source of ambient air lead at the present time. Also, during

the discussion, the information was mentioned that some of the calculations involved

in the test of burning waste oil at the Hawaiian electric plant apparently were in error. New data sheets have been released with these corrections, and the new figures

indicate that a maximum of 2.7 yg/m^ was found 1,800 meters downwind for normal burning operations, with figures considerably higher than these for soot-blowing periods.

Another important question which was addressed was the total energy conservation

aspect of recycling used oils. The Energy Research and Development Administration has

contracted for a study of this question, and preliminary indications are that, indeed,

recycling of used oil back to a high-quality lubricant requires less energy than

refining a high-quality lubricant from crude petroleum. However, this total energy

conservation aspect apparently depends a great deal on the refining methodology used,

since the energy requirements per barrel of crude were stated to differ significantly

among refineries. Some of these calculations went into detailed energy balances,

including solvent extraction refinery processes using furfural extraction, followed by

additional solvent extraction, with hydrotreating and dewaxing, etc., with the result

that substantial amounts of energy are expected to be saved by re-refining, rather

than burning and replacing the lube oil by the virgin product. This calculation

included losses in the acid-clay process (which are higher than any other re-refining

process) and assumed a water content of the used oil of about 7 percent and a light

petroleum fraction of about 3 percent. Also during the discussion some differing

calculations were discussed that had been made by the virgin refining industry, and

these calculations indicated that, while re-refining still appears to conserve energy,

the amount of saving is down to about 4 percent or 5 percent. There was some question

as to whether these particular calculations were on a very efficient refining operation versus many other companies which have less efficient virgin lubricating oil

refineries. A sensitivity analysis on the different variables considered in the first

set of energy calculations indicated that the quoted savings of 4 percent or 5 percent

were for the lowest case; and, for the average or the best situation, the savings

could be considerably higher. Another aspect that was brought up on the question of

energy savings was whether the energy cost of a failed piece of equipment was considered in these calculations. It was acknowledged that such energy costs were not

considered, but that effective quality control on a re-refined oil product should be

able to bring these costs in line with similar costS' for virgin lubricating oils.

Some of the economic questions which were discussed included the ability of

retail customers to recognize a quality oil. It was reported in one paper that a study of over 600 people who were queried as to why they bought a particular

123
lubricating oil for their automobile indicated that brand name was the preferred

determinant, with price a distant second. It was suggested that re-refiners could

break into the quality oil market most easily by having their product marketed under

a national brand, e.g., marketed by a major refiner.

It was also mentioned that currently the strongest area for re-refining is custom

re-refining or re-refining for industrial, commercial, or fleet-type operators. In this commercial area, the re-refiner can offer personalized service and long-time

effective relationships in order to obtain and retain these markets. A case in point

used to illustrate this is the use of re-refined oil by the City of San Diego. During

the energy crisis, this city had difficulty obtaining bids for their lubricating oil

products. A local re-refiner bid and, after some investigation, this supplier was accepted and even now retains the market for the entire fleet of city vehicles. This

is, in effect, not a closed-loop system in that the re-refiner bid on an equal basis

with all other lube sources, and no requirement to pick up and/or reprocess the existing city waste oil product was involved in the contract. However, once the quality of

the re-refiner's product was established through testing and use, the purchaser was happy to consider the re-refined oil on an equal basis with all other lubricating oil sources. The widely disseminated and favorable publicity for the re-refiner has also

apparently resulted in improved marketability of their products throughout the area. Finally, it was pointed out in some detail that there is a large number of

economic and political factors which interplay in the area of re-refining, including

legislation, economic questions, disposal of hazardous waste materials, marketability,

and consumer acceptance. There was extensive discussion on the question of whether

it was economic or practical to try to market a recycled oil at the highest quality

levels. This discussion acknowledged the possibility of doing almost anything if

economics, cost, practicability, etc., were not taken into consideration. The example

was quoted that even though a man can be put on the moon, moon travel was not an established transportation means. As a result of this comment, there was a general

question brought up as to whether everybody agreed that re-refined oil was really

capable of being formulated into a high-quality engine oil. In the ensuing discussion.i

it was asked if there were anyone in the room who did not agree that this could be I done, i.e., did everyone agree that a used crankcase lubricating oil could be re- i refined into a high-quality motor oil. The response indicated that all agreed that j this, indeed, was the case. However, several statements were made that the economics | indicated to them that the most reasonable position to take was that used oil should ! be recycled into fuel or industrial oils, depending upon which was most reasonable for | a particular situation. It was felt that the economic cost of testing would be a deterrent to assuring suitable quality control in the re-refined motor oil field.

Indeed, several statements were made that a re-refined automobile crankcase oil made

an excellent base oil for many different types of industrial and hydraulic oils.

Another aspect of the economic factors influencing re-refining and recycling discussed

| was the government "interference" in the mid-1960 's which eliminated favorable tax

treatment and effectively taxed re-refiners more than virgin oil refiners and the

Federal Trade Commission trade regulation which prescribed unfavorable labeling of all

recycled lubricating oil products.

It was readily apparent during all these discussions that there were many areas which affected the oil recycling industry, and the difficulty of working with all of

these factors simultaneously has created problems in many areas for the re-refining

industry.

124
SESSION VII

PROBLEMS AND NEEDS IN ESTABLISHING QUALITY FOR RECYCLED OIL PRODUCTS

125

National Bureau of Standards Special Publication 488. Proceedings of

a Workshop on Measurements and Standards for Recycled Oil held at NBS,

Gaithersburg, Maryland, November 22 and 23, 1976. (Issued August 1977)

DISCUSSION

SESSION VII. PROBLEMS AND NEEDS IN ESTABLISHING QUALITY

FOR RECYCLED OIL PRODUCTS

This session was a free and open discussion, with no formal presentations. All

of the previous subjects were discussed, to a greater or lesser extent, with an emphasis on motor oils as the subject of primary interest. Summaries of these discusI sions are included below.

