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NBS SPECIAL PUBLICATION 661

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

ASTM/NBS

Basestock

Consistency

Study Data

100

,U57

No. 561

1933
NATIONAL BUREAU OF STANDARDS

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the Institute for Computer Sciences and Technology.

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J&ATLOUPX BUREAU

Sfff. STANDARDS

LIBRARY c

ASTM/NBS Basestock

Consistency Study Data

S.J. Weeks, D.A. Becker, and S.M. Hsu

National Measurement Laboratory

National Bureau of Standards

Washington, DC 20234

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

NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director

Issued October 1 983
Library of Congress Catalog Card Number: 83-600590

National Bureau of Standards Special Publication 661

Natl. Bur. Stand. (U.S.) Spec. Publ. 661, 482 pages (Oct. 1983)

CODEN: XNBSAV

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 1983

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

Price $9.50

(Add 25 percent for other than U.S. mailing)
FOREWORD

by

National Bureau of Standards

The National Bureau of Standards (NBS) initiated the Recycled Oil Program in 1976 under the

Energy Policy and Conservation Act (P.L. 94-163, section 383). The Act directs NBS to develop test procedures that can be used to determine the substantial equivalency between recycled and virgin oil

products. In 1978, NBS concluded the first phase of the program, recycled oil used as burner fuel

(NBS Technical Note 1130), and the phase two work on automotive crankcase lubricants was initiated.

NBS interacted extensively with various companies and organizations in American Society for

Testing and Materials (ASTM) Committee D-2 on Fuels and Lubricants. In 1979, a task force was formed

in ASTM Committee D-2, Technical Division P on Recycled Petroleum Products, Section II on Used Oils

and Basestocks, to examine the consistency of the current production basestocks from re-refineries.

The joint ASTM/NBS study began in March, 1980 and was concluded in March, 1981. During this period,

monthly production samples of re-refined and virgin base oils from 10 companies were shipped to NBS,

and coded samples were sent out to fourteen participating laboratories for various analyses. Over

fifty tests were performed on these coded samples over the thirteen month period. The test data

collection and collation was initially conducted by Mobil Oil Corp. The data were transferred to NBS

in March 1982 for further compilation and analysis. NBS, however, under administrative guidelines,

terminated the Recycled Oil Program in September 1982. The Department of Energy under its Office of

Industrial Programs, awarded a research contract to the Chemical Stability and Tribology Group at NBS

to conduct extensive statistical analyses and develop correlation methods and models to fully utilize

such valuable data.

This report is the first one issued under the DOE contract. The main purpose of this report is to make available an invaluable data base to all interested parties for immediate reference and

application. No attempt has been made in this report to make conclusions as to the consistency of the

lubricating base oils nor is it meant that any should be inferred without careful analysis of this

complex body of information. The order in which the data is arranged, the summary statistics and the

plots are presented in a manner which is amenable to data analysis. NBS welcomes any comments,

suggestions or constructive critiques from the readers concerning future data analysis.

Stephen M. Hsu Group Leader

Chemical Stability and Tribology Group

National Bureau of Standards

iii
FOREWORD

by

American Society for Testing and Materials

Committee D2, Technical Division P

The contents of this report, i.e., data on characteristics and month-to-month consistency of re- refined and virgin basestocks, are the fruit of hard work by many individuals and organizations.

Following the first meeting of Technical Division P in December 1977, minutes of early meetings

and correspondence show an immediate, broad, and deep interest in basestock characteristics and

consistency. In 1978, a letter from M. E. LePera, U.S. Army, MERADCOM, addressed to the Chairman, N. A. Hunstad, of Technical Division B, on Automotive Lubricants and the Chairman, P. L. Strigner, of

Technical Division P, undoubtedly planted the seed when he said that "a new basestock characterization

methodology was urgently needed." His reference was to basestocks for engine oils. His need was for

revisions to the important, well-known specification for automotive engine oil, MIL-L-46152. He was moving in response to the Resource Conservation and Recovery Act of 1976 (PL 94-580) which required

government standards-writing agencies "to revise specifications to allow use of recycled materials to the maximum extent possible" without jeopardizing the intended use of the item. It was uncertain as to what the expression "basestock characterization methodology" embraced. Assuming that it embraced

basestock characteristics, interactions with additives and consistency, then these were in a large measure not well understood for lubricating basestocks, especially for re-refined base oil.

In late 1978, Technical Divisions B and P created a joint task group under the chairmanship of H.

E. Tiffany, API, to aid T. Bowen, U.S. Army, MERADCOM, who was charged with revising MIL-L-46152. A number of methods to characterize basestocks, and especially basestock consistency, were mentioned as being important. Taking the comments into consideration, a revised specification (MIL-L-46152A) was issued which did not exclude re-refined basestocks. It did identify a number of important basestock

characteristics for all basestocks, irrespective of origin, i.e., tests and limits but failed to address the question of basestock consistency owing to the absence of adequate guidelines.

Early in 1979, K.A. Frassa, Mobil Oil, who had attended the December, 1978 meeting of Division P, sent a letter to me in which he made four key points. (1) He stated "I believe it is generally

accepted that good re-refining processes can produce satisfactory re-refined oil; however, the con- sistency of production is not known." (2) He observed that a parallel activity was underway in NBS. (3) He suggested co-operation with NBS. (4) He suggested the formation of a task group under Section

II of Division P to pursue this activity.

NBS had been charged under the Energy Policy and Conservation Act of 1976 (PL 94-163, Section

383) "to 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." D. Becker of NBS was placed in charge of the NBS Recycled Oil Program to develop the test procedures—clearly a formidable task.

The officers of Division P (Dr. J. Comeford, Vice Chairman; R. F. Pedall, Secretary; and myself)

promptly agreed to deal with K. Frassa' s suggestions by the next meeting of the division. The

interest in a basestock consistency study in cooperation with NBS was spontaneous. Logically, a task

group was formed under the joint sponsorship of ASTM and NBS with K. Frassa as chairman, and lodged in Section II whose chairman was C. Thompson of DOE, BETC. The magnitude of the undertaking was evident.

The cooperating individuals and their organizations are listed elsewhere, all of whom are thanked a thousandfold for their very worthwhile contributions.

It is appropriate to also acknowledge the fine efforts of W. Starr also of Mobil Oil who

succeeded K. Frassa as chairman of the task group and who issued periodic comprehensive progress

reports.

Of course, it is appropriate to acknowledge the important efforts of D. Becker and co-workers of NBS who arranged for the collection and distribution of the large array of samples and who are now arranging for the publication of this report. Subsequent reports which will deal with in depth

examinations of the data and their significance may also be published by NBS. We hope to have a final

report as well, published by ASTM, possibly as a Special Technical Publication (STP).

iv
The data contained herein are expected to have far reaching applications in specifications,

including MIL-L-46152 and its revisions. The huge quantities of samples on hand at NBS also have

great value for other studies, e.g., of the consistency of finished products and the effect of basestock on additive performance. Indeed, Section IV of Technical Division P in cooperation with

Technical Division N on Hydraulic Fluids has already been using them to formulate hydraulic fluid

samples from re-refined and virgin basestocks in order to study the comparative properties of these

products and consistency.

Paul Strigner, Chairman,

Technical Division P

v
CONTENTS

Page

Foreword (National Bureau of Standards) iii

Foreword (American Society for Testing and Materials) iv

I. The ASTM/NBS Basestock Consistency Study 1

A. Organization and Scope 2

B. Data Presentation 2

II. Rheology 4

A. Kinematic Viscosity at 40 °C and 100 °C 5

B. Viscosity Index 25

C. Low-Temperature Viscosity by Brookfield Viscometer 35

D. Apparent Viscosity by Cold Cranking Simulator 46

E. Critical Starting Temperature by Cold Cranking Simulator 72

F. Borderline Pumping Temperature by Mini-Rotary Viscometry 75

III. Physical Properties 79

A. API Gravity 80

B. Boiling Range Distribution by Gas Chromatography 86

C. Cloud Point . . 126

D. Pour Point 129

E. Color 132

F. Fire Point 138

G. Flash Point 141

H. Odor Comparison 144

I. Refractive Index 146

IV. Chemical Properties 149

A. Carbonyl , Nitrates, Tertiary Carbon and P-O-C Absorption by Infrared Spectrometry . . 150

B. Carbonyl and Nitrates by Differential Infrared Absorption Spectrometry 162

C. Saponification Number 168

D. Total Acid Number 171

E. Nitrogen 174

F. Sulfur 177

G. Oxygen 180

H. Halogens 183

I. Carbon Residue 190

J. Water 193

K. Ethylene Glycol 196

L. Sulfated Ash 199

M. Total Metals 202

N. Metals 205

0. Silicon 219

V. Hydrocarbon Type Analysis 220

A. Saturates 221

B. Aromatics by LC, TLC, UV, MS, and Extraction 240

1. Monoaromatics 250

2. Diaromatics 263

3. Triaromatics 276

4. Polycyclic Aromatics 279

5. Polycyclic Aromatics and Polars 285

C. Polars by LC and TLC 295

D. Sulfur Compounds by MS 303

E. Isoprenoid Ratio by nmr 305

F. Linear/Total Hydrocarbon by nmr 308

G. Polyisobutylene by nmr 311

VI. General Performance Tests 312

A. Demulsibility 313

B. Filterability 349

C. Sediment 368

D. Foaming Tendency 371

E. Rust 380

F. High Temperature Copper Corrosion 386

G. CD/SE Additive Compatibility 387

H. Storage Stability 395

vi
Page

VII. Oxidation and Wear Bench Test Performance 405

A. Rotary Bomb Oxidation Test (RBOT) 406

B. Turbine Oil Oxidation Stability Test (TOST) 412

C. Antioxidant Capacity 415

D. Load Wear Index (LWI) 418

E. Differential Scanning Calorimetry .• 421

F. Lubricant Thermal Oxidation Test (LUBTOT) 430

G. Oxygen Uptake Test 433

H. Sequence III Simulator 439

Appendix I. Sample Numbering System and Data Table for Repeated Samples A-l

Appendix II. Test Methods and Summaries A-7

Appendix III. Additional Data A-29

Acknowledgment A-33

vii

I

THE ASTM/NBS BASESTOCK CONSISTENCY STUDY

1
I. The ASTM/NBS Basestock Consistency Study

A. Organization and Scope

As described in the two forewords, the study was co-sponsored by the American Society for Testing

and Materials (ASTM) and the National Bureau of Standards (NBS). Under the various government Acts

(Energy Policy and Conservation Act of 1975, Resource Conservation and Recovery Act of 1976, and Oil

Recycling Act of 1980), the recycling of lubricating oil has been encouraged. One of the main concerns both in government and industry, is the lack of a technical data base on the consistency in

quality of the re-refined lubricating base oils. The possibility of contaminants, either intermittent

or otherwise, in the used oil collected for re- refining causes concern that batch-to-batch variation

of re-refined base oils may have a significant affect on the finished oil performance.

Historically, the virgin base oil companies are required to maintain constant crude source and

the same processing technology to maintain quality control after extensive performance evaluations.

Control of feedstock consistency for re-refined base oils is more difficult. Studies in the past have

established that a properly re-refined basestock can be formulated to give comparable engine test and

field performance to a similarly formulated virgin base oil.

This consistency question was addressed in a cooperative study begun in March 1980 under the

sponsorship of ASTM and the National Bureau of Standards. In this 13-month study, four virgin oil and

six re-refined oil companies submitted monthly production samples to NBS. There, the samples were

subdivided, coded, and sent to 14 participating laboratories for analysis of the physical and chemical

properties as well as for evaluation in various bench tests. An eleventh control sample was sent monthly for reference.

Various re-refining processes included in the study are: acid/clay; clay treatment; short path

distillation; pretreat/vacuum distillation/clay finish; pretreat/hydrogenation. The processes for the

virgin base oils are mainly solvent extraction/distillation with and without the hydro- finishing step.

Since it is not clear what physical and chemical properties of the base oils are important in

quality control, a total of over fifty tests measuring over sixty-four characteristics were performed

by the participating laboratories. Some tests, because of their complexity, time requirement and/or

cost, were conducted only on predetermined selected samples.

The participating laboratories were Bartlesville Energy Technical Center; Chevron USA; Filmite

Oil Corporation; Gulf Research and Development Corporation; Lubrizol Corporation; MERADCOM (U.S.

Army); Mobil Research and Development Corporation; Motor Oils Refining Company; National Bureau of

Standards; National Research Council of Canada; Savant, Inc.; Shell Research Ltd: (Thornton); Suntech

Group; and Texaco, Inc.

B. Data Presentation

The data are grouped into six main catagories: (1) rheology; (2) physical properties; (3)

chemical properties; (4) hydrocarbon type analysis; (5) general performance tests; and (6) oxidation

and wear bench tests. Within each category, test results are arranged according to the similarity of

the tests or test properties.

In the tables, a single dash, - , means no sample exists for that oil and month, and a double

dash, — , means no analysis was performed on that sample for the specific test.

For each test or each property tested by several laboratories or several methods, the data are grouped together for easy comparison. Each test, whenever applicable or feasible, has (1) a data

table arranged in a month vs. oil source matrix, (2) a plot of the data vs oil source indicating the

range and data distribution, and (3) a time series plot showing variation as a function of time for

each oil source. The time series plot is intended to be a simple graphical display useful for initial

data analysis to aid in revealing various features of the data. In the time series plots, virgin

basestocks are plotted using solid lines and re-refined basestocks are plotted using dashed lines.

These plots show the relative numerical range and variability between the re-refined and the virgin

base oils. It is not intended to show each individual time series plot for each oil. The summary

statistics (mean, standard deviation, minimum and maximum) appear at the bottom of each table when

applicable. The calculation of these values simply ignores any non-numeric code (e.g. > or letters).

In the data tables, oil I is the internal reference oil sent out each month from the same drum to establish test repeatability. A casual examination of the data reveals that apparent variability in

2
the data could be derived from: (1) test method precision; (2) operator error (outlier); (3) pro- duction sample variability. Even after the inconsistent samples have been determined, questions such

as the significance of the test result, and what is truly being measured and how the measured property

relates to performance or quality remain to be answered. In addition, product performance can only be

measured when the basestocks are compounded with additives. Therefore, only those characteristics

affecting the additive response may be the controlling parameters in monitoring consistency. At this

time, such a commonly recognized set of properties does not exist.

Based on the these considerations, interpretation of the data presented here should be conducted

with extreme care, lest false conclusions be derived.
II

RHEOLOGY

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550

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500-

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450

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140
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153
INFRARED ABSORPTION AT 5.8 MICROMETERS

15.0

OIL

154
INFRARED ABSORPTION AT 6.2 MICROMETERS

155
INFRARED ABSORPTION AT 8.15 MICROMETERS

156
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157
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15.0

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158
INFRARED ABSORPTION AT 6.2 MICROMETERS
INFRARED ABSORPTION AT 8.15 MICROMETERS
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1 S.0-i

MONTH

161
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SATURATES BY ASTM D2007

232
SATURATES BY ASTM D2549

90

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SATURATE HYDROCARBONS BY TLC/FID

234
SATURATES BY HPLC

OIL

235
SATURATES BY ASTM D2007

MONTH

236
SATURATES BY ASTM D2549

90

MONTH

237
SATURATE HYDROCARBONS BY TLC/FID

95

MONTH

238
SATURATES BY HPLC

MONTH

239
f o CO o o in CO o 0 0 9 CO • a • 9 tO 1 1 1 1 1 1 1 1 l 1 in 1 • 9 9 ro in a i\l CM •* CM (VI • (VI s y(

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CP • o < • o • </> / • LU • in 01 CM in CO If) vO vO CT> • < • I o o a • • • • • a 1 • a • • 00 L0 • • • CO 0 ifl iO ro CM ro ro CM CO CM CM in • • • • 0 CM cm CM CM CM CM CM CM CM CM CM CM CM . ro CM CM • Q CM a LU • z • »-l • LL • UJ • a I vO in o vO i£i o O N O o CO N o in • 1 • 15 a 0 • • e a 0 0 • 0 • a • • • o t • • hi a 3 CM in ro LO --f ro CO CM CM ro • • • CM N • a. CM CM CM CM CM CM CM CM CM C\J CM CM CM t CM CM •*

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AROMATICS BY ASTM D2007

244
AROMATICS BY ASTM D2549
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246
AROMATICS BY ASTM D2007

35

MONTH

247
AROMATICS BY ASTM D2649

MONTH

248
AROMATIC HYDROCARBONS BY TLC/FTD

25 —i

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249
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258
AROMATICITY (MONO-RING) BY UV

259
MONOAROMATICS BY HPLC

25.0

22.5-

20.0-

17.5 —

15.0 —

12.5

260
AROMATICITY (MONO-RING) BY UV

MONTH

261
MONOAROMATICS BY HPLC

SB

0 2 4 6 8 10 12 14

MONTH

262
CO • ro CO 4 t ^ • • | i | | | i 1 1 1 • • • # _

## • >. s cr a o s o o CO o CO CO CO • vO "0 • • • CO

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CM • N in CM *0 *o If) e

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s; to • Q 0 " ° 1-0) > < _B 00 h • u • o CM CM CM «0 N CO ro * • CO • H Z Z I

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cr< • • O O O o O o o O O o > • UJ • CO CD CO CO CO CO CO CO CO CO CD to to • z UJ z

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HI • < • cr cr > z -J

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263
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264
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266
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267
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268
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269
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AROMATICITY (DI—RING) BY UV

272
DIAROMATICS BY HPLC

273
AROMATICITY (DI—RING) BY UV

3.0

MONTH

274
DIAROMATICS BY HPLC

MONTH

275
•••• •••••** CM *•6•••

ro CM • * • • 1 I 1 1 1 1 1 i i 1 • • * o • c 0 * ° •• •• •• °0 > •0 ° 0 IT * • O • u * * 0 o <r ro ro ro ro ro ro ro ro to ro ro • <"M ro 0 < • o o • 0 0 * 0 * ° • 0 • • ro o • • * • V) • • 0 • o t j£ * CD • <J • • • O 0 • -I • 1- • • • 10 • * UJ • if) : • < • I • ro CM CM CM CM cm CM CM CM CM CM CM • ro CM ro • CD O 0 0 0 0 0 0 0 e • • CM o • • • • • Q ; • LU • 2 • • • • • U- IS • • LU * • CC I • t ro ro 10 <tf ro ro ro ro ro rn ro o N • UJ 0 o • • o • 9 • t 0 0 o • * ro o • • •• ••• *0* 0 * •*

'. r, ••• °o• • Q • LL o CM cm eg CM <M CM CM CM CM CM CM ro CM • 2 • o o * • • • 0 t 0 • • * • o • • • H • • 0 • to • O •• > •• *• • u • 0 • z • • • UJ • • * • h- • • UJ * • CO • o CM cm CM rvi CM (M CM CM CM • O o CM •

""J ° B 3 0 ° o 0 • • I • 1 • CM o • • • to • Q 0 : « & 0 • o > * *

(X s • I'- 0 • • St LL! • • • U • 0 • o O • LL • : ^ • LU ' w 3 ro CM cm CM CM n C\J CM ro CM CM ro CM • ro lO CM ro • CC CM o • UJ X • • • n • CO a • * • < o • * • CD CL • 0 • H * • (0 cj • • CD LU • • Z a • • • N. CO • —i

mi

O o • S • • Q o o ° • * * • • • 0 9 0 o • • *4 o • • • H > • • 0 • • (/) • * • < • * 00 * 0 1= • • * • • o • • • H 3 =) <-< CM CM w4 CM (M 0 z • to • <J 3 O * e * * * 0 0 * o * * o • LU • • CD • to ° a • < • 0 < • CD • * U * • • • Z, • • * M • z • t3 • 0 i—« • a —s —1

CM • ro CM • a • CD I 0 • • • o A • 0 0 0 • • • o • • • i • > • • * 0 6-1 * * • a 0 * • •• s * • *0 • >• * • • h- * • M • • < o —)

CM CM CM CM • ro ID CM * * 0 • • • * 0 • • 0 • • • o 0 1 • < I u

CI 0 00 »e < * 0 O O o o o O O O O O > K • UJ CO CO © CO CO CO CO CO CD CO CO CO CO • Z UJ Z X

(/) < Q

LU • < na

a > z _!

