1、Designation: D 6335 09Standard 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 oforiginal adoption or, in the case
2、of 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 automotiv
3、e 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 to 65 mg total deposits.NOTE 1Operational experience with the test method has shown thetest method to be applicable to en
4、gine oils having deposits over the rangefrom 2 to 180 mg total deposits.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.2.1 Milligrams (mg), grams (g), millilitres (mL), and litresare the units provided, because they are a
5、n industry acceptedstandard.1.2.2 ExceptionProvided psig 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 an
6、d 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 isolates the depositorrod casing from the voltage applied to the deposi
7、tor 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 flow of specimen around theoutside of the rod.2.1.4 drain tubethe tube
8、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 the deposits col-lected on the filter cartridge.2.1.7 pumpthe gear pu
9、mp 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 reactor chamberthe reservoir that contains thebulk of the sample throu
10、ghout 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 reactor contents.2.1.11 rod depositsthe mass, in milligrams, of the depo
11、s-its collected 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 of the depositor rod casing.2.1.14 thermocouple lock collara
12、 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 a temperature of 100Cthat contains ferric napthenate and i
13、s 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, the depositor rod rinsed ofoil residue and dried and the gr
14、oss 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.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and i
15、s the direct responsibility of SubcommitteeD02.09.0G on Oxidation Testing of Engine Oils.Current edition approved June 1, 2009. Published July 2009. Originally approvedin 1998. Last previous edition approved in 2003 as D 633503b.2TEOST is a trademark of the Tannas Co. (Reg. 2001396), Tannas Company,
16、4800 James 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 15096-0001.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM Internat
17、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and Use4.1 The test method is designed 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 t
18、ool.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, or housevacuum.5.4 Magnetic stirrer and stir bars.5.5 Digital timer.5.6 Petroleum and temperature resis
19、tant 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 lockfitting.5.13 Graduated Cylinder150 mL.5.14 BeakersOne small (for example, 25 mL). One bea-
20、ker large enough to clean the depositor rod casing (forexample, 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.5.19 Steel Wool4/0 (ultra fine).5.20 Brass Brush0.22 caliber.5.21 Glass Syringe100 L.5.22 Tannas one piece cartrid
21、ge filters. (OptionalItems5.8, 5.9, and 5.10 are not needed if the optional Tannasone-piece cartridge filters is used.)45.23 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 diameter or length
22、of approximately 7 to 10 cm and notched in two diametricallyopposed places to prevent the rod from rolling. (See Fig. 2.)4The 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, p
23、lease provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.FIG. 1 Thermo-oxidation Engine Oil Simulation Test (TEOST)D63350926. Reagents and Materials6.1 Nitrous Oxide (N2
24、O)USP compressed gas cylinder,medical grade.6.2 Moist AirHydrocarbon-free air regulated to 103.4 kPa(15 psig) before the flow meter and then bubbled throughapproximately 30 mL of water in a small Erlenmeyer flask.6.3 Ferric NaphthenateSix percent iron content in min-eral spirits.6.4 Cyclohexane or H
25、eptaneIndustrial grade.6.5 Low Deposit Reference OilCG-1 reference oil4is 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 Reference OilCF-1 referenceoil4is a pe
26、troleum 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.47. Calibration7.1 The TEOST instrument is calibrated by performing theprocedure described in Section 8. At th
27、at point, either a low orhigh deposit reference oil shall be run. The results shall bewithin the repeatability limits established by 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 repea
28、tability 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 the operationsmanual. It is rec
29、ommended that this calibration be done everysix months.8.2 Thermocouple DepthThe thermocouple depth setting(distance from tip to locking collar) should be determinedusing the procedure in the operations manual. The depth settingshould be checked daily and should be redetermined whenevera new thermoc