I The session started with a brief description by the moderator on his perceptions

of some of the basic assumptions that could be described at the present time. These

assumptions are: (1) the legislation under which the National Bureau of Standards

I (NBS) is working is clearly supportive of the concept of recycling used petroleum oils;

I (2) used oil collection and waste management methods are going to improve with time,

I producing a larger feedstock volume for the various end uses considered; (3) the major

foreign system that effectively recycles used lubricating oils (West Germany) seems to

! work very well in practice, and this system is partly supported by a tax on virgin

lubricating oil which helps to pay for recycling or disposal of the used oil; and

(4) the Congress of the U.S. has mandated that the Federal Government will become

involved in this subject area. These assumptions will have to be realized and accepted

I by everyone in order to work together to try to obtain the best possible solution to

j the existing problems. Where oil recycling goes from here depends a great deal on the

, manufacturers, the refiners, the re-refiners, the consumers, and everybody else working together to try to get the most beneficial use out of this natural resource,

consistent with reason and common sense. With those comments, the floor was opened to discussion

.

j The first area of discussion was on the subject of labeling requirements and

I their effect on consumers. A major oil company representative discussed some of their

I considerations as to whether to get into marketing a re-refined lubricating oil and

product and stated that one of the important reasons why they did not try to market

that product was because an independent survey of consumers had indicated that the

labeling requirements were such that it was virtually impossible to eliminate a very

negative consumer bias against the oil. Consumers in general felt that it would be a "rip off" if a re-refined oil were sold to them for the same price as a virgin oil,

despite any quality claims. In addition, that same representative briefly described

the field tests his company had made with the re-refined oil on which it had acquired

the SE qualifications. It was put into 51 pursuit vehicles for the California Highway

j Patrol, for about 25,000 miles each. The condition of the used oils were monitored,

j but there were no engine inspections at the end of the test. As far as could be

determined, this re-refined oil had completely satisfactory performance in this field

test

.

' There was also some discussion about the future availability of used oil feedstock. Due to improved lubricating characteristics of the existing lubricating oils,

the drain intervals have been extended significantly and will continue to be extended

in the future. In addition, in some industrial applications tighter lubricating

systems are being acquired and, for example, chemical process pumps were described

which now use lube-for-life bearings instead of recirculating oils. Therefore, it was suggested that these forces would tend to offset the increased number of vehicles and

equipment and reduce or hold constant the total volume of used oil expected to be

available. However, it was also acknowledged that relatively small portions of the

existing used oils are actually collected and recycled; and, therefore, the total

potentially available feedstock for recycling is still rather large compared to existing volumes.

Another important area of discussion centered upon the question of whether current requirements for oil quality would be relaxed in order to encourage Vhe effective

I reuse of recycled oils. Significant concern was expressed by a number of engine

manufacturers that this, in effect, would be the case and that reduction of lube oil

j quality would essentially negate many years of difficult and expensive work trying to

! extend drain intervals, maintenance intervals, and the general quality of lubrication

for their equipment. The response to this concern by the NBS personnel indicated that

the term "substantial equivalence" means just that, that the recycled oil will be

required to perform on a equal basis with the virgin oil product. A re-refiner

127
commented that the re-refining industry as a whole is not looking to lower the

standards or products, but, in fact, is looking at this program to enable the quality

of performance in the re-refining industry to be raised. If the high-quality lube

oil markets are essentially closed to re-refiners, there is little incentive to work

at improving their product. It was also mentioned that it was important to consider

requiring only meaningful tests, tests which can effectively measure the useful

quality of a lubricating oil for a particular end use. There was also discussion on the subject of what would happen in the future if,

for example, the virgin oil industry or equipment manufacturers developed new tests

to measure overall performance or, conversely, if individual tests were upgraded to new and different conditions . The concern was that the NBS program would provide a set of tests, go out of business, and leave the industry hanging, dependent upon those

particular tests without the mechanism for updating them. This was acknowledged as an area of concern, but this also supported the concept that the various industries involved should become more involved with effective utilization of used oils and provide,

with the Federal Government, a mechanism through the American Society for Testing and

Materials (ASTM) or through the Federal test and specification system to tie new test

procedures into existing on-going programs.

The question of applicability of the existing ASTM or Federal tests to recycled

oils was also discussed. There was some concern shown by NBS that some of the existing virgin oil test methods may not be valid for used oils or recycled oils. A case

in point is the ash method which is currently specified for virgin fuel oil. With the

trace metals present in used oil, the standard ash method may not be applicable, but

would require the sulfated ash method, if found valid, or some other new test.

Another example would be the copper strip corrosion method and whether a recycled oil

product would react in a similar way to the virgin oil product and, if not, whether

the resulting corrosion test value would be acceptable for a specification which was developed for a virgin oil product. Several people spoke to this concern, most of

whom stated that they had been using existing ASTM methods for used oil or recycled

oil products quite successfully, and that most of these tests seem to be applicable

and valid for recycled oils. The comment was also offered that, in general, recycled

oils may very well require one or more additional tests besides all the tests required

for virgin oils. These additional tests may be needed to monitor some characteristic

of the recycled product that is normally always at an acceptable level for a virgin

product. These individuals could not think of a test which was applied to a virgin

oil but which would not be required for a similar recycled oil product.

Another subject which received considerable discussion was the monitoring of

basestock for motor oils. This basestock will be considered by the NBS program because

for an SA oil, a straight mineral oil, the basestock is the end product. It had been

pointed out by a number of people that the monitoring of basestock between primary

quality-defining tests could be an effective way to evaluate the variability of the

re-refined product. There was concern voiced from the military as to methods for

monitoring basestock for virgin oils also; some means to identify and demonstrate con- sistency of virgin oil basestock would be extremely useful with regard to the military

specification. Presumably, similar types of methods could be used on re-refined oils

also

There was a great deal of discussion on the American Petroleum Institute (API)

service classification system, especially as it applies to the SE classification.

Much of this discussion was in trying to understand the various workings of this

classification system. It finally was clarified to where it was understood that there.

is no formal SE spproval system which looks at oils and provides a stamp of approval,

except as you apply for the Qualified Products Listing for military approval. That

was stated as the only way that an outside body can be used to render a judgment for

all to see and indicate that this is, in fact, an SE/CC oil (e.g., for MIL-L-46152)

In these discussions, it came out that any individual or company who is willing to legally stand behind his oil can put the SE classification on the can. He thus assumes

the warranty for his product and, obviously, is liable to litigation if the product

causes problems which are traceable to a quality lower than was stated. At this point,

a re-refiner spoke up and commented that he had been told unequivocably many times

that in order to put an SE on the container, you would absolutely have to pass the

engine sequence tests. The comments in response to this were that it may not be

"correct" to do so, but there is no legal requirement that these tests be passed. In effect, this is because there is nobody monitoring the marketplace to determine the

quality of the lubricating oils on the marketplace. It was then stated that in the area of military specifications, in order to qualify for a particular military specification and be put on to the Qualified Products List, the test data must be supplied

to the qualification committee and the results passed on by that committee. However,

128
I there is nothing that requires the manufacturer to pass these tests and bring the oil

j before the military board in order to put on the can that this meets or exceeds a

j particular military specification, and it is perfectly legitimate if he feels like

doing it. The military apparently does not have any way to stop him as long as he is

willing to stand behind it. This is essentially the same as was stated for the SE

and the SE/CC classifications. In fact, of course, a can containing a statement that

it meets a certain specification is certainly not a qualified product, and this product has not demonstrated the performance that would be required for these tests.

