1、Designation: D 6335 03bAn American National StandardStandard Test Method forDetermination of High Temperature Deposits by Thermo-Oxidation Engine Oil Simulation Test1This standard is issued under the fixed designation D 6335; the number immediately following the designation indicates the year oforig
2、inal adoption 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.1. Scope*1.1 This test method covers the procedure to determine theamount
3、of deposits formed by automotive engine oils utilizingthe thermo-oxidation engine oil simulation test (TEOST2).3Aninterlaboratory study4has determined it to be applicable overthe range from 10 to 65 mg total deposits.NOTE 1Operational experience with the test method has shown thetest method to be ap
4、plicable to engine oils having deposits over the rangefrom 2 to 180 mg total deposits.1.2 The values stated in SI units are to be regarded as thestandard.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 t
5、his standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Terminology2.1 Definitions of Terms Specific to This Standard:2.1.1 ceramic isolatorthe fitting that compresses theo-ring into the depositor rod casing and is
6、olates the depositorrod casing from the voltage applied to the depositor rod.2.1.2 depositor rodthe steel rod on which the deposits arecollected. It is resistively heated through a temperature cycleduring the test.2.1.3 depositor rod casingthe sleeve that surrounds thedepositor rod and allows the fl
7、ow of specimen around theoutside of the rod.2.1.4 drain tubethe tube connecting the outlet of thedepositor rod casing to the reaction chamber.2.1.5 end capthe fitting to tighten the ceramic isolatorsdown onto the o-rings at the ends of the depositor rod casing.2.1.6 filter depositsthe mass in mg of
8、the deposits col-lected on the filter cartridge.2.1.7 pumpthe gear pump that controls the flow rate ofsample through the depositor rod casing.2.1.8 pump inlet tubethe tube connecting the reactorchamber to the pump.2.1.9 pump outlet tubethe tube connecting the pump tothe depositor rod casing.2.1.10 r
9、eactor chamberthe reservoir that contains thebulk of the sample throughout the test. It has a drain valve forremoving sample at the end of the test and an inlet valve foradding gases to the sample. The chamber contains a magneticstir bar well in the bottom in which a stir bar is placed to mixthe rea
10、ctor contents.2.1.11 rod depositsthe mass in mg of the deposits col-lected on the depositor rod.2.1.12 rod o-ringsthe o-rings that seal the outside of therod and the depositor rod casing to prevent sample leaks.2.1.13 side nutthe fitting creates a seal to prevent sampleleaking from the front holes o
11、f the depositor rod casing.2.1.14 thermocouple lock collara fitting that tightens onthe thermocouple to ensure the thermocouple is at the correctdepth when placed inside the rod.2.1.15 total depositsthe rod deposits plus the filter depos-its.3. Summary of Test Method3.1 A sample of the engine oil at
12、 a temperature of 100Cthat contains ferric napthenate and is in contact with nitrousoxide and moist air is pumped at a set flow rate past a tareddepositor rod. The rod is resistively heated through twelve, 9.5min temperature cycles that go from 200 to 480C. When thetwelve cycle program is complete,
13、the depositor rod rinsed ofoil residue and dried and the gross rod mass obtained. Thesample is flushed from the system and filtered through a taredfilter. The mass of deposits on the rod plus the mass of depositson the filter is the total deposit mass.4. Significance and Use4.1 The test method is de
14、signed to predict the high tempera-ture deposit forming tendencies of an engine oil. This testmethod can be used to screen oil samples or as a qualityassurance tool.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility
15、of SubcommitteeD02.09 on Oxidation.Current edition approved May 10, 2003. Published July 2003. Originallyapproved in 1998. Last previous edition approved in 2003 as D 633503a.2TEOST is a trademark of the Tannas Co. (Reg. 2001396).3The Development of Thermo-Oxidation Engine Oil Simulation Test (TEOST
16、),Society of Automotive Engineers (SAE No. 932837), 400 Commonwealth Dr.,Warrendale, PA 15096-0001.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021391.1*A Summary of Changes section appears at the end of this standard.Copyr
17、ight ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Apparatus5.1 Thermo-oxidation engine oil simulation test (TEOST)test instrument.55.2 Balance, capable of weighing to the nearest 0.1 mg.5.3 Vacuum Source, hand held, floor model, or housev
18、acuum.5.4 Magnetic stirrer and stir bars.5.5 Digital timer.5.6 Petroleum and temperature resistant o-rings.5.7 Ceramic isolators.5.8 Polypropylene filters.5.9 Plastic filter holder.5.10 Plastic Petri Dishes, for filter storage.5.11 Filtering Flask1000 mL.5.12 Graduated Filter Funnel500 mL with Luer
