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664 Lubricant Additives: Chemistry and Applications

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manufacture and modi cation, Appl Catal A: Gen, 221, 429–442, 2001.

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oxidation, J Org Chem, 17, 5396–5400, 1995.

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666 Lubricant Additives: Chemistry and Applications

63. Waynick, J., The development and use of metal deactivators in the petroleum industry a review, Energy

Fuels, 15(6), 1325–1331, 2001.

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ungstechnik, 42(1), 26–30, 1995.

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Part 8

Methods and Resources

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669

Testing Methods for Additive/

Lubricant Performance

Leslie R. Rudnick

CONTENTS

27.1 Summary of Standard Test Methods and Speci cations ....................................................669

27.1.1 American Society for Testing and Materials ........................................................669

27.1.2 CEC Test Methods ................................................................................................. 674

27.1.3 General Motors ....................................................................................................... 675

27.1.4 Society of Automotive Engineers ........................................................................... 676

27.1.5 Miscellaneous Test Methods .................................................................................. 676

27.1.6 Federal Supply Class 9150 Product Commodities .................................................677

27.1.7 Speci cations Having Cross-Reference among JIS, ASTM, and Others ..............679

27.2 Abbreviations Used ............................................................................................................. 682

Ack nowledgment s ..........................................................................................................................683

This chapter contains a selection of many of the most commonly used test methods and speci -

cations selected from the United States, Europe, and Japanese lubricant testing methods. These

include methods, standards, and speci cations from the American Society for Testing and Materi-

als (ASTM), Federal Test Method (FTM), Military (Spec) (MIL), Conseil Européen de Coordina-

tion pour les Dévelopments des Essais de Performance des Lubri ants et des Combustibles pour

Moteurs (CEC), Deutsches Institute für Normung (DIN), Japan Petroleum Institute (JPI), as well as

Federal Supply Class 9150 commodities. Some cross-references are also given.

ASTM publishes an Annual Book of ASTM Standards. Petroleum Products, Lubricants, and

Fossil Fuels, Volumes 5.01–5.04, in which a complete list of ASTM methods pertaining to lubricants

may be found.

27.1 SUMMARY OF STANDARD TEST METHODS AND SPECIFICATIONS

27.1.1 A

MERICAN SOCIETY FOR TESTING AND MATERIALS

D 56 Standard test method for  ash point by tag closed tester

D 86 Standard test method for distillation of petroleum products

D 88 Standard test method for viscosity Saybolt seconds universal

D 91 Standard test method for precipitation number of lubricating oils

D 92 Standard test method for  ash and  re points by Cleveland open cup

D 93 Standard test method for  ash point by Pensky–Martens closed tester

D 94 Standard test method for saponi cation number of petroleum products

D 95 Standard test method for water in petroleum products and bituminous materials by distillation

D 97 Standard test method for pour point of petroleum products

(continued)

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670 Lubricant Additives: Chemistry and Applications

D 130 Standard test method for the detection of copper corrosion from petroleum products by the copper

strip tarnish test

D 150-98 (2004) Standard test methods for AC loss characteristics and permittivity (dielectric constant) of solid

electrical insulation

D 156 Standard test method for Saybolt color of petroleum products (Saybolt chromometer method)

D 189 Standard test method for Conradson carbon residue of petroleum products

D 217 Standard test method for cone penetration of lubricating grease

D 257-99 Standard test methods for DC resistance or conductance of insulating materials

D 287 Standard test method for API gravity of crude petroleum and petroleum products (hygrometer

method)

D 445 Standard test method for kinematic viscosity of transparent and opaque liquids (and the calculation

of dynamic viscosity)

D 482 Standard test method for ash from petroleum products

D 524 Standard test method for Ramsbottom carbon residue of petroleum products

D 525-05 Standard test method for oxidation stability of gasoline (induction period method)

D 566 Standard test method for dropping point of lubricating grease

D 567 Standard test method for calculating viscosity index

D 611 Standard test method for (1993)el aniline point and mixed aniline point of petroleum products and

hydrocarbon solvents

D 664 Standard test method for acid number of petroleum products by potentiometric titration

D 665 Standard test method for rust-preventing characteristics of inhibited mineral oil in the presence of water

