ASTM D7528-17a Standard Test Method for Bench Oxidation of Engine Oils by ROBO Apparatus.pdf

1、Designation: D7528 17aStandard Test Method forBench Oxidation of Engine Oils by ROBO Apparatus1This standard is issued under the fixed designation D7528; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A

2、number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThis test method is written for use by laboratories that make use of ASTM Test Monitoring Center(TMC)2services (see Annex A1 Annex A4).

3、The TMC provides reference oils, and engineering and statistical services to laboratories that desireto produce test results that are statistically similar to those produced by laboratories previouslycalibrated by the TMC.In general, the Test Purchaser decides if a calibrated test stand is to be use

4、d. Organizations such astheAmerican Chemistry Council require that a laboratory utilize the TMC services as part of their testregistration process. In addition, the American Petroleum Institute and the Gear Lubricant ReviewCommittee of the Lubricant Review Institute (SAE International) require that

5、a laboratory use theTMC services in seeking qualification of oils against their specifications.The advantage of using the TMC services to calibrate test stands is that the test laboratory (andhence the Test Purchaser) has an assurance that the test stand was operating at the proper level of testseve

6、rity. It should also be borne in mind that results obtained in a non-calibrated test stand may notbe the same as those obtained in a test stand participating in the ASTM TMC services process.1. Scope*1.1 This test method describes a bench procedure to simu-late the oil aging encountered in Test Meth

7、od D7320, theSequence IIIG engine test method. These aged oils are thentested for kinematic viscosity and for low-temperature pump-ability properties as described in the Sequence IIIGA enginetest, Appendix X1 of Test Method D7320.1.2 UnitsThe values stated in SI units are to be regardedas standard.

8、No other units of measurement are included in thisstandard.1.2.1 ExceptionsThere are no SI equivalents for someapparatus in Section 6, and there are some figures where inchunits are to be regarded as standard.1.3 This test method is arranged as follows:SectionScope 1Reference Documents 2Terminology

9、3Summary of Test Method 4Significance and Use 5Apparatus 6Reagents and Materials 7Hazards 8New and Existing Test Stand Calibration 9Procedure 10Cleaning 11Calculations and Determination of Test Results 12Report 13Precision and Bias 14Keywords 15AnnexesASTM Test Monitoring Center: Organization Annex

10、A1ASTM Test Monitoring Center: Calibration Procedures Annex A2ASTM Test Monitoring Center: Maintenance Activities Annex A3ASTM Test Monitoring Center: Related Information Annex A4Reaction Vessel Annex A5Reaction Vessel Head Annex A6Reaction Vessel-to-Head Seal Annex A7Agitator Turbine Blade Annex A8

11、Agitator Packing Gland Annex A9Nitrogen Dioxide Graduated Tube Annex A10Vacuum System Plumbing Annex A11Vacuum Trap Condensers Annex A12Setting the Vacuum Control Valve Annex A13Appendixes1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubric

12、ants and is the direct responsibility ofSubcommittee D02.B0.07 on Development and Surveillance of Bench TestsMethods.Current edition approved Oct. 1, 2017. Published October 2017. Originallyapproved in 2009. Last previous edition approved in 2017 as D7528 17. DOI:10.1520/D7528-17A.2Until the next re

13、vision of this test method, the ASTM Test Monitoring Centerwill update changes in the test method by means of information letters. Informationletters may be obtained from the ASTM Test Monitoring Center, 6555 Penn Ave.,Pittsburgh, PA 15206-4489. Attention: Administrator. This edition incorporatesrev

14、isions in all information letters through No. 16-1.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internatio

15、nally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1SectionSample Preparation and Addition Appendix X1Cha

16、rging the Liquid Nitrogen Dioxide Appendix X2Nitrogen Dioxide Precision Needle Valve Appendix X3Example of an Assembled ROBO Apparatus Appendix X4Information Package to Aid Setting Up a New Robo Apparatus Appendix X51.4 This standard does not purport to address all of thesafety concerns, if any, ass

17、ociated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific warning statements are given in Sections 7 and 8.1.5 This international st

18、andard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2.

