1、Designation: D 7528 09Standard Test Method forBench Oxidation of Engine Oils by ROBO Apparatus1This standard is issued under the fixed designation D 7528; 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.INTRODUCTIONAny properly equipped laboratory, without outside assistance, can use the procedure described inthis test method. However, the ASTM Te
3、st Monitoring Center2(TMC) provides reference oils and anassessment of the test results obtained on those oils by the laboratory. By these means, the laboratorywill know whether its use of the test method gives results statistically similar to those obtained byother laboratories. Furthermore, variou
4、s agencies require that a laboratory utilize the TMC services inseeking qualification of oils against specifications. For example, the U.S. Army imposes such arequirement in connection with several Army engine lubricating oil specifications.Accordingly, this test method is written for use by laborat
5、ories that utilize the portions of the testmethod that refer to the TMC services. Laboratories that choose not to use the TMC services maysimply ignore these portions.This test method may be modified by means of information letters issued by the TMC. In addition,the TMC may issue supplementary memor
6、anda related to the method.1. Scope1.1 This test method describes a bench procedure to simu-late the oil aging encountered in Test Method D 7320, theSequence IIIG engine test method. These aged oils are thentested for kinematic viscosity and for low-temperature pump-ability properties as described i
7、n the Sequence IIIGA enginetest, Appendix X1 of Test Method D 7320.1.2 UnitsThe values stated in SI units are to be regardedas standard. 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 w
8、here inchunits are to be regarded as standard.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-bility of regul
9、atory limitations prior to use. Specific warningstatements are given in Sections 7 and 8.1.4 This test method is arranged as follows:SectionScope 1Reference Documents 2Terminology 3Summary of Test Method 4Significance and Use 5Apparatus 6Reagents and Materials 7Hazards 8Reference Oil Testing and Tes
10、t Stand Calibration 9Procedure 10Cleaning 11Calculations and Determination of Test Results 12Report 13Precision and Bias 14Keywords 15AnnexesReaction Vessel Annex A1Reaction Vessel Head Annex A2Reaction Vessel-to-Head Seal Annex A3Agitator Turbine Blade Annex A4Agitator Packing Gland Annex A5Nitroge
11、n Dioxide Graduated Tube Annex A6Vacuum System Plumbing Annex A7Vacuum Trap Condensers Annex A8Setting the Vacuum Control Valve Annex A9AppendixesSample Preparation and Addition Appendix X11This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is th
12、e direct responsibility of SubcommitteeD02.B0.07 on Development and Surveillance of Bench Tests Methods.Current edition approved April 15, 2009. Published June 2009.2ASTM Test Monitoring Center, 6555 PennAvenue, Pittsburgh, PA15206-4489.www.astmtmc.cmu.edu.1Copyright ASTM International, 100 Barr Har
13、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.SectionCharging 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 X52.
14、 Referenced Documents2.1 ASTM Standards:3D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4485 Specification for Performance of Engine OilsD 4684 Test Method
15、for Determination of Yield Stress andApparent Viscosity of Engine Oils at Low TemperatureD 5293 Test Method for Apparent Viscosity of Engine Oilsand Base Stocks Between 5 and 35C Using Cold-Cranking SimulatorD 7320 Test Method for Evaluation of Automotive EngineOils in the Sequence IIIG, Spark-Ignit
16、ion 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. D 41753.1.2 reference oil, na
17、n oil of known performance char-acteristics, 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. D 41753.1.3 non-reference oil, nany oi
18、l other than a referenceoil, such as a research formulation, commercial oil or candidateoil. D 41753.1.4 test oil, nany oil subjected to evaluation in anestablished procedure. D 41753.2 Definitions of Terms Specific to This Standard:3.2.1 aged oil, na test oil after it has been subjected to the40-h
19、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 C with air flowingacr
20、oss 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 calculate evaporative loss
21、.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 generates aged oilscompar
22、able 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 D 7320) engine tests, respectively.5.3 This bench te
23、st procedure has potential use in specifi-cations and classifications of engine lubricating oils, such asSpecification D 4485.6. 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
24、 aminimum indication resolution 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.The lower half has an
25、 Instatherm7,8coating, rated at approxi-mately 400 W, for heating the test mixture.Adiagram is shownin Fig. A1.1.6.4 Vessel HeadThe vessel head is a stainless steel plateof sufficient diameter to completely cover the lower glassvessel and provide ample material for a sturdy mountingsystem. Reimel Ma
26、chine, Inc. part number RMI-1002-DH7,9has been shown to be suitable for this application. The vesselhead may also be constructed as described in Annex A2. Usersmay also source some parts from Reimel Machine, Inc. andsome in-house. Ensure the plate has a center hole for anagitator shaft and threaded
27、ports to allow filling and for theattachment of air/nitrogen dioxide lines, vacuum control andrelief valves, and a temperature probe. Fig. A2.1 defines thelocations of these ports. Mill the bottom surface of thisstainless steel plate to accept a polytetrafluoroethylene (PTFE)ring seal for centered a
