ASTM D6335-2018 red 1250 Standard Test Method for Determination of High Temperature Deposits by Thermo-Oxidation Engine Oil Simulation Test.pdf

1、Designation: D6335 16D6335 18Standard 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

2、 case 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 the amount of deposits formed by au

3、tomotive engine oils utilizing thethermo-oxidation engine oil simulation test (TEOST2).3 An interlaboratory 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 the test method to be app

4、licable to engine oils having deposits over the range from2 mg to 180 mg total deposits.1.2 The values stated in SI units are to be regarded as standard.1.2.1 Milligrams (mg), grams (g), milliliters (mL), and liters are the units provided, because they are an industry acceptedstandard.1.2.2 Exceptio

5、nPounds per square inch gauge (psig) is provided for information only in 6.2.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvir

6、onmental practices and determine theapplicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards,

7、Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Terminology2.1 Definitions of Terms Specific to This Standard:2.1.1 ceramic isolator, nthe fitting that compresses the O-ring into the depositor rod casing and isolates the depositor rodca

8、sing from the voltage applied to the depositor rod.2.1.2 depositor rod4, na patented, specially made, numbered, and registered steel rod (used once for each test) on which thedeposits are collected. It is resistively heated through a series of twelve temperature cycles during the test to temperature

9、sestablished and controlled by a thermocouple inserted to a pre-determined depth in the hollow rod.2.1.3 depositor rod casing, nthe sleeve that surrounds the depositor rod and allows the flow of the test oil up and around theoutside of the rod at a flow rate such that every volume element of the tes

10、t oil is exposed to the same heating cycle.2.1.4 drain tube, nthe tube connecting the upper outlet of the depositor rod casing to the reaction chamber.2.1.5 end cap, nthe fitting to tighten the ceramic isolators onto the O-rings at both ends of the depositor rod casing.2.1.6 filter deposits, nthe ma

11、ss in milligrams of the deposits collected after test on a special multi-layer filter cartridge usedonce for each test.2.1.7 pump, nthe gear pump that is used to control the flow rate of the test oil through the depositor rod casing.1 This test method is under the jurisdiction ofASTM Committee D02 o

12、n Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of SubcommitteeD02.09.0G on Oxidation Testing of Engine Oils.Current edition approved Oct. 1, 2016June 1, 2018. Published November 2016July 2018. Originally approved in 1998. Last previous edition approved in 20092016

13、 asD6335 09.16. DOI: 10.1520/D6335-16.10.1520/D6335-18.2 TEOST is a trademark of the Tannas Co. (Reg. 2001396), Tannas Company, 4800 James Savage Rd., Midland, MI 48642.3 The Development ofThermo-Oxidation Engine Oil SimulationTest (TEOST), Society ofAutomotive Engineers (SAE No. 932837), 400 Common

14、wealth Dr.,Warrendale,PA 15096-0001.4 The sole source of supply of the apparatus known to the committee at this time is Tannas Co., 4800 James Savage Rd., Midland, MI 48642. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters. Your comments wi

15、ll receive careful consideration at a meeting of the responsible technicalcommittee,1 which you may attend.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be tec

16、hnically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of thi

17、s standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.1.8 pump inlet tube, nthe tube connecting the reactor chamber to the pump.2.1.9 pump outlet tube, nthe tube connecting the pump to the depositor rod casing.2.1.10 reactor cha

18、mber, nthe heated reservoir that contains the bulk (approximately 100 mL) of the 116 mL of test oil samplecirculated past the deposit rod during the test. The reactor is equipped with a magnetic stir-bar to continuously mix the chambercontents.2.1.10.1 DiscussionIn the reaction chamber, moist air an

19、d nitrous oxide are each bubbled at a controlled rate of 3.5 mLmin through a channel openingat the bottom of the reaction chamber. This channel is also used to drain the test oil from the reaction chamber for filtration whenthe test is completed.2.1.11 rod deposits, nthe mass, in milligrams, of the

20、deposits collected on the depositor rod.2.1.12 rod O-rings, nthe O-rings that seal the outside of the rod and the depositor rod casing to prevent sample leaks.2.1.13 side nut, nthe fitting creates a seal to prevent sample leaking from the front holes of the depositor rod casing.2.1.14 thermocouple l