D 874 Standard test method for sulfated ash from lubricating oils and additives

D 877-02e1 Standard test method for dielectric breakdown voltage of insulating liquids using disk electrodes

D 892 Standard test method for foaming characteristics of lubricating oils

D 893 Standard test method for insolubles in used lubricating oils

D 942 Standard test method for oxidation stability of lubricating grease by the oxygen bomb method

D 943 Standard test method for oxidation characteristics of inhibited mineral oils

D 972 Standard test method for evaporation loss of lubricating greases and oils

D 974 Standard test method for acid and base number by color-indicator titration

D 1091 Standard test methods for phosphorus in lubricating oils and additives

D 1092 Standard test method for measuring apparent viscosity of lubricating greases

D 1093 Standard test method for acidity of hydrocarbon liquids and their distillation residues

D 1159 Standard test method for bromine numbers of petroleum distillates and commercial aliphatic ole ns

by electrometric titration

D 1160 Standard test method for distillation of petroleum products at reduced pressure

D 1209 Standard test method for color of clear liquids (platinum cobalt scale) (APHA color)

D 1238 Standard test method for  ow rates of thermoplastics by extrusion plastimeter (melt index) (or ISO

1133–1991)

D 1264 Standard test method for determining the water washout characteristics of lubricating greases

D 1217 Standard test method for density and relative density (speci c gravity) of liquids by Bingham

pycnometer

D 1268 Standard test method for leakage tendencies of automotive wheel bearing greases

D 1296 Standard test method for odor of volatile solvents and diluents

D 1298 Standard test method for (1990)el density, relative density (speci c gravity), or API gravity of crude

petroleum and liquid petroleum products by hydrometer method

D 1331 Standard test method for surface and interfacial tension of solutions of surface-active agents

D 1358 Standard test method for (1995)el spectrophotometric diene value of dehydrated castor oil and its

derivatives

D 1401 Standard test method for water separability of petroleum oils and synthetic  uids

D 1403 Standard test methods for cone penetration of lubricating grease using one-quarter and one-half scale

cone equipment

D 1478 Standard test methods for low-temperature torque of ball bearing grease

D 1480 Standard test method for density and relative density (speci c gravity) of viscous material by

Bingham pycnometer

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Testing Methods for Additive/Lubricant Performance 671

D 1481 Standard test method for density and relative density (speci c gravity) of viscous material by Lipkin

bicapillary pycnometer

D 1500 Standard test method for color of petroleum products (ASTM color scale)

D 1646 Standard test method for rubber viscosity, stress relaxation, and prevulcanization characteristics

(mooney viscometer)

D 1662 Standard test method for active sulfur in cutting oils

D 1742 Standard test method for oil separation from lubricating grease during storage

D 1743 Standard test method for corrosion preventive properties of lubricating greases

D 1744 Standard test method for determination of water in liquid petroleum products by Karl Fischer reagent

D 1747 Standard test method for refractive index of viscous materials

D 1748 Standard test method for rust protection by metal preservatives in the humidity cabinet

D 1831 Standard test method for roll stability of lubricating grease

D 1947 Standard test method for load-carrying capacity of petroleum oil and synthetic  uid gear lubricants

D 2007 Standard test method for characteristic groups in rubber extender and processing oils and other

Petroleum-derived oils by the clay–gel absorption chromatographic method

D 2070 Standard test method for thermal stability of hydraulic oils

D 2155 Discontinued from 1981, replaced by E 659

D 2161 Standard practice for conversion of kinematic viscosity to Saybolt universal viscosity or to Saybolt

Furol viscosity

D 2265 Standard test method for dropping point of lubricating grease over wide temperature range

D 2266 Standard test method for wear preventive characteristics of lubricating grease (four-ball method)

D 2270 Standard test method for standard practice for calculating viscosity index from kinematic viscosity at

40 and 100ºC

D 2272 Standard test method for oxidation stability of steam turbine oils by rotating bomb

D 2273 Standard test method for trace sediment in lubricating oils

D 2500 Standard test method for cloud point of petroleum oils

D 2502 Standard test method for estimation of molecular weight relative molecular mass of petroleum oils

from viscosity calculation

D 2509 Standard test method for measurement of load-carrying capacity of lubricating grease (Timken

method)

D 2512-95 (2002) Standard test method for compatibility of materials with liquid oxygen (impact sensitivity threshold

and pass–fail techniques)

