1、Designation: D 3607 08An 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 adoption or, in the c
2、ase 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.1. Scope*1.1 This test method covers a standardized procedure forremoving volatile materials such as
3、 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 isrequired either Test Methods D 322 or D 3525 shall be used.NOTE 1Test Method D 322 determines the amou
4、nt 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 required to be known, theuser of this test method is advised to determine which method is to beuse
5、d. 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 given in parentheses are for informationonly.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
6、s 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 warnings, see 6.1 and 8.5.2. Referenced Documents2.1 ASTM Standards:2D 322 Test Method for Gasoline Di
7、luent in Used GasolineEngine Oils by DistillationD 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 3525 Test Method for Gasoline Diluent in Used GasolineEngine Oils by Gas ChromatographyD 4057 Practice for Manual Sampling of Petroleum
8、 andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. 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
9、are removed by the application ofheat while passing an inert gas through 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 lubricatin
10、g oils from gasoline engines.4. Summary of Test Method4.1 A known weight 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 themechanic
11、al shear stability or oxidative stability of the oil isbeing monitored by 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.)6.2 Rotameters or Nitrogen Flo
12、wmeters3, one or more, eachcapable of supplying 400 cm3/min of nitrogen at atmosphericpressure.NOTE 3If several rotameters are available, it is preferable to controlthe nitrogen flow with an individual rotameter to each tube. Consistent1This test method is under the jurisdiction of ASTM Committee D0
13、2 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved Feb. 1, 2008. Published March 2008. Originallyapproved in 1977. Last previous edition approved in 2003 as D 360797(2002)e1.2For referenced ASTM standards, v
14、isit 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.3The sole source of supply of the apparatus known to the committee at this timeis Brooks Instr
15、ument 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 consideration at ameeting of the responsible technical committee,1which you may attend.1*A
16、Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.flow rates can be maintained to several tubes by one rotameter if thenitrogen pressure is controlled in a common manifold t
17、o all tubes.6.3 Connecting Tubing, of 4.8-mm (316 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. Asm
18、any as eight tubes can usually be handled in a typicalapparatus 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 s
19、ample tube whenconnected to the nitrogen flow assembly 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
20、 Device, for oil bath. When stripping severalsamples 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 P
21、ointThermometer having a range from 25 to 105C or some othernon-mercury containing temperature measuring device capableof operating in the same temperature range. See Section 11,where the data presented is derived using mercury-in-glassthermometers only. Data obtained using other temperaturemeasurin
22、g shall have equal to or better accuracy.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.7.2 The sample should be well mixed by physical agitation
23、for at least 1 min immediately before selecting the aliquot fortesting.8. Procedure8.1 Turn on the heater and 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
24、by 150-mm glass tube together withthe 5-mm glass tubing to be used with it for nitrogen inlet flow.Weigh the assembly to the nearest 0.1 mg.FIG. 1 Schematic of Test ApparatusD36070828.3 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 contain
25、ing 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 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
26、shouldbe maintained to each tube. (WarningUsing pressurized gasis hazardous.)8.6 Attach the nitrogen delivery flexible tubing to the 5-mmgas inlet tubing 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
27、the nitrogen flow rate toapproximately 50 cm3/min and maintain this lesser rate until frothingsubsides before increasing it to 400 cm3/min. Frothing will 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 of
28、f the heater, thermoregulator, stirrer, and nitrogenflow, remove the flexible tubing from the glass inlet tubes, andremove the sample tubes (still containing 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,
29、 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,the sample should be reheated to about 60C and filtered while still warmbefore undertaking the kinematic viscosity measurement. This is espe-cially i
30、mportant if the used oil contains solid particles. See Test MethodD 445 for determining the kinematic viscosity and filtering of the oil.9. Calculation9.1 Calculate the volatile contaminants content of thesample as weight percent volatile contaminants as follows:Volatile contaminants, mass % 5 A 2 B
31、!/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 contaminants 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. Preci
32、sion and Bias11.1 The following criteria should be used for judging theacceptability of results (95 % confidence) (Note 8 and Note 9).(WarningThe information provided here was obtained usingmercury-in-glass thermometers only and may not be applicablewhen other temperature measuring devices are used.
33、)11.1.1 RepeatabilityThe 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 c
34、ase in twenty: 0.27 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
35、 value only in one 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 v
36、iscosity determinations 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 differen
37、ce in themeasured kinematic 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 p
38、recision of kinematic 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
39、 used engine oils has 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 contaminationD3607083SUMMARY OF CHANGESSubcommittee D02.06 has identified the location of
40、 selected changes to this standard since the last issue(D 360797(2002)e1) that may impact the use of this standard.(1) Removed references to mercury thermometers and Speci-fication E 1.(2) Reworded thermometer specification in 6.9.(3) Reworded precision statement in 11.1.ASTM International takes no
41、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 any such patent rights, and the riskof infringement of such rights, are entirely their own responsi
42、bility.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 invited either for revision of this standard or for additional standardsand should be addressed to
43、 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 received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the addr
44、ess 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 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).D3607084
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