21、ock collar, na fitting that tightens on the thermocouple to ensure the thermocouple is at the correct depthwhen placed inside the rod.2.1.15 total deposits, nthe rod deposits plus the filter deposits.3. Summary of Test Method3.1 A 116 mL sample of the engine oil to be tested containing 100 mgkg ferr

22、ic napthenatenaphthenate is put into the reactionchamber and heated and stirred at a temperature of 100 C.100 C. Nitrous oxide and moist air are injected from a bottom channelopening, each at a flow rate of 3.5 mLmin. This catalyzed oil is pumped past a tared depositor rod that is resistively heated

23、 throughtwelve, 9.5 min temperature cycles that go from 200 C to 480 C. When the twelve-cycle program is complete, the depositor rodis rinsed of oil residue and dried and the gross rod mass obtained. The remaining test oil sample, including washing from thedeposit rod, is flushed from the system and

24、 filtered through a tared filter. 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 designed to predict the high temperature deposit forming tendencies of an engine oil subject to the addedoxidizing stress o

25、f a turbocharger. This test method can be used to screen oil samples or as a quality assurance tool.5. Apparatus5.1 Thermo-oxidation engine oil simulation test (TEOST) test instrument.4 See Fig. 1.5.2 Balance, capable of weighing to the nearest 0.1 mg.5.3 Vacuum Source, hand held, floor model, or ho

26、use vacuum.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 Filtering Flask1000 mL.5.9 Graduated Filter Funnel500 mL with Luer lock fitting.5.10 Graduated Cylinder150 mL.5.11 BeakersOne small (for example, 25 mL). One beak

27、er large 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 Brush0.22 caliber (5.588 mm).5.18 Glass Syringe100 L. (OptionalA calibr

28、ated pipet can also be used with chemically inert disposable tips.)D6335 1825.19 One-piece disposable multi-layer cartridge filters.45.20 Flow Meterscapable of measuring 0 mLmin to 10 mLmin of gas.5.21 Weighing Boatlight, circular or oblong open container, preferably made of aluminum with a diameter

29、 or length ofapproximately 7 cm to 10 cm and notched in two diametrically opposed places to prevent the rod from rolling. (Seerolling (seeFig. 2.) or a suitable weighing device capable of preventing the rod from rolling and from losing any deposits.5.22 Wire Roda clean, thin (about 1 mm diameter), s

30、omewhat flexible, stainless steel wire rod (approximately 150 mm inlength) for dislodging any deposits adhering to the filter funnel 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 regu

31、lated to 103.4 kPa (15 psig) before entering the flow meter and then bubbled throughapproximately 30 mL of water in a small Erlenmeyer flask before combining with the nitrous oxide and entering the reactionchamber.6.3 Ferric NaphthenateSix percent iron content in mineral spirits.6.4 Cyclohexane, Hep

32、tane, or Other Alkane Hydrocarbon Solvent of Equivalent VolatilityReagent grade. (WarningFlammable.) Cyclohexane is the only allowed naphthenic hydrocarbon. Do no use other naphthenic or any aromatic hydrocarbons.Throughout the further description of the test, the solvent selected is referred to as

33、“hydrocarbon solvent.”6.4.1 The volatility of the hydrocarbon solvent selected should ensure timely evaporation from the deposits on the rod and filter.In general, the higher the purity of the solvent, the more quickly the solvent should evaporate.6.5 Low Deposit Reference OilCG-1 reference oil4 is

34、a petroleum oil capable of generating total deposits with a target in the20 mg to 30 mg range. The acceptable deposit deposit target and acceptable range of a specific lot is provided by the supplier ofthat lot.FIG. 1 Thermo-oxidation Engine Oil Simulation Test (TEOST)D6335 1836.6 Intermediate Depos

35、it Reference OilCF-1T33C-1 reference oil4 is a petroleum oil capable of generating total deposits witha target in the 50 mg to 60 mg range. The acceptable deposit deposit target and acceptable range of a specific lot is provided bythe supplier of that lot.6.7 Pump Calibration FluidTPC.47. Calibratio