There was another extensive discussion on the subject of warranties and the

effect of a non-SE oil affecting the warranty for an automobile or other vehicle.

This disucssion can be summarized by stating that apparently the warranty generally

i guaranties only workmanship and materials; and, if there is a substantial flaw in a

! particular engine which would cause it to fail, the manufacturer really does not care

I whether a virgin oil or a re-refined oil was used or what quality level was used.

I They should repair or replace that particular problem. However, if the workmanship

and materials of the engine were of an acceptable level and the customer, through

I abuse or through use of the wrong lubricating oil--virgin or re-refined- -causes fail-

! ure in an engine, the manufacturer is not going to accept the warranty for that

I failure. If a particular lubricating oil product actually caused a failure in an

I engine still under warranty, the manufacturer would tell the consumer to go see the

' oil company, it is their fault. It was suggested that this holds true for both virgin

! oils and re-refined oils.

I One additional participant spoke up at that point and commented on how difficult

I is it to try to pin down a particular failure to a specific cause. The illustration

was made that even though a mechanic had told him about what was suspected to be the

cause, in general the relatively unsophisticated consumer is not willing to pursue

the question of trying to obtain redress from the engine manufacturer or lubricant

manufacturer unless that failure were absolutely unequivocab le . The cost of expert

testimony would be greater than the repair, not even considering loss of vehicle time.

I There was discussion on the subject of what the re-refiner could do in order to

i become more involved with the "system," the working relationship between oil companies,

I additive manufacturers, and engine companies. The response was that the ASTM meetings

are open to everyone and that re-refiners or anyone else are strongly encouraged to attend, to participate, and to work together for the good of the industry in general.

It was also pointed out that the ASTM is an excellent way for smaller organizations

with limited technical facilities to pick up large amounts of technical data and

sophistication from the larger companies which are supporting much of this testing

research which is discussed in the ASTM, the Society of Automotive Engineers, the

American Society of Lubrication Engineers, and other such organizations.

There was substantial discussion on the question of the exclusionary clause

against re-refined oil in military specifications for engine oils. The statement was made that the problem is not so much that the re-refining industry is concerned about

attempting to sell lubricating oil to the government; in general, they are too small

for that type of operation. However, it was pointed out very dramatically that the

very fact that the prohibition exists in the military specifications is a strong

deterrent to the public and private sectors against utilizing re-refined oils. It was described that there are many times when, for example, a fleet could use re-refined

oil but when this re-refining arrangement is discussed with the fleet operator one of

the first comments made is, "Does it meet the military specification?"

Finally, there was discussion on the experiences and data which have been generated over many years on the application and usefulness of virgin lubricating oils.

One participant described when the military required virgin oil producers to obtain

base oil samples from various refineries all over the world and then a large series

of tests was run with many of these (refined by a solvent extraction technique)

.

These oils were then tested with a certain additive package. All of this background

information existjS on virgin oils; these experience and data just do not exist for

re-refined oils at the present time. It was obvious that the military is very con- cerned about potential applications of re-refined oils wihout enough background

information to be able to effectively evaluate their operability in use. One of the

most important considerations in this background data is the consistency that can be

expected from re-refiners on a long-term basis.

The workshop ended on the afternoon of November 23, 1976, with participants

agreeing in general that useful and informative discussions had taken place. A

number of comments were also received which indicated that additional such meetings

in the future would be helpful, and this possibility is b^ing explored.

129
Mr. Robert Teasley of Cummins Engine. Company makes a point

during the workshop discussion.

Messrs. Peter Asseff of

The Lubrizol Corporation

and William Katzenstein

of Chrysler Corporation

listen during a presentation .

130
APPENDIX I

Reprinted From Commerce America—August 16, 1976

OVMERCE

^IVCRICA U.S. Department of Commerce / August 16, 1976

A. -M. FORMERLY COMMERCE TODAY

•TheBeseansh

llssoGlaie;

GalalKt For^

imimv/ ^
The Rcsoareh

Associate;

mnRmiiaritir

Breeds

Respect

Alma Coats is a chemist witli Hooker

Chemical currently working as a Research Associate

for the Society

of the Plastics

Industry. COMMERCE AMERICA, AUGUST 16, 1976

Just as exchanges of people can improve rela- tions between countries, assignments of employees are leading to increased understanding be- tween business and government in this country. The Research Associate Program at Commerce's

National Bureau of Standards is helping to build

this understanding by allowing U.S. firms and busi- ness associations to send technical employees to use the elaborate facilities at NBS laboratories in Boulder, Colorado, and Gaithersburg, Maryland. The program enables scientists and engineers from the private sector, both domestic and foreign, as well as state and local governments and occasionally the academic community, to work on a full-time basis for specified periods at NBS on

projects of mutual interest to NBS and the sponsor. The base criteria for a program are simple: it must have nonproprietary objectives; it must be

within the .scope of NBS activities and interests; and it must offer the prospect of publishable re- sults of interest and significance to the industrial and technical communities represented, and thus

ultimately to the public. The programs start when convenient to both parties and may last from a few months to several

years. They may be staffed 'by one or many Associates. The American Dental Association research

unit, something of an unusual case, currently has

22, including physical chemists, ceramists, metallurgists, dentists, crystallographers, a mathematician, and supporting personnel. A Research Associate must have appropriate aca- demic background and sufficient experience to per- form independent research in the field covered by

the program. The sponsor and NBS must agree on

the associate's qualifications and acceptability for the assignment. "My experience here is going to prove very val- uable to my company when I return," says Alma

Coats of Hooker Chemical. "This definitely needs

to be an ongoing program, because of the improved

technology that's developing all the time. I'm go- ing to make a firm recommendation to my company

that they continue to make use of this program by

sending someone else here after I finish." "The facilities here are .so much better," says Randall Lawson, a Research Associate from the Gypsum Association who is trying to devise a test measuring the fire-resistive properties of gypsum

board products. "Also, the quality of the staff is excellent. There's a much broader range of techni132
cal knowledge available here than you would find

in any industrial research situation." "The equipment and people that are available here can't be duplicated anywhere else," says Alan

