1、Designation: D 128 98 (Reapproved 2003)e1An American National StandardStandard Test Methods forAnalysis of Lubricating Grease1This standard is issued under the fixed designation D 128; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.e1NOTEWarning notes were editorial
3、ly moved into the standard text in July 2003.1. Scope1.1 These test methods for analysis cover greases of theconventional type, which consist essentially of petroleum oiland soap. The constituents that can be determined are soap,unsaponifiable matter (petroleum oil, and so forth), water, freealkalin
4、ity, free fatty acid, fat, glycerin, and insolubles.NOTE 1Any of the test methods described herein are best used by anexperienced grease analyst who may also be able to make appropriateadaptations of the techniques as occasion requires.1.2 A supplementary test method is provided in AppendixX1. This
5、test method is intended primarily for application togreases containing thickeners that are essentially insoluble inn-hexane, and to greases that cannot be analyzed by conven-tional methods because of the presence of such constituents asnonpetroleum fluids or nonsoap-type thickeners, or both. Insome
6、cases, these constituents can react with strong acid oralkaline solutions.1.3 These test methods appear in the following order:SectionsAsh Determination 7-11Insolubles, Soap, Fat, Petroleum Oil,and Unsaponifiable Matter12-20Free Alkali and Free Acid 21-23Water 24Glycerin (Quantitative) 25-291.4 This
7、 standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices, and determine the applica-bility of regulatory limitations prior to use.1.5 The values stated
8、in SI units are to be regarded as thestandard.2. Referenced Documents2.1 ASTM Standards:D 95 Test Method for Water in Petroleum Products andBituminous Materials by Distillation2D 156 Test Method for Saybolt Color of Petroleum Prod-ucts (Saybolt Chromometer Method)2D 217 Test Methods for Cone Penetra
9、tion of LubricatingGrease2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (the Calculation of Dynamic Viscos-ity)2D 473 Test Method for Sediment in Crude Oils and FuelOils by the Extraction Method2D 1078 Test Method for Distillation Range of VolatileOrganic Liquids3D 1193
10、Specification for Reagent Water4D 1353 Test Method for Nonvolatile Matter in VolatileSolvents for Use in Paint, Varnish, Lacquer, and RelatedProducts33. Terminology3.1 Definitions:3.1.1 asphalt, na dark brown-to-black cementitious ma-terial in which the predominating constituents are bitumens.3.1.1.
11、1 DiscussionAsphalt can be a natural product or amaterial obtained from petroleum processing.3.1.2 candle pitch, na dark brown-to-black, tarry or solid,by-product residue from soap and candle stock manufacture,refining of vegetable oils, refining of wool grease, or refining ofrefuse animal fats.3.1.
12、3 cup grease, nany lubricating grease having physicalproperties, such as consistency and texture, suitable for its usein spring-loaded or screw-type lubricating cups.3.1.3.1 DiscussionCup greases are predominantly NLGINo. 3 or 4 calcium greases, but grease types other than calciumare also used.3.1.4
13、 degras (wool fat, wool grease, wool wax), nafat-like material comprised primarily of sterols, other higheralcohols, and fatty acids, obtained from the solvent extractionof sheeps wool.1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and are th
14、e direct responsibility of Subcommit-tee D02.G0 on Lubricating Grease.Current edition approved May 10, 2003. Published July 2003. Originallyapproved in 1922. Last previous edition approved in 1998 as D 12898.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 06.04.4Annual
15、Book of ASTM Standards, Vol 11.01.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.5 free alkali, nin lubricating grease, unreacted basic(alkaline) material present in the product.3.1.5.1 DiscussionMany greases are made with a sli
16、ghtexcess of alkali to ensure complete saponification. Free alkaliis determined by acidification of a solvent-thinned specimenand back titration with standardized, alcoholic potassiumhydroxide. It is expressed in terms of the predominating alkaliand a mass % of the total grease composition (for exam
17、ple,mass % lithium hydroxide).3.1.6 free fatty acid, nin lubricating grease, unreactedcarboxylic acid(s) present in the product.3.1.6.1 DiscussionSome greases are made with a slightexcess of carboxylic acid to ensure a non-alkaline product.Free fatty acid is determined by neutralization of a solvent