D 2549-02 Standard test method for separation of representative aromatics and nonaromatics fractions of high-

boiling oils by elution chromatography

D 2595 Standard test method for evaporation loss of lubricating greases over wide temperature range

D 2596 Standard test method for measurement of extreme-pressure properties of lubricating grease (four-ball

method)

D 2602 Replaced by D 5293, standard test method for apparent viscosity of engine oils at low temperature

using the cold-cranking simulator

D 2603-01 Test method for sonic shear stability of polymer-containing oils

D 2619-95 (2002)e1 Standard test method for hydrolytic stability of hydraulic  uids (beverage bottle method)

D 2620 Discontinued from 1993, replaced by D 5293

D 2622 Standard test method for sulfur in petroleum products by x-ray spectrometry

D 2625 Standard test method for determining endurance life and load-carrying capacity of dry solid  lm

lubricants (Falex method)

D 2670 Standard test method for measuring wear properties of  uid lubricants (Falex method)

D 2710 Standard test method for bromine index of petroleum hydrocarbons by electrometric titration

D 2711 Standard test method for demulsibility characteristics of lubricating oils

D 2714 Standard test method for calibration and operation of the Falex block-on-ring friction and wear

testing machine

D 2766 Standard test method for speci c heat of liquids and solids

D 2782 Standard test method for measurement of extreme-pressure properties of lubricating  uids (Timken

method)

(continued)

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672 Lubricant Additives: Chemistry and Applications

D 2783 Standard test method for measurement of extreme-pressure properties of lubricating  uids (four-ball

method) (load wear index)

D 2786-91 (2001)e1 Standard test method for hydrocarbon types analysis of gas–oil saturates fractions by high ionizing

voltage mass spectrometry

D 2878 Standard test method for estimating apparent vapor pressure and molecular weights of lubricating oils

D 2879 Standard test method for vapor pressure–temperature relationship and initial decomposition

temperature of liquids by isoteniscope

D 2887 Standard test method for boiling range distribution of petroleum fractions by gas chromatography

D 2893 Standard test method for oxidation characteristics of extreme-pressure lubricating oils

D 2896 Standard test method for base number of petroleum products by potentiometric perchloric acid

titration

D 2982 Standard test method for detecting glycol-base antifreeze in used lubricating oil

D 2983 Standard test method for low-temperature viscosity of automotive  uid lubricants measured by

Brook eld viscometer

D 3120 Standard test method for trace quantities of sulfur in light liquid petroleum hydrocarbons by

oxidative microcoulometry

D 3228 Standard test method for total nitrogen in lubricating oils and fuel oils by modi ed Kjeldahl method

D 3232 Standard test method for measurement of consistency of lubricating greases at high temperatures

D 3233 Standard test method for measurement of extreme pressure of  uid lubricants (Falex method)

D 3238 Standard test method for carbon distribution and structural group analysis of petroleum oils by the

ndM method

D 3244 Standard test method for standard practice for utilization of test data to determine conformance with

speci cations

D 3336 Standard test method for life of lubricating greases in ball bearings at elevated temperatures

D 3427-03 Standard test method for air release properties of petroleum oils

D 3525 Standard test method for gasoline diluent in used gasoline engine oils by gas chromatography

D 3527 Standard test method for life performance of automotive wheel bearing grease

D 3704 Standard test method for wear preventative properties of lubricating grease using the (Falex) block

on ring test machine in oscillating motion

D 3705 Standard test method for misting properties of lubricating  uids

D 3711 Standard test method for deposition tendencies of liquids in thin  lms

D 3829 Standard test method for predicting the borderline pumping temperature of engine oil

D 3850-94 (2000) Standard test method for rapid thermal degradation of solid electrical insulating materials by

thermogravimetric method (TGA)

D 3945 Standard test method for shear stability of polymer-containing  uids using diesel injector nozzle

(deactivated 1998, replaced by D6278)

D 4047 Standard test method for phosphorus in lubricating oils and additives by quinoline

phosphomolybdate method

D 4048 Standard test method for detection of copper corrosion from lubricating greases

D 4049 Standard test method for determining the resistance of lubricating grease of water spray

D 4057 Standard test method for standard practice for manual sampling of petroleum and petroleum products