Meierhofer of the Manmade Fiber Producers Association, who is trying to establish the fire hazard

potential of the different apparel fibers. "It was

somewhaf of a transition at first, learning the gov- ernment's way of doing things, but it's worked out

quite nicely." "The task of developing standards for consumer

products is very difficult, and both industry and government are faced with serious problems in this area," says Joe Dort of Sears, Roebuck. He is trying to develop tests to accurately predict the

service life of small appliances. "Lab tests are

difficult to relate to actual use by consumers, since the amount of time an appliance is operated and

the treatment it receives varies from user to user. We're trying to devise tests that come as close as

possible to the reality of actual use and abuse by

a consumer." The advantages of having a company scientist or engineer working on non-proprietary matters (re- search that will not be held secret) at NBS have

attracted more than 400 companies and trade organizations and some 1500 individuals to the Bureau

since the program began in 1920. Some of the advantages are obvious. There is the use of the NBS computer and libraries, the

laboratories and special research facilities that are

difficult to match Einywhere else. There is the ad- vantage of working with the NBS staff, which in- cludes many scientists of recognized importance in their fields. A Research Associate remains the employee of the sponsoring organization. His employer pays his salary, fringe benefits and travel, and makes ar- rangements as necessary for temporary relocation

of the Research Associate for the period of his as- signment to the program. "As to salary level there are no requirements,"

says Peter R. de Bruyn, the NBS liaison officer who

coordinates the program. "But we do suggest that they be comparable to the levels of the people

they'll be working with. That way nobody feels any resentment about different compensation for doing essentially the same job." The sponsors also pay for any special supplies or

services required by their associates, such as computer time, unusual or expensive materials, or the

use of technician assistance, just like any NBS unit would. NBS provides, at no cost to the sponsor, technical

supervision, office and laboratory space, routine

supplies and services, and the use of available re- search equipment not normally subject to time or usage charges. "Everybody carries his share of the load and

everybody benefits," says de Bruyn. Each memo of agreement setting up a research

associate program assigns a specific NBS supervisor to each associate, assuring the sponsoring

organization that their employee will not fall be- tween the cracks, and will know where to turn with problems. "Many of these associates are people on whom

the company has had an eye for some time as potential comers, and quite a few of them come home

to promotions. Consequently, especially in firms that have continuing programs or have run pro- grams in the past, these assignments tend to be

looked on as a plus and the competition for them

can get pretty intense," says de Bruyn. "They also value the acquaintances they make

among their contemporaries—both the other associ- ates and the government specialists they work with —which will prove useful later." A recent listing contained 21 projects currently

in progress, with 5 of them, involving Research

Associates, dealing with problems associated with

fire. Why the emphasis on fire? There are probably many reasons, but almost certainly one of them is the fact that it is possible at NBS to conduct full scale "burns" of rooms and vehicles inside a 6,500 cubic meter test chamber—a facility that most

companies do not have. Other associates are studying the impact resist- ance of eyeglass lenses, the criteria for perform- ance of automatic data processing systems, the measurement of paper characteristics, energy con- servation in mobile homes, and dental materials. Found a home Many firms run a succession of programs, usually

of about two years duration. Armstrong Cork has had at least one associate here for the past 40

years. The longest-running association on a continuing

basis is with the American Dental Association, which dates back to 1929. This association has

. . . the advantages

are obvious.

There is the use

of the NBS

computer and

libraries, the

laboratories

and

special research

facilities . .

.

Dentist Dr. George

Paffenbarger Is a Senior Research

Associate

representing the American Dental

Association.

COMMERCE AMERICA. AUGUST 16, 1976

133
Work on consumer product

technology

is just

beginning . .

produced more than 600 publications, including

books, reports and articles in various professional

journals. There are other places, of course, where this work could be done, but, notes Dr. George Paffenbarger, senior research associate of the ADA unit, "In no instance would the ADA have the facilities, or expertise, or large laboratories such as are avail- able here at the National Bureau of Standards." "Thus far there's been a very minimum of trouble." reports de Bruyn. "The thing's been running

for more than 55 years without becoming ossified, which^is more than you can say about many pro- grams, in or out of government. This program has been climbing steadily since 1970. We're pleased, and a little bit puzzled, because it's all happened

during a period when everyone' was crying that they were 'research poor' and firms were generally lowering their research goals." "Actually, I've got one of the easiest sales jobs

in the world. I'm trying to sell people something

they've paid for already—with their taxes. These

facilities are available and waiting for them.

"This program is open to all: our problem is get- ting the word around.

"It takes a while to convince scientists that

you're going to represent them and their capabilities correctly. The steady increase in the number

of calls I receive from technical people around the Bureau, suggesting areas that might prove promising for a research associate project, is the best evidence to me that the program has really caught

on."We're not in competition with private labs. What we offer is an unbiased source that everyone's

willing to accept. All of the results of the pro- gram are published, and industrial labs can then

pick up the technology that has been developed and profit from it. "In some cases, it could even ultimatelv provide

the basis for an entirely new industry. "New measurement technology is the end product. What has evolved from the program to date? Among other things, a new Standard Reference

Material for steels based on work done by a U.S. Steel Research Associate. And, through the contri- bution of a Research Associate sponsored by IBM,

a secondary standard computer amplitude tape is now available to industry as a regular Standard

Reference Material. "What each associate is seeking is a new meas- urement procedure in a highly specialized area, that will be acceptable to everyone in the field. They're looking for a test that you can plug every

piece of a particular material into. Since both in- dustry and government have had a hand in it, these

associations usually result in very rational stand- ards that protect the public interest without hin- dering industry. "The results are available to all. We want every- one to use our stuff. For example," de Bruyn goes

on, "John Robertson was a research associate from Dow Chemical. He brought ten years of experience

in the energy conservation field to NBS. He'd been dreaming up ways to conserve energy years before any of the rest of us even dreamed about an energy

crisis. Well, John put his decade of experience into our Energy Conservation Program Guide for Industry and Commerce, a guidebook especially designed

to help smaller and medium-sized firms get a handle

on their energy problem. That was an extremely

generous contribution by one firm to all of industry." The Atomic Industrial Forum's agreement calls for research into measuring techniques for radioactive pharmaceuticals, an area which is "pretty

crucial to the public that the situation is properly

handled," de Bruyn points out. The National Microfilm Association sent a Research Associate to NB§ with a major problem:

the microfilm on which the Library of Congress was

preserving the nation's priceless documents had, unaccountably, started to deteriorate. The problem was traced to a gas evolving from the cardboard

storage containers. Sub.stituting stainless steel containers solved the problem. However, not all Research Associates produce such dramatic fruit. Nor are the solutions often that

simple. "It's usually a matter of the dat^ that's de- veloped here ultimately filtering down to the public in the form of products incorporating it. Much

of this material is significant scientifically, but very

little of it has any dramatic one-shot impact," says de Bruyn. A number of governmental agencies have used

the program: In 1930 the Port of New York Authority sent specialists down to do some research

