1、Designation: D 3607 97 (Reapproved 2002)e1An American National StandardStandard Test Method forRemoving Volatile Contaminants from Used Engine Oils byStripping1This standard is issued under the fixed designation D 3607; 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 editorially moved into the standard text in March 2003.
3、1. Scope1.1 This test method covers a standardized procedure forremoving volatile materials such as gasoline and water fromused engine oils prior to further oil analysis.1.2 It also provides an estimate of such volatiles in usedengine oils.1.3 When an accurate value of the gasoline contaminant isreq
4、uired either Test Methods D 322 or D 3525 shall be used.NOTE 1Test Method D 322 determines the amount of gasoline bydistillation with water. Test Method D 3525 determines the amount ofmaterial boiling below the boiling point of ntetradecane by gas chroma-tography.NOTE 2When the amount of gasoline is
5、 required to be known, theuser of this test method is advised to determine which method is to beused. There are cases where D 3525 may be set as the referee method.1.4 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.5 This standar
6、d 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 consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.For specific precauti
7、onary statement, see 6.1 and 8.5.2. Referenced Documents2.1 ASTM Standards:D 322 Test Method for Gasoline Diluent in Used GasolineEngine Oils by Distillation2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (the Calculation of Dynamic Viscos-ity)2D 3525 Test Method for Gaso
8、line Diluent in Used GasolineEngine Oils by Gas Chromatography3D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products3D 4175 Terminology Relating to Petroleum, PetroleumProducts, and Lubricants3D 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3E1Specification
9、for ASTM Thermometers43. Terminology3.1 Definitions:3.1.1 stripping, nthe process whereby volatile fractionsare removed from a liquid material.3.1.1.1 DiscussionIn this test method, lighter componentssuch as water and gasoline are removed by the application ofheat while passing an inert gas through
10、the liquid.3.1.2 used oil, nany oil that has been in a piece ofequipment (for example, an engine, gearbox, transformer, orturbine) whether operated or not.3.1.2.1 DiscussionThis test method refers specifically toused lubricating oils from gasoline engines.4. Summary of Test Method4.1 A known weight
11、of sample is heated to 90C under anitrogen flow for 4.5 h, cooled, and reweighed.5. Significance and Use5.1 The removal of volatile materials such as gasolinedilution from used engine oils is especially important if themechanical shear stability or oxidative stability of the oil isbeing monitored by
12、 measuring a kinematic viscosity change inthe oil after it has been used in a gasoline engine.6. Apparatus6.1 Nitrogen Cylinder, equipped with regulator.(WarningUsing pressurized gas is hazardous.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants a
13、nd is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved Dec. 10, 2002. Published March 2003. Originallyapproved in 1977. Last previous edition approved in 1997 as D 360797.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 0
14、5.02.4Annual Book of ASTM Standards, Vol 14.03.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Rotameters or Nitrogen Flowmeters5, one or more, eachcapable of supplying 400 cm3/min of nitrogen at atmosphericpressure.NOTE 3If seve
15、ral rotameters are available, it is preferable to controlthe nitrogen flow with an individual rotameter to each tube. Consistentflow rates can be maintained to several tubes by one rotameter if thenitrogen pressure is controlled in a common manifold to all tubes.6.3 Connecting Tubing, of 4.8-mm (316
16、 in.) inside diameterand 7.9-mm (516 in.) outside diameter is a convenient size.NOTE 4No tolerances for the dimensions of the I.D. and O.D. of thetubing are given because these are nominal sizes.6.4 Sample Tubes or Test Tubes, glass, 25 by 150-mm. Asmany as eight tubes can usually be handled in a ty
17、picalapparatus assembly (Note 3).6.5 Tubing, glass, 5-mm outside diameter, 3-mm or smallerinside diameter and about 200 mm long, for nitrogen flow intothe sample in the above tubes. This tubing should be longenough to rest just off the bottom of the sample tube whenconnected to the nitrogen flow ass
18、embly with the flexibleconnecting tubing.6.6 Oil Bath, with suitable cover for inserting glass sampletubes. Rubber O-rings or rubber stoppers between the tops ofthe tubes and the cover are convenient for steadying andpositioning the tubes.6.7 Stirring Device, for oil bath. When stripping severalsamp
19、les at once, the use of a magnetic stirrer and stirring baris convenient as their use allows more room for the sampletubes.6.8 Thermoregulator and Heater, capable of maintainingthe oil bath at 90.0 6 0.2C.6.9 Thermometer, such as ASTM Medium Aniline PointThermometer having a range from 25 to 105C an
20、d conform-ing to the requirements for Thermometer 34C as prescribed inSpecification E1.NOTE 5A typical schematic arrangement of the apparatus is shown inFig. 1.7. Sampling7.1 Using Practices D 4057 (Manual) or D 4177 (Auto-matic) obtain a representative sample of the material to betested.5The sole s