OaH > u z CD LU » » Q 0 < a < 3 3 D LU u a LU < LU < • 2 O 2 < -) -> < o z Q LL H

LO

276
AROMATICITY (TRI—RING) BY UV

0.40

0.35-

0.30-

0.25

0.20

0. 15-

0. 10

277
AROMATICITY (TRI—RING) BY UV

0 2 4 6 8 10 12 14

MONTH

278
•••••• • © CM

O • r- 0»a

r ] • • ^ • CM 1 i 1 1 1 1 i 1 1 1 in 10 • o CM in • • • • • • * • • • *~* — • • • —* ••• > •

or • o • t ") • CO

O * ro o o N • o o co t- • • <o 00 CO 1 1 CM i 1 03 1 03 • N if/ 00 < • • • • • • 1 1 • i 1 • 1 • • • \0 10 • • or • 10 • ro CM CM CM CM CM CM • • • ro • * CM to • u < • o J • i- • 10 • 111 t 01 • 10 10 •* 0» CO • CO It cr • < . X • in 1 N 1 1 in ! 0> co • X • e 1 | 1 | ! • j | • • CM • ** —*

CM • • ~" CJ • Q • UJ • z •• u. • ID • a • CO CM in m N • o co ro CJ • i • U) • \0 1 1 CD 1 1 ID 1 1 l!) 1 1 C7> • ro in OJ • LU 1 1 e 1 1 • 1 1 I in 0 • a • 10 ro ro ro • • t W •* •*

ro •• • cm CO CO <t •o • CM 00 • u. 1 o 1 1 in 1 1 N 1 * o • 00 N o • • | 1 1 0 j 9 I • *0 CM

CM "* • CM ••• • ID • in * «• CO ro o CO • CM 1 1 o 1 1 CM 1 1 CM 1 1 1 • o O CM | | 1 1 1 CM • • CM CM CM CM • • CM CM •

CM •••• U. • <0 N ro 00 • O 10 • UJ | ro . ( I ] 1 1 CO • CM • a. • • | 0 1 1 • 1 • • in • 1 • CM —< —' t * • — CM •••

10 •••• • toN CM <* t <t in ro < • • ro 1 1 ro 1 1 * 1 1 to 1 1 tO • •o CM ro

ro • • a • • 1 1 • 1 1 • 1 1 1 1 • t •* • • • • • a •••

a* • ^

t-X • o • N —i vO • 00 in w • K • CO 1 1 N 1 1 ro 1 1 CO 1 1 • in o N • 10 > u • • 1 1 • 1 1 » 1 1 1 i t t o 10 9 • H • UJ m — * • z • to JJ ID • < H • CD z • o • z u •• 13 •o CM © • in •0 pj • CT • 1 1 1 •* 1 1 P>- 1 1 in 1 1 O CM <t • m CD 1 1 • 1 1 i 1 1 • 1 1 • • vO * • • > • a < • O • a • < • u •• • CO 00 in o CO M • • < • en 1 1 1 1 O 1 1 1 1 * • o «• J 1 1 • 1 1 • 1 • 1 1 • a CM • 0 u • >U>

_lu

M «• • a • • o o o o o o o O o o > • ID • CO 00 co CO oo CO CO 00 CO cn 00 CO CO • z UJ z X

10 • H < a <

111 • < • a.a > z J

a 1- > U z CD C£ • UJ •

1- • a < a < LU

u o UJ < ID < • o < -> -> < 10 o z Q "5 u. 10

279
a••• o O CM

N • N

O o CM • a * . h- O N • 01 pa P> • • <0 co h- • s pa £> co • • 10 1 i I 1 1 1 1 1 1 1 in in • LO in e & V 0 e a L0 O 9 0 O ••

pa) pa)a

api

a pa pa > •• a

r. • a

"> o o in in vO fv

N

N CM • ro in • o O in 10 OJ ro ro m • CO LO CM < • • CO 'O CO V- o CO N • pa) vO o

a. • 10 o m in in 10 1 1 1 1 m | m

m • CO Pat L0 >0 o • * © a o c a 1 1 • 1 1 • 1 a a a in o a a

CD • u 0 —a pa f* PH pa) ph paaa

a pa pa < • o pa) J • i- • in • 01 • 10 o O in CO O • CO 0i CO • < • I • ro n ® O • N « O ro i0 • ro vO CT1 » m 1 I 10 1 i 1 I If) 1 1 in • K in m • Q 1 1 0 1 1 1 1 1 a • in o a » • LU 0 —« pa a a a pa PO • z =^ • M • IL • LU • a • in « N CM CM • o O IT) • i • U CO CO n O • iO pa N CO • LU • « CO co CO N • o i0 CO • or • in 1 1 CO 1 1 in 1 1 m I 1 in • f- L0 in • J 0 [ 1 0 1 | 1 1 0 1 1 a • tf) o a a o 1 ^a —I paj a 0 © PH aa •

=-a > •a• o O CD O (M lO «h a in in

O

Q • • Li. o <M ==a CO CO

O • CM CO CO CO 3 • 0 f*, CO 0> -0 00 • ~* o vO Oi h • © IP | 1 If) 1 1 in 1 1 in 1 LO L0 • CO pa 10 m • :> o j 1 a I 1 • 1 1 a s a • 10 o t a • .,..„ i—i H pa a a o -« aa > aa o • Z 0 e UJ <? • h ro • • LU o 10 CM <* o vD OJ n

Ifl • o IM CMO <f 0i CM OJ

0. • o —< N o co o vO r~ «a| en t=a • o *0 1 I 10 1 1 in 1 1 in 1 1 1 • 03 L0 i0 z • a o 1 I a 1 1 a 1 1 • m O • a u • pH pal -« » • —<

-a

u co • 99 • * *-a u z o D • N LO CM IM

N • 4) o N

H • LU o Ch £> (M in • 0J co in 0-

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t- o w X •

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N • C0 10 r-- in

V

u • o ID oj pH o • co o in S t=-J • • Q o in IM 0J pa a l>- -a 0)

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a 10 o • 9 «x s •

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u 1 1 LO 1 I in 1 1 io 1 OJ 10 10 > • 10 1 1 « 1 1 • 1 1 a a in o - a a • < aa pa pal a • o <-« a-*l > • CO aa 0• z a • *aa) • o r>- iM N • m <* t«- l»- u. • a co ao 0> N • o «s N co u • CD f» L0 O • •o ro O N • > ° 1 1 1 in 1 1 m 1 1 L0 1 in • in n in in K | 1 a 1 0 1 1 0 I j in o a a

LU ^> pa pa

a 0 a

Q

a pa Z a

LU

aa o N

O in r\l LO • co

O > • < o 4 O N •o L0 • O • CO 1 oj 1 1 O 1 1 N 1 1 * • co i0 CM 00

t— ID I I LO 1 1 in 1 1 in 1 1 in • in

:> o 0 o a • 10 o a

a < » a

U-UJ aa • a a o o O O o o o o o O >

i- • LU • CO co CO CO co CO CO CO CO co co 00 CO

a z LU Z X

10 • 1- < a e-i <

LU • < • a.

a > Z J L5

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a

1- • Q 0 « a < D

D -> LU <J o LU < LU < • S O

•a s -i --> < to o z O LL t-co

280
POLYCYCLIC AROMATIC CONTENT BY IP346

281
REFRACTIVE INDEX PCA EXTRACT

1 .650

o

St

T,

GO2

1 .600

1 .575-

1 .550-

1 .525-

1 .500

282
POLYCYCUC AROMATIC CONTENT BY IP346

283
REFRACTIVE INDEX PCA EXTRACT

o

N

Q

ss

GOZ

P

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1 .625-

1 .600 —

.575

550-

525-

500

284
(/) w

</) <

m

1/1 COzN

10 CO < zsu

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a

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CO

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t • I CO

ro

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I • I

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•>

1- . • UJ • CO CD CO 00 00 CO 00 00 oo 00 CD oo 00 • z LU z X

CO • < Q <

lu • • < • cc a > z -1 13 a H > u z CO cc • Ul •

t- • a • < a D r> UJ o UJ < UJ < • o < -) -i < CO o z Q u. ST

in <o

285
u

z

UJ CO

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CO

UJ CO

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in to

CD

r-J

o o o O o o o O o o

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CO • • 1- < D <

UJ • • < a or > z -1 15 a I- > CJ Z CO a • LU s

t- • • a o < a < r> 3 LU u o LU < LU < • o

0 ? < S i -> < 10 o z Q -1 LL s: •

ST

n m

in in

286
Q

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uj 10

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10 _l Z 0. a i u* x U H O i H ~-

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aoI > o O o o o o o o o o > H • • UJ CO CO CO CO CO CO CO CO CO CO CO CO • z UJ Z X

10 • t t- < a <

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a • UJ • s s

1- • • < a < r>

D UJU o UJ < UJ < • Q • ZL < s: -> < in o z o u. ST

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287
oZ CO w s H X

Ul

u

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1- • • UJ t CO (0 to 00 00 03 co CD CD oo CO 00 00 • Z LU Z X

00 • • 1- < O <

UJ • • < o a (£ >- z a C5

a 1- > o z CO

a • UJ • s

<l- • 0 < a < O yj

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D UJ < yj < • Q 0 s < -) -> < 00 o Z o "1 1L ST

288
>QO

I->z

UJ

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IS) <f> z z a x o uJ * a o x QK -» w

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in I 10 » o o o O o o o o o o •> K • • UJ • CO 00 00 00 ao 00 00 00 00 00 00 00 00 • z UJ z

V) • < Q <

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in o m o — O

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289
>QDK

(/) CO£ > s u u Z _l

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1- • CO •*

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s: • • 1 1 1 (M 1 CO 1 1 1 1 1 1 • 10 OD CM o • • 1 1 1 r\J 1 1 1 ! 1 1 1 1 • o CM Cvl a • « CM O • 0 < • > •

-i • a • a • • • o o o O O o o o o o >

h- ! • LU o CD CD co co CO CO co CO CO CO CO co CO • Z 111 z X

(0 • • 1- < a <

UJ • • < o Ct a. > z _! IS

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1- • • Q • <t Q. < D 3 LU o o Lu < LU < • a » E «t E -> -i < 10 o z o u. 5! •

ST

O '•0 in - — N

CM l\J

290
>-QDH

(/) 00 > V U (J z _J

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CD < Z £ S2 in

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1- • • UJ • 00 CO CO CO CO CO CO CO CO CO CO CO CO • z UJ z X

co • • t- < Q <

UJ • • < • a ct > z _l

a > u Z CD UJ t 1- • • < a < O UJ o o UJ < UJ < • s o < 5. -) -i < CO o z Q U. ST

291
>aD

tCO to£

CO *« Z H o s u —

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CO LU LU CO

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CO CO m < Z £ V2 CO K 00

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O o o o O o o o o o •> K • • LU CD CO CO CD CD 00 (X) 00 00 CD oo oo CD • Z LU z X

CO • • 1- < a <

LU • • < o a

a >- Z J IS

aH > l_l z ID LU £

t- • • Q o < a < -> LU CJ o LU < LU < • £ a o ? < -> < CO o z c LU ST

•* rc\i <t

292
POLYAROMATICS & POLAR BY HPLC

293
POLYAROMATICS & POLABS BY HPLC

\

V

MONTH

294
•••••* * • 1 i * g 1 i 1 1 1 1 • 1 « OJ 10 * • it * * # CO *•*•*** . cco ** *• J •• OJ 11 11 m 1 m 11 m j * * • m OJ •

"J *

EX /A * O S/~r CD • \J ^ • O

-J • H• m 1 i i 1 1 1 # ifi • 0* 1 i CD i - 1 1 1 GO ! " o GO • < • X • • * • s • • a• OJ • z * LL • UJ 1 1 I 1 • or • cm 1 ro f <* 1 10 1 o ! o N o • 1 • KD • • t 0 • • • <t OJ • ill (VI oj OJ oj • • or OJ J 1l 1 m 11 CM 1! j i (0 iC • u. t • • 0 • e • * o • ;* • ID l 11 11 !1 I | i i • ID ro • • • O • e j* ** • u. • in j 11 11 to 11 11 * I| IT) i • l • 10 10 • UJ • • • • • • o •*•••*• * u) Ii I!) 11 10 11 LP J i • I • LO 10 * * * * * * 0 lO 0 •* t o •**

A. * 1 1 1 . ' * • o i 10 t 1 10 1 1 10 ! • f\l

N •• CO » u • • • LU • (/) • <• CO 1^O • z o 1 1 1 1 1 i OJ • o > 1 1 N 1 1 1 1 1 CD 10 • Q • cc. • • • • * * * • 00 ro • » CD • • • **** * . 1 1 1 1 i • * » ^ 1 i 1 1 1 1 1 10 I • OJ * 1 • * 10 * I

££

<lua • » o o o O o O o O o o >

i- » UJ GO CO CO CO GO CO CO CO CO oo CO CO CO • z UJ z

to I H < o

LU » < or

a > z J 19

a > u z CD cr • UJ • » Q • < a < D D LU u o LU < UJ < • a < -> -i < in o z o LL h295
o O o o o O O o o o o

0>

1- • • UJ o co CO CO co CO CO co co CD co co co CO • z UJ Z X

10 • • 1- < Q <

UJ . • < • a a > z J o a l- > u z CD a. • UJ • 2 H • • Q i <* a < D D UJ u UJ < UJ < • s Q

o 2 < E -5 -5 < CO o z a -> IL ST

o —

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in -<

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296
- I

I O I

I • I CM

• • • • O O o o o o o o o o

•> K . • UJ • CO CO CO CO CO CO CO CO CO CO CO CO CO • z UJ z

Ul • • t- < a M <

W • • <£ • cr a >- z -J 13 a > u z CO UJ •

t- • • Q • < o_ < UJ u o UJ < UJ < • E D < -> ~) < to o z Q -5 U. ST

o <t

CO ~

m o

i0~ in

297
298
POLARS BY ASTM D2007

3.0

2.5

2.0-

1.5

.0-

0.5

0.0

299
POLAR COMPOUNDS BY TLC/F1D

3.0

300
POLARS BY ASTM D2007

301
POLAR COMPOUNDS BY TLC/FTD
1-1

</> u

UJ HI go a

< CO

CD CO

CO co m <

Z Z \

7

t- 6

CO Q. < a

. o o o o O o o o o o

•>

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10 • < a

UJ • • < • a. ct > z J a > Z m a • UJ • 1- • • a • < a < D D UJ u o UJ < UJ < • o

< 1 -) < co o z Q -> IL ST

o o - ro

303
01 a. z i- O W u zo * cc U l- 0 u K UJ

</i

a

III 01 w< 01< mz — s e z a

ha

01

— <

01

UJz

UJXaox

t-NZ

UJm• • • o o o o o O o o o o o •> K • • UJ 3 CD CO co CO co CO CO co CO CO co 00 • z LU Z

01 • < a <

UJ • . < o Ct IX > z -J e>

a

K > z m

a • UJ

t- • • o 0 < a < "I IUu UJ < UJ < • s a • s «r s -> 01 a z a -J IL ST

304
>ZW

I-10

t-* tozo

<j*UOK

10

111 10<

El

CO

CD > z a S H z w H S

co o < cc\-u

UJa

co

vO (\l i -> o* I • I o I n i i • I I N I O | I • I

>0O |I

<0 I • I

CM I • I O- I I • I I

ro I -

ro I r- i • i - • O o o o O O O o o o >

t- • • u • 00 oo GO 00 CD CD CD 00 CO 00 00 CO • z UJ z X

co • < D <

111 • • < • tx or >- z J 13

a t- > z CQ

a • HI • s

h- • • Q . < a < UJ o 111 < HI < • Q < -> 1 < 10 o z Q -> U. ST n in

CM 0>

-H

O 0

CM

N

CM

O s in

CM

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in - ro

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N o -i * in

CM •* 00 —

CM -i

>0 CM N CM — o

>0 o

COo —

<»• ro o —

0> CM — o

305
ISOPRENOID RATIO

2.00

1.75

S 1.25—1

.00—1

0.75

0.50

306
ISOPRENOH) RATIO

307
U V

o a. K K

10 LU UJ £

CO O

< a m i-o

CO LU m a

2 co £ t- I— e

co c <

o o CO CO N o

• 0 SI • ! I • I I • • • • CO • • f- 0> in i 1 N | i in • • 10

CO

• I O I CM

• I O I CM

in

i • t

o O o o o O o O o o o H • :. CO CO CO co CO CO CO co co co CO co co CO • • hUJ • • < o a CL > z -1 U> a K > u z CO or 1- . a < 3 UJ U o UJ < LLl • 2 4 -> -i < CO O z -) LL

CM -

00 -i

vO O - CM

« 0>

\0 o — CM

-t O

in cm — CM

N O

« CM

o> in — (M

z x w <

308
LINEAR/TOTAL HC RATIO

309
LINEAR/TOTAL HC RATIO

MONTH

310
<J > O X

t- V10 UJ uj 2:

1/) o < a

(D |_o

CO UJ

CD 0- Z U1 s2 U

1- e

</> c < 3Nm • O

O 0 0 OO

O 0 0 0 i >

1- • • UJ • CD CO CO co CO CO CO CO CO CO CO CO CO • Z UJ z X

to . < O <

UJ • • < 1 a. (X > z -1

a

H > u z CD

a • UJ • s E

h- • • < a < UJ

u 0 UJ < UJ < • E a < —> < w 0 z 0 IL

ST

311
VI

GENERAL PERFORMANCE TESTS

312
•••••• • • • • • o o • • • i o I I 1 1 1 1 1 1 1 1 o o • • • o o • i >0 vO vO • o vO •0 • • A A A • •o A A • A •• > •• a • o • • • • • • • • • • • • • • • • Cvl CVI • • • • CM CM CM vO LO CO o ro N o • t vO O < ro •o vO CM o

oc • in

A

A CM CM

A o • *

CO • u < • o

_l . 1- • 10 • UJ • 10 • • • • • • « • a i • • in CO • • • < • I • o o o o O CO CO o o o O o o • t CO o • CD • <0 vO <0 V0 vO vO <0 <0 vO vO •o • ro IP • A A A A A A A A A A A • in A • a • UJ • z • u. • LU • or. » • • t • 0 • 0 0 • • • • vO • 1 • i i 13 » N o o O o o o CM o CM O O • t N O • LU vo <o <o vu vO >o vO CVJ VO • in CM ^0 • a ••• A A A A A A A A A • CM A > •••• • • • • • • • t • • » 0 e • • o o • a • • LL » O o o O o o o o O o o O o • • o o • • vQ vO <0 vO •o vO <o vO vO VO >0 vO VO • o o

(- • A

A

A

A

AA

A

A

A

A

AAA • vO

A

A •• A > •• z •

UJ •• > LU t • • • • s o 'ii t • » •* l 0 10 • • O O O o O in o If) o 1 1 1 • • • in O

»-i • « vO i0 vO •* CM vO CM vO

to • • AA

A

AA CM

A z • o •• o • ¥ •* • (J • a a • u. • * * • • • • • • ® • • • o o • • i— * LU O o

IT, • a • * vO vO 2 s s vO 0 s s vO • o vO -0

111 1- • • AA

A

AA

A

A

A

A

AA

AA • <oAA

co • A < < •

CD •

10 z •

CD o • Z N-l • » • • • • • • • « • • • • • 03 • \ CO • vO vO in in vO <* N vO in K • o • s -I • • a OJ f- v0 CM H •

10 • < LU •

-1 •• E • O

ro • • • • • • • • • • • e • • • • >0 in • • • \r o CM ro ro CM CM vO in • Cvl o O • to i u vO CO in vO

(- • 111

A

A • V) z • <

i—i • CO x • H H • o • • t • • • • • • • # • • • • • a. > i CO CVI •* CO r0 O CM •* v0 CM CM o • • • CO O

UJ • CO

—<

CM Cvl vQ • CO ro vO CD • > A . A • • • > • 1- •

t-t • _l • • • • • • • • • • • • • • • • Cvl CM • s i—i • • < > * * CM 1/) ro N ro o ro ro CM * • • CM O

OD CM

10JZ

LU • • • o • • o o O o o O O O o o >

1- • UJ • CO CO CO CO CO CO CO CO CO CO CO CO CO • z LU Z

10 < Q <

UJ • < • a. cc >- z J 15 0-

H > i_> z CD a. • LU • i- • a • < a. < 3 D LU u o LU < LU < . Q • X < x -> -» < to o z Q -> LL K

00

313
0 o o • o O 0 C vO • © A • M>o 1 • TMi 8 * • * • ft OJ

<r • 1 H sD

Li. • u)A

O • is. m • U < • Q

-j • H • ID • (/) » • • < • i • o O

O • CD ft vQ v0 o A * A • Q • Z •

5-1 *

h"l • | * ^5 i cu

Q

Q t UJ * o « *

if °

j"! oQ o A * A 0 - >Z

LU

t- UJ 0 Uj o O M o vQ

'./" e A * A o 0

<t CJ * Q •

cj Z • Q K • IL 1 ft 9 * • uJ Nl ' n o o

rn • CC

TMj • A

A

A • z

CD o *

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CD

J c J! i ^ 0 q 1 i Q <">J *

LLO •** v< « ro ft O 0 • 0 • H" • 1 N o ro •

J{? * m Z • <

*=, • CD E • w • Z • m

CM • o 0 • • a o | CM

UJ • M • CO

S3 ft >

Z> #

h- * » * >

ft *•* J

a

a 0 0 • < o pj ro

mw

-j

UJQ o O

O o H • UJ ft CO CO © w

UJ • < I X

a >

h- • a » < a < < I I I I I I I e 0 4 s It) CO CO o ro

rt

A o 0 e 1 o o O CO O O o

'0 <C ** '0 >0

AAA

A

A

A o 9 0 • e o (VI o o O OJ O

v0 >o <-s

V

A

AA

A

A • 0 • 9 o O o o a o o O

4> £ \0 cO 0 .0 A A A A A A A 8 9 0 0 o • o OJ in CO in O

•0 <* <\i <G A A • 0 • o e • o o O O o O O 0 O •o '0 MO & A A A A A A A 9 « CO 01 CO e O • o 0 % ft ro N OJ in in • e N CO •* CO CM ron 0 a o N in m <t O o O o o O o

co co CO CO CO CO CO z J a H > -

UJ

O UJ

-) -> < U1 z o 0 ft 0 o o 0 I 1 O o • t O o

tO *0 • A A • A • a • in I 4) o • <0 o

OJ

A f\j CNJ I • • • ft • o O O • • CO o

10 vO vO • o A A • If) 1 6 • • • in • • o o O • « 9 CO o

CM \Q • in CM A A • CM

A c o « * o O o I ft o o VJ '£> uO ft •-0 /\ A A 9

CM • 0 1 1 1 • in O

CM yQ

CM

A 0 © 0 O o • ft o O O • o o O i-0 vO • o A ^ 1

/\ • • • • m 9 • o in If) • o CO kO CM • • ft • m CO • 0 ft CM O O in A

(J <t o • t o • o t CO O

C\jJ *o * A • A 0 • • • • 0 (M ro • 0 • CM ro CM>

CO CO CO • z UJ z X < a < z LU UJ • < UJ < • s a

Li- in

314
« • B • • Q • o i | t | 1 1 1 1 o • * Q o • o 0 • A f • Q » * _ B m _ B • CM o CO CO CO _ ro CO o • GO _

<t * CM • (0 i A A CM

Q • ^

CD • o • D i • t— • to • in • to • 9 0 • • • t © • C> • • < • x 9 O o o o o o o Q o o o o • o • CD • <0 « v0 »0 *0 CM €> ^0 s ^0 <» • CM • A A A A A A A A A A A A • 10

A • Q t UJ • z • M • u. • UJ • tx • • • • • • • • 8 • • S3 • • N • t • 1 • m; o o o ro o o o CM o o o • © c • UJ *0 v0 •0 v0 • Ol. # A /\ /\ /\ /\ A A o fVI A > -_ , # # # o B B Q Q _ > U- o Q Q _ o • B * _ • ^0 *0 *0 *0 >o v0 • In *0 * A A /\ A A • »0 A A

tovz # UJ B

[— • UJ t • - _

_ - ro #

</) • o Q CO CO

Q

N 10 | lO

vO 1 0 10

(/) » A

A

A CM z #

l_J 1• t» Q 1B a • u. o ® • • • • o « i | • • o O • 9 K • UJ • 1-1 • O O o O O o o O O o O o o • • • o o

(/) • \0 >o

A*

•0 LU a* 1 ^ A A • A

I/) < -

CD

Q ••

COCD

J

B

_ # - B

B * Cg f « \ t to L0 10 00 CO 00 U") to • B ^0 UJ • o 0J CO CM

I—ID u_oJE • tj

ro • o « • # • • 9 • 1 # # CM t H* © ro to 10 Q 10 N * CM o • (0 • u *0 o lO

I— • UJ

A

A • 10 z t < • CD * 7^~

ro • tD * . . B

B

B • « OJ 1 ' J* m - in t CD 1 tM o

CD ** ^ A CM

l_ *

^.^— * * B • • # • • ro ro ro (M fO • B CM

CD

CO£

UJ • «• •* • Q • • o O o o O o o O o o > • UJ • CO GO CO CO 0) CO CO CO CO CO CO CO CO • z UJ z X

10 < Q <

UJ • < or > z -1

a > u z CD cr • UJ s:

K • a • < a < D

DD UJ o UJ < UJ < • 2 a < 3 "> < to o z Q u.

