1、Designation: D2272 11Standard Test Method forOxidation Stability of Steam Turbine Oils by RotatingPressure Vessel1This standard is issued under the fixed designation D2272; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method2utilizes an oxyge
3、n-pressured vessel toevaluate the oxidation stability of new and in-service turbineoils having the same composition (base stock and additives) inthe presence of water and a copper catalyst coil at 150C.1.2 Appendix X1 describes a new optional turbine oil(unused) sample nitrogen purge pretreatment pr
4、ocedure fordetermining the percent residual ratio of RPVOT value for thepretreated sample divided by RPVOT value of the new(untreated) oil, sometimes referred to as a “% RPVOT Reten-tion.” This nitrogen purge pretreatment approach was designedto detect volatile antioxidant inhibitors that are not de
5、sirablefor use in high temperature gas turbines.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3.1 ExceptionOther units are provided in parentheses(psi, grams, and inches), because they are either the industryaccepted sta
6、ndard or the apparatus is built according the figuresin this standard, or both.1.4 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 dete
7、rmine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 6.2, 6.4, 6.5, 6.6, and 6.10.2. Referenced Documents2.1 ASTM Standards:3B1 Specification for Hard-Drawn Copper WireD943 Test Method for Oxidation Characteristics of Inhib-ited Mineral OilsD1193 Speci
8、fication for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4742 Test Method for Oxidation Stability of GasolineAutomotive Engine Oils by Thin-Film Oxygen Uptake(TFOUT)D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Eval
9、uate AnalyticalMeasurement System Performance2.2 Energy Institute Standard:4IP 229 Determination of the relative oxidation stability byrotating bomb of mineral turbine oil3. Summary of Test Method3.1 The test oil, water, and copper catalyst coil, contained ina covered glass container, are placed in
10、a vessel equipped witha pressure gauge. The vessel is charged with oxygen to a gaugepressure of 620 kPa (90 psi, 6.2 bar) (see Eq 1), placed in aconstant-temperature oil bath set at 150C or dry block taken to150C (Fig. 1 and Fig. 2), and rotated axially at 100 rpm at anangle of 30 from the horizonta
11、l.3.2 The number of minutes required to reach a specific dropin gauge pressure is the oxidation stability of the test sample.100 kPa 5 1.00 bar 5 14.5 psi (1)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of Subc
12、ommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved May 1, 2011. Published May 2011. Originallyapproved in 1964. Last previous edition approved in 2009 as D227209. DOI:10.1520/D2272-11.2von Fuchs, G. H., Claridge, E. L., and Zuidema, H. H., “The Rotary BombOxidation Test for Inhi
13、bited Turbine Oils,” Materials Research and Standards,MTRSA (formerly ASTM Bulletin), No. 186, December 1952, pp. 43-46; vonFuchs, G. H., “Rotary Bomb Oxidation Test,” Lubrication Engineering, Vol 16,No. 1, January 1960, pp. 22-31.3For referenced ASTM standards, visit the ASTM website, www.astm.org,
14、 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 Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.1*A Summary of Changes s
15、ection appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and Use4.1 The estimate of oxidation stability is useful in control-ling the continuity of this property for batch acceptance o
16、fproduction lots having the same operation. It is not intendedthat this test method be a substitute for Test Method D943 or beused to compare the service lives of new oils of differentcompositions.4.2 This test method is also used to assess the remainingoxidation test life of in-service oils.Method
17、A5. Apparatus5.1 Method A, Liquid Bath RPVOTOxidation Vessel,Glass Sample Container with Four-Hole PTFE Disk, Hold-Down Spring, Catalyst-Coil, Pressure Gauge, Thermometer,and Test Bath as described in Annex A1. The assembledapparatus is shown schematically in Fig. 1 and Fig. A1.6.5.2 Method B, Dry B
18、lock Bath RPVOTSee Section 13 forthis additional option.FIG. 1 Schematic Drawing of the Rotary Vessel Test ApparatusFIG. 2 RPVOT Metal Block Bath InstrumentD2272 1126. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests in the final cleaning stages. Unless o
19、therwiseindicated, it is intended that all reagents conform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society where such specifications areavailable.5Other grades may be used, provided it is firstascertained that the reagent is of sufficiently high purity t
20、opermit its use without lessening the accuracy of the determi-nation.6.2 Isopropyl Alcohol, reagent grade. (WarningFlammable. Health hazard.)6.3 Liquid Detergent.6.4 n-Heptane, 99.0 minimum mol % (pure grade).(WarningFlammable. Health hazard.)6.5 Oxygen, 99.5 %, with pressure regulation to 620 kPa (
21、90psi, 6.2 bar). (WarningVigorously accelerates combustion.)6.6 Potassium Hydroxide, Alcohol Solution (1 %)Dis-solve 12 g of potassium hydroxide (KOH) pellets in 1 L of theisopropyl alcohol. (WarningFlammable. Health hazard.)6.7 Silicone Carbide Abrasive Cloth, 100-grit with clothbacking.6.8 Silicon
22、e Stopcock Grease.6.9 Wire Catalyst, Electrolytic Copper Wire, 1.63 6 1%mm (0.064 6 1 % in.) in diameter (No. 16 Imperial StandardWire Gauge or No. 14 American Wire Gauge, 99.9 % purity,conforming to Specification B1. Soft copper wire of anequivalent grade may also be used.6.10 Acetone, reagent grad
23、e. (WarningFlammable.Health hazard.)6.11 Reagent Water, conforming to Specification D1193,Type II.7. Sampling7.1 Samples for this test method can come from tanks,drums, small containers, or even operating equipment. There-fore, use the applicable apparatus and techniques described inPractice D4057.8