28、ttachment of the glass vessel as3For referenced ASTM standards, visit the ASTM website, 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 Internati
29、onal, 400 Commonwealth Drive, Warrendale, PA15096-0001, http:/www.sae.org.5Kinker, B. G., Romaszewski, R. A., and Palmer, P. A., “ROBOA BenchProcedure to Replace Sequence IIIGA Engine Test,” Journal of ASTM Interna-tional (JAI), Vol 4, No. 10, 2007, Paper ID JAI 100916. Available online fromwww.astm
30、.org.6The sole source of supply of the apparatus known to the committee at this timeis Ace Glass, Inc., P.O. Box 688, 1430 NW Blvd., Vineland, NJ 08362-0688.7If you are aware of alternative suppliers, please provide this information toASTM. Your comments will receive careful consideration at a meeti
31、ng of theresponsible technical committee1which you may attend.8Instatherm is a registered trademark ofAce Glass, Inc., P.O. Box 688, 1430 NWBlvd., Vineland, NJ 08362-0688.9The sole source of supply of the apparatus known to the committee at this timeis Reimel Machine, Inc., 2575 Wyandotte Rd., Willo
32、w Grove, PA 19090.D7528092described in Annex A3. Reimel Machine, Inc. part numberRMI-1007-DH7,9has been found suitable for this purpose.6.5 Stirrer MotorAn electric motor with drill chuck colletcapable of sustained operation at 200 6 5 r/min.6.6 StirrerAn 8-mm diameter stainless steel rod, 30-mmlong
33、 with a means of attaching a blade assembly at the bottom.The turbine blade assembly diameter is 2.58 in. with 1.4-mmthick blades attached at a 45 pitch with an overall blade heightof 0.985 in. Construct the stirrer as described in Annex A4.Reimel Machine, Inc. part number RMI-1001-DH7,9has beenfoun
34、d suitable for this purpose. Attach the stirrer to the reactorhead by means of a packing gland constructed as described inAnnex A5. Reimel Machine, Inc. part number RMI-1004-DH7,9has been found suitable for this application. Attach thestirrer to the stirrer motor by inserting the 8-mm steel rodthrou
35、gh the opening in the reactor head and the packing gland,and insert PTFE rope packing to create a seal. Position theblade 6 mm from the bottom of the vessel.6.7 Air Supply SystemCapable of delivering an uninter-rupted flow of dry air into the test oil via a subsurface feedthroughout the reaction tim
36、e period. An in-line, desiccant-charged, drying system has been found suitable. Ensure thesubsurface feed tube opening remains below the surface of thetest fluid for the duration of the test.NOTE 1As the amount of test oil remaining at the end of the test is notalways known at the beginning of the t
37、est, it is advisable to configure thedry-air tube location such that the opening of the 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-
38、mL capacity, with 0.1 mL graduations andhaving appropriate provisions for connection to the reactionvessels subsurface gas delivery systemsee Annex A6 formore details. By receiving liquid phase nitrogen dioxide froma gas bottle, this tube allows measurement of nitrogen dioxidedepletion from the tube
39、 over the course of the reaction.6.9 Temperature Control SystemA controller and probecapable of being programmed to control reaction temperaturevia low output wattage at or below 40 VAC and with anoperational hysteresis of 0.1 C using an on/off algorithm.Alternatively, a proportional-integral-deriva
40、tive (PID) algo-rithm may also be used. Position the temperature probe tip sothat it 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 v
41、iew of precision thatthe temperature is always monitored and controlled at thespecified 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 Serie
42、s, Order number 2C-17),7,10having a scale of 0.4 to4 Standard Cubic Feet per Minute (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 a3
43、8-in. inside diameter or larger. The machinedfitting for the bottom of the flow meter 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
44、flow rate. However, the definitions ofstandard conditions vary. In this method, the flow meter is calibrated withair at standard conditions defined as a temperature of 70F, a pressure of14.6 psia and 0 % relative humidity.6.10.2 Airflow Meter, with a scale calibrated in mL/min formeasuring subsurfac
45、e 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 6 0.1 SCFMwith 61 kPa vacuum for 40 h. Instructions for constructing thevacuum plumbing for t
46、he vessel are given in Annex A7.Asexplained inAnnexA7, it is critical to follow these instructionsprecisely.6.12 Vacuum Control ValveA stainless steel needle valvewith14-in. outside diameter tube connections and a flowcoefficient (Cv) of 0.37. A McMaster-Carr Supply Companyneedle valve part number 4
47、5585K867,11has been found suit-able for this application.6.13 Vacuum Trap SystemSupplies coolant at an inlettemperature 35D70 000ADetermine by Test Method D 445.BDetermine by Test Method D 4684.CThis viscosity is commonly referred to as the Mini Rotary Viscometer (MRV)viscosity (see also 12.2.1.1).D
48、Yield stress may be missed due to Test Method D 4684 test variability.D75280949.2.2.1 Transmit results to the TMC within 5 days of testcompletion via electronic data transfer protocol as outlined inthe Data Communication Committee, Electronic Test ReportTransmission Model (ETRTM). The ETRTM can be o
49、btainedfrom the TMC.29.2.3 Evaluation of Reference Oil Test ResultsThe TMCevaluates the reference-oil test results for both operationalvalidity and statistical acceptability. The TMC may consultwith the test laboratory in case of difficulty, as follows:9.2.3.1 Upon receipt of the reference-oil test results fromthe test laboratory, the TMC will evaluate the laboratorysreported operational parameters for compliance with the cur-rent test method. For operationally valid tests, the TMC willthen evaluate the pass/fail parameters for statistical validit