10

315
CO

O 0 • a 0 o 0 • • • • =i • c < > I o O O O O O O CM O O O O O O t o cm O

on

a <0 vO CM vD -0 <V S o CM • A A A A A A A A A A A A • li)

A • a « • 9 • 0 • • • • IP •

CM

O CD CM

O CO o CM o O • • 0 N o A A A CVJ vOA » a c a • • • e • 0 • 0> CM a a • 1 ; r- O O O ID O O O CM O r> O O • a o o a UJ vD •O o <o «J o CM «£> <o • 10 CM vO • IX A A A A A A A A A • •if CM A > 0 0 • o l a a a • a • « • • O O a a Q • U. o O O o O o O O o O O o O O • a • O O 3 c •© O >0 v0 -0 >£> O *£> <o -0 O <0 • O >£> 1- o A A A A A A A A A A A A A • <0 A A

10

A >Dz

UJH • UJ o • • a • 0 c 0 a

a

a <M GO

a 10 0 O O O o CM CO CO CP in O 1 1 1 • 0 • ir. O • €> o >0 CM >£> ro v0

10 o AAAAA tf CM

A z o a <f u Q

i>: U s o H • LL

a • • • • • • • a • 0 a

a CM v£> • • K 00 • UJ • HI O O O O o o o O O o O O • o

10 <t • a. vD

O >£> vO >0 vO vO £> v0 0 • O

n

a

UJ

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AAAA

A

A

AA

A

A

A • m

A

a o 0 • a « a • m CO • * • a. ; I CM O IP If) O CM CM <* o • • • o o

UJ • 03 CM ro CM

O

a o n o

CO • > A • CM

A

D

1->K

-1 o aa

a

a

a

a 0 • a • CM

a

a < o CD co <f in ro CM «t

a

a CM

O

CD o O

O

O o O o O o o o •>

1- • • UJ

a CO CO CO co CO CO CD CD co CO CO co CO

a z LU z X

CO • < Q <

UJ

a • < a

aa z _J

a h- > u Z cc CL

a LU

a s s

1- . • Q o < a <t 3 3 3 UJ

u o UJ < UJ < • Q o 5 <r 2 -l "J < to o z a LL ST

31 fi
DEMULSIBILITY, TUBE 1

317
60

50 —

DEMULSIBILITY, TUBE 2

2

O

J, P

m

a

2S

COo

z

%

40

30

20-

10 —

0

0 2

B

4

D

6

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OIL

8

G H

10

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12

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318
DEMULSIBILITY, TUBE 3

60

50 —

40 —

30 —

20-

10

0

0 2

B

T T

4 6

D I E F

OIL

T T

8 10 12

G H J K

319
DEMULSEBILITY, TUBE 4

OIL

320
DEMULSIBILTTY, TUBE 1

MONTH

321
DEMULSIBILITY, TUBE 2
DEMULSIBILITY, TUBE 3

# ( t • o | 1 l 1 1 | •• A > # Q # 9 • OJ OJ —<

LO

Q • ¥

CD • U < • Q • H • (/) t LU • if) • • • • • • < • I • o O o o o GO CO • CO • i0 »0 • A A A A A • Q • LU • Z • LL • LU • (X ( _ # „ e _ # • f • 19 « CD o O O ro o o • UJ vO \0 *0 <o • or # A A A A A > # # 0 0 0 Q • u. • O Q o o o o Q • vQ >o vO vO

j— • A

A

A

A

A

A

A

If) > # z

Ijj 1- • lit • • 0 0 g

_ to • O Q LO * »o CVI <>

If) • A

A

A

A zu o #•

*£.

Q • u ' o • LL H> • LU • O o O o o o o

(0 to • CL * o *0 *0 *£> UJ < • A A A A A A

A

to

(X) LU (0 # z m • • # # # 10 LO vO • Q OJ Q

to< J£ •t ¥

ro • <J • O • • _ • « • Q • (— • N ff) C\J t- • to • U • LU z • to * 4 • CO • z . • t3 # B #

LJJ • a. > 1 <* 00 ro o

CD • CD -* - • > _

>.

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-1 • • • • • • • < • LO N ft

CO< toJ

a>LUQ • O o o O o O

O

K » LU CO CO oo GO CO CO CO

I/) LU • < • CL (X > z J 0. • Q • < a < o LU < -) -J < to 9 O

O • 0 1 1 1 o o • • 9 o o

<0 o • o vO <o A A • 10 A A A

a • • • 9 • CVJ CVJ 9 0 CO o ro o • 0 vO O

<0 -0 OJ o <) A A OJ OJ A 1 • • • in 00 * o o o o O o • • 0 CD o

«f) •o <0 •D • ro in 0 A A A A A A • u> A 0 • « 0 9 oo <) 0 a o OJ o O • 0 0 0) O

to o C\J 10 to • in CVI vO A A A A • <f CM A 0 • 0 9 • • o o 0 0 O o o o O O • 9 9 o o

<£> il 10 • o A A A A A A • o A

A

A o 9 N 0 0 K in o 1 1 • O

CM <JD

A CMA 0 • 9 9 • • O © 0 O o o O o O • o O

vQ tO *0 0 • o >0 A A A A A A • vO A A A • t 9 in 0 0 N * N in OO • t •

00 CM • • 9 • • 0 • <* o • •

in in ro 9 • OJ CO OJ 9 9 • • 0 9 <t 0 0 * CXI CM O 9 9 9 00 o

C\| <\J *0 • 00 ro A 0 A • • o 9 OJ OJ •

ro o ro ro OJ . OJ o

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09 9 o o o >

CO oo 00 CO 00 00 • z UJ z X < o < H > u z CD UJ • u o UJ < UJ < • a o 2 Q -> u. yV)

325
• • • * •• ••• c. * • Jt. 1 i 1 I * ° 0o0* •*

CO> ''' * 0 _

r 0 * • • * » f\l r MJ 00 < * • —1 (\l • y • • u e < • o J l~ e' • CO a * UJ • cn • • t • 0 0 • • < • X • o O o o O O • CD • to «o v£i c /\ • O • LU 0 • z • U_ • LU * • T u> O o o O o • UJ • t0 tO • a. *

<*° 0 > ° • * * * * * 19 Q • LL. t Q o o Q o D 0 e O 43 \Q '0 A A A

A 00 • ° • * * Z ° * UJ * * • HIUJ O 3 o ° • © © * « * • o O o o CM 1i s • k0 v0 <£) CM ° • .- ( t A A A 0 • 9* * * * Q ° *

cjj 0 p _* 0 ° 0 0 1— • LU « O O O o o O

'0

UJ < 0 e A

A

AA

AA

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if) • • I CQ • * UJ 0 i— ° •

in ° • z 3 0 I ° • 8 0 • • s * • N CO

*^ lL • Q C\l o

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'"f • *

C\J • o • o • • o •

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N CD CD

CD • HI • ID 3 • > 0 h- ° e • I > 0 I 0 * -1 * • e » • • < • CM

N lO

COMw • _J

^3

21UJO o O o o O o o O h • UJ I 00 CO CD CD CO CO CO

UJ • < a > Z J 13

a • Q < a < D UJ o ST < 2 -) < CO

326 • • • o o 9 • 1 1 1 o O • 0 o O

vOO 9 o 0 o A A • A A A » • • • 00 CO 9 9 oo o ro co O i : 9 « o

>£> <o c* « A A CM A • t CO o 9 9 o O o o O o • 9 9 CO O

M5 <0 -0 iC vO • (0 X)

A

AA

A

A

A • 10 9H

A • « • • • 9 • • O CM o o o O 9 9 • O

^0 CM * • in CM <o A A A A • CM A 1 • • • • o O • O o O a O O 9 0 o O 0 « vO i0 o 10 A A A A A A • i£> A A A o 9 CM 9 •

CO 10 o i 1 • • e 10 o

<£> CM CM <0 A cv A 0 » • • 9 9 O o 9 9 Q o O o O O 9 • 9 o o

<£> <0 <0 VO 9 o vO <0 A A A A A A • •o A A A 9 9 9 9 O <f OO o in vO . 9 <t <0

CO CM e 9 • • 9 9 0> 9 9 in 10 0> t 9 • CM

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r-l

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ro VO 9 o K) A 9 CM iH A

CO ro n CM C\l ro 9 9 • CM 0>

ro

99 o o O >

oo oo CO CO CO CD 9 Z ID Z X

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a < h > U z CD a • UJ o o LU < LU < 9 S Q o z Q LL S 9 K

10 1
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vQ *** * CP A OJ *^

Q • ¥ • o • o # 1- • 10 • UJ • (0 • • t • » e • t • • • • O • • • < • I • O 0 0 0 0 Q Q • CO • O SO vO « i0 s cvj s s s s tO CVJ • A A A A A A A A A A A A • to A • Q • UJ • 2 • LL • UJ • cr a • • • • • 9 • • • t • • • • • t • VJ O 0 0 ro O 0 CVJ s? O • 0 • UJ l0 \Q qj \£) •D IO CVl • CL 9%

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A • # # # " * * * * % * Q • u. • o O 0 Q 0 O O *•* ~? 7: *o 43 vO • -0 t A A A A A ** A A A * A •

l/i o #

LU|— • UJ # ro f «

</) 2 ~r CO LO

O 1 1 1 • 10 i ^ n vO >"\J tO ro tO • A A A, z . o o a <fQ

(JQ 5" \ , # 0 0 _ ( # * O • 1- H • UJ M • O O 0 O O O O O O O O O O • • 0 0

co CO • or sO (0 vD ^0 i0 ^0 vO «o

O • 0 *0

UJ * * A

A

AAAA • A

A

10 /\ <m ctUJ V)

COz * # ro » o IP to in \0 CO CO CO O 10 CO • jr t_J CO 0 OJ

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Q

(/) < gN • ¥

ro • u• o O CO • • o • K to ro fO N in *0 LO • • CVJ t- • (0 (0 ro • UJ • 4 • CD • *" • O m 9 # # CVJ •

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__ pn . on

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CD • w • CD *** *"* C\J

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•£> • Al A • * **

_J * * * * _ 0 CO 1 • to ro ro OJ ro * CVJ CD • ro

to

-1

UJo • » o 0 0 0 0 0 0 O O 0 >

t- » UJ CO CO CO 00 CO CO CO CO CO CO CO CO CO • Z UJ z

10 < 0 <

UJ • < * a ct > z J 0 a > u z CD

a t UJ • » O » < a < UJ U 0 UJ < LU < • 0 < ") < CO O z 0 LL h327
00

,:. 9 9 0 9 9 O o 9 9 9 O 1 1 1 1 1 1 1 1 1 1 O o • 9 • o o o • -0 '0 o • o vO *0 I 9 A A A • <0 A A 9 A

B 9o ©0> •9 ao •• 9 ~) 9 • c 0 • • 9 o 9 9 9 • © • • in 9 • 0 CVI CM CD CM O co o CM O O • 9 • N o < • 9 —

CVI 94 —* <o <0 94 •

tr . to

A

A CM 99]

A o • ¥

to • u < 99 K 9 tO 9 UJ • w • • 0 o • • 9 0 9 • • 9 9 • 10 9 • < » I e O O o o O o CM o O o O o o • 9 9 CM o 9 CD 9 K0 -0 <£) CM VD o k0 %0 <0 • N o CVI <0 • A A A A A A A A A A A A • in A • a • LU o Z 0 t=J o LL • LU • a • 9 0 0 0 • 0 • 0 0 o • 9 o - 9 9 9 | 9 (J o Q ID o o o CM o ro o o • 00 9 LU <0 •0 •o >0 CM •o <o • <o CM vo ° a •0 A A A A A A A A A • * CVI A > *99 9 9 c. 0 o o • 9 • s • -f • 9 9 o o 9 9 Q 0 • LL • o O O o O o o o O O o o o • 9 9 o o 3 • vO >0 tQ vO vO vO *0 III 9 o <0 o n A A A A A A A A A A A A A • <0 A A

to 9 A > 9| u 9 z •

lu 9

(=* • • LU 9 9 o • 9 9 9 9 9 9 0 CM co 9 9

Lfl 9 9 O

O o o CO CO o IT)

O | 1 I 9 9 10 o

tl 9 o €> *£> o <J c\J <* *0 ro o

10 • » A

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A z -> • o o • u * • 99 94 • ¥ Q o 9 o z • LL © o • • • 9 9 • 9 9 0 9 • • o 9 9 H H t LU 9 94 0 © O o o o o o o o O O o o • • X o

to to • a.

O vO (0 >£> o 0 *0 o • <0

UJ 4 * A

A

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AAAA

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A • 10

A

W< ~ 9

CD Q" 9 99 LU «

CO 1- I (D < » Z 2 S 1 0 • 0 o 0 t 0 9 • • 9 9 co ro 9 9 0 O h- in vD N o ro L0 9 • 0 ro X j_ • • Q 9 —* 9 CO •4) CM

hO

if)

a < _l 9 E 9 N 0• ¥

ro • o - 0 0 0 0 • 0 • • 0 9 • 9 CVI • • Q 9 ^_ 3 kQ D ro ro ro o CO 00 • ro 03 9 If) » U 10 — 9 LU z • If)

1=4 • < s 9 CD 99 Z • L5 9 9 • 9 « 9 9 9 9 • • O 0 to cn 9 9

LLI • a 3 I in CM o IT) to o CM CM <* o • 9 9 o o m • CD 94 CM ro CM •0 • o ro 3 9 > A • C\J A

i= 9•

c> 9 > 9

1- • 94 • J 9 j a

O • o 0 • • 9 9 9 9 0 9 • CO 94 9 9

*4 9 i < > *- CO in o ro

N <t • • 9 CM » ro 9 CM

to *

-I3

LU 99 99 Q O O o O o o o o o o >

l~ i LU i GO oo co CO CO co CO co 00 CO CO 00 • z LU z

tn ' 1- < < Q <

UJ < i a £1 > z _J <J

a 1- > u z CD

a • LU 9 E H a i < a < 3 3 LU U o LU < LU < • z Q s < s 3 < to o z Q IL 1-

10

32P.
DEMULSIBILITY, TUBE 1

63

50

40 —

30

20-

10-

0

*

1 r

8

G H

0 2

A B

4

C D

6

E

OIL

10

J K

12

329
DEMULSIBILITY, TUBE 2

60

o

50

40

30

20

10

0

0 2

a

4

D

6

E

OIL

8

G H

10

J K

12

330
DEMULSE3IUTY, TUBE 3

60

w

<

S

COo

H

2

50-

40

30

20-

10 —

0

0 2

A B

4

D

6

E F

OIL

8

G H

10

J

12

K

331
DEMULSEBILITY, TUBE 4

60-

50 —

40

30-

20

10

0

e 2

B

4

D

6

E

OIL

8

G H

10

S

12

332
DEMULSIBILITY, TUBE 1

MONTH

333
DEMULSIBHJTY, TUBE 2

334
DEMULSIBILITY, TUBE 3
DEMULSIBILTTY, TUBE 4

MONTH

336
a

m 9 a • o i 1 t | # • vO a • A aa > #

q;o • • • • % # • a

CO o 00 o o < # m> D A A o • *

CD • <J < • O • (- • in • LU • 10 • • • • © 9 • < • I • O o O o o o o • CD • >0 vO •0 >0 <o >o ^0 • A A A A A A A • Q • LU • Z • U. • LU # cr • • a o • a • • • I • u> • CO O O o IT) o o • UJ <0 VO <0 <o *o • a. aa A A A A A

>•

©•• • • • • © 9 m

Q

a • LL • O

O o o o o o a • <0 <0 MJ •o \0 >£> 'O

H # • A

AA

A

A

A

A

(/)

a > # u # z

LU # • LU t • © 0 © 9 01 a • O o o o o ro o • to m> >0 \0 *0

10

A • A

A

AA

AA z a o •

(J • •• a

sCag o • LL • t ( 9 0 © • LU • >—t • O o o o o o o

00 • OZ • <o <0 MJ mj M) vO CI UJ • A A A A A A A

00

a < o # as It ©a to Q a CO # Z # • • 9 a

© • ©

N ta 0> >0 00 00 10 a • Q CM t- a 10 # < < a

LU • *

orCD • 9 • a 0 0 • • h- • 0> o * If) <* o • 10 • U o

h- • UJ

A • in z • < • CO •• o o 0 0 9 • • a • 1 o MJ in C\J LU • CD — CM CM

CD • >

1-

aa > a 1- • J 9 • • • • 9 9 « • < • in N ro mj <t 0>

CO

If) JZ

UJQ • o O o o o o o H • LU • GO CO CO CO CO 00 CO W • 1-

LU . < • a: a. > z J

a

K • Q • < a < D LU < s. -> 1 < in 9 9 9 o o 9 1 1 1 1 O O © o o

<0 • o o <0

AA 9 A

A

A • 9 9 9 9 • 00 0> • o LO L7> o n • 9 00 o

CM <o >0 r*. CM MJ A A OJ c\j A • 9 9 9 9 o O • • o o o o o o • 9 • o o

•o <0 (0 <0 vO •V 9 o MJ MO A A A A A A 9 >0 A A A • 9 • CM o • O D o o O 9 9 00 o

rvi « • 10 MO

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^0 >£> & '.0 0 9 o MJ

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vO MO A CM A

© 0 o • o 9 9 o O 9 o o O o O O 9 • 9 o o

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00 in 00 CO

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O

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O 9 9 no o O i * o MO A 9 CM A • Q • 9 9 CM 10 0 • in m OU o • O o o C\J It) o * (0 in MO A © CM A « • 9 9 n CM •

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m • 9 9 r«l • O o o >

03 00 00 oo CO CO 9 z LU z < Q <

1- > <J z CO a. • LU 9 O o LU < LU < • D o z O -> LL s • 1-m

337
9 4 9 • • iL' J o 1 i I 1 1 1 • o vO • « A 9••

a*> ••

or •• • "5 0 0 c • © 9 • • © m 0> o CD 0* c < • 9 ~* -4 HO

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J 0 o © • < • I o O O o O o o o • CD © hQ kO hQ hQ HO hO hO • • A A A A A A A • Q • ID • z • LL • UJ • or o ® 0 • 0 * • I • 13 o o O O o • UJ hO HO HO HO • a ••• A A A A A > ©• • • • • 9 • • U. • o o O o o o o D • 9 o vO <3 h0 hO hO * © A A A A A A A

(fl • > •• U • z

ID • H • • UJ • • 0 • 0 m • . o O O o O

m

O

M

© • >0 nO -0 HQ hO •* hO

in • o AAA

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AA zo • u • 99 * •• u • o • u. « 9 0 • • 9 • H • LU • w o O O O o o o o m • or o hO -o hO HO o hO HO m © © A A A A A A A m rH • < O • o ••

