1、Designation: D2619 09Standard Test Method forHydrolytic Stability of Hydraulic Fluids (Beverage BottleMethod)1This standard is issued under the fixed designation D2619; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method2covers the determination of thehydrolytic stability of petroleum or synthetic-based hydraulicfluids.NOT
3、E 1Water-based or water-emulsion fluids can be evaluated by thistest method, but they are run “as is.” Additional water is not added to the100-g sample. In these cases, the person requesting the test needs to let thetest operator know that water is present.1.2 The values stated in SI units are to be
4、 regarded as thestandard. The English units given in parentheses are providedfor information only.1.3 This 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
5、 practices and determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in 3.1, 6.1, 6.3, 6.9 and Annex A1.2. Referenced Documents2.1 ASTM Standards:3D130 Test Method for Corrosiveness to Copper from Pe-troleum Products by Copper Strip TestD974 Test M
6、ethod for Acid and Base Number by Color-Indicator Titration3. Summary of Test Method3.1 A copper test specimen and 75 g of test fluid plus 25 gof water (or 100 g of a water-containing fluid) are sealed in apressure-type beverage bottle. The bottle is rotated, end forend, for 48 h in an oven at 93 C
7、(200 F). Layers are separatedand the weight change of the copper specimen is measured.The acid number change of the fluid and acidity of the waterlayer are determined. (WarningIn addition to other precau-tions, because this test method involves the use of a glass bottlethat may contain approximately
8、 200 kPa (2 atm) of air andwater vapor at temperatures up to 93 C, a full face shield andheavy woven fabric gloves should be worn when handling orworking with the heated and sealed sample container.)4. Significance and Use4.1 This test method differentiates the relative stability ofhydraulic fluids
9、in the presence of water under the conditionsof the test. Hydrolytically unstable hydraulic fluids form acidicand insoluble contaminants which can cause hydraulic systemmalfunctions due to corrosion, valve sticking, or change inviscosity of the fluid. The degree of correlation between thistest metho
10、d and service performance has not been fullydetermined.5. Apparatus5.1 Air Oven, convection, adjusted to 93 6 0.5 C (200 61 F).45.2 Pressure-Type Beverage Bottles,5200-mL (7-oz).5.3 Capping Press, for bottles.5.4 Rotating Mechanism, for holding bottles and rotatingend over end at 5 r/min in oven.5.5
11、 Bchner Funnel and Filter Flask.5.6 Water Aspirator.5.7 Typewriter Brush.5.8 Separatory Funnel, 125-mL.5.9 Balance, sensitive to 0.2 mg.5.10 Caps, for sealing bottles.5.11 Inert Seal, for cap gasket, 0.127-mm (0.005-in.) thickfluorocarbon seal.6. Reagents and Materials6.1 n-Heptane.(WarningFlammable
12、, harmful if inhaled,skin irritant on repeated contact, aspiration hazard; see A1.1.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.N0.08 on Thermal Stability.Current edition approved Dec. 1, 2
13、009. Published February 2010. Originallyapproved in 1967. Last previous edition approved in 2002 as D261995(2002)1.DOI: 10.1520/D2619-09.2This test method is a modification of Federal Test Method Standard No. 791a,Method 3457 for Hydrolytic Stability.3For referenced ASTM standards, visit the ASTM we
14、bsite, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4The sole source of supply of the apparatus known to the committee at this timeis Falex Corp. 1020 Airpark Dr.