19、lockfitting.5.13 Graduated Cylinder150 mL.5.14 BeakersOne 25 mL. One 600 mL.5.15 Graduated Cylinder10 mL.5.16 Erlenmeyer Flask50 mL.5.17 Adjustable hex wrench.5.18 Pipe Cleaners3 3 304.8 mm (12 in.).5.19 Steel Wool4/0 (ultra fine).5.20 Brass Brush0.22 caliber.5.21 Glass Syringe100 L.5.22 Tannas one
20、piece cartridge filters. (OptionalItems5.8, 5.9, and 5.10 are not needed if the optional Tannasone-piece cartridge filters is used.)55.23 Flow Meters, capable of measuring 0 to 10 mL of airper min.5.24 Weighing Boat, light, circular or oblong open con-tainer, preferably made of aluminum with a diame
21、ter or lengthof approximately 7 to 10 cm and notched in two diametricallyopposed places to prevent the rod from rolling. (See Fig. 2.)6. Reagents and Materials6.1 Nitrous Oxide (N2O)USP compressed gas cylinder,medical grade.6.2 Moist AirHydrocarbon-free air regulated to 103.4 kPa(15 psig) before the
22、 flow meter and then bubbled through 30mL of water in a 50 mL Erlenmeyer flask.5The sole source of supply of the apparatus known to the committee at this timeis Tannas Co., 4800 James Savage Rd., Midland, MI 48642. If you are aware ofalternative suppliers, please provide this information to ASTM Int
23、ernationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee1, which you may attend.FIG. 1 Thermo-oxidation Engine Oil Simulation Test (TEOST)FIG. 2 Weighing Boat and RodD 6335 03b26.3 Ferric NaphthenateSix percent iron content in min-er
24、al spirits.6.4 Cyclohexane or HeptaneIndustrial grade.6.5 Low Deposit Reference OilCG-1 reference oil5is apetroleum oil capable of generating total deposits in the 20 to30 mg range. The acceptable deposit range of a specific lot isprovided by the supplier of that lot.6.6 Intermediate Deposit Referen
25、ce OilCF-1 referenceoil5is a petroleum oil capable of generating total deposits inthe 50 to 60 mg range. The acceptable deposit range of aspecific lot is provided by the supplier of that lot.6.7 Pump Calibration FluidTPC.57. Calibration7.1 The TEOST instrument is calibrated by performing theprocedur
26、e found in Section 8-16 for both a low and a highdeposit reference oil. The results shall be within the repeat-ability limits established by the supplier of the reference oils.7.2 The calibration should be performed a minimum ofevery three months, as recommended by the instrument manu-facturer.7.3 I
27、f the repeatability is not within the established limits,the instrument setup steps in Section 8 should be performed.Then the reference oil should be rerun.8. Setup of the Test Instrument8.1 Pump Speed CalibrationThe pump speed should becalibrated using the instructions found in Annex A1. It isrecom
28、mended that this calibration be done every three months.8.2 Thermocouple DepthThe thermocouple depth setting(distance from tip to locking collar) should be determinedusing the procedure in Annex A2. The depth setting should bechecked daily and should be redetermined whenever a newthermocouple is ins
29、talled.8.3 Power AdjustmentsThe procedure for making poweradjustments is given in Annex A3. It is recommended that thepower adjustments be made by a qualified instrument techni-cian.8.4 Verify that the temperature program shown in Table 1 isentered. When verifying the temperature program, alwayspres
30、s RETURN when assured soak is displayed.9. Assembly of Apparatus9.1 Assemble the TEOST system by placing the reactionchamber in the bolt seats on the TEOST platform with the drainand gas inlet tubing facing the right side of the instrument.9.2 Connect the pump inlet tube to the outlet connection oft
31、he reaction chamber and the inlet connection of the pump.Finger tighten the connections.9.3 Connect the pump outlet tube to the outlet connection ofthe pump, and place a 10 mL graduated cylinder directly underthe open end of the pump outlet tube.9.4 Place the lid containing the thermocouple on the r
32、eac-tion chamber, making sure that the thermocouple is touchingthe bottom of the reaction chamber.9.5 Wrap the heating jacket around the reaction chamberand secure it with the provided straps. Connect the heatingjacket and the thermocouple to the labeled connections on theback wall of the instrument
33、. The connectors shall be insertedand twisted to obtain a proper connection. Use the reactortemperature controller to set the temperature of the reactionchamber to 100C.9.6 Connect the gas tubing to the reaction chamber, and setthe flow meters for the moist air and N2O to 3.5 mL/min. Theseare allowe
34、d to flow to purge out the lines before the test begins.NOTE 2Be sure the valve on the reaction chamber is pointing up toallow the gases to enter into the chamber.10. Sample Preparation10.1 After thoroughly mixing the test sample, use a gradu-ated cylinder to measure 116 mL of the fluid and pour it
