1、Designation: D2619 09 (Reapproved 2014)Standard 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 revisi
2、on, the year of last 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 h
3、ydraulicfluids.NOTE 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
4、SI units are to be 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
5、 safety and health 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 Petro-leum Products by Copper Str
6、ip TestD974 Test Method 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 i
7、n an oven at 93 C (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 otherprecautions, because this test method involves the use of aglass bottle that may conta
8、in approximately 200 kPa (2 atm) ofair and water vapor at temperatures up to 93 C, a full faceshield and heavy woven fabric gloves should be worn whenhandling or working with the heated and sealed samplecontainer.)4. Significance and Use4.1 This test method differentiates the relative stability ofhy
9、draulic fluids 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
10、 thistest method 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/
11、min in oven.5.5 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.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsan
12、d is the direct responsibility ofSubcommittee D02.N0.08 on Thermal Stability.Current edition approved Oct. 1, 2014. Published November 2014. Originallyapproved in 1967. Last previous edition approved in 2009 as D2619 09. DOI:10.1520/D2619-09R14.2This test method is a modification of Federal Test Met
13、hod Standard No. 791a,Method 3457 for Hydrolytic Stability.3For referenced ASTM standards, visit the ASTM website, 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.4T
14、he sole source of supply of the apparatus known to the committee at this timeis Falex Corp. 1020 Airpark Dr., 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 meet
15、ing of theresponsible technical committee,1which you may attend.5Bottles can be obtained from beverage distributors.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.11 Inert Seal, for cap gasket, 0.127-mm (0.005-in.) thickfluorocarbo
16、n seal.6. Reagents and Materials6.1 n-Heptane. (Warning Flammable, harmful if inhaled,skin irritant on repeated contact, aspiration hazard; see A1.1.)6.2 Phenolphthalein, 1 % alcoholic solution.6.3 Potassium Hydroxide (KOH), 0.1 N aqueous solutionstandardized to within 0.0005 N.(WarningCaustic.)6.4
17、Copper Strip (QQ-C-576A), 16-22 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 co
18、ncentrations may cause unconsciousness 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,
19、 but do not dry.7.2 Determine 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 t
20、o a clean surface withthe steel 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
21、the inert seal and place in 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.
22、7.8 Open the bottle and decant 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 thec
23、ombined water washings. Dry 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
24、other fluids may emulsify withwater 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
25、, remove the water wash,and 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 to
26、tal acid number of the filtered 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 com
27、bined waterwashes and then 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
28、solution to theappearance of a pink phenolphthalein end point which persistsfor 15 s. Calculate the water layer acidity as follows:Total Acidity, mg KOH 5 A 2 B!N# 356,100 mg/Eq1 L/1000 mL!(1)where:A = millilitres of KOH solution required for titration of thesample,B = millilitres of KOH solution re
29、quired for titration of 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 p
30、er square centimetre and appearance asdetermined using the ASTM Copper Strip Corrosion Standard,following the interpretation guidelines in Test Method D130,Section 11.F 5 C 2 D!/E (2)where:C = final weight of copper specimen, mg,D = initial weight of copper specimen, mg,E = surface area of copper sp
31、ecimen, cm2, andF = weight 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
32、.3 Weight change of copper strip in milligrams persquare centimetre, and8.1.4 Appearance of strip as per the instructions in TestMethod D130.D2619 09 (2014)29. Precision and Bias69.1 The precision of this test method is based on aninterlaboratory study of D2619-95 (Note 4), Standard TestMethod for H
33、ydrolytic Stability of Hydraulic Fluids, 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 strip( Cu, mg/cm2), five laboratories obtained two replicate testresults
34、from each of two operators for every material, whileone laboratory obtained just two replicate test results (from oneoperator) for each material. For TAN, four laboratoriesobtained two replicate test results from each of two operatorsfor every material, while one laboratory obtained just tworeplicat
35、e 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 of the participating labs routinely test phosphate esters, and as aresult used only n-heptane for cl
36、eaning the strips in this study.Furthermore, none of the round robin test fluids was phosphate ester-based. Therefore, this precision statement cannot necessarily be extrapo-lated to phosphate ester fluids or to procedures using 1,1,1-trichloroethanesolvent.NOTE 5The data used to generate Tables 1-3
37、 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 they differ by morethan the “r” value for that material; “r” is the intervalrepresenting the critical di
38、fference 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 judged notequivalent if they differ by more than the “R” value for thatmaterial; “R” is the interval rep
39、resenting 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 these two state-ments would have an approximate 95% probability of beingcorrect.9.2 BiasAt the time of t
40、he 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 through statis-tical examination of 310 results, from six laboratories, on fivematerials. These five fluids
41、 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 oilFluid 4 A failing zinc dithiophosphate-containing formulation in mineral oilFluid 5 A passing zinc d
42、ithiophosphate-containing formulation in syntheticbase oils (poly-alpha-olefin and complex ester)6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1676.TABLE 1 (delta) Cu (mg/cm2)FluidAverage, XRepeatabilityStandard Deviation,
43、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 0.0193 0.0441 0.0540TABLE 2 H2O Acidity (mg KOH)FluidAverage
44、,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 0.5146 0.9190 1.44095 0.6533 0.2929 0.4413 0.8202 1.2355TABL
45、E 3 (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 0.1403 0.1403 0.3927 0.39274 0.5155 0.0904 0.1095 0.2530 0.3066
46、5 0.0220 0.0479 0.0639 0.1342 0.1788D2619 09 (2014)39.3.1 To judge the equivalency of two test results, it isrecommended to choose the fluid closest in characteristics tothe test fluid.9.4 The precision statement from the 1995 round robin isincluded in Appendix X1. Also included is a comparison ofth
47、ose results with the latest precision statement.10. Keywords10.1 beverage bottle; copper corrosion; hydraulic fluid;hydrolytic stabilityANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 n-Heptane A1.1 Keep away from heat, sparks, andopen flame.Keep container closed.Use with adequate ventilation
48、.Avoid prolonged breathing of vapor or spray mist.Avoid prolonged or repeated skin contact.A1.2 1,1,1-Trichloroethane A1.2 Avoid prolonged or re-peated breathing of vapor or spray mist.Use only with adequate ventilation.Eye irritation and dizziness are indications of overexposure.Do not take interna
49、lly. Swallowing may cause injury, illnessor 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 sp