15、, Sugar Grove, IL 60554. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.5Bottles can be obtained from beverage distr
16、ibutors.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Phenolphthalein, 1 % alcoholic solution.6.3 Potassium Hydroxide (KOH), 0.1 N aqueous solutionstandardized to within 0.0005 N.(WarningCaustic.)6.4 Copper Strip (QQ-C-576A), 1
17、6-22 B and S gage, 13 by51 mm.6.5 Steel Wool, grade 1-medium fine.6.6 Litmus Paper.6.7 Filter Paper, Whatman No. 41.6.8 Anhydrous Sodium Sulfate (Na2SO4).6.9 1,1,1-Trichloroethane (optionalfor use when the testfluid is a phosphate ester). (WarningHarmful if inhaled,high concentrations may cause unco
18、nsciousness or death;contact may cause skin irritations and dermatitis, may producetoxic vapors if burned, eye irritant; see A1.2.)7. Procedure7.1 Fill the pressure beverage bottle with distilled water andallow to stand overnight. Drain and rinse with fresh distilledwater, but do not dry.7.2 Determi
19、ne the total acid number of the test fluid inaccordance with Test Method D974.7.3 Weigh 75 g of test fluid and 25 g of distilled water (orin the case of water-containing fluids, 100 g of the test fluid) to0.5 g into the beverage bottle.7.4 Polish the copper test specimen to a clean surface withthe s
20、teel wool and wash with n-heptane. (Warningsee 6.1.)Dry and weigh to 0.2 mg. Immediately immerse the copperspecimen in the fluid in the beverage bottle. Avoid specimencontact by handling the cleaned copper test strip with cottongloves or filter paper.7.5 Prepare a disk of the inert seal and place in
21、 a new bottlecap. Seal the bottle using the cap with the gasket.7.6 Place the bottle in the rotating mechanism in the ovenadjusted to 93 6 0.5 C (200 6 1 F). Allow to rotate, end forend, at 5 r/min for 48 h.7.7 Remove the bottle and place on an insulated surfaceuntil cool.7.8 Open the bottle and dec
22、ant the contents (except for thecopper specimen) into a 125 mL separatory funnel. Allow thelayers to separate and remove the aqueous layer (Note 2). Washthe oil layer with 25 mL portions of distilled water, repeatinguntil the washings are neutral to litmus paper. Save thecombined water washings. Dry
23、 the washed fluid with anhy-drous sodium sulfate or by vacuum dehydration (Note 3), orboth. Filter the fluid through filter paper to remove the sodiumsulfate solids.NOTE 2For water-containing fluids, there will be no separation, andso this step should be bypassed. Certain other fluids may emulsify w
24、ithwater and not separate during this step. In either of these cases, nodetermination of water acidity will be conducted and a remark should beinserted into the test report to this effect. If the fluid sample is heavier thanwater, drain the fluid from the separatory funnel, remove the water wash,and
25、 return the fluid to the separatory funnel for repeated water washes.NOTE 3Mechanical stirring for 1 h with the anhydrous sodium sulfatedries the fluid efficiently. Add sufficient sodium sulfate with swirling untilit no longer forms clumps in the fluid.7.9 Determine the total acid number of the filt
26、ered fluid inaccordance with Test Method D974. The acid number of thefiltered fluid is compared to that of the original fluid (deter-mined in 7.2) and the change recorded.7.10 Rinse the copper test specimen and beverage bottlewith distilled water and n-heptane into the combined waterwashes and then
27、return to the separatory funnel. Separate thelayers and wash the aqueous phase with one 50 mL portion ofn-heptane.7.11 Transfer the water layer to an Ehrlenmeyer flask.Determine total acidity by adding 1.0 mL of phenolphthaleinsolution and titrating rapidly with 0.1 N KOH solution to theappearance o
28、f a pink phenolphthalein end point which persistsfor 15 s. Calculate the water layer acidity as follows:Total Acidity, mg KOH 5 A B!N# 3 56,100 mg / Eq1 L / 1000 mL!(1)where:A = millilitres of KOH solution required for titration of thesample,B = millilitres of KOH solution required for titration of
29、theblank, andN = normality of KOH solution.7.12 Wash the copper specimen with warm n-heptane,followed by warm 1,1,1-trichloroethane (if using).(Warningsee 6.9.) Brush with a short bristled typewriter-type brush while washing. Dry and weigh. Report weightchange in milligrams per square centimetre and
30、 appearance asdetermined using the ASTM Copper Strip Corrosion Standard,following the interpretation guidelines in Test Method D130,Section 11.F 5 C D! / E (2)where:C = final weight of copper specimen, mg,D = initial weight of copper specimen, mg,E = surface area of copper specimen, cm2, andF = weig
31、ht change, mg/cm2.8. Report8.1 The report shall include the following:8.1.1 Acid number change of fluid in milligrams of KOHper gram,8.1.2 Total acidity of water in milligrams of KOH, or if thiscould not be determined because no separation occurred, aremark to this effect.8.1.3 Weight change of copp
32、er strip in milligrams persquare centimetre, and8.1.4 Appearance of strip as per the instructions in TestMethod D130.9. Precision and Bias69.1 The precision of this test method is based on aninterlaboratory study of D2619-95 (Note 4), Standard TestMethod for Hydrolytic Stability of Hydraulic Fluids,
