1、Designation: D2603 01 (Reapproved 2013)Standard Test Method forSonic Shear Stability of Polymer-Containing Oils1This standard is issued under the fixed designation D2603; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the evaluatio
3、n of the shearstability of an oil containing polymer in terms of the permanentloss in viscosity that results from irradiating a sample of the oilin a sonic oscillator. This test method can be useful inpredicting the continuity of this property in an oil where nochange is made in the base stock or th
4、e polymer. It is notintended that this test method serve to predict the performanceof polymer-containing oils in service.1.2 Evidence has been presented that correlation betweenthe shear degradation results obtained by means of sonicoscillation and those obtained in mechanical devices can bepoor. Th
5、is is especially true in the case of automotive engines.Further evidence indicates that the sonic technique may ratedifferent families of polymers in a different order than me-chanical devices.2,31.3 Because of these limitations, the committee underwhose jurisdiction this test method falls has devel
6、oped analternative shear test method using a diesel injector nozzle, TestMethod D3945. While that test method has found some utilityin the evaluation of crankcase oils, the stress imparted to thesample has been found to be insufficient to shear polymers ofthe shear-resistant type found in aircraft h
7、ydraulic fluids.1.4 This test method is used for polymeric additivespecifications, especially in the hydraulic fluid market.1.5 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are provided forinformational purposes only.1.6 This standard does not purp
8、ort 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.2. Referenced Documents2.1 ASTM Standards:4D44
9、5 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D3945 Test Method for Sheer Stability of Ploymer-Containing Fluids Using a Diesel Injector Nozzle (With-drawn 1998)5D6022 Practice for Calculation of Permanent Shear StabilityIndex3. Summary
10、 of Test Method3.1 A convenient volume of polymer-containing oil is irra-diated in a sonic oscillator for a period of time and the changesin viscosity are determined by Test Method D445. Standardreference fluids containing either a readily sheared or shear-resistant polymer are run frequently to ens
11、ure that the equip-ment imparts a controlled amount of sonic energy to thesample.NOTE 1The conditions to obtain the data for the precision statementwere a 30mL sample, 10 min, and at 0C.4. Significance and Use4.1 This test method permits the evaluation of shear stabilitywith minimum interference fro
12、m thermal and oxidative factorswhich may be present in some applications. Within thelimitations expressed in the scope of this test method, it hasbeen successfully applied to hydraulic fluids, transmissionfluids, tractor fluids, and other fluids of similar applications. Ithas been found applicable t
13、o fluids containing both readilysheared and shear-resistant polymers. Correlation with perfor-mance in the case of automotive engine applications has, todate, not been established.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricantsand is the direct r
14、esponsibility of SubcommitteeD02.07 on High Temperature Rheology of Non-Newtonian Fluids.Current edition approved May 1, 2013. Published August 2013. Originallyapproved in 1967. Last previous edition approved in 2007 as D2603 01 (2007).DOI: 10.1520/D2603-01R13.2The Effects of Polymer Degradation on
15、Flow Properties of Fluids andLubricants, ASTM STP 382,ASTM, 1965.Available fromASTM Headquarters, 100Barr Harbor Drive, West Conshohocken, PA 19428, www.astm.org.3Shear Stability of Multigrade Crankcase Oil, ASTM DS 49, ASTM, 1973.Available from ASTM Headquarters, 100 Barr Harbor Drive, West Conshoh
16、ocken,PA 19428, www.astm.org.4For 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.5The last approved version of th
17、is historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Sonic Shear Unit, fixed frequency oscillator and sonichorn.5.2 Auxiliary EquipmentTo facilitate uniformperformance, th
18、e following auxiliary equipment is recom-mended:5.2.1 Cooling Bath or Ice BathTo maintain a desiredtemperature such as 0C.5.2.2 Griffn 50 mL Beaker, borosilicate glass.5.2.3 Sonic-Insulated BoxTo enclose the sonic horn toreduce the ambient noise level produced by the sonic shearunit.5.3 ViscometerAn
19、y viscometer and bath meeting the re-quirements of Test Method D445.6. Reference Fluids6.1 The primary reference fluid is ASTM Reference FluidA,6a petroleum oil containing a polymer capable of beingbroken down by turbulence at high rates of shear. This oil hasthe following typical properties:Petrole
20、umBaseReferenceFluid AViscosity at 100C, mm2/s (cSt) 5.4 10.8Viscosity at 40C, mm2/s (cSt) 32 586.2 A second reference fluid is ASTM Reference Fluid B,6a petroleum oil containing a polymer capable of being brokendown by turbulence at high rates of shear. This oil has aviscosity of about 13.6 mm2/s (
21、cSt) at 40C.7. Calibration of Apparatus7.1 The reference fluid provides a practical way to definethe performance (severity level) of a sonic oscillator unit sothat satisfactory comparison can be made between tests run ondifferent days in the same unit and between tests run withdifferent units.7.2 Th
22、e decrease in viscosity observed for a given polymer-containing oil on irradiation in an oscillator unit depends on anumber of factors; these include sample volume, irradiationtime, and oscillator power setting. These parameters can bevaried in order to increase or decrease severity of test exposure