relating to bridge towers, and in 1940 the Florida

Citrus Commission did an analysis of citrus juices. Universities, too, occasionally make use of the pro- gram, such as the time Yale sent a technical team down to do optics research. Work on consumer product technology is just beginning, and an associate from Sears, Roebuck

has been assigned to NBS Gaithersburg headquarters since last November. Sometimes these agree- ments turn into two-way streets, with the govern- ment sending a specialist out to work in private

laboratories. This has happened in the Sears case, with an NBS scientist being assigned to Sears under the provisions of the Federal Training Act. "He's learning how they do it in industry, which we need to know if we're going to deal with the consumer product problem realistically," says de Bruyn. Research Associate Programs still have rather informal beginnings. The initiative may come from

either industry or the Bureau, depending upon who

first conceives a project that might be of interest

to the other. Representatives of a prospective sponsor get to- gether with the appropriate members of the NBS

staff at the invitation of either party to discuss the

details of a potential program. Dc Bruyn works

with them to establish a mutually acceptable proj- ect definition, statement of objectives, and work

plan. Following this, with the assistance of members of the NBS legal, patent, budget and accounting staffs, he negotiates with the sponsor's management personnel a Memorandum of Agreement

describing the program and setting forth the terms and conditions governing the relationship between

the sponsoring organization and NBS. To sum it up, "The Research Associate Program

helps give each of us a mutual perspective as to what the others' problems are, says Sear's Joe Dort.

"If government and industry understand each

other, they should be able to work out solutions that are beneficial to both, and eventually the

public, because that's what it's all about." -^r COMMERCE AMERICA, AUGUST 16, 1976

134
APPENDIX II

Report 2127

INVESTIGATING WASTE OIL DISPOSAL BY DIRECT INCINERATION

Maurice E. LePera and Gerald DeBono

February 1975

Approved for public release; distribution unlimited.

. S. ARMY MOBILITY EQUIPMENT RESEARCH AND DEVELOPMENT CENTER

FORT BELVOIR, VIRGINIA

Retyped from best available copy.

135
CONTENTS

Section Title Page

I INTRODUCTION

1 . Background 1

II INVESTIGATION 2

2. Details of Test 2 a. Plant Facilities/Operation 2 b. Waste Oil Collection 2 c. Fuel and Stack-Emission Sampling 3 3. Results o£ Test 3

III CONCLUSIONS

4. Conclusions 9 APPENDIX

SAMPLING AND ANALYTICAL METHODS 12

136
TABLES

Table Title Page

1 Comparison o£ APG Waste Oil with Other Sources 2

2 Comparison of APG Waste Oils 3

3 Identification of Fuel Oil/Waste Oil Samples 4

4 Inspection Properties of Fuel Oil and Waste Oil

Samples 5

5 Combustion-Emissions Results from APG Messhall

(Bldg. 4219) 6

6 Stack Emissions Data from APG Messhall '(Bldg. 4219) 7

7 Properties of 271 Waste Oil Blend vs VV-F-815C

Limits 10

8 Metal Analysis of "Products" Used in CombustionEmissions Test 11

137
INVESTIGATING WASTE OIL DISPOSAL BY DIRECT INCINERATION

I. INTRODUCTION

1. Background. The Facilities Engineering Directorate at Aberdeen Proving

Ground (APG) , Maryland, initiated a program in 1968 to dispose of generated waste oil

by blending with a No. 6 Fuel Oil (Federal Specification VV-F-815C). Approximately

40,000 gallons of waste oil have been consumed each year in this manner at the main

APG powerhouse facility. Since No. 6 Fuel Oil is a relatively viscous product, no problems were encountered with the waste oil disposal system. In August 1972, it was reported that APG would be changing from No. 6 to No. 2 Fuel Oil (Federal Specification VV-F-815C] as a result of air pollution abatement legislation restricting the

level of- sulfur in the fuel. Because of the obvious difference in properties (other

than sulfur content) between No. 2 and No. 6 Fuel Oil, this office became concerned

that continuance of the waste oil disposal system could:

• cause stratification and/or sedimentation problems due to the

difference in gravity (waste oil is generally higher than No. 2 Fuel Oil) leading to potential malfunctioning of the burner

no z zles .

• create excessive stack emissions exceeding the air pollution

standards either due to improper combustion (i.e., nozzle

deposits) or from the composition/concentration of the waste

product itself.

In April 1973, this office conducted an initial waste oil incineration program at the main powerhouse facility (Bldg. 345) at APG. The stack emissions, monitored by US Army Environmental Hygiene Agency (AEHA) emissions specialists, were measured

while No. 2 Fuel Oil and No. 2 Fuel Oil containing approximately II waste oil were

burned. 1 In summary, there was no significant difference in the emissions levels

between the neat fuel and the fuel adulterated with waste oil. Furthermore, the APG

facility engineer reported that incineration of this mixture did not create any burner

nozzle maintenance problems. There were, however, several shortcomings in this initial

program. Since the mixing of the waste oil with the base fuel oil was extremely difficult to control, only an estimate of the percent of waste oil reaching the burner during the steady-state emissions test could be obtained. Also, the low concentration of

waste oil may not have been a significant contaminant when compared to the tank-bottom

residue of the No. 6 Fuel Oil remaining in the main storage tank from previous years.

Finally, the introduced waste oil generated at APG was not considered to be representative of typical waste oils due to its unusual lightness (i.e., low viscosity, high

API gravity, low ash, etc.). An analysis of this waste oil compared with other waste

oils reported in the literature brings attention to this point (Table 1) . A review of

the results of this initial emissions test, the physical arrangement of the burnerboiler system, and the atypical properties of the waste oil indicated the need for a , second combustion-emissions program to establish baseline parameters for this waste f oil disposal system. This report describes the results of the second combustionemissions test conducted at APG.

^G. E. DeBono, "Investigating Waste Oil by Combustion," CCL Interim Report No. 3008,

AD No. 772911, January 1974

138
Table 1. Comparison of APG Waste Oil with Other Sources

Waste Oil

Source/ Re f er ence

Kin. Vis.

@100°F,

D 445

°API

Gravity

D 287

Water ^ Sediment

,

D 1796

Sulfur

,

% Wt,

D 129

Total Ash,

% Wt,

D 482

Sulfated Ash,

% Wt,

D 874

APGi 7.34 32 .

0

1.4 0.21 0 . 50

\ ^ J 53.3 24 .

6

0 .-6 0 . 34 - - 1 . 81 57.7 26 .