'/i

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CD • 2 s • 0 9 • • • 9 9 • o hO CM CO HO o S VI » • Q CM 9* h < © < — •• <

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ft • u a • o o o • • 0 • 9 • 1- 0 J* O * CD o • 10 • (J o H • UJ A • 10 2 . < M • CD E 0 - - • z

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CO • > D • h • >M

—1

© » © • 9 9 • < © m 10 10 o

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->n

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a

h • a o < a < 3 3 CU • s < 5 -J -) < w • « 9 O

O • 9 I 1 1 1 o o • • • o o

HQ <0 • o h0 H.0 A A • HQ A A A 9 0 • 9 • • • • N O o c t • o

CM >Q -<

a • CO CM hO

AA CM CM

A 0 • • 9 « 9 O O • 9 O O o o O o • 9 • O o

hO HQ HQ hO hO h0 • o <0 HO A A A A A A • HO A A A

Ci o • • o O • • O o CM O O • • 0 o

hO "* hO CM nT' hO • nO CM HO A A A A • <M A 9 9 • • o o • o o Q o o O • • • o o

HO <0 -0 hO -0 HO • o hO <0 A A A A A A • to A A A • • • O cD o 1 1 t • • • HO o

hO s «0 A <t CM A 9 9 o O • o O o o o O • 0 o o

hO hQ hO hO hQ n0 • o hO hO A A A A A A • nO A A A 9 © • 9 • • hO - •

CD IT o CD

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CD

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338
saasg » a

a

Q s ¥ • O 1 i I I | 1 1 1 i I o O a o a • vO vO vO • 0 a » A A A * A a A aa •a> aa

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vo vO *Q *0 v£J CVJ vO vO • vO CVJ vO • a. a A A A A A A A A A a (M A a! a a a • a • • a O o s • LL » O O O O o o O o o o O O O • a • Q o > >0 vO <o <o vO vO vO •£> VU a O *0 • A A A A A A A A A A A A A • vO A A •# A asaa • LU 1 a • • • e « a • ro vO » „ « » o O O O o N O O vO o 1 1 1 • a vO o • vO lQ >0 *£> T •* • A A A A A A A <f rvj a•a U- a • t a a a a o a a a a • a O o • LU a i O O O O O O O o o O O O o • o o a q; a vO \0 vO vO *0 \Q vO vQ vO vO vO * o vO • A A A A A A A A A A A A A • vO

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a

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to

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A

aa < a 1U • * a • (J

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a

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ID e CO CvJ CvJ CvJ CvJ

n CM ID vO • CO 10 >U CO • > A • CVJ A ,aaa _J a a a a a a a a a a a a • a a N a a a < a ^ •0 4> 10 L0 \0 vO fs. 10 CO m * • . a CO m * r>

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DD o O LU < LU < • Q • s < 2. "> < CO o z Q LL E • H

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339
••0•• ft ft • • • o • • • • * 8 O 1 i 1 1 1 1 1 1 1 1 o o • • • o o • o ,Q >0 * • o vO • o A A A • i0 A A • A 3 c• > •* or • o I a e ft c 0 0 • ft 0 * • t • t •

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t\l

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cr • 10A

A

A

A CVI CV)

A

Q • *

CD • o < • O J • t~ • 10 • UJ • 00 ft o 0 0 • • » 0 e • • o O • • <t ' X • o O o O o O c O O o o o O • • O O • m o >0 O « « cO >o vD vD cO <0 <0 • o •0 >0 o A A A A A A A A A A A A A • <0 A A • Q A • LU • Z • N* • LL • LU • X ft ft « 0 • • a ft • • e • • • • t • 1 • VP • 03 O O O O o O o LO o O • • • co O • LU iO >D o o vO cO o C\J iU <0 • <o • cr ••• A A A A A A A A A • * CVI A > •••• 0 • 9 • • • 0 • o • s e • • o o • • Q • • LU o O O o O o o O O o o o O O • ft • o o D • o vO *0 .0 o C *0 cO O -0 « <o • o •Q O H • 0 /\ A A A A A A A A A A A A • A A

CO ! A > • U • z •

111 •• o LU

a o ft ft • « • ft • o • L0 ro • • W • o o O O o O o ru iG o 1 1 1 • • • O

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AA

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UJ ft • A

A

A

A

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A

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A

LO 0 A < o •

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•H • CO Q • m • z 2 • -' 0 • • 0 • • o e 0 • • « • 00 • 9 \ H ft o O p* O CO O O O • • • o z co • • o © —» H CO —<

—a <0 • L0 £> « • A • -ft A

to • < ••

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or • cj

CD • O ft 9 o • • • • o ft • • • © • • N CVI • 9 • I- < O o CD in 10 CD CO O • • • o • to ' u <0 • * o >0 • LU A A • CM A • W z • < • CD E c• Z • M • L5 • • 9 • 0 • c •>• •* • • • a ft | 3 a- r\J L0 (VI O O CD O • • • CM o

cu CM CM Cvf CM ^0 in CO <0 • O

N «

CD • > A

A « ro pal

A • h •• > • H ••

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CT 9 s ft* •

a)-J3

2.LUQ • s O o o O o o o o O o >

t~ > LU • 00 CD CD CD co CO CD co 00 0D co co 03 . z LU Z X > h- < a <

LU > < i a

a > z J 15

a

H > CJ z CQ or • LU • h • a » < a < O D LU U UJ < LU < • Q . 5 < -l -1 < 10 z Q LL H

co
DEMTJLSIBILITY, TUBE 1

60

50

40

30-

20 —

I

10

0

0 2

B

4

D

6

E

OIL

T

8

H

10

341
DEMULSIBILITY, TUBE 2

<

m

o

COP

60

50

40 —

30 —

20

10

0

0 2

B

4

D

6

E

OIL

8

G H

10

J K

12

342
DEMULSIBUJTY, TUBE 3

60

50

<

O

H

00w

H

Z

40 —

30-

20 —

10-

0

0 2

A B

4

D

6

E

OIL

1 1 1 r

8 10

G H J K

12

343
DEMULSD3ILITY, TUBE 4

<u

m

o

H

W

H

P

60

50

40

30-1

20

10-

0

0 2

B

4

D

6

E F

OIL

8

C H

10

S

12

K

344
DEMULSIBIUTY, TUBE 1
DEMULSIBUJTY, TUBE 2
DEMULSIBILITY, TUBE 3
DEMULSIBILITY, TUBE 4

348
•••••••• 1 i 1 1 1 1 t 1 1 I LL \ • o •0 • • • Z 1 • • » • • 1 <* ••

*• ••

(X • Q • • • < • ro LL in LL LL CO ro • ro o 10 i0 CC • CO • • • • • • Z • • z z • • • • t Q • ¥ • • —1 CO • <J —• < • O • H • (/) • LU • V) m < • I • CD LL ro u_ LL LL LL LL LL ro LO ro ro • • Z z Z z Z Z z • • *

<U CM 0 • Q • ro ro • • ro • LU • Z • j-t • IL • LU • 0. * • 1 • LU • CM CO to LL o LL LL OJ in in to in • LO CM UJ • CC • • • Z • Z 9 Z 0 • • * • • in CO • 0 • ro OJ N • • * • » CO in ** Q *•

>• • Q X • • ll D 1- • • LL OJ LL ro LL LL ro LL o LL • <* ro ro

LU • • Z • z • • z • • Z • Z • Z • CO ro • • ro OJ OJ *-* d- • 0 LO • OJ > • j— • z • LU • h U- • • LU • UJ • • OJ CD CO >0 LL o ^* CO I ! 1 • >^ CO CO z • • • • • t • Z • 0 G ro CO • 0 z < • • OJ vD ro CO • • CO

'-1 CM

CD •

Lit ••• LL

(~ CX • LU » 1 CO LU • CC CO <=i m CO 1 N • —'

ID

H • • • • • 9 • • • • 0 • o • • LO • (0 UJ • \Q OJ *-• • • • • »H OJ

CD o •

CC • CO U •

CD • z • s • 1 • 3) • • Q • (\J is in ro ro in 1 • CM • • • • • • • © • * • • * CO • 9

u")

O • • • < • OJ •• z

UJ • o • • ! Q • CO in CM o 1 (M ro OJ • n ** LU • LU • • • • • • • ° • ° • * • * N OJ • 0 CO • 10 t ro CM ro * 10 • < ro in M

O) • CD E •

*** • z • o • CC Z * t-t » CD • 1 in o O in

m in o D • > • • • • • • • • • • • * OJ o » ro ro • ro • H ^ • •

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CD * • N in ro ro <* in in • < o ro < t • • * • • • • • • • • t • • N N • CC OJ

LU • (M CM in OJ K • 9* •

U. • • O o o o o o o o o o > K » LU • CD CO GO 00 CO CO CO CO CD CD CO CO CO • Z LU z X

CO < Q <

LU • < • cr cr > z J o a t- > U z CD CC • LU t • Q < a < D LU V O LU < LU < • S D < ") ") < CO o z Q LL 1-

CO

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404
VII

OXIDATION AND WEAR BENCH TEST PERFORMANCE

405
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to

412
TOST

2500

2000-

K

3

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1500

1000

500

413
TOST

2500 —

i

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MONTH

414
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in 0> If) (VI rj • o o N 1 1 1 1 o o • o o o o o o • o o o o • • • • •

in ID

N o II) • N C\J CM o O o o o o • o o o o o o o o o • o o O o • • • • • • • • • 0 m If) If) • CO <!• O o o o o o o • o o O o o o o o o • o o O o e • • • • • •

CO 0*

CO CO • in CO CO CM o o o o o • o o n o o o o o o • o o o o 0 • * 6 • • • 0 • •

in CO CM ro CM CM eg • CM s o o o o o o • o o o o o o o o o o • o o o o • • •

CO

to t/l t0 «tN in in o o o 1 - j o o w o o o o o o o 0 * a 1 * •

If) o o o o o o o • O o a o o o o o o o • o o o o 0 © © • • • « • 0 0

If) CMo o o o o o • o o O

O o o o o o o • o o o o t o • • • • • 9 • •

If) If)

O o n o o o o o o • o O o o o o o a o o • o o o o 0 * * • • • • • * N CM ro ro r\J m • n CM o o o o o o • o o o o o o o o o o • o o o o 0 • • • • 9 • t • o o

pM o o O o O o o • o o o o o o o o o o • o o a o • 9 « • 0 o o o • >

a) 00 CO CD en CO • z UJ z < a < K > u z CD a. • LU • z u o LU < UJ < • X a o z o U. U)

415
ANTIOXIDANT CAPACITY

0.04

0.03-

0.02

0.01 -

0. 00

416
ANTIOXIDANT CAPACITY

0.04

MONTH

417
0•1?* '

("Pi in

C1 CD * y r 0 | I I 1 1 t I 1 • 1 % ro » o LO 1 * o LO c ro ro (T) ro ro

Q ro

N

ccp

v ^ o X) CM • OJ J , .1 ° 1 * .1 in < 0 ^ 1 1 1 t t 1 1 o • *o * to 1 n") CM OJ ro OJ • Q OJ ro O * ¥ ro

03

<C • o

-J • H • 10 o LL1 1 4 OJ CO CD OJ • < ! x ' 0 ) 0 1 1 • 1 1 • 1 0 1 • in t • • m • OJ 1 1 1 1 in i [ GO ! CO 1 • t CO CO ro ro OJ ro ro ro OJ ro • o ro • UJ • z • lift LU t CC r — ro o OJ • 1 • • 1 « 1 • 1 i • 1 * • in n • • • 111 1 t 1 i ! 1 1 CD • • • • a • FO c\j OJ C\J Oi 0J • OJ ro :

OJ 1 OJ <\ LO • CO in ^ • U- o o i i I • 1 1 • 1 • • £> • • o £ i i o ! ! ! 1 CD • • o

ro ro ro ro ro ro • ro ro ro

ro

p UJ

Q CD * 0 i • i i 1 i ! i • • * IP Oi in j i i CD 1 * in

CM

w OJ

N CM OJ CM

eg o• u. o IN CO o OJ • CO CO • UJ i " • • 1 • t i • i I I • • CD > • • • (1 1 ! 1 i o 1 i 1 * (0 0 OJ m OJ OJ CNJ • OJ OJ ro *•©* * _

OJ CO OJ

rl

CD

_ 1 * 1 . ro • * J cr ' I I • e 0 ro OJ ro rn <T mm OJ ro 0 ro • ¥ • u ? * P aj "- . OJ m .1 i _f 1 i * .1 1 * n *

OJ tn 1 l <r in 1 1 . 1 1 • • V)

Cl *UJ ° rn rn r\i ro OJ • W

E~ * m

(/) •

<E • O CO u) CO r0 If] CO OJ ro CO

13 • a 0 | • 1 • 1 » 1 e t • t 1 • in • • • *-• • CD 1 o 1 o 1 CO j 1 10 1 1 • • • CO N • ^ ro ro rn OJ ro ro OJ ro • ro ° LUQ *0 0 ^0 * Cl ) t * l B 1 1 1 I 1 • <—i * * o 1 ' 1 1 1 I 1 •

UJ 0 ro OJ OJ CD OJ ! OJ U M

-J • o O o O o o o o o o o > H • UJ I CO CO CO CO CO CD CO CO cc CO CO CO CO • Z LU z X

00 < a <

UJ • < o a

a > z —1 a

K > u z CD cr • LU • 2 Q o < a < D LU u o HI < LU < • 0 < i -> < CO o 2 Q LL H

LO

41

a
LOAD WEAR INDEX

O

419
420
••••• • • • • • ro 10 » * • 1 i 1 1 1 1 1 1 1 1 CM * • 9 1 •1 • • CM (M (VI • CM (M CM • (VI z •••

•*> •*

cr • o • • * • * • • • • • • • • • • • • • CVl * • h • • CO CO (VI CO o VO CM CO CO • • • CO CO < • • ro (VJ ro (VI ro (VI (VI (M CM <* CO CM • CD 10 H <t a • 10 CM o • id CD • U < • o

-1 • h* • CO • UJ • CO • • • • • • a 1 • 9 ro • < . I • (VI CO (VI CO •0 <± N CM ro 10 10 « • • • CD 0 » oj • (VI (VI (VI (VJ CM (VI CM CM CM CM ro CM • ro

(VI • C'J • UJ • z • LL *• /VQl ' 10 * * • • • e l • a * • • • 1 a> 9 ° • 1 » o (VJ ro o CM CO 00 CO CM CD • UJ • (M (VI CM 0,| co ro • a ••* > *••• • • • • • • • « o • • cO CM 1 • Q • • u. CO CM CM N CO N o 00 • 9 • CM iD • • (VI (VI CM ro CM CM (M CM ro CM ro ro ro • cr. CO c\J * CM 10

>- •• o • z •

UJ • • h- • • • • 0 0 • o o • a 9 O in 9 9 CO • • CO vO O N C\J ro —1 O i0 i i l • • a ro M • • (VJ (VI ro CM ro ro ro CM ro CM "J CM ro CO • CM z • o • u • •« * it • u • 0 • LL • 9 • 9 • • • • e • * 0 • • • a* O • 9 H • UJ • *—» • s O CO 10 10 it) in • 0 co CJ • 01 • (VI (VI ro CM CM CM CM CM CM CM CM CM ro • i0 m CM ro UJ to • CM CO Q • < •

CD ^ • Z • CO •

CD • Z w • • © • • ° • • I c o o • • • CD • • s • • CO CO CM CO rcl CO a> 10 00 CO ro • • • CM ro o • • o • (VI (VI ro ro CM CM CM (M CM cm CM ro • CD CM CM CO

1- • CM co 0- • < • LU • > •• o • o • • • • * • • • • 0 © 1 • 9 N • 9 Q • H (VJ CO o ro, O o • • • CO o Q • CO • o • (VI CM (VI ro (VI CVJ CM CM (M CM CM * t 10 cO ft < • UJ CM • CO + • < • CO JM • z o • w• CD • • • • • 0 • • • • • • • CM CD * * • cr • 1 (J> CO (VI CM CM CM r*- • 9

111 • M 1 CD (VI (VI CM (VI (VI CM CM CM CM CM CM • ro CM CM * > CM

r- • Z • a ••• 9 • • • • • • • • • • • • CD LO • • u • • < • o o N CO '0 CD • * O O • • * N O •

IN I U

CO •• a • o o o O O o o o O O > • UJ • CO CO CO CO CO CO CO CO CO CO CD CO CO • Z UJ z X

to • 1- < Q <

UJ • < • a. a. > 2 -J 13

a »- > u z CO

a • UJ

H • Q • < a < o UJ

O o UJ < UJ < • Q < -) 1 < to o z Q -J LL K

01

421
**• * • • ro If) * • * ro O • • • o ! m i 1 1 1 i 1 i i o O • ro ro o O CM CM • o CM CM CM

[VO • 0 o u

J c • • CM CM • • ? ' ' CM CM O o o ~* • • • CM r i ft] O ro i CM CM CM i .i CM CM CM CM CM CM CM • CM CM o • ^

CM 5 * ri * i =J • r* • UJ

to t c l e • c • 0 o N • • < • I e CO LO (0 If) <r O o CD ro 0 • in • CD. o O o O O CM CM CM CM ro O • O n • cm CM CM CVJ CM CM CM CM CM CM CM CM CM • CM • o CM • LU * ^ • LL • UJ • a • 0 • 4 • » • a « • • • t m • . • I t CVJ o go OJ 0» o in • • • *

(Y 5 r1 j? o CM i-t • ro LO o (VI • Li ° • cm CM CM CM iM CM CM CM CM • CM *° CM * 0 0 * * ° * • * t> LO • • * LL o IJ) CO CO • CO

D CM o CM CM CM • to o CM h 0 CM CM OJ CM CM rM CM CM CM CM CM CM CM • CM ° CM zu * • LU w * * * 0 * • * o ro CP ao %0 (> 00 ro N • CP o o o 1 1 1 • ro © • CM CM CM rM CM CM CM CM CM CM CM * * 0 * * 0 * * CM • • UJ J O o c> CO S • CT o O a> CO Q"> CD o O CO t * CO

UJ • —a - CM

LQ ° CD ** °0 CD 9 Z • * * • • • © * • • CM CM • • ° ^!

rn rn • N * © CJ» r\ 0* ex • CP o

r- • 0 c—.