18、-thinned specimen with standardized, alcoholic potassium hy-droxide. Regardless of the actual composition of the carboxylicacid(s), it is expressed as free oleic acid and as a mass % of thetotal grease composition.3.1.7 insolubles, nin lubricating greases analysis, thematerial remaining after the ac
19、id hydrolysis, water extraction,and solvent extraction of soap-thickened greases.3.1.7.1 DiscussionConsisting of such products as graph-ite, molybdenum disulfide, insoluble polymers, and so forth.3.1.8 lubricating grease, na semi-fluid to solid product ofa dispersion of a thickener in a liquid lubri
20、cant.3.1.8.1 DiscussionThe qualifying term, lubricating,should always be used. The term, grease, used without thequalifier refers to a different product, namely certain natural orprocessed animal fats, such as tallow, lard, and so forth.3.1.9 mixed base, adjin lubricating grease, the descriptionof a
21、 thickener system composed of soaps of two metals.3.1.9.1 DiscussionAlthough mixed-base grease can bemade with soaps of more than two metals, in practice, such israrely, if ever, encountered. All of the soaps need not bethickeners, although the major soap constituent will be onecapable of forming a
22、lubricating grease structure. Because themixed soaps are seldom present in equal amounts. The pre-dominant soap is referred to first.NLGI Lubricating Grease Guide53.1.10 montan wax, na wax-like material comprised pri-marily of montanic acid and its ester, higher aliphatic alcohols,and resins obtaine
23、d from the solvent extraction of lignite.3.1.11 neutralization number, nof petroleum oil, thequantity of acid or base required to titrate to neutrality andexpressed as equivalent milligrams of potassium hydroxide pergram of sample. D 8043.1.12 NLGI, nNational Lubricating Grease Institute.3.1.13 NLGI
24、 number, na numerical scale for classifyingthe consistency range of lubricating greases and based on theTest Methods D 217 worked penetration.NLGI Lubricating Grease Guide3.1.14 non-soap thickener (synthetic thickener, inorganicthickener, organic thickener), nin lubricating grease, any ofseveral spe
25、cially treated or synthetic materials, exceptingmetallic soaps, that can be thermally or mechanically dispersedin liquid lubricants to form the lubricating grease structure.NLGI Lubricating Grease Guide3.1.15 residuum, na liquid or semi-liquid product ob-tained as residue from the distillation of pe
26、troleum andconsisting primarily of asphaltic hydrocarbons.3.1.15.1 DiscussionAlso known as asphaltic oil, asphal-tum oil, liquid asphalt, black oil, petroleum tailings, andresidual oil.3.1.16 rosin oil, na viscous, oily liquid obtained as acondensate when the residue (rosin) from turpentine produc-t
27、ion is subjected to dry, destructive distillation.3.1.16.1 DiscussionAlso used to describe specially com-pounded oils having a rosin base.3.1.17 saponification, nthe interaction of fats, fatty acids,or esters generally with an alkali to form the metallic salt,which is commonly called soap.3.1.17.1 D
28、iscussionSoap thickeners are most often madeby in situ saponification in the lubricating grease base oil.However, the use of pre-formed soaps is also common;dispersion is effected by mechanical means and usually withheat. NLGI Lubricating Grease Guide3.1.18 single base, adj in lubricating grease, re
29、lating to athickener comprised of soaps of only one metal.3.1.19 soap, nin lubricating grease, a product formed inthe saponification (neutralization) of fats, fatty acids, or estersby inorganic bases.3.1.20 Soxhlet apparatus, na device, usually of glass,used to extract soluble material from a mixtur
30、e of soluble andinsoluble (generally solid) materials, by passing a volatilesolvent through the sample and recirculating the solvent byrefluxing.3.1.21 tar, na brown or black, bituminous, liquid orsemi-solid comprised primarily of bitumens condensed in theprocessing of coal, petroleum, oil-shale, wo
31、od, or other organicmaterials.3.1.22 thickener, nin lubricating grease, a substancecomposed of finely divided solid particles dispersed in a liquidlubricant to form the products structure.3.1.22.1 DiscussionThe thickener can be fibers (such asvarious metallic soaps) or plates or spheres (such as cer
32、tainnon-soap thickeners), which are insoluble or, at most, only veryslightly soluble in the liquid lubricant. The general require-ments are that the solid particles be extremely small, uniformlydispersed, and capable of forming a relatively stable, gel-likestructure with the liquid lubricant. D 2173
33、.1.23 thimble, nin Soxhlet apparatus, a closed-end po-rous cylinder used to hold the material to be extracted, usuallymade of thick matted filter paper but sometimes made ofceramic.3.1.24 total fluid constituent, nin lubricating greaseanalysis, the n-hexane-soluble material extracted from thelubrica