0

1 . 80

55.1 25.0 -- 0.21 1 .61

(3) 26.7 4.8 0 .26 0 .40

248 24.6 0.6

256 25.0 1 .62

161 27.9 2.4 1 .10

24.8 18.0 2 .16

(5) 0 .44 1 .43 1.69

Patuxent N.A.S. 60 . 3 28 .1 Trace 0.35 0 .95

I ^G. E. DeBono, "Investigating Waste Oil By Combustion," CCL Interim Report No. 3008,

AD No. 772911, January 1974.

^Anonymous , "Final Report of the API Task Force on Used Oil Disposal," American

Petroleum Institute, New York, N.Y., May 1970.

I ^M. Liberman, "Combustion and Heat Recovery of Air Force Waste Petroleum Oils and

1 Lubricants," Air Force Weapons Laboratory Report No. AFWL-TR- 73-244 , February 1974.

'*S. Chansky, W. McCoy, and N. Surprenant, "Waste Automotive Lubricating Oil as a Municipal Incinerator Fuel," Environmental Protection Technology Series Report No. EPA-R2-73-293, September 1973.

^G. A. Chappell, "Waste Oil Processing," Commonwealth of Massachusetts, Division of

Water Pollution Control Publication No. 6 72 2 - 41 - 100 - 4 - 73 -CR , January 1973 .

II. INVESTIGATION

2. Details of Test. The details of the test are as follows.

a. Plant Facilities/Operation. The powerplant system at the APG Messhall

(Bldg. 4219) was selected for this second combustion-emissions test because the fuelsystem design offered a simple and accurate method for controlling the waste oil/fuel

oil ratio. The burner system consisted of three five-tube, high-pressure boilers and

three oil-fired, low-pressure, rotary-cup KEWANEE burners. This system, originally

designed to burn a No. 4 or a No. 5 Fuel Oil, was rated at 86.3 hp, 30,808.5 pounds

I of steam/hour, and 4,500,720 Btu. For this test, the fuel was to be metered directly

I to the burners from a 1200-gallon tank truck not only permitting accurate mixing of

the desired fuel oil/waste oil ratio, but also controlling delivery to the burners

during the steady-state emissions test.

b. Waste Oil Collection. The waste oil used in this test was considerably

heavier than that used in the previous test at the APG powerhouse. ^ To insure that a sufficiently "heavy product" was tested, the waste oil was collected in 55-gallon

drums located at the main APG Post Exchange Service Station. It consisted almost

entirely of drained crankcase oil from commercial - des ign vehicles with trace amounts

of antifreeze and hydraulic brake fluid and some transmission fluid. In addition,

I some water contamination occurred from improper drum covering and/or closure procedures

I since the drums were positioned outside. This water, after settling, was pumped out

i prior to the combustion-emissions test to insure that the water contaminant did not

^G. E. DeBono, "Investigating Waste Oil by Combustion," CCL Interim Report No. 3008,

AD No. 772911, January 1974.

139

4
3 influence the resultant stack emissions. A comparison of the characteristics of this

collected "referee - type" waste oil versus the waste oil used in the initial program is

shown in Table 2

Table 2. Comparison of APG Waste Oils

Kin. Vis. Gravity,

@100°F, °API

D 445 D 287

Initial Combustion 7.34 32.0

Test

Second Combustion 86.7 24.9

Test

Water § Sulfur Total Asli Ramsbottom

Sediment % Wt , % Wt, Carbon Residue

D 1796 D 129 D 482 D 524

1.4 0.21 0.50 0.89

0.1 0.39 1.60 4.36

c. Fuel and Stack-Emission Sampling. To assess the effect of this referee

waste oil on combustion of No. 2 Fuel Oil, the AEHA again participated in monitoring

stack emissions. As before, two series of emissions tests were required. The first

series of tests was made while No. 2 Fuel Oil obtained from the 10 , 000 - gal Ion underground storage tank located at the messhall facility was burned. Samples of this base

fuel were obtained from the sampling valve adjacent to the burner system and from the

underground storage tank prior to the baseline combustion-emissions test. Using this

base fuel, AEHA personnel monitored the stack emissions during three 2-hour runs. The

details of the emissions stack sampling/analysis procedures performed by AEHA are presented in the Appendix.

The second series of combustion-emissions tests was made while the

referee waste oil/fuel oil blend was burned. A 1200-gallon tank truck containing 200

gallons of waste oil and 800 gallons of No. 2 Fuel Oil served as the temporary mixing

reservoir. The resultant blend was pumped to the burner system from the bottom of

the tanker via tubing. The 200 gallons of referee waste oil, collected in four 55-

gallon drums, was sampled prior to mixing to assess the variation in composition and

the occurrence of stratification. To possibly avoid any stratification occurring within the tanker, the waste oil from the four drums was pumped into the tanker at different time intervals. Although this precaution was taken, it was anticipated that

stratification could occur due to the wide differences in API gravity between the waste

product and the No. 2 Fuel Oil. In view of this, the waste oil/No. 2 Fuel Oil mixture

was sampled at three levels in the tank truck top, middle, and bottom prior to initiation of the steady-state emissions tests. With this 201 volume "nominal blend" of

waste oil in No. 2 Fuel Oil being used, the second series of combustion-emissions

tests was monitored by AEHA personnel during the three 2-hour runs. Details on the ' fuel oil samples, waste oil, and waste oil/fuel oil sample blends obtained during this

second combustion-emissions test are provided in Table 3 with the analyses of the I samples presented in Table 4. Accordingly, the emissions measured during this second i combustion-emissions test by AEHA at the messhall facility are tabulated in Tables 5 | and 6 . I

3. Results of Test. The analysis data on the "collected" waste oil samples I indicated that stratification was occurring within the four drums. For that reason, i the composite sample was taken (Sample No. 5, Table 5) to characterize the collected

j waste product. As noted, this composite waste consisted primarily of crankcase drains \ as evidenced by its high viscosity and low API gravity.' After the 200 gallons of i, waste oil were introduced into the tank truck containing the 800 gallons of No. 2 Fuel

[ Oil, the sample analysis indicated that satisfactory mixing had not occurred since the f top, middle, and bottom samples (Samples 7, 8, and 9) revealed the waste product to be

j stratifying. Although the nominal concentration of waste oil was 201, the fuel oil/ | waste oil blend was being fed to the burner system via a connection located at the

bottom of the tanker. Because of this apparent stratification, the burner system was

in fact combusting a fuel oil/waste oil blend of something in excess of the selected

201 volume ratio. Since the burner system was being fed primarily a "bottom sample"

of fuel oil/waste oil during the three 2-hour runs of stack emissions measurements,

the amount of waste oil in the No. 2 Fuel Oil for this "bottom sample" was determined

by preparing known blends of waste oil in No . 2 Fuel Oil. The kinematic viscosity for

each of these blends was determined and plotted on a graph (see Figure) . From this

140
4

graph, the concentration which corresponded to the viscosity o£ the bottom sample

(Sample No. 9) was interpolated and found to be 271.