23、.Tuning of the oscillator-horn combination is also required inorder to assure efficiency of energy coupling between the twounits. The procedure described in 7.3 and 7.4 is recommendedfor establishing a reproducible performance level for a givenunit.7.3 Introduce 30 mL of a reference fluid into the 5
24、0-mLGriffin beaker. Immerse the beaker in ice water or in anotherconstant temperature bath until sample fluid level is below theliquid level in the bath. The beaker shall be positioned in avertical position in the bath. Secure beaker in this position andcondition the sample for 10 min before commenc
25、ing exposure.Immerse the sonic horn into sample fluid until tip is exactly 10mm below surface of fluid (see Fig. 1). The horn shall bepositioned in a vertical position in the fluid and centered in thebeaker (a weighted ringstand may be used to support the hornin this position). Irradiate the fluid f
26、or 10 min at a preselectedpower setting. Experience has shown that with some instru-ments this may require readjustment of the controls duringirradiation to maintain the preselected power. Determine thedecrease in reference fluid viscosity. Repeat as necessary todetermine the proper power setting to
27、 produce a viscositychange at 40C of 15.0 % (60.5 %). Use this power setting forsubsequent test runs. Daily recalibration of the apparatus isrequired because the power setting required to produce a statedviscosity loss will probably vary from day to day. Experiencewith a given apparatus set will det
28、ermine whether morefrequent calibration is required. Calibration in this manner willassure that repeatable severity levels are established for anypredetermined set of test parameters.7.4 This procedure can be used to establish severity levelsappropriate for the requirements of a variety of applicati
29、ons.Once the conditions for a given severity level have beenestablished, it is possible to compare the shear stability offluids at one or more irradiation times. If calibration at6This fluid can be obtained from Evonik OilAdditives USA, Inc., 723 ElectronicDr., Horsham, PA 19044-2228.FIG. 1 Schemati
30、c of Sonic Probe Type Apparatus, SupportSystems, Cabinet and Power SupplyD2603 01 (2013)2conditions other than 15.0 % 6 0.5 % decrease of referencefluid viscosity at 40C are employed, that fact shall be includedin the test report.NOTE 2For interlaboratory comparisons, the laboratories shoulddefine a
31、 common severity level in terms of a specified viscosity loss of thereference fluid occurring in a given irradiation time with a given volumeof sample. For example, “the reference fluid should undergo a viscosityloss of 15 % when a 30 mL sample is treated for 10 min.”Alternatively, two or more labor
32、atories can define equivalent operatingconditions by a curve of percent viscosity loss of a reference fluid as afunction of irradiation time. Power setting and sample size are varied untileach laboratory finds a combination that satisfies two or more points onthe reference curve. This procedure prov
33、ides a comparison of the shearstability of an unknown fluid with that of the reference fluid over a rangeof irradiation times.8. Procedure8.1 Clean the sonic horn with a suitable solvent and cali-brate the apparatus as described in 7.3 and 7.4. Introduce 30mL of the sample into a clean 50-mL Griffin
34、 beaker andimmerse in the constant temperature bath at the desiredtemperature (0C unless otherwise specified). The beaker mustbe in a vertical position. Allow the sample to equilibrate for 10min. Immerse the sonic horn in the fluid as described in 7.3.Irradiate the sample at exactly the same energy
35、level and forthe same time as determined in 7.3 and 7.4. Upon completionof irradiation, remove the sample and clean the sonic horn witha suitable solvent.8.2 Determine the viscosity of the sample by Test MethodD445 before and after irradiation.9. Calculation9.1 Calculate the percentage loss of visco
36、sity as follows:Viscosity loss, % 5V02 Vf!/V0#3100 (1)where:V0= viscosity of oil before irradiation, mm2/s (cSt), andVf= viscosity of oil after irradiation, mm2/s (cSt).The permanent shear stability index (PSSI) may also becalculated in accordance with Practice D6022, provided thebase fluid viscosit
37、y is known.10. Report10.1 Report the result for the sample and the specifiedreference fluid as the percentage loss of viscosity at 40C in 10min. If other irradiation times/temperatures for determinationof viscosity or reference fluids are employed, the report shallindicate those facts.11. Precision
38、and Bias711.1 RepeatabilityThe difference between two indepen-dent results obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial would, in the long run, in the normal and correctoperation of the test method, exceed 1.6 percentage loss unit
39、sonly in one case in twenty.11.2 ReproducibilityThe difference between two indepen-dent results obtained by different operators working in differentlaboratories on identical test material would, in the long run, inthe normal and correct operation of the test method, exceed 3.3percentage loss units o
40、nly in one case in twenty.11.3 BiasThe procedures in this test method have no biasbecause the results can be defined only in terms of the testmethod.12. Keywords12.1 shear stability; sonic shear test; viscosity stableASTM International takes no position respecting the validity of any patent rights a
41、sserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time
42、 by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will re
43、ceive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received 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 In
44、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).7Supporting data are available from ASTM Headquarters. Request RR:D02-1264.D2603 01 (2013)3
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