34、ting grease sample.3.1.24.1 DiscussionTypical materials include petroleumoil, non-petroleum fluid, soluble fats, and soluble additives.3.1.25 total n-hexane-insoluble material, nin lubricatinggrease analysis, that portion of grease (excluding free alkali)that is essentially insoluble in n-hexane.5Av
35、ailable from National Lubricating Grease Institute, 4635 Wyandotte St.,Kansas City, MO 64112-1596.D 128 98 (2003)e123.1.25.1 DiscussionTypical materials include thickeners,fillers, inorganic salts, asphaltenes, or any combinations ofthese (also includes insoluble materials found in the analysis ofco
36、ntaminated grease). Free alkali content is generally insignifi-cant.3.1.26 unsaponifiable matter, nin lubricating grease, or-ganic materials, either added or found with fatty materials,which do not react during saponification.4. Significance and Use4.1 These test methods can be used to identify and
37、estimatethe amount of some of the constituents of lubricating greases.These test methods are applicable to many, but not all, greases.4.2 Composition should not be considered as having anydirect bearing on service performance unless such correlationis established.NOTE 2Details on other test methods
38、for grease analysis can be foundin other reference material.6,7,85. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the America
39、n Chemical Society,where such specifications are available.9Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water
40、shall be understood to mean reagent water conformingto Specification D 1193, Type III.5.3 AcetoneAmerican Chemical Society Reagent GradeAcetone. (WarningExtremely flammable. Vapors may causeflash fires.)5.4 Alcohol (50 %)The alcohol shall be prepared fromcommercial 95 % ethanol or denatured alcohol1
41、0,11(WarningFlammable. Denatured. Cannot be made non-toxic) by distilling from NaOH and neutralizing exactly withNaOH or KOH using phenolphthalein as the indicator.(WarningIn addition to other precautions, avoid skin con-tact or ingestion.) Dilute with an equal volume of water.5.5 Ammonium Carbonate
42、(NH4)2CO3.(WarningHarmful if swallowed.) (WarningHarmful if swallowed.)5.6 Butter Yellow Indicator (0.02 g/mL)Toluene solution(WarningFlammable. Vapor harmful) ofp-dimethylaminoazobenzene. (WarningSuspected carcino-gen. In addition to other precautions, avoid inhalation or skincontact.)5.7 t-Butyl A
43、lcohol, melting point 24 to 25.5C (WarningFlammable liquid; causes eye burns).5.8 Carbon Disulfide (CS2). (WarningExtremely flam-mable. Poison. Vapor may cause flash fire. Vapor harmful.Capable of self-ignition at 100C or above. Harmful or fatal ifswallowed. May be absorbed through the skin.)5.9 Eth
44、yl Ether.(WarningExtremely flammable. Harm-ful if inhaled. May cause eye injury. Effects may be delayed.May form explosive peroxides. Vapors may cause flash fire.Moderately toxic. Irritating to skin.)5.10 n-hexane, high-purity grade,11,12conforming to therequirements of Table 1. (WarningExtremely fl
45、ammable.Harmful if inhaled. May produce nerve cell damage. Vaporsmay cause flash fire.)5.11 Hydrochloric Acid (37 %)Concentrated acid (HCl).(WarningPoison. Corrosive. May be fatal if swallowed.Liquid and vapor cause severe burns. Harmful if inhaled.)5.12 Hydrochloric Acid, Standard Solution (0.5 N)P
46、repare and standardize a 0.5 N solution of HCl.5.13 Hydrochloric Acid (10 %), a solution containing 10 %by weight of concentrated HCl in water, with a permissiblevariation of 0.5 %.5.14 Hydrochloric Acid (1 + 3)Mix one volume of con-centrated HCl (37 %) with three volumes of water.5.15 Methyl Red In
47、dicator Solution.(WarningFlammable. Avoid skin contact or ingestion.)5.16 Nitric Acid (1 + 4)Mix one volume of concentratednitric acid (70 %) (WarningPoison. Corrosive. Strong oxi-dizer. Contact with organic material may cause fire. May beharmful if swallowed. Liquid and vapor cause severe burns)wit
48、h four volumes of water.5.17 Phenolphthalein Indicator SolutionThe phenol-phthalein solution shall be prepared by dissolving 1.0 gphenolphthalein (WarningIn addition to other precautions,6Stanton, G. M., “Examination of Grease by Infrared Spectroscopy,” NLGISpokesman, Vol 38, No. 5, August 1974, pp
49、153165.7Stanton, G. M., “Grease Analysis, a Modern Multitechnique Approach,”Preprint NLGI Annual Meeting, Oct 2629, 1975.8Bonomo, F. S., and Schmidt, J. J. E., “Development of Schematic AnalyticalProcedures for Synthetic Lubricants and Their Additives,” WADC Technical Report54-464, Part IV, July 1957 (U.S. Government No. AD-130922).9Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Soc
