1、Designation: D 2619 95 (Reapproved 2002)e1An American National StandardStandard Test Method forHydrolytic Stability of Hydraulic Fluids (Beverage BottleMethod)1This standard is issued under the fixed designation D 2619; the number immediately following the designation indicates the year oforiginal a
2、doption or, in the case of revision, 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.e1NOTEWarning notes were placed in the text editorially in May 2002.1. Scope1.1
3、This test method2covers the determination of thehydrolytic stability of petroleum or synthetic-base hydraulicfluids.NOTE 1Water-base or water-emulsion fluids can be evaluated by thistest method but are run “as is.” Additional water is not added to the 100-gsample.1.2 The values stated in SI units ar
4、e to be regarded as thestandard. The inch-pound units given in parentheses areprovided for 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
5、and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in 3.1, 6.1, 6.3, 6.4, and Annex A1.2. Referenced Documents2.1 ASTM Standards:D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and the Calculat
6、ion of DynamicViscosity)3D 974 Test Method for Acid and Base Number by Color-Indicator Titration33. Summary of Test Method3.1 The sample of 75 g of fluid plus 25 g of water and acopper test specimen are sealed in a pressure-type beveragebottle. The bottle is rotated, end for end, for 48 h in an oven
7、 at93C (200F). Layers are separated, and insolubles areweighed. Weight change of copper is measured. Viscosity andacid number changes of fluid and acidity of water layer aredetermined. (WarningIn addition to other precautions, be-cause this test method involves the use of a glass bottle thatmay cont
8、ain approximately 200 kPa (2 atm) of air and watervapor at temperatures up to 93C, a full face shield and heavywoven fabric gloves should be worn when handling or workingwith the heated and sealed sample container.)4. Significance and Use4.1 This method differentiates the relative stability of hy-dr
9、aulic fluids in the presence of water under the conditions ofthe 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 t
10、histest and service performance has not been fully determined.5. Apparatus5.1 Air Oven, convection, adjusted to 93 6 0.5C (200 61F).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 rpm in oven.
11、5.5 Centrifuge, 1500 rpm.5.6 Centrifuge Tubes, cone-shaped, 100-mL.5.7 Filtration Assembly,6stainless screen/glass, membranetype 47-mm diameter.5.8 Typewriter Brush.5.9 Separatory Funnel, 125-mL.5.10 Microscope, for 203 magnification.5.11 Balance, sensitive to 0.2 mg.5.12 Caps, for sealing bottles.1
12、This 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 Jan. 15, 1995. Published March 1995. Originallypublished as D 2619 67. Last previous edition D
13、2619 88 (1994)e1.2This test method is a modification of Federal Test Method Standard No. 791a,Method 3457 for Hydrolytic Stability.3Annual Book of ASTM Standards, Vol 05.01.4An acceptable commercial unit is available from Falex Corp. 1020 Airpark Dr.,Sugar Grove, IL 60554.5A 200-mL (7-oz) glass Coca
14、 Cola trademarked bottle has proven satisfactory.Bottles can be obtained from beverage distributors.6A Millipore XX10 047 30 or equivalent has proven satisfactory.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.13 Inert Seal,7for c
15、ap gasket.5.14 Membrane Type Filter,8cellulosic, 5-m porosity,47-mm diameter.6. Reagents and Materials6.1 n-Heptane.(WarningFlammable, 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 a
16、queous solutionstandardized to within 0.0005 N.(WarningCaustic.)6.4 1,1,1-Trichloroethane.(WarningHarmful if inhaled,high concentrations may cause unconsciousness or death;contact may cause skin irritations and dermatitis, may producetoxic vapors if burned, eye irritant; see A1.2.)6.5 Copper Strip (
17、QQ-C-576A), 16-22 B and S gage, 13 by51 mm.6.6 Steel Wool, grade 1-medium fine.6.7 Litmus Paper.7. Procedure7.1 Fill the pressure beverage bottle with distilled water andallow to stand overnight. Drain and rinse, with distilled water,but do not dry.7.2 Weigh 75 g of test fluid and 25 g of distilled
18、water to 0.5g into the beverage bottle.7.3 Polish the copper test specimen to 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 test fluids in the beverage bottle. Avoidspecimen contact by handling the
19、cleaned copper test strip withcotton gloves or filter paper.7.4 Prepare a disk of the inert seal6and place in a new bottlecap. Seal the bottle using the cap with the gasket.7.5 Place the bottle in the rotating mechanism in the ovenadjusted to 93 6 0.5C (200 6 1F). Allow to rotate, end forend, at 5 r
20、pm for 48 h.7.6 Remove the bottle and place on an insulated surfaceuntil cool.7.7 Open the bottle, empty the contents into a 100-mL,cone-shaped centrifuge tube, and centrifuge for 10 min at 1500rpm. Decant the separated water and emulsion layers and setaside. (A pipet can be used as an alternative m
21、ethod to removethe water layer without centrifuging, provided a clear waterseparation results by sample settling.)7.8 Filter the fluid oil layer through a membrane filterweighed to 0.2 mg. Transfer the fluid layer to a 125-mLseparatory funnel. Rinse the filter flask with 25 mL of distilledwater and