C\J CM CM CM CM • (\j (J «e6* ^

Zl • Q CM • 1- o C\| CM o o Uj O ro O o J, O t • • o v0

UJ • 10 • U • CO 00 a> CO CO CO 00 CO CD CO

O CO • to CO J. CD • LO * • <

4: • CD

,£- Lu * CD ro CM • a 03 ro CM LO CJ* 0> ro o LO N Ln • • • CM

UJ • CD " I OJ rx) CO CO CO CO CO o CDO 0' COO

<f) • ^ CJ • CO Z 0 M wz •••9- * 3 © • 1 * * * 0 * 9 1 * * ro CD * < * • < o ro LO CM o o o LP CO CM • * CM O & o o O e> o o o o O O o 0* • LO o

i-i o r\j CM CM CM CM CM CM CM f\J -4 • © CM X 9 CM Q

LJ

U)Q t o O o o o o o o O O O > • UJ CO CO CO CO CO CO CO CO CO CD CO CO CO • Z LU z X

U) < Q <

LU • < a > z _!u

a > U z CO LU 9 2 • Q • < 0. < UJ U o UJ < LU < • o o s < -> -> < i/) o z a IL s • K

cn

422
• • * p. i * • o '0 10 • t a • in < 1 1 i • 1 .1 m m • ro r # • CM CM CM • In "J v OJ z s« ••> *# o:o • ) * • • # t _ • & vO CO CO 0> CO CO ro Ov LO • m ro < • in • 10 if: 10 10 in in If) 0

CVJ Oj cm CM CM CM CM s CM OJ CM (M CM • CM

a • ¥ CM

CD • U < © D • t- • W • LU • in • • • t • • t • • O LO * 2 • X • vO 10 in tO CO vO ao CO <o rj CM • aj ro

ID in LO (0 u" 10

m «r LO »0 10 • vO rn '-'j CVi CVJ CM CM CM CM CM OJ CM CM CM CM • 10 CM CM • Q CM • LU • Z• H• LL • LU • Lf. • • z • i> • • • • • a • • CO • 9 • | o CO CM CO t 00 • LU • 'U vD l 0 10 to vO vjj iQ <y vQ to * o LO vfj * CM CM CM CVJ OJ CM CM 04 CM OJ CM OJ CM • vO OJ CM •

CM # * Q • Li. • CO 4- 10 ro yD ro O 10 o ro m • ao *0 (0 10 • ro 0 • oj CVJ CVI oi <\J CM EM OJ OI w CM OJ CM •

IS

CM CM s > s O » Z

LU

B I- • LU t • 0 0 # # °j t

l/> # • N vO CO CO CO lO LO qn M • tn in in lo 10 jv 10 ) i N LO

LO • CM CVJ CM 10 °J !, 2 to OJ U Q • U • •« M ¥ U • u B Q t LL • • # 0 _

if) vO ( 1- 01 • LU • H • CVJ o ro <t o rvj ro <\! N 0 • O o

co o • QC • in if) in 10 10 LO if> LO LO LO 10 10 • ro CM in -0 Ui • OJ CM CM CM CM CvJ CM * m CM CM

1/) OJ <

CD •

Q. #

(/) CD # z > t B 9 00 o 9 X • o o o vO o . o CD o «-) • vO <f V- • O • 10 in LO ^> in if) m <j to LO 10 • OJ LO 1- • CVJ OJ oj CM OJ OJ OJ OJ CM CM OJ CM * CM OJ

(/)

Q OJ < Q< • ¥ • <J J • O • • • ® • 0 • « 0 0 • • • hN 0 • • H • a* CO CO o o O ro o • 0 • s ro o • to • u • 4- to 10 in <? 10 (0 tn 10 • 10 • IU • CVJ OJ CM CM OJ OJ CM OJ CM OJ CM CM CM • CM ^J • if) CM # • < a • CO

LLI • z

1- t w • KD • • 9 • • u • • 0 • 0 • • LO • - • CL oj ro OJ ro CM ro • • LU • ao J! * 1 10 10 in m in m m to 10 LO LO 10 * CM LO in W • > CVJ CM OJ Oj OJ OJ OJ CM * LO CM OJ Z OJ (jzo _ o 0 « # # 0 4) • • B s < • < t o CO *0 vO ro ro r> CM • m • ro CM Q • <f in ^I <t <f 10 • N OJ LO • • CVJ CVJ CM CM CM CM OJ CM CM CM CM OJ OJ • CM OJ CM ou

LO • o # o o O O O O o O O o > • LU • CO CO 00 CO CO CO CO CO CO CO CO CO CO • Z LU Z X

to < a <

LU • < • a:

a > z -J o a > (J z CD rx • LU

K • < a < o LU

U o LU < LU < • Q < ) < (f) a z a -> LL CO

423
DSC INDUCTION TIME

424
DSC ONSET TEMPERATURE

U

u

w

X

a

w

240

230

220

210

425
DSC ONSET TEMPERATURE WITH ADDITIVE

265

260-

o

H

m

255

250 -J

245

240

426

.A
DSC INDUCTION TIME

53

MONTH

427
DSC ONSET TEMPERATURE

428
DSC ONSET TEMPERATURE WITH ADDITIVE
• t 40 <3" 1 | 1 | I 1 ) s o | • o 4 10 j • to <}• LO >ao # • > © 0 • e 0 c • • 0 .j • * LO o t o OJ ro OJ 4' OJ CD CO o (J* OJ CO

ro OJ OJ CM OJ ro ro OJ ro ro ro CM

a • 10 ro Q • ^

CO • W < • O j * H • (0 • UJ t CO o o c 0 • • • o • • • • < i X 9 O ^0 10 ro o 10 03 < • • 10 • CD OJ CVJ m OJ CM CM CM 04 CM CM OJ 04 • ro

CM • a • UJ • z • t=* • u_ • UJ • a 0 0 • • • 9 t 0 • • ro • • • t • u o ro o o ro 10 to O o CM 1 • • 10 o • LU CM ro CM <f rO to ro ro CM 1 • ro ~* LO • II ,1

ro > «_ . _ . .., B 0 o ft 0 0 OJ Q • LL O GO o CO o H o ro | • o m ^> ro OJ <f CM } « jt ro LO _ OJ

I/)

>-u if) 0 z u

LU h- h • UJ • • 0 • 0 0 0 0 0 CO 10 #

(/) LO rO CD LD ro o <_) 1 1 | o *

OJ ro LO ro ro ft. 10

[/) OJ 2U < u a • •* ^ X uu u. o « o • 9 0 _ 0 B f t #

i— _J • UJ • o o LO OJ C\J OJ

O • Q

to < • a • ro <j- ro ro ro <t ro * o ro 10

LU

COa •

«t UJ

03x •# to a

ID |=Z 0 e 9 0 o _ 9 m CO _ o O <f t\j OJ CO If) 10 • OJ s u • Q o CM CM ro OJ OJ OJ OJ OJ CM ro OJ • 10 s h • OJ a • < LU * • u h • o , 0 • • • • • a • 0 • • • • • o 10 • • • f- in LD L> C7i CO CO o N co • • • 10 • (0 • <J ® ro OJ ro OJ ro OJ ro ro ro • OJ • LU ro a • (0

LU • < Q • CD X • z < • o 3 g 0 CO

II • CC o 1 0* OJ ro. \£, CO CO * * _ 1 o • CD m OJ ro OJ OJ ro Al to rn

if) z<Ju

ii 0 « ( 0 0 « 0 - # CO « < o OJ 10 CO 10 CO OJ OJ N o • CO CM o ro OJ OJ OJ ro ro ro ro ro ro ro • - rO

i—

ED

^> • • 0 eo J o o O o o o o o o o o > H • UJ • OJ 00 00 00 CO CO CO GO CO CO CO CD CO • Z IJJ z

l0 < Q <

LU • < * cr tx. > z J e>

a

H > (J z CD CL • UJ • £ h • Q • < CL < D LU U a UJ < LU < • • £ < -5! "> < CO o z a LL h

430
LUBTOT

H

<

O

w

o

o

50

40

30-

20

10

0 2

B

4

D

G

E

OIL

8

C E

10 12

431
LUBTOT

0 2 4 6 8 10 12 14

MONTH

432
o

i-<

> a

Q m

O X

I- o

10> . o to Z GO UJ <

I10 CVJ w O

H 10

10 a m x

(0 w

<

CD UJ

10

• o o o o o o o o o o

•>

• 00 CO CO CO CO CO CO CO CO 00 00 CO CO • Z UJ z

(0 • < a <

lit • • < i a DC >- z _l o a t- > u z CD 0L. I UJ • z

1- • • Q • < a < D D UJ u o UJ < UJ < • s: a

< "» 1 < (0 o z Q -> U. ST

10 ~

o —

t • 10 *

CO —

0> tN If)

If) -

• •

If) >0

<o eg

CM —

- CO

• •

433
w

LUKa > < Q Q D « H X

10

O > —

<J • z w

ai or H I

ini- o

i/i

— z s O OJ u o * i/) u a. o LU h t-

</>

H

LU -I 10 w <

1/1 in z m o z a s m s iu

i- a. W< w> o O o o O o o o o o o

1- • • LU CD co co CO CO co CO CO oo co CO CO CO CO • • 1- w • • < » a a > Z CQ _l 15 a t- > u z a

t- • • a o < a 3 3 3 LUU o UJ < LU < o S < 1 -> < 10 z Q IL • • to

«* -I o ro - 0*

in

—

ro \0 • • roz x H <

434
OXYGEN UPTAKE TEST

9—

r

435
OXYGEN UPTAKE TEST

m

w

H

436
OXYGEN UPTAKE TEST

MONTH

437
438
• O in *

LT>

O « |{) i i 11 • 1 in 7| * CM Lf) * * * • • • 0* * 1 0>

QO • "> • O in

Q o o o in in in Lf 1 in * _ . 1 o ^ * | ® in L0 in C\J C\J CM • <j o

J. • * * * * * * 00 <j\ LP o 0* <£} CD CT' — °» * '0 o O *

?*» CO *• u

_j • CO • LU • 00 o L0

m o in in

O o O to

m o in • CM o tn f < • I • in N N in CM CM o in o CM o CM • 10 o • CD s • t * • 0 • • • CM <t • o O o o» O o CO 0* CO 0» a» • • CO a> • Q • LU • LL • LU • a • o o o o o o in in o o m o o • O o o • 1 • L5 • o in in in in in o o o in • U) o in • LU • • • • • • • • 0 • • • o in • • • CL • o o> CO a") CO ao o> • CO o n> • • o in o s

LO lO o in o in • 'C? 0> o in * * ^ u^ o CM • m CO in 0 • • 00 CO » aj CT1 _ • LU LO 10 m * o LO

r\i CM in * LP 1 0 e jj * n\ _

0' G'< 0 0* v0 . 19

_

**

to

to • < •

U") ' O ! lO • UJ * m Q O • n\

]£ • £1 * • o 0 * * * cj» o o CO CO CO CO CP 0 Z * » 10 o o o C tn in o o L0 o o in • o o U • • N in o in o o o CM o LO CM o o LO i D * * ° * -5 * * * m CO * O * •' m ** CO _ • * * 0s * CO

III * , <^ • ^

CO • O • O in inO

O o o U) o in in

O uo • o yo o Ln • h= i O r*- h- L0 in in o C\J tn L0 CM • o CM LO N • CO o U » • 0 • t • • • CM 0 • UJ n> 0* CO 00 o> • CO O 1 *

!i* Q\ * w • 5CD • _ *

tn 6 in

jf* L0 ~?

_

m ID L0 10 uo • CO

Q LO < *• nrLL ' m ° 1 in _ m r^ m

-J * • UJ • 0 • • r — o CO CO o CD (J, o> • 0 CO Z • O * CO **•* J in 10 in o —

tn

_

10 10

_

in • CO LO • • < in w o o o N o CM • CO o a N

LU • • • • • • • • • • • o (0 o (7* o o GO CO CO CO CO o > CO Q> Z CO

LUu

LU •

00 • O o O o O o o O o o > H » LU » CO 00 CD CO CO CO CO CO CO CO CO CO • z LU z X

co < a <

LU • < • a

a > z -1 10

a > u z CD UJ • K • Q • < a < D D UJ U o LU < LU < • Q < -) -> < 00 Q z Q li. H

co

439
SEQ HI SIMULATOR

440
SEQ m SIMULATOR

MONTH

441
L
Appendix I

Sample Numbering System

and

Data Table for Repeated Samp!

A-1
APPENDIX I

The sampling number system appears in the Table AI-1 below. All sample numbers are preceded by

a two letter code BC for identification purposes. Oils A - D and Oil I are virgin base oils. Oils

E - H, J and K are re-refined base oils. Each sample number is a separate sample. The laboratories

performing the analyses were at liberty to run multiple analyses per sample and report the average

value or all values. The data presented in the body of this publication together with the appendices

comprise all the test information received from the analytical laboratories.

Duplicate samples (BC7169, BC7174) were sent for analyses for Oil I, March 80. Triplicate samples

(BC7248, BC7423, and BC7426) were sent for analyses for Oil F, June 80. Samples BC7423 and BC7426 were

sent for analyses approximately eight months after sample BC7248.

In the body of the publication the values listed for Oil I, March 80 and Oil F, June 80 are the

average values for the replicate samples. In order for a complete data analysis the value for these

five oil samples are listed in Table AI-2 below. They are grouped according to the major divisions

listed in the Table of Contents.

TABLE AI-1

ASTM/NBS BASESTOCK CONSISTENCY STUDY

SAMPLE NUMBERING SYSTEM

VIRGIN BASE OILS REF RE-REFINED BASE OILS

DATE/OIL A B C D I E F G H J MAR 80 7168 7170 7171 7174 7187 7186 7172 7173 7233 APR 80 7199 7202 7201 7198 7200 7204 7203 7205 7197 7240

MAY 80 7230 7231 7232 7229 7228 7227 7234 7235 7226 7246 JUN 80 7242 7243 7236 7241 7238 7237 7248 7244 7239 7251

JUL 80 7255 7256 7249 7257 7252 7254 7250 7258 7253 7272

AUG 80 7263 7265 7267 7269 7266 7262 7270 7271 7268 7264

SEP 80 7290 7293 7284 7285 7287 7288 7292 7289 7286 7346

OCT 80 7343 7337 7340 7341 7345 7342 7339 7338 7344 7373

NOV 80 7348 7354 7349 7350 7351 7347 7385 7352 7353 7380

DEC 80 7375 7378 7379 7377 7372 7376 7388 7374 7371 7384

JAN 81 7387 7381 7383 7382 7390 7397 7386 7389 7405

FEB 81 7404 7403 7400 7402 7399 7421 7401 7398 7414

MAR 81 7417 7419 7420 7422 7415 7424 7425 7418 7416

K 7245

7413

7427

NOTE: SAMPLE NUMBER BC7169 WAS A DUPLICATE SAMPLE FOR OIL I (MAR 80)

SAMPLE NUMBER BC7423 WAS A TRIPLICATE SAMPLE FOR OIL F (JUN 80)

SAMPLE NUMBER BC7426 WAS A TRIPLICATE SAMPLE FOR OIL F (JUN 80)

FOR CASES IN WHICH DUPLICATE OR TRIPLICATE SAMPLES OCCURRED AN AVERAGE VALUE WAS RECORDED

Table AI-2

II. RHE0L0GY

Test

Brookfield Viscosity (cP) 0°F

-20°F

-40°F

Cold Cranking Simulator (cP) 0°C

- 5°C

-10°C

-15°C

-18°C

-20°C

-25°C

-30°C

-35°C

-40°C

^b BC7169

0 3030

23500

SOLID

P 410

640

1030

1830

2680

3550

7430

16900

S

S

BC7174

3080

28200

SOLID

405

625

1000

1800

2660

3550

7550

16800

S

S

BC7248

5160

28350

650000

610

930

1500

2550

4300

5600

11900

S

S

s

BC7423

4750

29100

543000

690

1040

1620

2720

4500

5800

12100

S

S

s

BC7426

4650

29100

632000

560

850

1340

2300

3850

5100

11000

S

S

S

A-2
Test 1 Ah RP71 fi9 RT71 74 Rr7?aft D u / c to RT74?'3 RC74?fi

Tr-it-iral Startinn Tpmn (°C} p - ?n . o3 _ on a _ i c c

J.D . D

- 1 fi 1 -17 4

Kinematic Viscosity (cSt) 40°C L 38.93 38.87 57.74 57.44 57.36

100°C 6.10 6.10 8.31 8.31 8.31

40°C P 66.67 38.86 57.45 57.38 57.58

lJ-KJKJ nn°rU fiD . inJ.U p; nft ftO. JU^n ft "311 ft ^i

Viscosity Index (units) L 101 101 114 115 115

P 0 101 114 115 115

Mini-Rotary Viscosity (°F) P +4. OA +1.7A -21. 6F -20. 6F -20. 2F

III. PHYSICAL PROPERTIES

Toct 1 co L Ldu RT71 fiQ RT71 DU / J. 74/ *T DU / £t-o RT74?^ DU

/

H£

o

RT7d?fi

nri APT ul dv 1 tvLy f °APT V. " ' 1 J

)L 9Q Q 9Q Q ?Q 7 ?q 7 M CJ?9 ft . o ?Q ft

Rni 1 i nn Danno c t yi hi it i on ( ® P

"\ DU 1 I lily r\aliyc UlbU 1UUL1UH ^ \j J U . J 1L jjj ODO ?7fl ?71 ?70

X OJJ oT7fi / o ?Q? ?9?

D }ftft ^Qft JJU JJO 3Rft

1 Cl 4i n JO^ft"}J JOT 3ft4 JO3ft7/ 41 ft 497 di n HJ.U 41 ? 30 431 439 428 428 431

40 442 451 445 443 447

50 453 461 462 458 463

60 463 471 477 473 480

70 474 482 497 491 500

80 486 494 521 515 528

502 511 560 555 575

95 517 528 575 575 575

Cloud Point (°F) M 22 20 20 18 18

Pour Point (°C) L -7 -9 -30 -21 -21

Color (ASTM Color Units) L 2.5 2.5 4.5 5.0 5.0

M 2.0 2.5 4.5 4.5 4.5

Fire Point (°F) L 500 495 500 500 490

Flash Point (°F) L 465 475 460 465 450

20 Refractive Index (N

n

) N 1,4837 1.4837 1.4840 1.4840 1.4841

A-3
IV. CHEMICAL PROPERTIES

Test Lab BC7169 BC7174 BC7248 BC7423 BC7426

Carbon Residue L 0.05 0.10 0.21 0.24 0.23

Sulfated Ash L 0.00 0.00 0.13 0.13 0.13

Total Metals R 5 3 276 344 335

Saponification Number L 0. 16 0. 17 0. 55 0.92 0. 92

Total Acid Number L 0.01 0.01 0.18 0.18 0.18

IR Spectrometry 5 8 W 0 0 0. 96 0 0

6 2 0 0 1.42 2.15 2.0

8 15 0 0 0 0.3 0.2

10 3 0 0 0 0 0 DIR Spectrometry 5 8 1.72 0.5

6 23 0 0

Test Lab BC7169 BC7174 BC7248 BC7423 BC7426

Elemental Analysis

1. Atomic Emission Ca R 1 1 74 165 163

FePb -- -- — -- Mg

P <50 <50 100 57 65

SiNa 1 1 1 1 Sn 2 Zn 1 1 102 120 105

2. Chemiluminescence N L 29.00 29.00 27.00 21.00 19.00

3. Neutron Br N <. 07 <. 07 0. 93 0. 84 0. 90

Activation CI .42 .48 9.2 9.0 9.2 Na .98 1.03 0.9 0.82 0.84

K <1 <1 1 <1 <1

4. Oxygen Analysis 0 0. 18 0. 23 0. 19

5. X-ray S L 0.66 0.66 0.20 0.19 0.19

Fl uorescence CI <0.01 <0.01 <0.01 <0.01 <0.01

Molecular Analysis

1. Ethylene Glycol S <1 <1 <1

2. Water N 71 63 288 301 298

A-4
.1

V. HYDROCARBON TYPE ANALYSIS

Test Lab BC7169 BC7174 RP7?4fi D\> / ^ C O RT74?fi

Liquid Chromatography

1. Clay-Silica (ASTM D2007) Sat M 73. 0 7? ? Aro

Pol

2. Alumina-Silica (ASTM D2549) Aro V 26.3 28.5 20.1 20.9 20.5

Sat 73. 7 71 5 79 9 7Q 1 79 ^ Recovery 98.0 95.9 95.0 96.4 97.3

TLC/FID SAT HC U 80.0 82.8 84.6 84.6 83.5

ARO HC 17.8 16.2 13.5 14.3 15.0 POL CMPD 2. 2 0. 9

i i Hiahlv i i i y 1 1 i v POL i w l. CMPD win u Nn n i nuwn Nn

DMSO EXTRACT u 0. 99 1. 19 1.85 2.27

0.96 1.22 1.91 2.28

RI 1. 5625 1. 6109 1 5R47 1 ^790

MS Benzothiophenes V D D — —

Di- D fC H„ S^ ^ n 2n-12 D; Q ND

NMR L/T HC V 19 21 16.4 18.1 19.4

Isoprenoid ratio 0.8 0.7 1.14 1.01 0.98

PIB ND ND ~0.3 ND

UV Aromaticity mono- ring L 4.0 4.1 3.1 1.6 1.6

di-ring 1.6 1.7 1.7 0.9 0.9

tri-ring 0.3 0.3 0.3 0.1 0.1

VI. GENERAL PERFORMANCE TESTS

Test Lab BC7169 BC7174 BC7248 BC7423 BC7426

nomiilcnhil"i'f"\/ ucinu T i iho T i b i u i i i i uuc ± H O W >fiO FM >60 >60 >60 >60 >60

RK >fifl >60

Tube 2 H 2 0 >60 >60 >60 >60 >60

EM >60 >60 >60 >60 >60

BK >60 >60 >60 >60 >60

Tube 3 H 2 0 7 >60 >60 >60 >60

EM >60 >60 >60 >60 >60

BK >60 >60 >60 >60 >60

Tube 4 H 2 0 >60 8 >60 >60 >60

EM >60 11 >60 >60 >60 BK >60 >60 >60 >60 >60

A-5
Test Lab BC7169 BC7174 BC7248 BC7423 BC7426

Filterability Run 1 mg W 8.0 16.1 1.9 NF Time(s) 109.7 128.1 180.6 >1800 --

Run 2 mg 19.5 7.5 2.1 NF Time(s) 107.7 124.7 176.6 >1800

Run 3 mg 6.8 3. 5 1. 9 NF Time(s) 112.2 124.4 182.3 >1800

Foaming Seg I X 330-0 330-0 20-0 0-0 20-0

Tendency II 10-0 0-0 10-0 50-0 40-0

III 320-0 30-0 20-0 90-0 50-0

Rust A X L H M N N

B H H H H L

Sediment M 0.000 0.000 0.000 0.001 0.001

CD/SE Additive Compatibility WKl.RT X c C c C C 150°F c C/T c C/T C 32°F c C c C c 0°F c C/T c SZ SZ WK4.RT c C C/T C/T C/T

150°F C/T C/T C/T C/T C/T

32°F C/T C C C C/T

0°F r/T r/T r/T r r

VII. OXIDATION AND ADDITIVE RESPONSE TESTS

Test Lab BC7169 BC7174 BC7248 BC7423 BC7426

Antioxidant Capacity N 0. 003 0. 004 0. 004 0. 001 0. 001

DSC Induction Time N <1 <1 <1

Onset Temp. 192 192 221 220 219

DSC + Add Induction Time 24 24 34 32 30 Onset Temp. 251 252 255 256 255

Lubtot L 31 32 19 -- --

Oxygen Uptake Time 1L Oxy Z 6.0 5.8

Total Oxy 5.1 5.9 -- -- --

RBOT Run 1 M 141 143

Run 2 142 142

Seq. Ill Sim 0 9.25 9.00 9.25 9.50 9.50

TOST M 538 685

Load Wear Index Z 29.9 29.4
Appendix II

Test Methods and Summaries

A-7
APPENDIX II

The test methods used in this study are listed below grouped by major divisions corresponding to the

table of contents. When the test method is not readily available or when additional information is necessary for understanding the data presented, the method and/or summary is attached at the end of Appendi:

II as noted. An asterisk (*) denotes that the method is available on approval from the Chairman of the

appropriate ASTM Committee D2-RDD Division.