36、n7.1 The TEOST instrument is calibrated by performing the procedure described in Section 8. At that point, either a low orhighintermediate deposit reference oil shall be run. The results shall be within the repeatability limits established by the supplierof the reference oils.7.2 The calibration sho

37、uld be performed a minimum of every six months, as recommended by the instrument manufacturer.7.3 If the repeatability is not within the established limits, the instrument setup steps in Section 8 should be performed. Thenthe reference oil should be rerun.8. Setup of the Test Instrument8.1 Pump Spee

38、d CalibrationThe pump speed should be calibrated using the instructions found in the operations manual. Itis recommended that this calibration be done every six months.8.2 Thermocouple DepthThe thermocouple depth setting (distance from tip to locking collar) should be determined using theprocedure i

39、n the operations manual. The depth setting should be checked daily and should be redetermined whenever a newthermocouple is installed.8.3 Thermocouple CalibrationThe thermocouple shall be calibrated every six months or when replaced. This can be done byplacing the thermocouple into a liquid or sand

40、bath while simultaneously measuring the temperature by a certified liquid or digitalthermometer. The temperature controller may then be offset to display the correct temperature.8.4 Flow CalibrationEnsure the proper operation of the flow meters by connecting a digital flow meter to the output. The f

41、lowfor the air shall be 3.5 mLmin 6 1 mLmin and the N2O flow shall be 3.5 mLmin 6 1 mLmin.8.5 PID SettingsThe PID settings on the temperature controller MUST be set to Pb: 80, Re: 2.0, and Ra: 0.2. Consult the thespecified settings for a specific controller. Consult the individual unit operations ma

42、nual for further guidance.8.6 Power AdjustmentsThis procedure, used only for instruments made prior to 1999, is for making power adjustments andis given in the operations manual. It is recommended that the power adjustments be made by a qualified instrument technician.8.7 Verify that the temperature

43、 program shown in Table 1 is entered. When verifying the temperature program, always be sureNOT to select guaranteed or assured soak.9. Assembly of Apparatus9.1 Assemble the TEOST system by placing the reaction chamber in the bolt seats on the TEOST platform with the drain andgas inlet tubing facing

44、 the right side of the instrument.9.2 Connect the pump inlet tube to the outlet connection of the reaction chamber and the inlet connection of the pump. Fingertighten the connections.9.3 Connect the pump outlet tube to the outlet connection of the pump, and place a 10 mL graduated cylinder directly

45、underthe open end of the pump outlet tube.9.4 Place the lid containing the thermocouple on the reaction chamber, making sure that the thermocouple is touching thebottom of the reaction chamber.FIG. 2 Weighing Boat and RodD6335 1849.5 Wrap the heating jacket around the reaction chamber and secure it

46、with the provided straps. Connect the heating jacket andthe thermocouple to the labeled connections on the back wall of the instrument. The connectors shall be inserted and twisted toobtain a proper connection. Use the reactor temperature controller to set the temperature of the reaction chamber to

47、100 C.9.6 Connect the gas tubing to the reaction chamber, and set the flow meters for the moist air and N2O to 3.5 mLmin 61 mLmin. These are allowed to flow to purge out the lines before the test begins.NOTE 2Be sure the valve on the reaction chamber is pointing up to allow the gases to enter into t

48、he chamber.10. Sample Preparation10.1 Invert both the catalyst vial and the test sample container at least three times to ensure homogeneity of both componentsprior to use. After thoroughly mixing the test sample, use a graduated cylinder to measure 116 mL 6 1 mL of the fluid and pourit into a large

49、 beaker until only drips are coming from the graduated cylinder. UseAfter thoroughly mixing the catalyst, use a glasssyringe or an optional calibrated pipet to add 193 L 6 1 L of the approximately 6 % ferric napthenatenaphthenate solution tothe 116 mL of test fluid. The resulting concentration of iron in the test fluid will be about 100 mgkg.10.2 Use a magnetic bar and stirrer to mix the oil and ferric naphthenate for at least 5 min but not more than 15 min. Makecertain that a vortex is not created. Periodical