1、Designation: D7528 13Standard 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 n
2、umber 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 Test
3、 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, various
4、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 laborator
5、ies 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 memoran
6、da related to the method.1. Scope*1.1 This test method describes a bench procedure to simu-late the oil aging encountered in Test Method D7320, theSequence IIIG engine test method. These aged oils are thentested for kinematic viscosity and for low-temperature pump-ability properties as described in
7、the Sequence IIIGA enginetest, Appendix X1 of Test Method D7320.1.2 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 wher
8、e 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 regulato
9、ry 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 Test S
10、tand 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 A5Nitrogen D
11、ioxide Graduated Tube Annex A6Vacuum System Plumbing Annex A7Vacuum Trap Condensers Annex A8Setting the Vacuum Control Valve Annex A9AppendixesSample Preparation and Addition Appendix X1Charging the Liquid Nitrogen Dioxide Appendix X2Nitrogen Dioxide Precision Needle Valve Appendix X31This test meth
12、od is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.B0.07 on Development and Surveillance of Bench Tests Methods.Current edition approved May 1, 2013. Published June 2013. Originallyapproved in 2009. Last previous
13、 edition approved in 2009 as D7528 09. DOI:10.1520/D7528-13.2ASTM Test Monitoring Center, 6555 PennAvenue, Pittsburgh, PA15206-4489.www.astmtmc.cmu.edu.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken
14、, PA 19428-2959. United States1SectionExample of an Assembled ROBO Apparatus Appendix X4Information Package to Aid Setting Up a New Robo Apparatus Appendix X52. Referenced Documents2.1 ASTM Standards:3D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynam
15、ic Viscos-ity)D4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD4485 Specification for Performance of Active API ServiceCategory Engine OilsD4684 Test Method for Determination of Yield Stress andApparent Viscosity of Engine Oils at Low TemperatureD5293 Test Method for Appare
16、nt Viscosity of Engine Oilsand Base Stocks Between 5 and 35C Using Cold-Cranking SimulatorD7320 Test Method for Evaluation of Automotive EngineOils in the Sequence IIIG, Spark-Ignition Engine2.2 SAE Standard:4SAE J300 Engine Oil Viscosity Classification3. Terminology3.1 Definitions:3.1.1 candidate o
17、il, nan oil that is intended to have theperformance characteristics necessary to satisfy a specificationand is to be tested against that specification. D41753.1.2 reference oil, nan oil of known performancecharacteristics, used as a basis for comparison.3.1.2.1 DiscussionReference oils are used to c
18、alibratetesting facilities, to compare the performance of other oils, orto evaluate other materials (such as seals) that interact withoils. D41753.1.3 non-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
19、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 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
20、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 flowingacross the liquid surface under negative pressure. In addition,nitrogen dioxide and air are introduced below the reactionsurface
21、. After cooling, the oxidized, concentrated test oil issubjected to pertinent viscometric tests. Evaporated oil iscondensed in order to weigh it and calculate evaporative loss.5. Significance and Use5.1 This bench test method is intended to produce compa-rable oil aging characteristics to those obta
22、ined 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 oilscomparable to those from the Sequence IIIG engine test, themeasured increases in kinematic and MRV viscosity indicatethe tendency o
23、f an oil to thicken because of volatilization andoxidation, as in the Sequence IIIG and IIIGA(seeAppendix X1in Test Method D7320) engine tests, respectively.5.3 This bench test procedure has potential use in specifi-cations and classifications of engine lubricating oils, such asSpecification D4485.6
24、. 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 resolution of 0.001 g.6.2 Fume Hood, that vents to the outside atmosphere (seeSection 8).6.3 Reaction Vess
25、el (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 Instatherm8,7coating, rated at approxi-mately 400 W, for heating the test mixture.Adiagram is shownin Fig. A1.1.6.4 Vessel Hea
26、dThe vessel head is a stainless steel plate ofsufficient diameter to 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
27、 as described in Annex A2. Users may alsosource some parts from Reimel 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 p
28、robe. Fig. A2.1 defines the locations ofthese ports. Mill the bottom surface of this stainless steel plate3For 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 standa
29、rds Document Summary page onthe ASTM website.4Available from SAE International, 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 International(JAI),
30、 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 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 informa
31、tion toASTM. Your comments will receive careful consideration at a meeting 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
32、committee at this timeis Reimel Machine, Inc., 2575 Wyandotte Rd., Willow Grove, PA 19090.D7528 132to accept a polytetrafluoroethylene (PTFE) ring seal for cen-tered attachment of the glass vessel as described in Annex A3.Reimel Machine, Inc. part number RMI-1007-DH9,7has beenfound suitable for this
33、 purpose.6.5 Stirrer MotorAn electric motor with drill chuck colletcapable of sustained operation at 200 r/min 6 5 r/min.6.6 StirrerAn 8 mm diameter stainless steel rod, 30 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
34、.4 mm thick blades attached at a 45 pitch with an overallblade height of 0.985 in. (25.0 mm). Construct the stirrer asdescribed in Annex A4. Reimel Machine, Inc. part numberRMI-1001-DH9,7has been found suitable for this purpose.Attach the stirrer to the reactor head by means of a packinggland constr
35、ucted as described in Annex A5. Reimel Machine,Inc. part number RMI-1004-DH9,7has been found suitable forthis application. Attach the stirrer to the stirrer motor byinserting the 8 mm steel rod through the opening in the reactorhead and the packing gland, and insert PTFE rope packing tocreate a seal
36、. Position the blade 6 mm from the bottom of thevessel.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. Ensure thesubsurface f
37、eed 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 test, it is advisable to configure thedry-air tube location such that the opening of the tube is as clo
38、se 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 the reactionve
39、ssels 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 over the course of the reaction.6.9 Temperature Control SystemA controller and probecapable of being
40、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 is level with th
41、e 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 thespecified position insi
42、de 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 (SCFM), with14-in
43、. 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 shall accommoda
44、te the14-in. (6.35 mm) 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 flow me
45、ter 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 subsurface airflow of 185 mL/min in 10.3.1 and10.3.2.6.11 Vacuum SystemA pump with a free air capabi
46、lity 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 the vessel are given in Annex A7.Asexplained in AnnexA7, it is critical to follow these inst
47、ructionsprecisely.6.12 Vacuum Control ValveA stainless steel needle valvewith14-in. (6.35 mm) outside diameter tube connections and aflow coefficient (Cv) of 0.37. A McMaster-Carr Supply Com-pany needle valve part number 45585K8611, 7has been foundsuitable for this application.6.13 Vacuum Trap Syste
48、mSupplies coolant at an inlettemperature 35D70 000ADetermine by Test Method D445.BDetermine by Test Method D4684.CThis viscosity is commonly referred to as the Mini Rotary Viscometer (MRV)viscosity (see also 12.2.1.1).DYield stress may be missed due to Test Method D4684 test variability.D7528 134pri
49、or knowledge of acceptable results in assessing the testresults. The TMC will determine which specific reference oilthe laboratory shall test.9.2.1.2 Assign a test number to each ROBO test.9.2.1.3 During the time of conducting a reference oil test onone test stand, non-reference oil tests may be conducted onother previously calibrated stands.9.2.2 Reporting of Reference Oil Test ResultsReport theresults of all reference oil tests to the TMC according to thefollowing directive:9.2.2.1 Transmit results to the TMC within 5 days of testcompletion v