Test Method

II. RHEOLOGY

Brookfield Viscosity at

0, -20, -40 °F (cP)

Cold Cranking Simulator at

0, -5, -10, -15, -18, -20, -25,

-30, -35, -40 °C (cP)

Critical Starting Temperature

at 3500 cP (°C)

Kinematic Viscosity at

40, 100 °C (cSt)

Viscosity Index

Mini-Rotary Viscometer

BPT (°F)

III. PHYSICAL PROPERTIES

API Gravity (°API)

Boiling Range Distribution by GC,

0.5, 1, 5, 10, 20, 30, 40, 50,

60, 70, 80, 90, 95 °C and wt%

greater than 575 °C

Cloud Point (°C)

Pour Point (°C)

Color (ASTM Color)

Fire Point (°F)

Flash Point (°F)

Odor Comparisons to 100 Pale and

to 100 Neutral

20 Refractive Index (n^ )

ASTM D2983

Low-Temperature Viscosity of Automotive Fluid Lubricants

Measured by Brookfield Viscometer

^Modified ASTM D2602

1980 ASTM Proposed Test Method for Apparent Viscosity of

Motor Oils Between -40 °C and 0 °C Using the Cold Cranking

Simulator (and using scanning mode)

Calculated from Cold Cranking Simulator data using a regression fit based on the Walther Equation

ASTM D445 Test for Kinematic Viscosity of Transparent and Opaque

Liquids (and the Calculation of Dynamic Viscosity)

ASTM D2270

Calculating Viscosity Index from Kinematic Viscosity

ASTM D3829

Predicting the Borderline Pumping Temperature of Engine Oil

Summary explanation attached

ASTM D287 (or ASTM D1298) Test for API Gravity of Crude Petroleum and Petroleum

Products (Hydrometer Method)

*Modified ASTM D2887 Test for Boiling Range Distribution of Petroleum Fractions

by Gas Chromatography

Modified for determination of higher boiling components

and data processing

ASTM D2500 Test for Cloud Point of Petroleum Oils

ASTM D97 Test for Pour Point of Petroleum Oils

ASTM D1500 Test for ASTM Color of Petroleum Products (ASTM Color Scale)

ASTM D92 Test for Flash and Fire Points by Cleveland Open Cup

ASTM D92 Test for Flash and Fire Points by Cleveland Open Cup

Proprietary Test

ASTM D1218

Test for Refractive Index and Refractive Dispersion of

Hydrocarbon Liquids

A--8
Test Method

IV. CHEMICAL PROPERTIES

Carbon Residue (wt%)

Sulfated Ash (wt%)

Total Metals (ppm)

ASTM D524

Test for Ramsbottom Carbon Residue of Petroleum Products

ASTM D874 Test for Sulfated Ash from Lubricating Oils and Additives

Atomic Emission Spectrometry

Summary and Method Attached

Saponification Number (mg KOH/g)

Total Acid Number (mg KOH/g)

Elemental Analysis

1. Atomic Emission for Ca, Fe, Pb,

Mg, P, Si, Na, Sn, Zn (Ag, Cu,

Al , Ba, Ni , Cr, B, V, Mo, Cd,

Ti) (ppm)

2. Chemi luminescence (N) (ppm)

ASTM D94 Test for Saponification Number by Color-Indicator

Titration

ASTM D664 Test for Neutralization Number by Potentiometric Titration

Atomic Emission Spectrometry

Summary and Method Attached

*ASTM Proposed Test Method for Organically Bound Trace Nitrogen in Liquid Petroleum Hydrocarbons by Oxidative

Combustion and Chemi 1 umi nescence Detection

3. Neutron Activation for Br, CI,

Na, K (ppm)

4. Oxygen (ppm)

5. X-ray Fluorescence for S(C1) (wt%)

Molecular Analysis

1. Ethylene Glycol (ppm)

2. Water (Moisture) (ppm)

Infrared Spectrometry (absorbance)

Neutron Activation Analysis

Summary and Method Attached

Modified UOP 649-74

Total Oxygen in Organic Materials by Pyrolysis-Gas

Chromatographic Technique

Summary Attached

Modified ASTM D2622

Test for Sulfur in Petroleum Products (X-Ray Spectrograph!' c Method) Modified to use energy dispersive instead

of wavelength dispersive XRF. CI procedure similar to

S, but with 100 ppm limit of detection.

*ASTM Proposed Test Method for Trace Ethylene Glycol in Used Engine Oil

Modified ASTM D1744

Water in Liquid Petroleum Products by Karl Fischer Reagent

Modification described in Proceedings of the Conference on Measurements and Standards of Recycled Oil -IV, to be published

1983.

Infrared Spectrometry

Method Attached

A-9
Test Method

V. HYDROCARBON TYPE ANALYSIS

Liquid Chromatography

1. Clay-silica (ASTM D2007) for

saturates, aromatics and

polars (wt%)

2. Alumina- silica (ASTM D2549) for

saturates, and aromatics (wt%)

Liquid Chromatography/Mass

Spectrometry for saturates, mono- aromatics, diaromatics, polyaromatics (wt%)

Thin Layer Chromatography/Flame

Ionization Detection for saturate,

aromatic, polar and highly polar

compounds (wt%)

DMSO Extraction/Refractive Index for

polycyclic aromatic content (wt%)

Mass Spectrometry for Sulfur

compounds (ppm)

Nuclear Magnetic Resonance

Spectrometry for isprenoid and

linear/total hydrocarbon ratio

and PIB units (ppm)

Ultraviolet Spectrometry for Monodi-, and tri-aromatics (%)

VI. GENERAL PERFORMANCE TESTS

Demulsibility

Filterability

Foaming Tendency

High Temperature Copper Corrosion

CD/SE Additive Compatibility

Rust

ASTM D2007 Test for Characteristics Groups in Rubber Extender and

Processing Oils by the Clay-Gel Adsorption Chromatographic

Method

ASTM D2549 Test for Separation of Representative Aromatics and

Nonaromatics Fractions of High Boiling Oils by Elution

Chromatography

HPLC/MS Method: "Preparative Liquid Chromatography for

Fractionation of Petroleum and Synthetic Crude Oils," James W. Vogh and Jane S. Thomson, Anal . Chem . , 1981 , 53, 1345-1350.

TLC/FID: Thin Layer Chromatography with Flame Ionization

Detector

Summary of Method Attached

IP346

Polyclic Aromatics in Petroleum Fractions by Dimethyl

Sulphoxide-Ref racti ve Index Method

High Resolution Mass Spectrometry

Summary of Method and Results Attached

13 C Nuclear Magnetic Resonance Spectrometry

Summary of Method Attached

Determination of Aromaticity of Fuels and Lubricants by

Ultraviolet Spectroscopy, Interim Report AFLRL 103 Feb 1980

(Defense Documentation Center #ADA0 86654)

Summary of Method Attached

ASTM D1401 Test for Emulsion Characteristics of Petroleum Oils and

Synthetic Fluids

1) Sediment and Filterability of Industrial Oils

Method Attached

2) Proprietary Method

ASTM D892 Test for Foaming Characteristics of Lubricating Oils

Proprietary Method

Proprietary test, Storage at 70-80 °F of oil treated with

a typical SE/CD additive.

ASTM D665 Test for Rust-Preventing Characteristics of SteamTurbine Oil in the Presence of Water

A- 10
Test Method

Sediment

Storage Stability

Ambient, Cold and Sunlight Storage

ASTM D2273 Test for Trace Sediment in Lubricating Oils

Storage Stability

Summary of Method Attached

VII. OXIDATION AND ADDITIVE COMPATIBILITY

Antioxidant Capacity (mol-L)

Differential Scanning Calorimetry

Load Wear Index

Lubricant Thermal Oxidation Test

(LUBTOT)

Oxygen Uptake

Rotary Bomb Oxidation Test (RBOT)

Sequence III Simulator

Turbine Oil Oxidation Stability Test

(TOST)

Free Radical Titration Test: Ind. Eng. Chem. Prod. Res. Div. 17, 250(1978)

Summary and Method Attached

Differential Scanning Calorimetry

Summary of Method Attached

ASTM D2783

Measurement of Extreme-Pressure Properties of Lubricating

Fluids (Four-Ball Method)

To evaluate EP properties, oils containing a package which

satisfies the U.S. Steel 224 Specification. Load wear

index results are considered suspect if they differ by more than 5 kg.

Lubricant Thermal Oxidation Test

Summary Attached

Oxidator Test Summary of Method Attached

ASTM D2272 Test for Oxidation Stability of Steam-Turbine Oil by

Rotating Bomb

Proprietary test, scale 0-10 (10 = clean; >6.6 = Passing,

a form of hot tube test at elevated temperatures.

ASTM D943 Test for Oxidation Characteristics of Inhibited Mineral Oil

A-n
SUMMARY EXPLANATION OF MINI- ROTARY VISCOMETER ASTM D3829 METHOD

Border line pumping temperature (BPT) reported in °F also reports whether the oil exhibited

air-binding (A) or flow-limited (F) failure mode. In some cases the air-binding BPT and the

viscosity (flow-limited) BPT were within 0.5 °F. This is indicated in the data by #sign and the BPTs were averaged. All air-binding failure mode cases correspond to a yield stress of 105 Pa for the 30 g mass. All flow-limited failure mode cases were interpolated at an apparent viscosity of 30 Pa-s.

DESCRIPTION OF INFRARED ABSORPTION METHOD

FOR ANALYSIS OF USED ENGINE OILS

1. INTRODUCTION

1.1 This revision limits the application to oils of known additive composition or behavior to avoid errors in interpretation of test results. It also modifies the recommendations for adsorption

cell window materials and eliminates certain details that were incorporated in the original method in an attempt to make it applicable to marine diesel oils. For the latter products a new method is now available entitled "Infrared Analysis of Used Marine Diesel Lubricants." Numerous editorial changes

have also been made to help clarify the method.

2. SCOPE

2.1 This method is used to examine used lubricating oils from gasoline, natural gas, and diesel

engines (other than marine) by infrared absorption spectroscopy. The method indicates the degree of

oxidation and the relative amounts of olefins, nitrates, and nitro compounds. Water may often be

determined quantitatively and ethylene glycol is determined quantitatively.

2.2 In general, the method is limited to oils of known composition, containing only additives

which do not adsorb at wavelengths of interest (table 1) or additives whose absorption is known not to change significantly relative to the adsorption of the component being measured. Disregard of these

limitations may lead to uncertainty or errors in interpretation of test results. For example, the

depletion of an additive which adsorbs at 5.85 micrometers may balance the increase in absorbance

caused by oxidation of the oils and lead to the erroneous conclusion that little or no oxidation has

taken place. Similarly, in certain oils containing phenate additives, decomposition of the phenate

may yield a phenol absorption peak which will lead to an erroneously high water value.

3. OUTLINE OF METHOD

3.1 A differential spectrum of the used oils vs. a reference unused oil of the same type is

recorded between 2.5 and 15.0 micrometers. Oils which are opaque to infrared radiation are diluted

with a similar type of oil to obtain adequate transmittance. Absorbances are measured at specific

wavelengths and are related to components as shown in table 1. Water and gasoline fuel dilution are determined by reference to calibration curves.

4. APPARATUS

4.1 Infrared Spectrophotometer, dual beam. A Grubb Parsons G. S. 2A, a Perkin-Elmer Infracord

Model 137-B, or a Perkin-Elmer Grating Spectrophotometer Model 221 or 467 is suitable. Other

equivalent instruments also can be used.

4.1.1 Consult texts concerning general methodology of infrared absorption analysis for

discussions of apparatus, materials, and procedures.

4.1.2 The Infracord Model 137, with the slit width set at 25 and a slow scan speed, was

used in developing this method.

4.2 Absorption Cells, fixed thickness, 0.100 ± 0.005 mm pathlength (Note 1). Barium fluoride

and silver chloride windows are recommended for this method, but silver chloride may induce interference fringes with some oils. Sodium chloride and potassium chloride windows are acceptable for

samples which are nearly free of water; however, extended exposure to moisture will cause fogging

(Note 2). Irtran-2 windows are not recommended because the current composition of this material has

been found to yield intolerable interference fringes.

A^12
Table 1

Specific Infrared Absorption Bands and Used Oil Components

Band Wavelength

(micrometers)

2.90

6.05

5.85

6.10

6.10, 7.9, 11.6

6.4

12.40 & 12.80

9.30 & 9.70

Nature of Component

Water

Water

Oxidation Products

Olefins (a)

Organic Nitrates (b)

Nitro Compounds (b)

Gasol ine

Fuel Dilution (b)

Ethylene Glycol

Reported as Volume %

Absorbance/cm

Absorbance/cm

Absorbance/cm

Absorbance/cm

at each wavelength

Absorbance/cm

Volume %

Present or Absent

(a) Absorbance at 6.10 micrometers indicates olefins only when the 7.9 and 11.6 micrometer bands

(organic nitrates) are absent; if the 7.9 and 11.6 micrometer bands are present, olefins cannot

readily be determined with certainty.

(b) Not present in diesel oils.

Note 1 - Cell pathlengths between 0.095 and 0.105 mm are satisfactory, but the pair of cells

used for an analysis must not differ from each other by more than 0.002 mm. Use the thinner

cell for the reference oil.

Note 2 - Use extreme care in handling cells with halide windows. Do not subject barium

fluoride windows to mechanical or thermal shock. Do not touch sodium chloride or potassium

bromide windows with the fingers, and avoid exposing to the breath or other moist air; store these cells, while not in use, in a desiccator or in a tightly closed jar containing a desiccant. Store silver chloride cells in darkness.

4.3 Hypodermic Syringe, 1 mL.

5. MATERIALS

5.1 Reference Oils. Unused oils containing the proper concentrations of all the additives

contained in the formulations of the used oils to be analyzed.

6. PREPARATION OF CALIBRATION CURVES

6.1 Water Content.

6.1.1 Select a sample of used oil of the type to be analyzed which is shown by ASTM D95-IP

74 or an equivalent method to be free of water. Prepare standard blends of this oil containing 0.10,

0.20, 0.50, 1.0, 1.5, and 2.0 volume % water. Disperse the water in the oil by agitating with a high

speed mixer or a homogenizer-blender of the waring type.

Note 3 - Complete dispersion of the water in the oils is essential. Stable dispersions are obtained more readily with used oils than with unused oils.

6.1.2 With the spectrophotometer beams unobstructed, adjust the transmittance at 2.5

micrometers to 90% (0.05 absorbance). Fill the cell designated as "reference" with the oil used to make the water blends in Section 6.1.1 and the "sample" cell with one of the standard blends (Note 4).

Place each cell in the appropriate light path and scan the spectrum between 2.5 and 4.5 micrometers. Draw a straight baseline from the region of 2.5 micrometers to the region of 4.0 to 4.5 micrometers. Measure the net absorbance at 2.9 micrometers (peaked) and calculate the absorbance/cm for the

standard blend as follows:

A-13
where

a = absorbance/cm.

A = net absorbance at 2.9 micrometers, absorbance units,

b = length of cell path, cm.

Note 4 - Cells can be filled conveniently by dispensing oil droplets from the tip of a micro

spatula into the cell opening, and drawing the oil into the cell with mild suction. A syringe with a Luer-Lok type tip is also suitable. After filling, inspect the cell for the

presence of air pockets. If any are present, remove them with gentle suction or by

refilling with the sample.

6.1.3 Repeat Section 6.1.2 for all the prepared standard water blends. On linearcoordinate graph paper, plot the absorbance/cm values against the water contents of the blends and

draw a smooth line through the points.

6.2 Gasoline Fuel Dilution.

6.2.1 Accumulate a representative quantity of gasoline fuel diluent by running ASTM D322,

"Dilution of Gasoline-Engine Crankcase Oils," on at least 20 different samples of used oil and

compositing the distillates. Alternatively, distill one liter of a reference fuel and collect the

90-97% volume fraction. Blend the composite or the 90-97% distillate fraction into unused oil of the

type to be tested at the following concentrations: 1.5, 3.0, 6.0, 9.0 and 12.0% volume.

6.2.2 With the spectrophotometer beams unobstructed, adjust the transmittance at 2.5

micrometers to 90% (0.05 absorbance). Fill the "reference" cell with the unused oil, and the "sample"

cell with a fuel diluent oil blend (Note 4, Section 6.1.2), and record the spectrum between 11.0 and

15 micrometers. Repeat the scan with each blend.

6.2.3 Draw baselines between 11.2 and 14.1 micrometers on each scan and measure the net values at 12.4 and 12.8 micrometers (Note 5). Add the two values for each blend, convert the sum to absorbance/cm, and plot the values vs. concentrations by volume on linear-coordinate paper. Draw a smooth line through the points.

Note 5 - The fuel dilution is based on the measurement of aromatic bands commonly found in gasoline. Other bands indicative of fuel dilution occur at 11.8, 13.05, 13.55, and 14.4

micrometers. If experience shows that better correlation is obtained by using one or more

of these bands in addition to those at 12.4 and 12.8, the procedure may be extended to include them.

7. PREPARATION OF SAMPLE

7.1 Agitate the sample in the original container until all sediment is homogeneously suspended

in the oil (Note 6). If the original container is of opaque material, or if it is more than threefourths full, transfer the entire sample to a clear glass bottle having a capacity at least one-third

greater than the volume of the sample. Transfer all traces of sediment from the original container to the bottle by violent agitation of portions of the sample in the original container.

Note 6 - As used oil may change appreciably in storage, test the samples as soon as possible

after receipt.

7.2 Some used oils contain sufficient soot, etc. to render them opaque to infrared radiation.

If the maximum transmittance at 2.5 micrometers is below 30% (0.5 absorbance), dilute the used oil to

a known volume with unused oil having the same formulation. To avoid excessive loss of sensitivity,

do not dilute beyond 1:2. Multiply the results obtained by the appropriate dilution factor.

8. PROCEDURE

8.1 Gasoline Engine Oils. Fill the "sample" cell and the "reference" cell with the sample and

the corresponding reference oil, respectively (Note 4, Section 6.1.2). With the spectrophotometer

beams unobstructed, adjust the transmittance to 90% (0.05 absorbance) at 2.5 micrometers wavelength.

Place the cells in the spectrophotometer and record the spectrum between 2.5 and 15 micrometers.

Measure the net absorbance for the water peak as described in Section 6.1.2, and for the fuel dilution

A-14
peaks as described in Section 6.2.3. Measure the net absorbances for peaks at 5.85, 6.05, and 6.1

micrometers, based on a horizontal straight line tangent to the flat baseline of the spectrum in the

range 4.5 to 5.2 micrometers and extending to the 7.0 micrometer range. Measure the net absorbance

of the peaks at 7.9 and 11.6 micrometers, using the appropriate baseline technique Section 14.2.2). Note the presence or absence of peaks at 9.3 and 9.7 micrometers having approximately equal absorbance

intensities which identify ethylene glycol.

8.2 Natural Gas Engine Oils. Fill the cells and adjust the spectrophotometer transmittance as described in Section 8.1. Place the cells in the spectrophotometer and record the spectrum between

2.5 and 12.5 micrometers. Measure the net absorbance at 2.90 micrometers as previously described in Section 6.1.2. Measure the net absorbance of the peaks at 5.85, 6.05, 6.1 and 6.4 micrometers, based

on a horizontal straight line tangent to the flat baseline of the spectrum in the area of 4.5 to 5.2

micrometers and extending to the 7.0 micrometers range. Measure the net absorbance of the peaks at

7.9 and 11.6 micrometers by a baseline technique. Absorption peaks of approximately equal intensity

occurring at 9.3 and 9.7 micrometers indicate the presence of ethylene glycol.

8.3 Diesel Engine Oils. Fill the cells and adjust the spectrophotometer transmittance as described in Section 8.1. Place the cells in the spectrophotometer and record the spectrum between

2.5 and 12.5 micrometers. Measure the net absorbance at 2.90 micrometers as previously described in Section 6.1.2. Measure the net absorbance of the peaks at 5.85, 6.05, and 6.1 micrometers, based on a horizontal straight line tangent to the flat baseline of the spectrum in the area of 4.5 to 5.2

micrometers and extending to the 7.0 micrometer range. Measure the net absorbance of the peaks at 7.9

and 11.6 micrometers by a baseline technique. Note the presence or absence of peaks at 9.3 and 9.7

micrometers having approximately equal absorbance intensities which identify ethylene glycol. If the

transmittance at any wavelength of interest is less than 30%, refer to Section 7.2.

9. CALCULATION AND REPORT

9.1 Convert the net absorbance values into absorbance per centimeter of cell pathlength.

9.2 Determine water and fuel dilution percentages by volume by reference to the respective

calibration curves, Section 6.

Note 7 - In the presence of high oxidation (absorbance at 5.85 micrometers) the water peak

at 2.9 micrometers may be influenced by the presence of oxidation products containing -OH and be high.

9.3 Report results as shown in table 1, Section 3.

SUMMARY OF ELEMENTAL ANALYSIS

BY

EMISSION SPECTROMETRIC PROCEDURE

This method covers the determination of twenty-one elements in new and used lubricating oils.

Summary

A graphite disc electrode rotating in a vertical plane partially immersed in the oil sample

serves as the lower electrode and provides continuous introduction of the sample into the arc gap. A controlled high-voltage arc between the upper and lower electrodes excites the sample. Spectral light

is generated and processed to discrete spectral light beams that are directed to certain photomultipl ier

tubes. The photomultipl ier tubes convert the spectral light to an electrical signal current. The amount of signal current is measured. Utilizing these measurements, the attached mini-computer and

peripheral hardware with software packages supplies a complete printout showing percent concentration

of the elements desired.