35、into a600-mL beaker. Use a syringe to add 193 L of the 6 % ferricnapthenate solution to the 116 mL of test fluid. The resultingconcentration of iron in the test fluid will be about 100 wt ppm.10.2 Use a magnetic bar and stirrer to mix the oil and ferricnaphthenate for at least 5 min but not more tha
36、n 15 min. Makecertain that a vortex is not created.10.3 After the stirring is completed, inspect the oil solutionby holding it up to a light to make sure it is homogenous. If not,stir for 5 min more.11. Procedure11.1 When the reaction chamber is 100 6 5C, pour the testsample into the reaction chambe
37、r. Using the speed dial on theTABLE 1 Temperature ProgramProgram Mode ValueSet point 0 200CTime 1 1.15 minSet point 1 200CTime 2 1.00 minSet point 2 480CTime 3 2.00 minSet point 3 480CTime 4 4.00 minSet point 4 200CTime 5 1.15 minSet point 5 200CTime 6 0 minCycles 12.00FIG. 3 Diagram of Depositor Ro
38、d AssemblyD 6335 03b3right side of the instrument, set the stir bar speed to 50. Thesample temperature should reach 100C in approximately 15min.11.2 Set the pump speed to 999, using the dial on the frontpanel of the instrument. Allow the pump to flush out 10 mL offluid into the 10 mL graduated cylin
39、der placed at the open endof the pump outlet tube. When flushing is complete, set thepump dial to 000 to stop the pump. Discard the 10 mL of oil.11.3 Use cyclohexane to rinse off an unused rod, both on theoutside and down the center. Clean each of the three sections ofthe rod with 4/0 steel wool by
40、stroking (up and down action)each section 20 times while turning the rod. Rinse the rod withacetone inside and out. Using a pipe cleaner soaked in acetone,clean the interior of the rod. Repeat the interior cleaning witha clean pipe cleaner through the rod in the opposite direction.Dry the rod with a
41、 vacuum while holding the rod between thethumb and index finger. Handle the rod as little as possible toavoid adding mass from oils on the skin and be sure not to setthe rod down until after a mass is taken. Take extra care not totouch the center area of the rod where the deposits are formed.Weight
42、the rod to 0.1 mg and record as the initial mass.NOTE 3Heptane may be substituted for cyclohexane throughout thetest. The use of heptane will require longer drying times.11.4 Slide the pre-weighed rod into the clean depositor rodcasing with an even amount of the rod protruding from eitherend. Slide
43、a new petroleum and temperature resistant o-ringover each end of the rod, and slide them up to the depositor rodcasing. Place the ceramic isolators over each end of the rodwith the thin portion pointing toward the end of the rod. Placethe nuts on the end, and start to secure them, but do not tighten
44、.Align the rod in the depositor rod casing until the shoulderbetween the deposit area and the bus bar connection areas ofthe rod can be seen through the inlet or outlet connections ofthe depositor rod casing. When this is achieved, the securingnuts may be tightened with a wrench.11.5 Place the depos
45、itor rod casing/test rod assembly verti-cally in the bus bars, and slide the overtemp thermocouple inthe bottom of the rod at the same time. Slide this in as far as itwill go without bending it (be sure the rod has not shiftedwithin the depositor rod casing). Make certain that the largerconnection o
46、n the depositor rod casing is at the top. Connectthe top end by placing the rod into the indentation of the busbar and swinging the cap over the rod. Insert the hex screw tobegin the securing process. The top of the rod should beapproximately 2 mm above the top of the circular bus bar cap.Tighten al
47、l four hex screws. The gap in the bus bar should bethe same on both sides of the depositor rod for the top andbottom bus bars. A solid contact between the rod and the busbars is all that is required.NOTE 4Do not overtighten.11.6 The open end of the pump outlet tube can now beconnected to the input c
48、onnection of the depositor rod casing.The drain tube may now also be connected to the outletconnection of the depositor rod casing and finger tightened.Use a wrench to tighten the end caps on the two open fronts ofthe depositor rod casing. The unit assembly should now becomplete.11.7 Set the pump di
49、al to 999 once again to complete thefluid flow through the entire system. When the system iscompletely filled with test fluid and the oil is flowing out of thedrain tube back into the reactor, set the pump dial to the settingdetermined from the pump speed calibration to give a flow rateof 0.49 mL/min (0.40 g/min flow rate with TPC pumpcalibration fluid).11.8 Place the depositor rod thermocouple down the centerof the test rod. A caliper may be used to ensure proper depth ofthe thermocouple as determined by the thermocouple depthcali
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