33、 con-ducted in 2006. Each of six laboratories tested five differentmaterials. Every “test result” represents an individual determi-nation. For H2O Acidity and weight change of the copper strip6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Researc
34、h Report RR:D02-1676.D2619 092(D Cu, mg/cm2), five laboratories obtained two replicate testresults from each of two operators for every material, whileone laboratory obtained just two replicate test results (from oneoperator) for each material. For D TAN, four laboratoriesobtained two replicate test
35、 results from each of two operatorsfor every material, while one laboratory obtained just tworeplicate test results (from one operator) for each material(Note 5).NOTE 4The purpose of the 1,1,1-trichloroethane solvent is to thor-oughly remove phosphate ester fluids from the copper strips; howevernone
36、 of the participating labs routinely test phosphate esters, and as aresult used only n-heptane for cleaning the strips in this study. Further-more, none of the round robin test fluids was phosphate ester-based.Therefore, this precision statement cannot necessarily be extrapolated tophosphate ester f
37、luids or to procedures using 1,1,1-trichloroethane solvent.NOTE 5The data used to generate Tables 1-3 are available fromASTM International Headquarters and may be obtained by requesting RR:D021676.9.1.1 RepeatabilityTwo test results obtained within onelaboratory shall be judged not equivalent if the
38、y differ by morethan the “r” value for that material; “r” is the intervalrepresenting the critical difference between two test results forthe same material, obtained by the same operator using thesame equipment on the same day in the same laboratory.9.1.2 ReproducibilityTwo test results shall be jud
39、ged notequivalent if they differ by more than the “R” value for thatmaterial; “R” is the interval representing the difference be-tween two test results for the same material, obtained bydifferent operators using different equipment in different labo-ratories.9.1.3 Any judgment in accordance with the
40、se two state-ments would have an approximate 95% probability of beingcorrect.9.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testmethod, therefore no statement on bias is being made.9.3 The precision statement was determined throug
41、h statis-tical examination of 310 results, from six laboratories, on fivematerials. These five fluids were the following:Fluid 1 A passing ashless formulation in mineral oilFluid 2 A passing zinc dithiophosphate-containing formulation in mineral oilFluid 3 A failing ashless formulation in mineral oi
42、lFluid 4 A failing zinc dithiophosphate-containing formulation in mineral oilFluid 5 A passing zinc dithiophosphate-containing formulation in syntheticbase oils (poly-alpha-olefin and complex ester)9.3.1 To judge the equivalency of two test results, it isrecommended to choose the fluid closest in ch
43、aracteristics tothe test fluid.9.4 The precision statement from the 1995 round robin isincluded in Appendix X1. Also included is a comparison ofthose results with the latest precision statement.10. Keywords10.1 beverage bottle; copper corrosion; hydraulic fluid;hydrolytic stabilityTABLE 1 D (delta)
44、Cu (mg/cm2)FluidAverage, DXRepeatabilityStandard Deviation,srReproducibilityStandard Deviation,sRRepeatabilityLimit,rReproducibilityLimit,R1 0.0219 0.0156 0.0180 0.0438 0.05052 0.0742 0.0438 0.0438 0.1226 0.12263 0.5283 0.0748 0.2051 0.2093 0.57414 3.6439 0.6490 0.8274 1.8172 2.31665 0.0161 0.0157 0
45、.0193 0.0441 0.0540TABLE 2 H2O Acidity (mg KOH)FluidAverage,XRepeatabilityStandard Deviation,srReproducibilityStandard Deviation,sRRepeatabilityLimit,rReproducibilityLimit,R1 2.3267 0.5684 1.1103 1.5916 3.10882 0.3458 0.2156 0.4694 0.6038 1.31433 15.2358 1.4479 3.6158 4.0542 10.12444 0.6025 0.3282 0
46、.5146 0.9190 1.44095 0.6533 0.2929 0.4413 0.8202 1.2355TABLE 3 D (delta) TAN (mg KOH/g oil)FluidAverage,XRepeatabilityStandard Deviation,srReproducibilityStandard Deviation,sRRepeatabilityLimit,rReproducibilityLimit,R1 0.0030 0.0750 0.0750 0.2100 0.21002 0.0130 0.0708 0.0895 0.1983 0.25053 0.4460 0.
47、1403 0.1403 0.3927 0.39274 0.5155 0.0904 0.1095 0.2530 0.30665 0.0220 0.0479 0.0639 0.1342 0.1788D2619 093ANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 n-HeptaneKeep away from heat, sparks, and open flame.Keep container closed.Use with adequate ventilation.Avoid prolonged breathing of vapor
48、 or spray mist.Avoid prolonged or repeated skin contact.A1.2 1,1,1-TrichloroethaneAvoid prolonged or repeated breathing of vapor or spraymist.Use only with adequate ventilation.Eye irritation and dizziness are indications of overexposure.Do not take internally. Swallowing may cause injury, illnessor
49、 death.Avoid prolonged or repeated contact with skin.Do not get in eyes.APPENDIX(Nonmandatory Information)X1. REPRODUCIBILITY INFORMATIONX1.1 Precision Statement from D261995 (ConductedUsing 1,1,1Trichloroethylene Solvent)X1.1.1 Table X1.1 shows recommended precision quantitiesfrom interlaboratory study of hydrolytic stability test method.X1.2 Comparison of Precision Statements fromD261995 and D261909X1.2.1 Table X1.2 compares the reproducibility for thechange in the weight of the copper specimen obtained in thecurrent study with those