30、ouple is installed.8.3 Thermocouple CalibrationThe thermocouple shall becalibrated every six months or when replaced. This can be doneby placing the thermocouple into a liquid or sand bath whilesimultaneously measuring the temperature by a certified liquidor digital thermometer. The temperature cont
31、roller may then beoffset to display the correct temperature.8.4 Flow CalibrationEnsure the proper operation of theflow meters by connecting a digital flow meter to the output.The flow for the air shall be 3.5 6 1 mL/min and the N2O flowshall be 3.5 6 1 mL/min.8.5 PID SettingsThe PID settings on the
32、temperaturecontroller MUST be set to Pb: 80, Re: 2.0, and Ra: 0.2. Consultthe operations manual for further guidance.8.6 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 p
33、ower adjustments be made by a qualifiedinstrument technician.8.7 Verify that the temperature 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 reactio
34、nchamber 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 ofthe reaction chamber and the inlet connection of the pump.Finger tighten the connections.9.3 Connect the pump outlet
35、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 reac-tion chamber, making sure that the thermocouple is touchingthe bottom of the reaction chamber.9.5 Wrap the heati
36、ng 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. The connectors shall be insertedand twisted to obtain a proper connection. Use the reactortemperature controller t
37、o 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 N2Oto3.56 1 mL/min.These are allowed to flow to purge out the lines before the testbegins.FIG. 2 Weighing Boat and RodTABLE 1 Temperature ProgramProgr
38、am 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 12.00D6335093NOTE 2Be sure the valve on the reaction chamber is pointing up toallow the gases to
39、enter into the chamber.10. Sample Preparation10.1 After thoroughly mixing the test sample, use a gradu-ated cylinder to measure 116 6 1 mL of the fluid and pour itinto a large beaker until only drips are coming from thegraduated cylinder. Use a syringe to add 193 6 1 L of theapproximately 6 % ferric
40、 napthenate solution to the 116 mL oftest fluid. The resulting concentration of iron in the test fluidwill 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 than 15 min. Makecertain that a vortex is not created. Periodically
41、move thebeaker around the stirrer (hence moving hte 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 ch
42、amber is 100 6 5C, pour the testsample, along with the stirrer bar, into the reaction chamber.Using the speed dial on the right side of the instrument, turn onthe stirrer. The older equipment has a stirrer control versus aswitch; this control must be set so that the stirrer is on but avortex is not
43、formed. The sample temperature should reach100C 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 comp
44、lete, set thepump dial to 000 to stop the pump. Discard the 10 mL of oil.11.3 Use cyclohexane or heptane to rinse off an unused rod,both on the outside and down the center. Clean each of thethree sections of the rod with 4/0 steel wool by stroking (up anddown action) each section 20 times while turn
45、ing the rod.Rinse the rod with acetone inside and out. Using a pipe cleanersoaked in acetone, clean the interior of the rod. Repeat theinterior cleaning with a clean pipe cleaner through the rod inthe opposite direction. Dry the rod with a vacuum or blowingdry air while holding the rod between the t
46、humb and indexfinger. Make sure to dry the center of the rod as well. Handlethe rod as little as possible to avoid adding mass from oils onthe skin and be sure not to set the rod down until after a massis taken. Take extra care not to touch the center area of the rodwhere the deposits are formed. We
47、ight the rod to 0.1 mg andrecord as the initial mass once the rod weight has come toequilibrium.NOTE 3Heptane may be substituted for cyclohexane throughout thetest. The use of heptane will require longer drying times.11.4 Inspect the bus bars to make sure they are clean. If not,clean the bus bars ac
48、cording to the operations manual. Slide thepre-weighed rod into the clean depositor rod casing with aneven amount of the rod protruding from either end. Slide a newpetroleum and temperature resistant O-ring over each end ofthe rod, and slide them up to the depositor rod casing. Place theceramic isol
49、ators over each end of the rod with the thin portionpointing toward the end of the rod. Place the nuts on the end,and start to secure them, but do not tighten.Align the rod in thedepositor rod casing until an even amount of the rod isprotruding from both ends (equally spaced) or the shoulderbetween the deposit area and the bus bar connection areas ofthe rod is centered in the inlet or outlet connections of thedepositor rod casing. When this is achieved, the nuts may betightened. See Fig. 3.11.5 Place the depositor rod casing/test
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