Standard materials are used to calibrate and develop analytical curves. These curves supply the

information necessary for converting the analytical data into percent concentration.

Apparatus

The apparatus includes the following:

A-15
HA- 10 Baird Spectromet 1000 direct reading spectrometer

RS-2 High speed digital readout

SCE-14 Spectrocomp system PDP - 8/A computer

Decwriter for printout

Material

s

Materials necessary are:

Disposable sample containers

Electrode rotating discs

Electrode rods

Standards

Standards used are Conostan metal lo-organic standards.

Base oil is used for preparing calibration standards.

Conostan C-21 standards are purchased at concentrations of 900, 100, and 50 parts per million

(ppm).

The C-21 Standards are blends of equal amounts of the following elements:

Ag Al B Ba Ca Cd Cr

Cu Fe Mg Mn Mo Na Ni

P Pb Si Sn Ti V Zn

Standards are prepared by weight using the purchased standards and base oil to make dilutions.

The series of standards used for analytical curves include concentrations covering 0 ppm, 0.1 ppm, 0.2

ppm, 0.5 ppm, 1 ppm, 2 ppm, 5 ppm, 10 ppm, 20 ppm, 50 ppm, 100 ppm, 450 ppm, 900 ppm. A daily adjust- ment standard is prepared.

Procedure

The optical portion of the spectrometer 1000 is adjusted before use to line up the optics to optimum position. The daily adjustment standard is burned three times or until three sets of results

are within the satisfactory limit of variance. The results are averaged and the computer adjusts the curves relative to these results. Next a standard with known levels is run and if significant differences from the values are found the daily adjustment standard is rerun.

Sample handling procedure requires that all samples should be mixed well before removing a portion for analysis. The sample is poured into a new sample container until the container is level

full. The full sample container is placed in the holder on the adjustable head of the stage in the

rotating disc electrode disc stand. Prior to putting the sample in this stand, one rotating disc

electrode and one rod electrode is placed in the holders and the gap is set. The stage is raised

until the rotating disc electrode dips about 2 mm into the sample of "oil." The sample containers and

electrodes are used once and discarded to prevent contamination. However, the long rod electrodes may

be reused by cutting away about 6 millimeters and reshaping the tip. Pushing the start button

activates the timing to sequence the system through Flush, Preburn, Expose and Measure modes. During

this sequence of modes of the system, data is accumulated, reduced, computed and printed out as element concentration for each of the twenty-one elements for which the readout is programmed.

Report

We report results in parts per million with the following exceptions.

For all elements except silver and phosphorus zero is reported for a readout of less than 0.5. Silver values are reported down to 0.1 mm. Phosphorus readouts below 50 are reported as less than 50 ppm (<50).

Total metals is the summation of all the detected metals plus phosphorus and silicon.

A-16
9

SUMMARY OF THE NEUTRON ACTIVATION ANALYSIS TEST

FOR CHLORINE AND BROMINE

In the neutron activation analysis (NAA) test method, the sample is irradiated in a neutron

source (usually a nuclear reactor, in order to obtain the required sensitivity) for a period of time

and, after withdrawing the sample, the resulting induced radioactivity is measured. This radioactivity is detected and quantitated using a high resolution germanium semiconductor detector. Each

element of interest may be uniquely identified through observation of its gamma-ray energy, half-life,

and also peak ratios if multiple gamma-rays are produced. The NAA method measures total chlorine and

total bromine in an oil sample, regardless of chemical form or location, and does not suffer from

significant problems with non-halogen additives or contaminants expected to be in re-refined or virgin

lubricating oil basestocks. The sensitivity of NAA for both chlorine and bromine is below 1 ug/g

using this analysis method.

The NAA method has been found to be both repeatable and consistent with results from other

analytical methods. Although not considered a routine analytical technique, the NAA method is straightforward and analyses can be obtained commercially. Although this procedure is not in ASTM

format or highly detailed, it provides sufficient information for an experienced individual to duplicate these analysis.

Experimental Procedure

Samples for Analysis: Oil samples to be analyzed must be representative of the bulk material in order to provide valid data. Non-homogeneous oils must be thoroughly mixed prior to sampling. Used

oils and/or heavily contaminated oils should be vigorously shaken in a paint shaker for 20 minutes

immediately before subsampling for analysis. To monitor the halogen blank values, a paraffin oil

(Fisher Scientific No. 0-119) was run in parallel with each set of oil samples.

Sample and Standard Irradiation: Both samples and standards were irradiated in NBSR small

screw-top rabbits which had been pre-cleaned with high purity nitric acid. These containers were held

in a fixed position by a heat sealed polyethylene snap-top vial which was placed in the bottom of a standard NBSR rabbit for irradiation. All irradiations were done in the RT-4 pneumatic tube facility

i of the NBSR (f = 1.3 x 10 13 N-cm 2 -s 1 ) for times from two to ten minutes.

After irradiation, the sample or standard was pipette transferred to a preweighed screw-top glass

vial for counting. The sample weights ranged from 2.3 to 2.9 grams. The standards used were twn aqueous solutions each of KBr and NaCl with the concentrations shown in Table I.

Table I

Standards Used for Analysis

Compound Cation (ug/g) Anion (ug/g)

KBr- I 319.42 692.79

KBr- I I 30.86 63.07

NaCl-I 584.41 901.22

NaCl-II 39.36 60.69

Counting Procedure: All samples were counted with the vials placed upright at 10 cm from a Ge(Li) detector. Replicate counts were taken at 20 cm and 30 cm for samples and standards with

sufficient activity. Two series of counts were done for each sample, one within the first hour

after irradiation to determine the 38 C1 activity, and the second a day later to determine to 82 Br. For each element, at least two characteristic gamma lines were monitored and in general more than

one count was taken in both counting series. The gamma lines and decay half- lives used are shown

in Table II.

A-17
Table II

Characteristic Radiation Measured

Elem. Nucl ide Half- Life E ,, KeV Ey2 , KeV E Y3- KeV

CI 38 C1 37.21 min 1642.42 2167.51

Br 82 Br 35.30 hr 554.35 776.52 1044 00

Na 24 Na 15.00 hr 1368.63 2754.03

K 42 K 12.36 hr 1524.67

The analyzer dead time was kept at below 5% and no correction was made for pulse pileup or for the

second order effect of the decaying source on the live time. The quantity deemed proportional to element mass was

NeXt

l (l-e_AA

)(l-e"

AT

)

where:

N = net counts in the gamma peak

k = the decay constant

t = irradiation time

A = counting live time

t-^ = time from end of irradiation to the start of count

Results: The measured concentrations of chlorine and bromine in nine oils are given in Table I The values given are a pooling of the results for the two or more gamma lines measured and for

multiple counts of each sample. Only one sample of each oil was measured. The uncertainty

quoted for the mean value is the larger of the observed range of the individual determinations

and the a priori statistical uncertainty of a single determination. This uncertainty should be

conservative estimate of the (la) precision of the values given.

Table III

Typical Elemental Concentration Results for

Halogen Analysis in Virgin and Re-Refined Basestocks

Sample# CI (ug/g) Br(ug/g)

AA 0.91 ± 0.06 <0.06

BB 0.42 ± 0.04 <0.07

CC 0.12 ± 0.02 <0.03

DD 0.12 ± 0.02 <0.03

EE 102.4 ±1.5 9.4 ± 0 2 FF 7.72 ± 0.15 1.54 ± 0 10 GG 0.48 ± 0.05 <0.07

HH 29.0 ± 0.5 0.84 ± 0 07

II 37.8 ± 0.5 1.62 ± 0 10

Paraffin Oil 0.12 ± 0.02 <0.03

Container 3.4 ± 0.1 0.07 ± 0. 03

The concentration measured for the Fisher paraffin oil may be considered an upper limit of the

procedure blank, which represents possible leaching of the irradiation container by the oils. For bromine, this blank is below the measurement sensitivity of 30 ppb. For chlorine, the

apparent 0.12 ppm blank may in fact be a trace impurity in the paraffin oil. As an absolute

upper limit on the procedure blank, an empty irradiation container was counted and the results

are shown in Table III. It should be noted that these results would occur as a blank only if the entire irradiation container were dissolved into the oil.

A-18
Conclusions: (1) The limit of measurement for chlorine and bromine is about 50 ppb, using the

present procedure. For bromine, the blank is at or below this level while for chlorine the

blank may be as high as 120 ppb.

(2) The post-irradiation transfer of the samples incurs the possible risk of loss of volatile

species, which could be serious for either CI or Br. However, no loss of CI or Br activity was

seen during a large number of analysis, and agreement is good with other analytical techniques

for chlorine in samples for which other techniques can be used.

SUMMARY OF TOTAL OXYGEN TEST

METHOD: MODIFIED UOP METHOD 649-74

The sample is pyrolyzed in a helium atmosphere in the presence of carbon. Oxygen is converted to carbon monoxide. A gas chromatograph is used to separate and quantify the evolved carbon monoxide.

The lower limit of detection is 0.1%. Precision = ± 5% of the 0 2 content. No correction is made

for H 2 0.

SUMMARY OF THIN LAYER CHROMATOGRAPHY WITH FLAME IONIZATION DETECTION (TLC/FID)

The separation is performed on a quartz rod coated with stationary phase material (e.g. silica

gel or alumina). The rod with the chromatographical ly separated hydrocarbon types is passed through

the flame of a hydrogen/air burner above which is a collector electrode. The ionization effect from

the combustion process is converted into a signal from which the chromatogram is recorded.

SUMMARY OF MASS SPECTROMETRY ANALYSIS

High resolution mass spectrometry analysis of the ASTM/NBS BCS oils has been carried out. Such

analyses were performed in order to identify any organic impurities such as anti-oxidants , plasticizers

,

acids, and halo-carbon solvents which may be present in the oil. The experimental conditions are described below.

Experimental Method

The instrument used for these experiments was an AEI MS50 mass spectrometer, operating in electron impact mode at a mass resolution of 1:20,000 under the following conditions; source temperature -250 °C, electron energy -70 eV, electron current - 100 uA, accelerating potential - 8000V. 20 pi of sample is heated in an oven which is at 270 °C and the resultant vapor allowed to flow into the mass spectrometer via a small leak. These conditions are designed to yield analysis of

a maximum portion of the sample without thermal degradation ("cracking") of the oil occurring and

using optimum mass resolution and sensitivity. Under these conditions approximately 85% of the

sample was analyzed in most cases. The exceptions were BC7186 (60%), BC7239 (70%), BC7240 (70%) and

BC7245 (55%). The figures in brackets represent the amount of sample analyzed. This may indicate

that these four oils contain high molecular weight impurities such as polymers.

Basestock

All the oils examined contained the expected paraffinic and aromatic species that contribute to "natural" hydrocarbon oils, although different mixes of paraffinic and naphthenic oils were observed.

No evidence was obtained for the incorporation of synthetic oil basestocks in the re-refined oils of a level of greater than 3%. However, some of the oils (BC 7171, BC7239, BC7241 and BC7243) contain

abnormally low levels of the C H„ series of ions which are usually characteristic of benzocycloJ n 2n-ll

paraffins (mono and di cyclic).

Molecular Weight Range

Under the conditions utilized it is not possible to give any accurate data on molecular weight.

However, three of the oils (BC7171, BC7186 and BC7243) were examined using chemical ionisation mass

A-19
spectrometry. This is a soft ionization technique, which concentrates a larger amount of the ion

current in the molecular ion region of the mass spectrum. This enables better data to be obtained on molecular weight, but sacrifices information on compound type. The results show the molecular weight

range of three oils examined to be BC 7171, 370-490 amu; BC 7186, 390-520 amu; BC 7243, 340-520 amu.

Sulphur Compounds

Sulphur compounds were detected in some of the oils examined. Doping experiments indicate that

the other ten oils probably contain less than 400 ppm of aromatic sulphur compounds. The oils con- taining sulphur compounds contained up to three types of compounds, benzothiophenes (in BC 7169, 7170,

7172, 7174, 7187, 7237, 7138, 7239, 7244, and 7246) dibenzothiophenes (in BC 7169, 7170, 7172, 7174,

7238, 7244, and 7246) and a series c

n H2n-i2S wnich maY be indanothiophenes (in BC 7169, 7237, 7238,

7244, 7245, and 7246). Approximate concentrations for BC 7284, 7372, 7374, 7356, 7415, and 7413 are reported.

Other Organic Compounds

For all but three oils, no compounds containing oxygen or nitrogen were observed. This means

that expected impurities such as phenols, amines and organic acids were present at less than 600 ppm

in the portion of the sample analyzed. However, we cannot eliminate the possibility that these types

of compounds have become bound to polymer or inorganic residues and have, therefore, not been

distilled into the mass spectrometer.

All the oils contained less than 500 ppm of antioxidant material, less than 300 ppm of halocarbon

solvents and less than 250 ppm of plasticizers such as phthalate esters.

Three oils did contain other organic compounds in addition to the hydrocarbons normally found in oils. BC 7418 has a range of compounds containing nitrogen and a combination of nitrogen and oxygen. This is consistent with the degradation of a PIB-succinimide during the rerefining process. BC 7293

contains sulphonic acids and BC 7248 contains naphthenic acids.

SUMMARY OF 13 C NMR ANALYSIS

13 C NMR spectroscopy analysis by this technique provides two types of information:

(1) the level of residual polyisobutylene additive(s)

(2) an estimate of differences in carbon types between the base oils.

(1) Analysis for polyisobutylene derivatives

The 13 C NMR spectrum of free polyisobutylene (PIB) or its derivatives is dominated by three

signals due to the C 4 polymer repeat unit. The -CH2

- signal at 6(c), 59 ppm is well resolved from the

mineral oil background and this has been used to determine the level of polymer in the oil. Most of

the samples showed no detectable PIB indicating levels <0. 5% w/w for total carbon in PIB/total carbon

in oil. The results for those samples where it was detected are reported, there appears to be a variation in polymer level.

(2) 13 C NMR analysis of base oil composition

Previous 13 C NMR work on mineral oils and re-refined oils has shown that two parameters can provide information on the origin of the crude oils from which they derive. These are:

(a) the integral of all linear hydrocarbon signals expressed as a proportion (%) of the total

aliphatic integral.

(b) the 'isoprenoid ratio' which is the ratio: signal intensity due to

+C/signal intensity due

to *C

(CH,) - CH - +CH,-CH,

+CH, - CH -(CH,)„

2 n | 2 2 2 j 2 n CH

3 CH

3 "(CH 9 ) n

- CH 9- *CH„ - CH - ^CH, - CH, (CH 0

) - I n 2

I CH

3 A-20
The results for the oils are reported. We estimate experimental errors as ±1% (for linear/total,

%) and ±0.05 (for isoprenoid ratio).

SUMMARY OF ULTRAVIOLET SPECTROPHOTOMETRY

This analytical method is used in direct oil analysis for the qualitative and semi -quantitative

determination of aromatic hydrocarbons. Within this chemical family the method is used for the

analysis of mononuclear (at a wavelength of 195 nm), dinuclear (at 225 nm) and trinuclear (at 255 nm)

aromatic hydrocarbons.

DESCRIPTION OF SEDIMENT AND FILTERABILITY OF INDUSTRIAL OILS

(MEMBRANE FILTRATION METHOD)

1. INTRODUCTION

1.1 This revision includes adaptations for testing hydraulic oils which contain wax.

2. SCOPE

2.1 This method is used primarily (a) to determine insoluble contaminants (sediments) suspended

in hydraulic oils (DTE) and way lubricants (Vactra numbered), and (b) to measure the f i lterabi 1 ity of

hydraulic oils. The test is intended for control of oil cleanliness to quality specifications. It can be used to measure the cleanliness and filterability of other products, e.g., circulating oils,

turbine oils, etc., and also basestocks.

3. DEFINITION

3.1 Filterability is the time required for a specified volume of sample, neat or diluted, to

pass through a micropore filter membrane under standard conditions of dilution, pore size, filter

diameter, vacuum, etc.

4. OUTLINE OF METHOD

4.1 A measured volume of sample is diluted with solvent and filtered through a membrane of

specified porosity. The amount of sediment that is retained is determined from the increase in weight

of the membrane. The filterability is determined by measuring the filtration time.

5. APPARATUS

5.1 Filtration Equipment.

5.1.1 Filter Holder, Pyrex, consisting of a 300 mL funnel, clamp and stainless steel disc

support.

5.1.2 Forceps, stainless steel.

5.1.3 Membrane Filters, plain, white, 47-mm diameter,

o 0.3 micrometer.

o 0.8 micrometer,

o 5.0 micrometer.

Assemble the apparatus using either a 500 mL or 1-liter suction flask.

5.2 Drying Oven, explosion proof, capable of maintaining a temperature of 75 ± 2 °C.

5.3 Vacuum Source, capable of maintaining constant vacuum of 125 mm and of 250 mm of mercury.

5.4 Weighing Dishes, aluminum.

5. 5 Stop Watch.

A-21
5.6 Separatory Funnel, 500 mL, with Teflon plug.

5.7 Wash Bottle, 500 mL.

6. REAGENTS

6.1 n-Pentane (for hydraulic oils.) ASTM specification given in D893, "Insolubles in Used

Lubricating Oils." Filter the n-pentane through a 0.3 micrometer membrane into a suction flask,

transfer and store in a solvent-rinsed glass container.

Note 1 - Prepare the suction flask and container as follows: Wash with warm, soapy water,

and rinse thoroughly with tap water, then with distilled water. Rinse several times with

small portions of reagent-grade acetone, and then several times with the filtered solvent.

6.1.1 Periodically determine a solvent blank by filtering 100 mL of n-pentane in the same manner as described for the sample in Section 8, except that a 0.3 micrometer membrane is used. If the increase in weight of the membrane exceeds 0.2 mg per 100 mL, the blank is considered unsatisfactory.

Reclean the apparatus and prepare fresh solvent. Repeat the blank determination.

6.2 Sovasol No. 2 or Precipitation Naphtha (for way lubricants).

6.2.1 Filter, store and test the solvent as described in 6.1 for n-pentane.

7. SAMPLE PREPARATION

7.1 Allow the sample to equilibrate to room temperature (24 ± 3 °C). Prior to further handling,

shake the container by hand for about 30 seconds to ensure that all sediment, if present, is uniformly

distributed.

Note 2 - If wax is present, the time-temperature conditioning of the sample can affect the test results significantly. The presence of wax may not be apparent unless the sample is allowed to stand in a cool state (room temperature) long enough for the wax to crystallize.

Samples which are suspected to contain wax, e.g. hydraulic oils, should be held at room temperature for 24 hours, shaken by hand for about 30 seconds and then tested. See Note 6.

8. PROCEDURE

8.1 Hydraulic Oils

8.1.1 Place a 0.8 micrometer membrane in an aluminum weighing dish with the correct side up (Note 3) and dry for 10 minutes in an oven at 75 ± 2 °C. Remove the dish and cool for about 10

minutes in a dust-free area, such as a covered drying block. Remove the membrane from the dish,

weigh to the nearest 0.1 mg and record the weight as Wx

. Place it correct side up on the stainless

steel support, attach the funnel, and clamp together.

Note 3 - The membrane must be placed on the stainless steel mesh filter support with the

correct side up. Failure to do this may result in incorrect filter times. In most cases,

the membranes as received are packed with the correct side facing up. In other cases, a written statement indicating the correct side is packed with the membranes. Handle the

membranes with forceps to avoid disturbing the filtering surface or altering the weight.

8.1.2 Measure 100 mL of the sample with a graduated cylinder into a separatory funnel (Note

about 30 seconds. Suspend the separatory funnel in such a manner that the bottom of the stem is approximately 1 inch above the filter membrane. Open the stopcock and introduce the mixture into the

filter cup.

Note 4 - If a funnel with a glass stopcock plug is used, lubricate the plug lightly with

pure mineral oil

.

Note 5 - The use of a separatory funnel is convenient but not mandatory. However, if the

oil -sol vent blend is mixed in a graduated cylinder (250 mL) and added directly to the

filter, a constant level must be maintained in the filter cup.

8.1.3 Apply a vacuum of 125 mm of mercury to the suction flask, and adjust the liquid flow

from the separatory funnel to maintain a constant level in the filter cup.

A-22
8.1.4 Measure and record the elapsed time required to filter the oil-pentane mixture as follows: Start the watch when the first drop appears through the apparatus. Stop the watch when all the solution has passed through the membrane, i.e., when the membrane first appears dry. Discontinue

the test if the filtration is not complete within 30 minutes. Record the elapsed time as "First 100

mL Filter Time."

Note 6 - To determine if a high filtration time is caused by wax (Note 2), heat 250 mL of

well -shaken sample to 50 °C, cool to room temperature and allow to stand one hour. Shake 30 seconds and test in the usual way. If the filtration time is substantially less than the

value obtained after the 24-hour conditioning, the presence of wax is likely. Report the

filtration times determined by the two tests, i.e. after 1-hour and 24-hour conditioning

periods, and the sediment measured after 1-hour conditioning.

8.1.5 If a second 100 mL filtering time is specified for the product, repeat 8.1.2, 8.1.3

and 8.1.4, using the same membrane, graduated cylinder and separatory funnel. Record the elapsed time

as "Second 100 mL Filter Time."