19、 Referenced Documents2.1 ASTM Standards:3D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D4175 Terminology Relating to Petroleum Products, LiquidFuels, and LubricantsD4485 Specification for Performance of Active API ServiceCategory Eng

20、ine OilsD4684 Test Method for Determination of Yield Stress andApparent Viscosity of Engine Oils at Low TemperatureD5293 Test Method for Apparent Viscosity of Engine Oilsand Base Stocks Between 10 C and 35 C UsingCold-Cranking SimulatorD7320 Test Method for Evaluation of Automotive EngineOils in the

21、 Sequence IIIG, Spark-Ignition Engine2.2 SAE Standard:4SAE J300 Engine Oil Viscosity Classification3. Terminology3.1 Definitions:3.1.1 candidate oil, nan oil that is intended to have theperformance characteristics necessary to satisfy a specificationand is to be tested against that specification. D4

22、1753.1.2 reference oil, nan oil of known performancecharacteristics, used as a basis for comparison.3.1.2.1 DiscussionReference oils are used to calibratetesting facilities, to compare the performance of other oils, orto evaluate other materials (such as seals) that interact withoils. D41753.1.3 non

23、-reference oil, nany oil other than a reference oil,such as a research formulation, commercial oil or candidate oil.D41753.1.4 test oil, nany oil subjected to evaluation in anestablished procedure. D41753.2 Definitions of Terms Specific to This Standard:3.2.1 aged oil, na test oil after it has been

24、subjected to the40 h aging process in a ROBO apparatus.3.3 Acronyms:3.3.1 ROBO, nRomaszewski Oil Bench Oxidation54. Summary of Test Method4.1 The test oil is combined with a small amount of ironferrocene catalyst and placed in a 1 L reaction vessel. Thatmixture is stirred and heated for 40 h at 170

25、C with air flowingacross the liquid surface under negative pressure. In addition,nitrogen dioxide and air are introduced below the reactionsurface. After cooling, the oxidized, concentrated test oil issubjected to pertinent viscometric tests. Evaporated oil iscondensed in order to weigh it and calcu

26、late evaporative loss.5. Significance and Use5.1 This bench test method is intended to produce compa-rable oil aging characteristics to those obtained with ASTMTMC Sequence IIIGA matrix reference oils 434, 435, and 438after aging in the Sequence IIIG engine test.5.2 To the extent that the method gen

27、erates aged oilscomparable to those from the Sequence IIIG engine test, themeasured increases in kinematic and MRV viscosity indicatethe tendency of an oil to thicken because of volatilization andoxidation, as in the Sequence IIIG and IIIGA(seeAppendix X1in Test Method D7320) engine tests, respectiv

28、ely.5.3 This bench test procedure has potential use in specifi-cations and classifications of engine lubricating oils, such asSpecification D4485.5.4 The results of this test method are valid when seekingqualification of oils against published specifications only whenrun on a test stand that has suc

29、cessfully met the calibrationrequirements specified under the TMCs ROBO test monitor-ing program.6. Apparatus6.1 Balances:6.1.1 Analytical BalanceCapable of weighing 200 g witha minimum indication resolution of 0.1 g.6.1.2 Analytical BalanceCapable of weighing 0.1 g with aminimum indication resoluti

30、on of 0.001 g.6.2 Fume Hood, that vents to the outside atmosphere (seeSection 8).6.3 Reaction Vessel (ACE Glass, Inc. part numberD120676),6,7a 1 L, thick-walled glass vessel having a nominal100 mm inner diameter and with a bottom, sample/drain valve.3For referenced ASTM standards, visit the ASTM web

31、site, 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.4Available from SAE International, 400 Commonwealth Drive, Warrendale, PA15096-0001, http:/www.sae.org.5Kinker,

32、 B. G., Romaszewski, R. A., and Palmer, P. A., “ROBOA BenchProcedure to Replace Sequence IIIGA Engine Test,” Journal of ASTM International(JAI), Vol 4, No. 10, 2007, Paper ID JAI 100916. Available online fromwww.astm.org.6The sole source of supply of the apparatus known to the committee at this time

33、is Ace Glass, Inc., P.O. Box 688, 1430 NW Blvd., Vineland, NJ 08362-0688.D7528 17a2The lower half has an Instatherm8,7coating, rated at approxi-mately 400 W, for heating the test mixture.Adiagram is shownin Fig. A5.1.6.4 Vessel HeadThe vessel head is a stainless steel plate ofsufficient diameter to

34、completely cover the lower glass vesseland provide ample material for a sturdy mounting system.Reimel Machine, Inc. part number RMI-1002-DH9,7has beenshown to be suitable for this application. The vessel head mayalso be constructed as described in Annex A6. Users may alsosource some parts from Reime

35、l Machine, Inc. and somein-house. Ensure the plate has a center hole for an agitator shaftand threaded ports to allow filling and for the attachment ofair/nitrogen dioxide lines, vacuum control and relief valves,and a temperature probe. Fig. A6.1 defines the locations ofthese ports. Mill the bottom