Table 3, Identification of Fuel Oil/Waste Oil Samples

Sample Date Sample Origin or Sampling

No. Sampled Type Location Depth Sample Description

10

8/20'/73 Waste Drum No. 1 Bottom

Oil

8/20/73 Waste Drum No. 1 Top

Oil

8/20/73 Waste Drum No. 4 Bottom

Oil

8/20/73 Waste Drum No. 4 Oil

8/20/73 Waste Drums No.

Oil 1,2,3, § 4

9/24/73

9/27/73

9/27/73

No. 2 Fuel Line

Fuel @ Messhall

Oil

No. 2 Fuel

Oil

No. 2 Fuel

Oil

Tank Truck

Tank Truck

9/27/73 No. 2 Tank Truck

Fuel

Oil

7/20/73 No. 2 Contractor's

Fuel Delivery

Oil Truck

Top

Middle

Top of Fuel

Tanker

Middle of

Fuel Tanker

Bottom of

Fuel Tanker

One of four drums of collected

waste oil for combustionemissions test.

Same as above.

One of four drums of collected

waste oil for combustionemissions test.

Same as above.

This was a composite sample

from all four drums of the

collected waste oil.

Fuel sample obtained prior to initial baseline emissions test

at messhall.

Sample taken from tanker con- taining 200 gallons waste oil

and 800 gallons fuel oil.

Same as above.

Same as above,

Sample taken of No. 2 Fuel Oil

delivered to messhall and other

APG facilities.

141
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142
Table 5. Combustion-Emissions Results from APG Messhall (Bldg. 4219)

Results Obtained

Allowable or No. 2 Fuel Oil No. 2 Fuel Oil + Test Parameter Legal Limit (No Waste Product) -w 201 Waste Oil

Emissions Rate:

GR/SCPl 20.03 0.047 0.262

lb/MBtu3 0.6 0.031 0.158

lb/hour --- 0.184 0.938

Visible Emissions No. 2 Max'* 0 0 Sulfur Content, °^ Wt 0 . 30 0. 20 0.35

Trace Metal Emissions,

GM/Day:

Lead --- 3.86 172

Calcium Nil 97

Zinc --- 1 410

Magnesium Nil > 37

^Corrected to 501 excess air, dry basis, 25°C., and 1 atmosphere.

^This limit, imposed by the State of Maryland, applies only to residual oil burning

equipment

.

^As specified in AR 11-21, Environmental Pollution Abatement.

"A maximum No. 2 rating on the Shell Bacharach Scale.

The net effect of this 271 waste oil on air pollution regulations was explained by AEHA in their emissions survey report. ^ This was explained in the

following manner:

f AR 11-21 Environmental Pollution Abatement limits emissions

from boilers in Bldg. 4219 to 0.6 Ib/MBtu.

• The State of Maryland Bureau of Air Quality Control limits

smoke emissions from distillate-fired boilers to a No. 2 rating on the Shell Bacharach Smoke Scale. No visible emissions are allowed except during start-up, and the sulfur

content of the fuel oil is limited to a maximum of 0.301 wt.

Residual oil burning equipment is limited to 0.03 GR/SCF.

In applying these limits to the initial combustion-emissions program wherein

1% waste oil was used at the main powerhouse facility (Bldg. 345), no violation of

any emission standards occurred. However, in reviewing the results from this latter

program in which 27% waste oil was consumed, there were indications that some emission

standards were violated. More specifically, the sulfur content of the waste oil/fuel

oil mixture was 0.35% (Note: a 0.30% maximum is permitted) and, more important, the

particulate emissions rate was 0.262 GR/SCF. (Note: a 0.03 maximum rate is permitted.) This value is 773% greater than the maximum allowable rate and represents a fivefold increase over the baseline level. However, AEHA concluded that no emission

levels were exceeded in this instance since there are no emission standards for No. 2 Fuel Oil. (Note: the 0.03 GR/SCF maximum applies to residual fuels only.) AEHA

personnel maintained the position that a fuel oil/waste oil blend must be considered

a distillate product if it meets the specification requirements given under Federal

Specification VV-F-815C, Fuel Oil, Burner. A tabulation of the inspection. properties

of this 27% waste oil/ fuel oil blend versus the specification limits in VV-F-815C is

^A. R. Paine and J. T. Higgins, "Air Pollution Engineering Special Study No. 21-015-

73/74, Waste Oil Utilization Program, Aberdeen Proving Ground," April and September

1973.

143
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8 DETERMINING THE CONCENTRATION OF WASTE OIL IN THE FUEL

PERCENT WASTE OIL IN NO. 2 FUEL OIL

Determining the concentration of waste oil in the fuel.

145
j

9

I shown in Table 7. The Maryland Bureau of Air Quality (MBAQ) initially informed this

office that a fuel could not be considered a distillate if it contains a non-distillate ! product such as waste oil. In view of this, their initial position was that the i particulate emissions rate for the 271 waste oil blend was in violation of the MBAQ

standards. However, in subsequent discussions between AEHA personnel and the MBAQ,

tentative agreement was reached in favor of AEHA's conclusions. (Note: the problem

of defining a distillate versus a residual fuel in terms of applying emission standards

has been presented to ASTM D-2 Technical Committee E on Burner and Diesel Fuel Oils

for an official ruling.)

The emission rates of the four trace metals analyzed showed a significant | increase when the 27% waste oil was introduced. These increases were anticipated due

to the nature of the "collected" waste product which had high concentrations of engine

oil drains. To provide additional information on this point, samples of the products

used in this combustion-emissions test and the previous program were analyzed for the ' four suspect metals: lead, zinc, calcium, and magnesium.'* The results of these

analyses are shown in Table 8. Since neither AR 21-11 nor MBAQ provides emission

standards for these or any trace metals, the obtained emission rates for all metals

were not considered to be in violation although the rate for zinc was relatively high, i

i As mentioned in the AEHA report,^ the combustion-emissions test program was conducted on a short-term basis to observe whether significant increases in particulate emissions would be evidenced with the addition of the waste oil component. No I attempt was made to assess the potential deleterious effects of waste oil combustion

on burner nozzles or heat-transfer surfaces of the boiler system. A previous study ' conducted for the State of Massachusetts revealed that attempts to combust 100% waste [ oil resulted in severe operating problems in a 50-hp Cleaver-Brooks boiler system.^

The results of the Massachusetts study emphasized the need to remove or separate the

j inorganic ash materials from the waste product prior to combustion. More recently, | under a USAF program addressing the feasibility of this approach, experimental com- bustion tests were performed using up to 101 waste oil in both No. 2 and No. 6 Fuel

Oil.^ The results of the USAF program revealed no short-term air pollution effects

or operational problems.