8.1.6 Rinse the graduated cylinder with about 20 mL of n-pentane and transfer this to the

separatory funnel (stopcock open) in such a manner as to rinse the wall. Repeat with two more 20 mL portions of n-pentane. When the filtration is complete, remove the separatory funnel and rinse the

wall of the filter cup with about 40 mL of n-pentane from the wash bottle. With the vacuum still

applied, remove the filter cup and wash the membrane with about 40 mL of n-pentane from the wash

bottle. Direct the stream from the periphery toward the center of the membrane.

Note 7 - Care must be taken to ensure that all the oil is washed through.

8.1.7 Gently remove the membrane with the vacuum still applied. Place it in the oven at

75 °C for 10 minutes, remove and cool in a dust-free area for 10 minutes. Weigh the membrane plus

sediment to the nearest 0.1 mg and record as W2

.

8.2 Way Lubricants.

8.2.1 Place a 5.0 micrometer membrane in an aluminum weighing dish and proceed as described

in 8.1.1.

8.2.2 Measure 75 mL of the sample into the separatory funnel and add 25 mL of prefiltered

Sovasol No. 2 or precipitation napththa. Proceed as described in 8.1.2.

8.2.3 Apply a vacuum of 250 mm of mercury to the suction flask. Proceed as directed in 8.1.3, 8.1.6, and 8.1.7, but substituting Sovasol No. 2 for n-pentane.

9. CALCULATION AND REPORT

9.1 Hydraulic Oils (DTE).

9.1.1 Calculate and report the sediment retained on an 0.8 micrometer membrane as follows:

ioo(w

2 -w

1

) Sediment, mg per 100 mL of oil =

V

where:

W-^ = weight of membrane, mg.

Vl^ = weight of membrane plus sediment, mg.

V = total volume of oil filtered, mL.

9.1.2 Report the elapsed time under 8.1.4 as "First 100 mL Filter Time." Note 6.

Note 8 - If the test was discontinued after 30 minutes because of plugging, report the

filter Time as 30+ minutes without reporting sediment weight.

A-23
9.1.3 Report the elapsed time under 8.1.5 as "Second 100 mL Filter Time." (Note 8).

9.2 Way Lubricants (Vactra numbered).

9.2.1 Calculate and report the sediment retained on a 5 micrometer membrane as follows:

Sediment, mg per 75 mL of oil, = W

?

- W,

SUMMARY OF STORAGE STABILITY TEST

Appearance, color and sediment of the samples as received is reported. The appearance code is given herewith. Color is performed according to ASTM D1500. Sediment is analyzed according to ASTM

D2273.

Storage Stability

Ambient Storage - One Year

This test simply involved the storage of 50 mL of the oil in a 100 mL brown glass bottle in an enclosed cupboard in the laboratory for one year. Results are tabulated for sediment after one year

and color after one year.

Cold Room Stability Test - One Year

Upon receipt the oil is visually examined for clarity and cleanliness. 100 mL of oil are then

stored in a 200 mL brown glass bottle in a cold room maintained at 40 °F. The oil is examined

visually monthly for precipitation, sedimentation and other changes. The cold room test is terminated

after one year.

The results are reported using the code given herewith. No effort was made to identify the

precipitates.

Sunlight Stability Test-One Year

Upon receipt the oil is visually examined for clarity and cleanliness. Color test, ASTM D1500,

and sediment test, D2273 are also performed. 200 mL of oil are then stored in an 200 mL clear glass

bottle in the laboratory on the ledge of the south window receiving the full effects of winter and summer sunlight. The oil is examined visually monthly for precipitation, sedimentation, and color

change. In addition after 6 months and one year, 50 mL are removed for an ASTM D1500 color test, and

ASTM D2273 trace sediment test. The sunlight test is terminated after one year.

The results are reported here on four sheets:

(1) Sediment after one year, (2) color after one year, (3) appearance after one year, and (4)

appearance showing month when precipitation first appeared.

The sunlight stability test is not sufficiently standardized; sunlight is not very reproducible.

It is not designed as either a consistency test stable to sunlight nor a quality test because base

oils are never put into direct sunlight in this way in glass vessels.

APPEARANCE CODE

OVERALL APPEARANCE DUE TO VERY FINE PARTICLES IN SUSPENSION

C - Clear; no visible evidence of particles in suspension, (a —

also indicates clarity or substantial clarity)

T - Translucent or hazy due to very fine particles in suspension.

0 - Opaque or cloudy due to very fine particles in suspension. EXTENT OF FLOCCULATION DUE TO COARSE PARTICLES (OFTEN AS CLUSTERS) IN SUSPENSION

TH - Trace haziness

TF - Trace flock; 10 to 50 specks approximately.

LF - Light flock; 50 to 100 specks approximately.

A-24
HF - Heavy flock; more than 100 specks.

P - Particles in suspension or settled sediment

DEGREE OF SEDIMENT OR STAIN

S - Brown stain on glass

TS - Trace sediment; few particles settled; less than 5% of bottom

covered.

LS - Light sediment; about 5% to 50% of bottom covered.

MS - Moderate sediment; about 50% to 100% of bottom covered.

HS - Heavy sediment; marked thickness of sediment, say over 1/16" thick.

MONTH OF FIRST APPEARANCE OF PARTICLES IN SUSPENSION OR AS SEDIMENT

This is indicated by number in box, e.g., "Oil G/March" in the cold

storage test shows "C/TF-6", which means that the oil is essentially

clear except for trace flocculation that first appeared in the 6th month.

A "C" indicates clear oil even after 1 year.

SUMMARY OF THE ANTIOXIDANT CAPACITY TEST PROCEDURE

This test was developed by Dr. Lee Mahoney and others at the Ford Motor Co., and details of the

apparatus and procedure can be found in the open literature (Industrial and Engineering ChemistryProduct Res. and Dev. 17, 250 (1978)).

This test method determines the antioxidant capacity of a lubricating oil by measuring the length

of an induction period preceding the rapid uptake of oxygen by the test solution when a small quantity

of oil is added to the system. This delay time is directly proportional to the antioxidant capacity

of the oil. The test solution consists of an oxidizable hydrocarbon, cyclohexene, and a free radical

initiator, azobis-isobutyronitrile, in a n-hexadecane-chlorobenzene solution. The principle of the

method is based upon the titration of the antioxidant species present in the oil by peroxy radicals

formed at a constant rate from the thermal decomposition of the initiator in the presence of dissolved

oxygen. At the end-point of the titration the solution begins to rapidly absorb oxygen by a chain

process. The decrease in oxygen pressure is monitored.

All of the chemicals used in this method needed to be further purified by recrystal 1 ization,

distillation and/or adsorption techniques. This includes the cyclohexene, chlorobenzene, n- hexadecane, azobis-isobutyronitrile, 2,6 di-t-butyl-4-methylphenol and 4,4' -methylene bis (2,6-di-tbutylphenol ). Further, it is necessary to calibrate the delay time with different known concen- trations of various antioxidants. At that time, measurement of the antioxidant capacity of various

re-refined and virgin lubricating oil base stocks, formulated with a "standard" additive package, were

made. It may be noted also that this test can be evaluated both before and after the oils have

undergone a bench oxidation test.

SUMMARY OF DIFFERENTIAL SCANNING CALORIMETRY METHODS

(Literature references "Characterization of Lubricating Oils by Differential Scanning Calorimetry,"

J. A. Walker and W. Tsang, SAE paper No. 801383, Fuels and Lubricants Meeting, Baltimore, MD, Oct. 20-23, 1980).

High pressure differential scanning calorimetry (DSC) has been used to characterize the oxidative

stability of formulated as well as virgin and recycled lubricating base stocks. At pressures of 0.7 - 3.4 MPa (50-500 psig) air or 0 2 , and temperatures near 200 °C, degradation occurs with significant

generation of heat. Experiments conducted in the temperature programmed mode give recognizably

different thermograms as well as onset temperatures for various lubricating oils. In the isothermal

mode induction time measurements were carried out with ASTM Engine Test Standard Reference Oils (R0)

which contain antioxidants and appear to correlate with multicycl inder engine sequence test results.

Under the same experimental conditions virgin base (VB) and recycled base (RB) stocks degradate too quickly to measure the induction time.

The speed, accuracy and experimental configuration of DSC measurements suggest its use not only

for elucidating fundamentals on the mechanism of hydrocarbon oxidation but also as a standard test

method.

The present studies are aimed at exploring the possibility of using DSC as a standard test method

for evaluating the oxidative stability of luricating oil, and further to use the technique to study

the basic mechanisms involved in hydrocarbon oxidation processes.

A^25
2. Experimental

All experiments were made using a DuPont Model 990 Thermal Analyzer with a model 910 high pressure

differential scanning calorimeter module, [a] The experimental procedure involves placing a 1 to 2 mg sample in an open aluminum pan, setting the pressure and the flow rate of the purged gas - air, oxygen,

or nitrogen - and then commencing the experiment either by running the temperature up to a preselected

value, holding it at this point and observing the reaction heat as a function of time (isothermal experiment), or by scanning at a programmed temperature rate and measuring the incremental heat change as a function of temperature rapidly raised to the isothermal temperature. At that time 0 2 was introduced

and the time scan started simultaneously.

A great deal of attention was given to finding the conditions that yielded an optimum amount of

reproducible information and indeed it proved to be possible to increase the precision by an order of

magnitude in comparison with the earlier work. The conditions and procedures that were used for these

studies are summarized below.

A Modified Procedure for Measuring Oxidative Stability by Induction

Time Method

Introduction:

A fundamental property of automotive lubricating oil is its ability to resist oxidation. This property

can give some indication as to its expected lifetime. To enhance performance antioxidants are among the

materials added to oils.

Procedure:

1. One to two milligrams of sample are placed in an open aluminum sample pan which is placed in the cell on the sample pedestal with an empty aluminum pan on the reference pedestal. The cell is closed

and the pressure cover is secured by three bolts tightened finger tight.

2. The cell is pressurized to 349 KPa (50 psig) with oxygen and purged by opening the vent valve.

The process is repeated with vent valve closed but with the exit valve open to allow a flow of 50 cm3 /min

of oxygen for about 30 sec.

3. The pressure [b] is then raised to 3.4 MPa (500 psig) the exit needle valve is adjusted for

dynamic flow of 50-100 cmVmin.

4. The initial temperature dial is set 10 °C below the desired isothermal temperature and the iso

button is depressed. When the uncontrol light goes out the temperature dial is reset to the isothermal

temperature (185 °C in this case).

5. When the uncontrol light goes out again, the start switch is depressed and the recorder pen is lowered simultaneously.

6. The scan continues until the antioxidant is consumed and is signified by an exothermic peak which

rises sharply from the base.

The time lapse between zero time and the extrapolated onset of the exotherm is the induction time.

If one allows the time base scan to continue until the exotherm returns to the baseline, the heat

generated by the reaction can be determined by the following formula: AH = |

(60BEAqs)

where A = Peak area in (cm2

) M = Sample mass in (mg)

B = Time base setting in (min/cm)

E = Cell calibration coefficient dimensionless (approx. 1.000)

Aqs = y-axis range setting in meal sec Vin

AH = Heat of reaction J/g (mcal/mg)

[a] Certain commercial materials and equipment are identified in this paper in order to specify adequately

the experimental procedure. In no case does such identification imply recommendation or endorsement by

the National Bureau of Standards, nor does it imply the material or equipment identified is necessarily

the best available for the purpose.

[b] For this general procedure, therefore, the pressure and temperature are dictated by the stability

of the material

.

A-26
A Modified Procedure of Oxidative Onset Temperature

Introduction:

This is a general procedure and adaptable to inhibited oils. The onset temperature is a measure

of the temperature at which oxidative degradation occurs.

Procedure:

1. One or two mg of sample are placed in an open aluminum sample pan which is then placed in the

cell on the sample pedestal with an empty aluminum pan on the reference pedestal.

2. The cell is pressurized to 700 KPa (100 psig) [c] with air and the flow is adjusted to 50-100

cnrVmin. Purging is not necessary for air. The heat control is set of 20 °C/min.

3. The cell is equilibrated at 100 °C for 2 mins. The heat switch is then depressed and the

recorder pen lowered.

4. The scan is continued until the antioxidant is consumed, which is signified by a sharply

rising exothermic peak. The onset temperature is the temperature at which the extrapolated onset

intersects the baseline.

[c] The pressure is arbitrary.

All experiments were carried out with flow rates of 50-120 cm3 /min (NTP). This was necessary to continually remove reaction products and to assure maximum contact between the sample and the reactive

gas. The pressures used in these experiment are a reflection of the need to obtain sharp onsets as well as maintaining details in the thermograms.

THERMAL OXIDATION LUBE OIL TEST ER

Summary of LUBTOT Test

LUBT0T is a modified JFOT test for investigating luricant deposition. This bench test has been

developed to provide initial screening for ground vehicle engine and gear lubricants. It is a high

temperature stability test with a hot spot temperature of 316 °C and an oil sump temperature of 93 °C. The test has a six hour duration using an oil flow rate of 180 mL/hr and an air flow rate of 10 mL/hr.

The oil is pushed upward outside a heated steel tube and the steel tubing is rated for color and

deposits.

A considerable number of tests were performed with the LUBTOT at controlled conditions in order

to generate data for subsequent correlations with available engine test data. LUBTOT tests were performed using numerous qualified specification products, several re-refined candidate MIL-L-46152

products, and re-refined basestocks without additives. Results showed the test can discriminate

lubricant quality level with reasonable repeatability.

The test method developed thus far does correlate with some of the Caterpillar single-cyclinder

reference tests; however, it does not correlate with the 1-D, 1-H, and 1-H2 test results performed on selected reference oils. Further development work is needed to attempt to correlate the LUBTOT

results with the two main reference tests, namely: the Caterpillar 1-G2 and the 1-H2 tests. LUBTOT

tests should be performed on oils that have "failed" the Cat 1-G2 and 1-H2 refarence tests. These

data will assist in developing an effective test procedure for "screening" candidate lubricants.

A limited number of tests were performed with re-refined oil basestocks and formulated oil. The

LUBTOT appears to be able to measure the consistency of basestock oils and determine the effectiveness

of the formulated oils evaluated.

LUBTOT appears to be an effective test device for evaluating lubricants regarding oil deposits

that are formed under a set of controlled test conditions.

A-27
REFERENCES

1. Hsu, S.M. , "Review of Laboratory Bench Test in Assessing the Performance of Automotive Crankcase

Oils, Lubrication Engineering 37, 722-731, 1981.

2. Cuellar, J. P., Montalvo, D.A. and Baber, B.B., "Studies with Synthetic Lubricants in the Hot Wall

Deposition Rig," Air Force Aero Propulsion Laboratory (AFAPL) Technical Report 72-25, 1972,

Wright-Patterson Air Force Base, Ohio.

3. D'Orazio A.J. , Karpovich, P. A. and Nowack, D.J., "A Study of the Factors Affecting Deposition

Characteristics of Synthetic Lubricants for Gas Turbine Engines," Naval Air Propulsion Test

Center (NAPTC), Technical Report PE-71, 1976, Trenton, New Jersey.

SUMMARY OF OXIDATOR TEST

The Oxidator test is similar in principle to a method described by Dornte in 1936 (1) and by

Denison in 1944(2). The stability of an oil is measured by the time required for consumption of a fixed volume of oxygen at 171 °C. The oil is vigorously stirred to saturate it with gas. The

pressure of oxygen is kept at one atmosphere by a gasometer immersed in water. Alternate evacuations

and fillings with oxygen charge the system with oxygen.

Results are reported as hours for 100 grams of oil to absorb one liter of oxygen. The actual test uses 25 grams of oil, and the results are corrected to 100 grams.

Procedure B

Used for evaluating base oils that will be used to formulate engine oils. An engine oil -type

catalyst is used. Oil temperature is 171 °C.

The engine oil -type catalyst is made up of metal napthenates patterned after the normal

distribution of metals in used crankcase oils after leaded gasoline engine tests. This catalyst

introduces soluble copper, iron, manganese, lead, and tin.

When this method is used for evaluating base oils for engine oil samples would be formulated with

an engine oil additive. Thus, the results would indicate response to a detergent-inhibitor package

rather than oxidation stability of the neat base oils. Based on results with three different

reference oils, the 95% confidence interval is about ± 5% of the actual results.

(1) Dornte, R.W. , Ind. Eng. Chem. 28, p 26 (1936).

(2) Denison, G.H., Jr., Ind. Eng. Chem. 36, p 477 (1944).

A-28
Appendix III

Additional Data

A-29
The following tables list additional data supplementary to the hydrocarbon analysis data in section V. These data include the percent recovery information for gradient elution chromatographic

methods. The data are useful for analysis and interpretation of the hydrocarbon type results

presented in section V.

Additional metal analysis data is also presented here.

Appendix III also provides a place to add new data which is considered to be necessary to evaluate the consistency of lubricating oil basestocks.

TEST: Metals (PPM) Atomic Emission Spectrometry [T3] LABORATORY: R

For all the Samples none of the following metals were detected except as noted.

Silver

Copper

Aluminum: BC7399, Oil I, Feb. 81, 1 ppm

Barium: BC7471, Oil J, Feb. 81, 1 ppm; BC7416, Oil J, Mar. 81, 1 ppm

BC7421, Oil F, Feb. 81, 1 ppm

Nickel

Chromium

Boron

Vanadium: BC7231, Oil B, May 80, 1 ppm

Molybdenum

Manganese

Cadi urn

Titanium: BC7198, Oil D, Apr. 80, 2 ppm; BC7200, Oil I, Apr. 80, 2 ppm

BC7202, Oil B, Apr. 80, 2 ppm

Phosphorus: BC7228, Oil I, May 80, <50 ppm; BC7227, Oil E, May 80, <50 ppm

BC7248, Oil F, June 80, <50 ppm

Iron: BC7338, Oil G, Oct. 80, 3 ppm; BC7205, Oil G, Apr. 80, <1 ppm

BC7244, Oil G, June 80, <2 ppm; BC7262, Oil F, Aug. 80, <1 ppm

BC7288, Oil F, Sept. 80, <1 ppm; BC7347, Oil F, Nov. 80, <1 ppm

A-30
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A-32
Acknowledgment

In a study of such scope of participation, it may not be possible to thank all the people who

have contributed to the study. The authors would like to thank all the base oil suppliers,

participating laboratories and Mobil Oil Corp., ASTM and NBS for their support and participation. The

three Task Force Chairmen: K. A. Frassa, W. C. Starr, and D. A. Becker who have spent many many hours

of work to make this study a success, deserve special commendation. On behalf of NBS, the authors

would like to thank Henrietta Brown, Denzil Mathews, and Art Cummings whose tireless efforts of

receiving samples, sending out samples and making sure that the right samples were received, have made

this study a reality. The aid received from the Statistical Engineering and Computer Services

Divisions at NBS, together with the work of Ying Leung and others, have made this massive compilation

possible. The general support and help from many in ASTM such as Paul Strigner (Technical Division P Chairman), Charles Thompson (Past Chairman of Tech P, Section II), George Booth III (Tech P, Section

II Chairman) and many others are gratefully acknowledged. Finally, the financial support from

Department of Energy, Office of Industrial Programs and Bartlesville Energy Technology Center is acknowledged with thanks.

A-33

ir U.S. GOVERNMENT PRINTING OFFICE : 1983 0 - 418-356
NBS-114A (REV. 2-8C) U.S. DEPT. OF COMM.

BIBLIOGRAPHIC DATA

SHEET (See instructions)

1. PUBLICATION OR

REPORT NO. NBS SP 661

2. Performing Organ. Report No. 3. Publication Date October 1983

4. TITLE AND SUBTITLE

ASTM/NBS Basestock Consistency Study Data

5. AUTHOR(S)

Stephan J. Weeks, Donald A. Becker, and Stephen M. Hsu

6. PERFORMING ORGANIZATION (If joint or other than NBS, see instructions) 7. Contract/Grant No. NATIONAL BUREAU OF STANDARDS

DEPARTMENT OF COMMERCE 8. Type of Report & Period Covered

WASHINGTON, D.C. 20234

FINAL

9. SPONSORING ORGANIZATION NAME AND COMPLETE ADDRESS (Street, City, State, ZIP)

Department of Energy/Bartlesvi 1 le Energy Technology Center

Bartlesville, OK 74005

10. SUPPLEMENTARY NOTES

Library of Congress Catalog Card Number: 83-600590

J Document describes a computer program; SF-185, FlPS Software Summary, is attached.

11. ABSTRACT (A 200-word or less factual summary of most significant information. If document includes a significant

bibliography or literature survey, mention it here)

ASTM and NBS co-sponsored a Basestock Consistency Study (BCS) to assess the quality

consistency of lubricating base oils. This study, which is the first of its kind,

will impact on developing basestock characterization methodology and on efficient

utilization of energy resources as well as their conservation through recycling.

The purpose of this publication is to present the ASTM/NB S BCS data for data analysis .

Monthly production samples from 6 re-refiners and 4 refiners were analyzed by 14

laboratories for a 13-month period. The results of over 55 tests are divided

according to 6 major categories: rheology, physical properties, chemical properties,

hydrocarbon type analysis, general performance tests, and oxidation and wear

bench tests. The data are presented in tabular and graphical form, which is

quite amenable to further data analysis.

12. KEY WORDS (Six to twelve entries; alphabetical order; capitalize only proper names; and separate key words by semicolons)

additive response; basestock; chemical properties; consistency; data; lubricants;

oil; petroleum; physical properties; re-refining

13. AVAILABILITY

| xl Unl imited

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