D 4172 Standard test method for wear preventive characteristics of lubricating  uid (four-ball method)

D 4294 Standard test method for sulfur in petroleum products by energy-dispersive x-ray  uorescence

spectroscopy

D 4310 Standard test method for determination of the sludging and corrosion tendencies of the inhibited

mineral oils

D 4485 Standard test method for standard speci cation performance of automotive engine oils

D 4624 Standard test method for measuring apparent viscosity by capillary viscometer at high temperature

and high shear rates

D 4627 Standard test method for iron chip corrosion for water-diluteable metalworking  uids

D 4628 Standard test method for analysis of barium, calcium, magnesium, and zinc in unused lubricating oils

by atomic absorption spectrometry

D 4629 Standard test method for trace nitrogen in liquid petroleum hydrocarbons by syringe/inlet oxidative

combustion and chemiluminescence detection

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Testing Methods for Additive/Lubricant Performance 673

D 4636 Standard test method for corrosion and oxidative stability of hydraulic oils, aircraft turbine engine

lubricants, and other highly re ned oils

D 4683 Standard test method for measuring viscosity at high shear rate and high temperature by tapered

bearing simulator

D 4684 Standard test method for determination of yield stress and apparent viscosity of engine oils at low

temperature (MRV TP-1 cycle)

D 4693 Standard test method for low-temperature torque of grease-lubricated wheel bearings

D 4739 Standard test method for base number determination by potentiometric titration

D 4741 Standard test method for measuring viscosity at high temperature and high shear rate by tapered plug

viscometer

D 4742 Standard test method for oxidation stability of gasoline automotive engine oils by thin- lm oxygen

uptake (TFOUT)

D 4781-03 Standard test method for mechanically tapped packing density of  ne catalyst particles and catalyst

carrier particles

D 4857 Standard test method for determination of coef cient of friction of lubricants using the four-ball wear

test machine

D 4871-88 Standard guide for universal oxidation/thermal stability test apparatus

D 4898 Standard test method for insoluble contamination of hydraulic  uids by gravimetric analysis

D 4927 Standard test method for elemental analysis of lubricant and additive components, barium, calcium,

phosphorus, sulfur, and zinc, by wavelength-dispersive x-ray  uorescence spectroscopy

D 4950 Standard classi cation and speci cation for automotive service greases

D 4951 Standard test method for determination of additive elements in lubricating oils by inductively

coupled plasma atomic emission spectrometry

D 5119 Standard test method for evaluation of automotive engine oils in CRC l-38

spark ignition engine

D 5133 Standard test method for low temperature, low shear rate, viscosity/temperature dependence of

lubricating oils using a temperature-scanning technique (scanning Brook eld test with gelation

index calculation)

D 5182 Standard test method for evaluating the scuf ng load capacity of oils (FZG visual method)

D 5183 Standard test method for evaluating coef cient of friction of lubricants using the four-ball wear test

machine

D 5185 Standard test method for determination of additive elements, wear metals, and contaminants in used

lubricating oils and determination of selected elements in base oils by inductively coupled plasma

atomic emission spectrometry (ICP-AES)

D 5293 Standard test method for apparent viscosity of engine oils between −5 and −30ºC using the cold-

cranking simulator

D 5302 Standard test method for evaluation of automotive engine oils in the Sequence VE spark ignition

engine

D 5306-92 (2002)e1 Standard test method for linear  ame propagation rate of lubricating oils and hydraulic  uids

D 5480 Standard test method for engine oil volatility by gas chromatography

D 5483 Standard test method for oxidation induction time of lubricating greases by pressure differential

scanning calorimetry

D 5533 Standard test method for evaluation of automotive engine oils in the Sequence IIIE spark ignition

engine

D 5570 Standard test method for evaluating the thermal stability of manual transmission lubricants in a cycle

durability test

D 5620 Standard test method for evaluating thin- lm lubricants in a drain and dry mode using Falex pin and

Vee block test machine

D 5621 Standard test method for sonic shear stability of hydraulic  uids

D 5704 Standard test method for evaluation of thermal and oxidative stability of lubricating oils used for

manual transmissions and  nal drive axles

D 5706 Standard test method for determining extreme-pressure properties of lubricating greases using a

high-frequency, linear-oscillating (SRV) test machine

(continued)

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