21、ource of supply of the apparatus known to the committee at this timeis Brooks Instrument Co., Inc., Hatfield, PA 19440, as Sho-Rate 50, Model 1350. Ifyou are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consider
22、ation at ameeting of the responsible technical committee1, which you may attend.FIG. 1 Schematic of Test ApparatusD 3607 97 (2002)e127.2 The sample should be well mixed by physical agitationfor at least 1 min immediately before selecting the aliquot fortesting.8. Procedure8.1 Turn on the heater and
23、thermoregulator of the oil bathand set the bath at 90.0 6 0.2C (Note 1). If a magnetic stirreris being used, ensure that it is properly positioned beneath theoil bath.8.2 Weigh the empty 25 by 150-mm glass tube together withthe 5-mm glass tubing to be used with it for nitrogen inlet flow.Weigh the a
24、ssembly to the nearest 0.1 mg.8.3 Add 25 mL of well-mixed sample to the assembly of 8.2and reweigh to the nearest 0.1 mg.8.4 Place the tubes containing oil into the preheated oil bath.The tubes should be positioned so that the entire oil sample isimmersed in the bath and between 20 and 40 mm of the
25、tubeextends above the bath oil level.8.5 Before connecting the gas inlet tubing, turn on thenitrogen flow and set it at 400 cm3/min. This flow rate shouldbe maintained to each tube. (WarningUsing pressurized gasis hazardous.)8.6 Attach the nitrogen delivery flexible tubing to the 5-mmgas inlet tubin
26、g in the sample tube and ensure that the inlettubing is resting just off the bottom of the sample tube.NOTE 6If excessive frothing occurs, decrease the nitrogen flow rate toapproximately 50 cm3/min and maintain this lesser rate until frothingsubsides before increasing it to 400 cm3/min. Frothing wil
27、l usuallysubside within 30 min.8.7 Maintain the 400-cm3/min nitrogen flow rate afterfrothing subsides for a total sparging time of 4.5 h.8.8 Turn off the heater, thermoregulator, stirrer, and nitrogenflow, remove the flexible tubing from the glass inlet tubes, andremove the sample tubes (still conta
28、ining the glass inlet tubes)from the oil bath.8.9 Wipe the outside of the sample tube completely dry,allow the assembly to cool to room temperature, and reweighto the nearest 0.1 mg. The oil sample in the tube is now free ofdiluent.NOTE 7If the kinematic viscosity of the stripped sample is desired,t
29、he sample should be reheated to about 60C and filtered while still warmbefore undertaking the kinematic viscosity measurement. This is espe-cially important if the used oil contains solid particles. See Test MethodD 445 for determining the kinematic viscosity and filtering of the oil.9. Calculation9
30、.1 Calculate the volatile contaminants content of thesample as weight percent volatile contaminants as follows:Volatile contaminants, mass % 5 A 2 B!/A 3 100 (1)where:A = weight of original sample, g, andB = weight of sample after stripping, g.10. Report10.1 Report the result as volatile contaminant
31、s content,mass percent ASTM D 3607.10.2 Report the time, if any, that a nitrogen flow rate of 50cm3/min was used due to excessive frothing.11. Precision and Bias11.1 The following criteria should be used for judging theacceptability of results (95 % confidence) (Note 8 and Note 9):11.1.1 Repeatabili
32、tyThe difference between successivetest 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 the following value onlyin one case in twenty: 0.27
33、 mass %.11.1.2 ReproducibilityThe difference between two, singleand independent results, obtained 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 following value only in one
34、case out oftwenty: 1.40 mass %.NOTE 8The precision reported here was obtained by a round-robinprogram using a stripping temperature of 87.8C and a stripping time of4.5 h. Kinematic viscosity results on the stripped samples were determinedat 98.9C.NOTE 9The precision of kinematic viscosity determinat
35、ions on oilsafter stripping by this test method will not usually be as good as theprecision stated in Test Method D 445. Results of duplicate strippingoperations on two portions of the same oil by the same operator in thesame laboratory should be considered suspect if the difference in themeasured k
36、inematic viscosities after stripping is greater than 1.4 % oftheir mean. Results on the same oil after stripping in each of twolaboratories should be considered suspect if the difference in the measuredkinematic viscosities after stripping is greater than 2.8 % of their mean.The precision of kinemat
37、ic viscosity measurements on gelled used engineoils may be much poorer than this. Gelled oils are defined as oils thatdevelop structure on standing, but that become much more fluid with lightagitation.11.2 BiasThe procedure in this test method for measuringvolatile contaminants in used engine oils h
38、as no bias becausethe mass percent of volatile materials can only be defined interms of the test method.12. Keywords12.1 contaminants; engine oils; gasoline dilution; used en-gine oils; water contaminationD 3607 97 (2002)e13ASTM International takes no position respecting the validity of any patent r
39、ights asserted 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 a
40、ny time 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
41、will receive 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
42、ASTM International, 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).D 3607 97 (2002)e14