22、add to the separatory funnel. Repeat the waterwashes of the oil in the separatory funnel until the washings areneutral to litmus. Save the combined water washings (Note 2).Dry the filtered, washed fluid by vacuum dehydration when incontact with anhydrous sodium sulfate (Note 3). Filter the fluidthro
23、ugh filter paper to remove the sodium sulfate solids.NOTE 2If the fluid sample is heavier than water, drain the fluid fromthe separatory funnel, remove the water wash, and return the fluid to theseparatory funnel for repeated water washes.NOTE 3Mechanical stirring for 1 h with the anhydrous sodium s
24、ulfatedries the fluid efficiently. This is done prior to vacuum dehydration.7.9 Determine the viscosity of the filtered fluid in accor-dance with Test Method D 445. Compare the result withviscosity of the original fluid sample and calculate the percent-age viscosity change at 40C (104F).7.10 Determi
25、ne the total acid number of the filtered fluid inaccordance with Test Method D 974. Acidity for the filteredfluid is compared to that of the original fluid and the acidnumber change recorded.7.11 Filter the water phase and the emulsion layer (whichusually contains the bulk of the insoluble material)
26、 through themembrane filter. Rinse the copper test specimen, pipet, centri-fuge tube, beaker, and beverage bottle with distilled water andn-heptane. Filter these washes through the membrane. Segre-gate the water wash. Then wash with 50 mL of n-heptane. Drythe membrane in a 60C (140F) oven and weigh.
27、 Calculate thepercentage of insolubles in the 75-g sample.7.12 Combine all the water portion and washes. Determinetotal acidity by adding 1.0 mL of phenolphthalein solution andtitrating rapidly with 0.1 N KOH solution to the appearance ofpink phenolphthalein end point which persists for 15 s.Calcula
28、te the water layer acidity as follows:Total Acidity, mg KOH 5 A 2 B!N 3 56.1 (1)where:A = millilitres of KOH solution required for titration of thesample,B = millilitres of KOH solution required for titration of theblank, andN = normality of KOH solution.7.13 Wash the copper specimen with warm n-hep
29、tane,followed by warm 1,1,1-trichloroethane. (WarningSee 6.4.)Brush with a short bristled typewriter-type brush while wash-ing in both solvents. Dry and weigh and examine under a 203microscope. Report appearance and weight loss in milligramsper square centimetre.8. Report8.1 The report shall include
30、 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,8.1.3 Weight change of copper strip in milligrams persquare centimetre, and8.1.4 Appearance of strip under 203 magnification.9. Precision and Bias9.1 The precision as deter
31、mined by statistical examinationof interlaboratory result is as follows:9.1.1 RepeatabilityThe difference between two test re-sults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and correct ope
32、ration ofthe test method, exceed the values given in Table 1 in only onecase in twenty, where:7A 0.127-mm (0.005-in.) thick fluorocarbon seal has proven satisfactory.8A Millipore SMWP 04700 or (5.0-m porosity) or equivalent has provensatisfactory. If there is a test fluid filter material incompatibi
33、lity a fluorocarbonmembrane may be used. A Millipore FSLW 04700 (3.0-m or equivalent porosity)has proven satisfactory for example with phosphate ester fluids.D 2619 95 (2002)e12X55 the average of the two test results9.1.2 ReproducibilityThe difference between two singleand independent results obtain
34、ed by different operators work-ing in different laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the values given in Table 1 in only one case intwenty, where:X55 the average of the two test resultsNOTE 4These data are based
35、on the use of a 200-mL (7-oz) glassbottle5at 93C (200F).NOTE 5The precision data were derived from cooperative testing byten laboratories on five reference fluids using the proposed hydrolyticstability test method. These reference fluids included four petroleum basedfluids (regular, ashless, antiwea
36、r and multipurpose) and one phosphateester. The data used to obtain Table 1 are available from ASTMInternational Headquarters and may be obtained by requesting RR:D02-1154.9.2 BiasNo statement on bias is possible, because there isno absolute value. The results are interpretable only withrespect to t
37、his test.10. Keywords10.1 beverage bottle; copper corrosion; hydraulic fluid;hydrolytic stabilityANNEX(Mandatory Information)A1. PRECAUTIONARY STATEMENTSA1.1 n-HeptaneKeep away from heat, sparks, and open flame.Keep container closed.Use with adequate ventilation.Avoid prolonged breathing of vapor or
38、 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 de
39、ath.Avoid prolonged or repeated contact with skin.Do not get in eyes.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of an
40、y such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are i
41、nvited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not receiv
42、ed a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of
43、this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE 1 Recommended Precision Quantities fromInterlaboratory Study of Hydrolytic Stability Test MethodPropertyRepeatability,rReproduci-bility, RCopper corrosion, mg/cm20.3X5 A0.9 X5Acid number change, mg KOH/g oil0.8 X51.9X5Total acidity of water layer, mg KOH0.8X51.3 X5AX5denotes mean value.D 2619 95 (2002)e13