I III. CONCLUSIONS

4. Conclusions. The two combustion-emissions programs conducted at APG demonstrated that waste oil can be incinerated as fuel -oil -blending components without

attendant stack emissions problems. However, the use of the 27% waste oil/fuel oil \ blend in the KEWANEE burner system produced emission rates which could be in violation ! depending on whether the particular waste oil/fuel oil blend is defined as a residual

or a distillate product. The high particulate emissions evidenced were in part attri- j butable to the rather inefficient operation of the rotary-cup atomizers employed in

j the burner system. This important variable involving burner-b.oiler configurations can | significantly affect and/or alter the emissions produced from the same waste oil/fuel ' oil mixture. It should be noted, however, that this combination of "heavy waste oil" ' and the burner system employing rotary-cup atomizers essentially represented a referee,

or "worst case," situation. Other burner systems employing the steam-assisted atom- , izers could be expected to produce substantially lower particulate emissions. These | limited data acquired from these two combustion-emissions tests further support the

need for additional test programs to quantify the relationships between particulate

emission rates, boiler-burner configuration and endurance, and long-term operation on waste oil/fuel oil blends to identify any potential burner nozzle and heat- transfersurface problem areas. '

'*G. E. DeBono, "Investigating Waste Oil by Combustion," CCL Interim Report No. 3008 , AD No. 772911, January 1974.

^A. R. Paine and J. T. Higgins, "Air Pollution Engineering Special Study No. 21-015- [ 73/74, Waste Oil Utilization Program, Aberdeen Proving Ground," April and September I 1973.

^G. A. Chappell, "Waste Oil Processing," Commonwealth of Massachusetts, Division of

Water Pollution Control Publication No. 6722-41-100-4- 73-CR, January 1973.

''M. Liberman, "Combustion and Heat Recovery of Air Force Waste Petroleum Oils and

Lubricants," Air Force Weapons Laboratory Report No. AFWL-TR- 73- 244 , February 1974. .

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12

APPENDIX

SAMPLING AND ANALYTICAL METHODS

1. Sampling Methods

a. Particulates

(1) The particulate train used consisted of a probe tip, heated stainless

steel probe, glass cyclone, and glass fiber filter in a heated chamber; four Greenburg Smith impingers in an ice bath; vacuum pump; gas meter; and calibrated orifice.

(2) Isokinetic sampling conditions were maintained as close as possible by

controlling pump vacuums in relation to pertinent system parameters so that the

velocity of the gas entering the probe tip was equal to the velocity of the surrounding gas stream. The gas velocity was determined by use of an S-type pitot tube.

Temperature was measured with a chromel-alumel thermocouple.

(3] The particulate was collected at several points across the stack diameter. Two diameters 90° apart were traversed. The number of sampling points was determined by the stack diameter and distance above and below flow disturbances. In this case, 10 points on each of two diameters were sampled for boilers in Bldgs. 345

and 4219.

B. Moisture. Moisture determination was made from the change in weight of the

impinger containing silica gel and the change in liquid volume of the other three.

Impingers 1 and 2 contained 100 ml of H2O, impinger 3 was empty, and impinger 4 con- tained silica gel.

c. Gaseous Sampling. A Mylar bag sample was collected concurrently with each

particulate sample. The sampling velocity was maintained proportional to stack gas

velocity for the entire test.

2. Analytical Methods

a. Particulates. Particulate determination was accomplished by measuring the

weight change of the particulate traps in the system. The glass cyclone and the

probe were washed with acetone. The washings were combined and dried to constant

weight and a final weight was taken. An acetone blank was also included. The glass

fiber filter was dried to constant weight in a desiccator and weighed. In accordance

with ASME Power Test Code 27,* condensible particulates collected in the impingers

were not included as particulate matter.

b. Moisture. Moisture content was determined by weighing four impingers before

and after sampling.

c. Gases. A Fisher-Hamilton Gas Partitioner was used to determine CO2, O2, N2

,

and CO in the Mylar bag samples.

•CrU.S. GOVERNMENT PRINTING OFFICE: 1 9 7 7-2 40- 848/2 93

*Power Test Code No. 27, "Determining Dust Concentration in a Gas Stream," adopted

29 April 1957, the American Society of Mechanical Engineers.

149
NPS-114A (REV. 7-73)

U.S. DEPT. OF COMM. BIBLIOGRAPHIC DATA

SHEET

1. PUBLICATION OR REPORT NO. NES SP-488

2. Gov't Accession

No.

3. Recipient's Accession No.

4. TITLE AND SUBTITLE

PROCEEDINGS OF THE WORKSHOP ON MEASUREMENTS AND STAITOARDS

FOR RECYCLED OIL

5. Publication Date August 1977

6. Performing Organization Code

7. AUTHOR(S)

D. A. Becker fRHitor^

8. Performing Organ. Report No.

9. PERFORMING ORGANIZATION NAME AND ADDRESS

NATIONAL BUREAU OF STANDARDS

DEPARTMENT OF COMMERCE

WASHINGTON, D.C. 20234

10. Project/Task/Work Unit No.

11. Contract/Grant No.

12. Sponsoring Organization Name and Complete Address (Street, City, State, ZIP)

Same as 9.

13. Type of Report & Period ' Covered Final

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15. SUPPLEMENTARY NOTES

Library of Congress Catalog Number: 77-600032

16. ABSTRACT (A 200-word or less factual summary of most significant information. If document includes a significant

bibliography or literature survey, mention it here.)

This publication is the formal report of the workshop on Measurements and

Standards for Recycled Oil, held at the National Bureau of Standards on November 22 and 23, 1976. There were seven sessions on specific subject areas at the meeting, with a total of 26 formal presentations, plus extensive discussion periods. The subject areas were as folloxjs: (I) The NBS

Responsibilities and Program, (II) Used Oil Reused as Fuel, (III) Recycled

Industrial and Hydraulic Oils, (IV and V) Recycled Engine Oils, (VI) Barriers

to the Utilization of Recycled Oils, and (VII) Problems and Needs in

Establishing Quality for Recycled Oil Products. Included in this volume are

the invited talks that were given and summaries of the extended discussions

that were held on each of these subject areas.

17. KEY WORDS (six to twelve entries; alphabetical order; capitalize only the first letter of the first key word unless a proper name; separated by semicolons)

Recycled oil; petroleum test methods; re-refined oil; petroleum standards; oil

specifications; industrial oils; fuel oil; engine oil; hydraulic oil; lubricating

oil; used oil; waste oil.

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