36、surface of this stainless steel plateto accept a polytetrafluoroethylene (PTFE) ring seal for cen-tered attachment of the glass vessel as described in Annex A7.Reimel Machine, Inc. part number RMI-1007-DH9,7has beenfound suitable for this purpose.6.5 Stirrer MotorAn electric motor with drill chuck c

37、olletcapable of sustained operation at 200 r/min 6 5 r/min.6.6 StirrerAn 8 mm diameter stainless steel rod, 300 mmlong with a means of attaching a blade assembly at the bottom.The turbine blade assembly diameter is 2.58 in. (65.5 mm) with1.4 mm thick blades attached at a 45 pitch with an overallblad

38、e height of 0.985 in. (25.0 mm). Construct the stirrer asdescribed in Annex A8. Reimel Machine, Inc. part numberRMI-1001-DH9,7has been found suitable for this purpose.6.6.1 Attach the stirrer to the reactor head by means of apacking gland constructed as described in Annex A9. ReimelMachine, Inc. par

39、t number RMI-1004-DH9,7has been foundsuitable for this purpose. Attach the stirrer to the stirrer motorby inserting the 8 mm steel rod through the opening in thereactor head and the packing gland, and insert PTFE ropepacking to create a seal.6.6.2 Position the blade 6 mm from the bottom of the vesse

40、l.6.7 Air Supply SystemCapable of delivering an uninter-rupted flow of dry air into the test oil via a subsurface feedthroughout the reaction time period. An in-line, desiccant-charged, drying system has been found suitable.6.7.1 Ensure the subsurface feed tube opening remainsbelow the surface of th

41、e test fluid for the duration of the test.Do not place the tube in the drain area of the reaction flask.NOTE 1As the amount of test oil remaining at the end of the test is notalways known at the beginning of the test, it is advisable to configure thedry-air tube location such that the opening of the

42、 tube is as close to theagitator and as close to the bottom of the reactor as practical (withoutcontacting the agitator or blocking the tube opening).6.8 Graduated Tube (Ace Glass, Inc., part numberD120677),6,712 mL capacity, with 0.1 mL graduations andhaving appropriate provisions for connection to

43、 the reactionvessels subsurface gas delivery systemsee Annex A10 formore details. By receiving liquid phase nitrogen dioxide froma gas bottle, this tube allows measurement of nitrogen dioxidedepletion from the tube over the course of the reaction.6.9 Temperature Control SystemA controller and probec

44、apable of being programmed to control reaction temperaturevia low output wattage at or below 40 V ac and with anoperational hysteresis of 0.1 C using an on/off algorithm.Alternatively, a proportional-integral-derivative (PID) algo-rithm may also be used. Position the temperature probe tip sothat it

45、is level with the bottom of the turbine blade with adistance of 8 mm between the probe center and the blade edge.6.9.1 As the temperature may not be uniform throughout thereactor, it is important from the point of view of precision thatthe temperature is always monitored and controlled at thespecifi

46、ed position inside the reactor. When reassembling thereactor for a new run, reposition the probe, if necessary, as it iseasily bent.6.10 Flow Meters:6.10.1 Acrylic Block Airflow Meter (King Instrument Co.,7520 Series, Order number 2C-17),10,7having a scale of 0.4 to4 Standard Cubic Feet per Minute (

47、SCFM), with14 in. NPTthreaded female pipe end. It is used for measuring air flow in10.3.2. The machined fitting for the top of the flow meter shallaccommodate the vacuum line from the condenser to thereactor with a38 in. inside diameter or larger. The machinedfitting for the bottom of the flow meter

48、 shall accommodate the14 in. vacuum control valve.NOTE 2SCFM is the volumetric flow rate of a gas corrected tostandardized conditions of temperature, pressure, and relative humidity,thus representing a precise mass flow rate. However, the definitions ofstandard conditions vary. In this method, the f

49、low meter is calibrated withair at standard conditions defined as a temperature of 70 F, a pressure of14.6 psia and 0 % relative humidity.6.10.2 Airflow Meter, with a scale calibrated in mL/min formeasuring subsurface airflow of 185 mL/min in 10.3.1 and10.3.2.6.11 Vacuum SystemA pump with a free air capability ofat least 160 L/min is required to ensure a constant air flowacross the reaction surface in the vessel of 2.0 SCFM 60.1 SCFM with 61 kPa vacuum for 40 h. Instructions forconstructing the vacuum plumbing for the vessel are given inAnnex A11