1、Designation: D6335 16Standard Test Method forDetermination of High Temperature Deposits by Thermo-Oxidation Engine Oil Simulation Test1This standard is issued under the fixed designation D6335; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the procedure to determine theamount of deposits formed by automotive
3、engine oils utilizingthe thermo-oxidation engine oil simulation test (TEOST2).3Aninterlaboratory study (see Section 17) has determined it to beapplicable over the range from 10 mg to 65 mg total deposits.NOTE 1Operational experience with the test method has shown thetest method to be applicable to e
4、ngine oils having deposits over the rangefrom 2 mg to 180 mg total deposits.1.2 The values stated in SI units are to be regarded asstandard.1.2.1 Milligrams (mg), grams (g), milliliters (mL), and litersare the units provided, because they are an industry acceptedstandard.1.2.2 ExceptionPounds per sq
5、uare inch gauge (psig) isprovided for information only in 6.2.1.3 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 and health practices and determine the applica
6、-bility of regulatory limitations prior to use.2. Terminology2.1 Definitions of Terms Specific to This Standard:2.1.1 ceramic isolator, nthe fitting that compresses theO-ring into the depositor rod casing and isolates the depositorrod casing from the voltage applied to the depositor rod.2.1.2 deposi
7、tor rod4, na patented, specially made,numbered, and registered steel rod (used once for each test) onwhich the deposits are collected. It is resistively heated througha series of twelve temperature cycles during the test totemperatures established and controlled by a thermocoupleinserted to a pre-de
8、termined depth in the hollow rod.2.1.3 depositor rod casing, nthe sleeve that surrounds thedepositor rod and allows the flow of the test oil up and aroundthe outside of the rod at a flow rate such that every volumeelement of the test oil is exposed to the same heating cycle.2.1.4 drain tube, nthe tu
9、be connecting the upper outlet ofthe depositor rod casing to the reaction chamber.2.1.5 end cap, nthe fitting to tighten the ceramic isolatorsonto the O-rings at both ends of the depositor rod casing.2.1.6 filter deposits, nthe mass in milligrams of thedeposits collected after test on a special mult
10、i-layer filtercartridge used once for each test.2.1.7 pump, nthe gear pump that is used to control theflow rate of the test oil through the depositor rod casing.2.1.8 pump inlet tube, nthe tube connecting the reactorchamber to the pump.2.1.9 pump outlet tube, nthe tube connecting the pump tothe depo
11、sitor rod casing.2.1.10 reactor chamber, nthe heated reservoir that con-tains the bulk (approximately 100 mL) of the 116 mLof test oilsample circulated past the deposit rod during the test. Thereactor is equipped with a magnetic stir-bar to continuouslymix the chamber contents.2.1.10.1 DiscussionIn
12、the reaction chamber, moist air andnitrous oxide are each bubbled at a controlled rate of3.5 mLmin through a channel opening at the bottom of the1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubc
13、ommittee D02.09.0G on Oxidation Testing of Engine Oils.Current edition approved Oct. 1, 2016. Published November 2016. Originallyapproved in 1998. Last previous edition approved in 2009 as D6335 09. DOI:10.1520/D6335-16.2TEOST is a trademark of the Tannas Co. (Reg. 2001396), Tannas Company,4800 Jame
14、s Savage Rd., Midland, MI 48642.3The Development of Thermo-Oxidation Engine Oil Simulation Test (TEOST),Society of Automotive Engineers (SAE No. 932837), 400 Commonwealth Dr.,Warrendale, PA 15096-0001.4The sole source of supply of the apparatus known to the committee at this timeis Tannas Co., 4800
15、James Savage Rd., Midland, MI 48642. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.*A Summary of Changes section ap
16、pears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1reaction chamber. This channel is also used to drain the test oilfrom the reaction chamber for filtration when the test iscompleted.2.1.11 rod deposits,
17、nthe mass, in milligrams, of thedeposits collected on the depositor rod.2.1.12 rod O-rings, nthe O-rings that seal the outside ofthe rod and the depositor rod casing to prevent sample leaks.2.1.13 side nut, nthe fitting creates a seal to preventsample leaking from the front holes of the depositor ro
18、d casing.2.1.14 thermocouple lock collar, na fitting that tightens onthe thermocouple to ensure the thermocouple is at the correctdepth when placed inside the rod.2.1.15 total deposits, nthe rod deposits plus the filterdeposits.3. Summary of Test Method3.1 A 116 mL sample of the engine oil to be tes
19、ted contain-ing 100 mgkg ferric napthenate is put into the reactionchamber and heated and stirred at a temperature of 100 C.Nitrous oxide and moist air are injected from a bottom channelopening, each at a flow rate of 3.5 mLmin. This catalyzed oilis pumped past a tared depositor rod that is resistiv
20、ely heatedthrough twelve, 9.5 min temperature cycles that go from200 C to 480 C. When the twelve-cycle program is complete,the depositor rod is rinsed of oil residue and dried and the grossrod mass obtained. The remaining test oil sample, includingwashing from the deposit rod, is flushed from the sy
21、stem andfiltered through a tared filter. The mass of deposits on the rodplus the mass of deposits on the filter is the total deposit mass.4. Significance and Use4.1 The test method is designed to predict the high tempera-ture deposit forming tendencies of an engine oil subject to theadded oxidizing
22、stress of a turbocharger. This test method canbe used to screen oil samples or as a quality assurance tool.5. Apparatus5.1 Thermo-oxidation engine oil simulation test (TEOST)test instrument.4See Fig. 1.5.2 Balance, capable of weighing to the nearest 0.1 mg.5.3 Vacuum Source, hand held, floor model,
23、or housevacuum.5.4 Magnetic stirrer and stir bars.5.5 Digital timer.5.6 Petroleum and temperature resistant O-rings.FIG. 1 Thermo-oxidation Engine Oil Simulation Test (TEOST)D6335 1625.7 Ceramic isolators.5.8 Filtering Flask1000 mL.5.9 Graduated Filter Funnel500 mL with Luer lock fit-ting.5.10 Gradu
24、ated Cylinder150 mL.5.11 BeakersOne small (for example, 25 mL). One beakerlarge enough to clean the depositor rod casing (for example,600 mL).5.12 Graduated Cylinder10 mL.5.13 Erlenmeyer Flask50 mL.5.14 Adjustable hex wrench.5.15 Pipe Cleaners3 mm 304.8 mm.5.16 Steel Wool4/0 (ultra fine).5.17 Brass
25、Brush0.22 caliber (5.588 mm).5.18 Glass Syringe100 L. (OptionalA calibrated pipetcan also be used with chemically inert disposable tips.)5.19 One-piece disposable multi-layer cartridge filters.45.20 Flow Meterscapable of measuring 0 mLmin to10 mLmin of gas.5.21 Weighing Boatlight, circular or oblong
26、 opencontainer, preferably made of aluminum with a diameter orlength of approximately 7 cm to 10 cm and notched in twodiametrically opposed places to prevent the rod from rolling.(See Fig. 2.)5.22 Wire Roda clean, thin (about 1 mm diameter), some-what flexible, stainless steel wire rod (approximatel
27、y 150 mmin length) for dislodging any deposits adhering to the filterfunnel walls into the filter cartridge.6. Reagents and Materials6.1 Nitrous Oxide (N2O)Compressed gas cylinder, 99.6 %purity or higher.6.2 Moist AirHydrocarbon-free air regulated to 103.4 kPa(15 psig) before entering the flow meter
28、 and then bubbledthrough approximately 30 mL of water in a small Erlenmeyerflask before combining with the nitrous oxide and entering thereaction chamber.6.3 Ferric NaphthenateSix percent iron content in min-eral spirits.6.4 Cyclohexane, Heptane, or Other Alkane HydrocarbonSolvent of Equivalent Vola
29、tilityReagent grade. (WarningFlammable.) Cyclohexane is the only allowed naphthenichydrocarbon. Do no use other naphthenic or any aromatichydrocarbons. Throughout the further description of the test,the solvent selected is referred to as “hydrocarbon solvent.”6.4.1 The volatility of the hydrocarbon
30、solvent selectedshould ensure timely evaporation from the deposits on the rodand filter. In general, the higher the purity of the solvent, themore quickly the solvent should evaporate.6.5 Low Deposit Reference OilCG-1 reference oil4is apetroleum oil capable of generating total deposits in the 20 mgt
31、o 30 mg range. The acceptable deposit range of a specific lotis provided by the supplier of that lot.6.6 Intermediate Deposit Reference OilCF-1 referenceoil4is a petroleum oil capable of generating total deposits inthe 50 mg to 60 mg range. The acceptable deposit range of aspecific lot is provided b
32、y the supplier of that lot.6.7 Pump Calibration FluidTPC.47. Calibration7.1 The TEOST instrument is calibrated by performing theprocedure described in Section 8. At that point, either a low orhigh deposit reference oil shall be run. The results shall bewithin the repeatability limits established by
33、the supplier of thereference oils.7.2 The calibration should be performed a minimum ofevery six months, as recommended by the instrument manu-facturer.7.3 If the repeatability is not within the established limits,the instrument setup steps in Section 8 should be performed.Then the reference oil shou
34、ld be rerun.8. Setup of the Test Instrument8.1 Pump Speed CalibrationThe pump speed should becalibrated using the instructions found in the operationsmanual. It is recommended that this calibration be done everysix months.8.2 Thermocouple DepthThe thermocouple depth setting(distance from tip to lock
35、ing collar) should be determinedusing the procedure in the operations manual. The depth settingshould be checked daily and should be redetermined whenevera new thermocouple is installed.8.3 Thermocouple CalibrationThe thermocouple shall becalibrated every six months or when replaced. This can be don
36、eby placing the thermocouple into a liquid or sand bath whilesimultaneously measuring the temperature by a certified liquidor digital thermometer. The temperature controller may then beoffset to display the correct temperature.8.4 Flow CalibrationEnsure the proper operation of theflow meters by conn
37、ecting a digital flow meter to the output.The flow for the air shall be 3.5 mLmin 6 1 mLmin and theN2O flow shall be 3.5 mLmin 6 1 mLmin.8.5 PID SettingsThe PID settings on the temperaturecontroller MUST be set to Pb: 80, Re: 2.0, and Ra: 0.2. Consultthe operations manual for further guidance.FIG. 2
38、 Weighing Boat and RodD6335 1638.6 Power AdjustmentsThis procedure, used only forinstruments made prior to 1999, is for making power adjust-ments and is given in the operations manual. It is recom-mended that the power adjustments be made by a qualifiedinstrument technician.8.7 Verify that the tempe
39、rature program shown in Table 1 isentered. When verifying the temperature program, always besure NOT to select guaranteed or assured soak.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 fa
40、cing the right side of the instrument.9.2 Connect the pump inlet tube to the outlet connection ofthe 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 directl
41、y underthe open end of the pump outlet tube.9.4 Place the lid containing the thermocouple on the reac-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 t
42、he heatingjacket and the thermocouple to the labeled connections on theback wall of the instrument. The connectors shall be insertedand twisted to obtain a proper connection. Use the reactortemperature controller to set the temperature of the reactionchamber to 100 C.9.6 Connect the gas tubing to th
43、e reaction chamber, and setthe flow meters for the moist air and N2O to 3.5 mLmin 61 mLmin. These are allowed to flow to purge out the linesbefore 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 Aft
44、er thoroughly mixing the test sample, use a gradu-ated cylinder to measure 116 mL 6 1 mL of the fluid and pourit into a large beaker until only drips are coming from thegraduated cylinder. Use a glass syringe or an optional cali-brated pipet to add 193 L 6 1 L of the approximately 6 %ferric napthena
45、te solution to the 116 mL of test fluid. Theresulting concentration of iron in the test fluid will be about100 mgkg.10.2 Use a magnetic bar and stirrer to mix the oil and ferricnaphthenate for at least 5 min but not more than 15 min. Makecertain that a vortex is not created. Periodically move thebea
46、ker around the stirrer (hence moving the magnet around thebottom) to ensure the best possible stirring.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 10
47、0 C 6 5 C, pour thetest sample, along with the stirrer bar, into the reactionchamber. Using the speed dial on the right side of theinstrument, turn on the stirrer. Older instruments have a stirrercontrol versus a switch; this control must be set so that thestirrer is on but a vortex is not formed. T
48、he sample temperatureshould reach 100 C in approximately 15 min.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 cylinder placed at the open endof the pump outlet tube. When flushing is complete, se
49、t thepump dial to 000 to stop the pump. Discard the 10 mL of oil.11.3 Use hydrocarbon solvent to rinse off an unused rod,both on the outside and down the center. Clean each of thethree sections of the rod lightly with 4/0 steel wool by stroking(up and down action) each section 20 times while turning therod. Rinse the rod with acetone inside and out. Using a pipecleaner soaked in acetone, clean the interior of the rod. Repeatthe interior cleaning with a clean pipe cleaner through the rodin the opposite direction.