24、. Preparation of Apparatus8.1 Catalyst PreparationBefore use, polish approxi-mately3mofthecopper wire with a silicon carbide abrasivecloth and wipe free from abrasives with a clean, dry cloth.Wind the wire into a coil having an outside diameter 44 to 48mm and weight of 55.6 6 0.3 g and stretched to
25、a height of 40to 42 mm. Clean the coil thoroughly with isopropyl alcohol,air-dry, and insert inside the glass sample container by aturning motion, if necessary. A new coil is used for eachsample. For extended storage, the prepared coil may bepackaged in a dry, inert atmosphere. For overnight storage
26、 (lessthan 24 h), the coils may be stored in n-Heptane.NOTE 1Commercially available and prepackaged coils prepared asdescribed in 8.1 can also be used for the test.68.2 Cleaning of VesselWash the vessel body, cap, andinside of vessel stem with a suitable solvent (for example,petroleum spirit, heptan
27、e, or acetone.) Wash with hot detergentsolution and rinse thoroughly with water. Rinse the inside ofthe stem with isopropyl alcohol and blow dry with cleancompressed air. Keep the plastic valve out of the hot detergentto prevent its deterioration. Failure to remove oxidation residuecan adversely aff
28、ect test results.8.3 Cleaning of Glass ContainerDrain and rinse with asuitable solvent (for example, non-reagent petroleum spirit,heptane, or acetone). Soak or scrub in an aqueous detergentsolution. Brush thoroughly and flush thoroughly with tap water.Rinse with isopropyl alcohol, followed by distil
29、led water andair dry. If any insolubles remain, soak overnight in an acid-typecleaning solution and repeat the above procedure starting fromthe tap water flush. Do not use chipped or cracked glassware.8.4 Cleaning of Polytetrafluoroethylene (PTFE) DiskRemove any residual oil with a suitable solvent
30、and clean bybrushing with detergent solution. Rinse thoroughly with tapwater, followed by distilled water rinse and air dry.9. Procedure9.1 ChargingWeigh the glass sample container with afreshly cleaned catalyst coil. Weigh 50 6 0.5 g of oil sampleinto the container; also add 5 mL of reagent water.A
31、dd another5 mL of reagent water to the vessel body and slide the samplecontainer into the vessel body (see Note 2). Cover the glasscontainer with a 57.2mm (214 in.) PTFE disk and place ahold-down spring7on top of the PTFE disk. Apply a thincoating of silicone stopcock grease to the O-ring vessel sea
32、llocated in the gasket groove of the vessel cap to providelubrication, and insert the cap into the vessel body.NOTE 2The water between the vessel wall and the sample containeraids heat transfer.9.1.1 Tighten the closure ring by hand. Cover the threads ofthe gauge-nipple with a thin coating of stopco
33、ck grease (PTFEpipe tape is a suitable alternative to the use of stopcock grease)and screw the gauge into the top center of the vessel stem.Attach the oxygen line with an inline pressure gauge to theinlet valve on the vessel stem. Slowly turn on the oxygensupply valve until the pressure has reached
34、620 kPa (90 psi, 6.2bar). Turn off the oxygen supply valve. Slowly release pressureby loosening the fitting or by using an inline bleeder valve.Repeat purging process two more times; purge step should takeapproximately 3 min. Adjust the regulating valve on theoxygen supply tank to 620 6 1.4 kPa (90
35、psi, 6.2 bar) at a roomtemperature of 25C (77F). For each 2.0C (3.6F) above orbelow this temperature, 5 kPa (0.7 psi, 0.05 bar) shall be addedor subtracted to attain the required initial pressure. Fill thevessel to this required pressure and close the inlet valvesecurely by hand. Open the pressure v
36、alve one more time andwatch the pressure gauge to make certain it is not decreasing.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for
37、LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.6Prepackaged coils were provided for RR:D02-1409.7PTFE disk with 4-holes and hold down spring were provided for RR:D02-1409.D2272 113
38、If not, then close the valve. If desired, test the vessel for leaksby immersing in water (see Note 3).NOTE 3If the vessel was immersed in water to check for leaks, dry theoutside of the wet vessel by any convenient means such as airblast or atowel. Such drying is advisable to prevent subsequent intr
39、oduction of freewater into the hot oil bath which would cause sputtering. For safetypurposes, a face shield is recommended during the charging process.9.2 OxidationBring the heating bath to the test tempera-ture while the stirrer is in operation. Switch off stirrer, insert thevessel into the carriag
40、es, and note the time. Restart the stirrer.If an auxiliary heater is used, keep it on for the first 5 min ofthe run and then turn it off (see Note 4). The bath temperatureshall stabilize at the test temperature within 15 min after thevessel is inserted. Maintain the test temperature within 60.1C(see
41、 Note 5).NOTE 4The time for the bath to reach the operating temperature afterinsertion of the vessel may differ for different apparatus assemblies andshould be observed for each unit. The objective is to find a set ofconditions that does not permit a drop of more than 2C after insertion ofthe vessel
42、 and allows the vessel pressure to reach a plateau within 30 minas shown in Curve A of Fig. 3.NOTE 5Maintaining the correct temperature within the specifiedlimits of 6 0.1C during the entire test run is an important factor assuringboth repeatability and reproducibility of test results.9.3 Keep the v
43、essel completely submerged and maintaincontinuous and uniform rotation throughout the test.Astandardrotational speed of 100 6 5 rpm is required; any appreciablevariations in this speed could cause erratic results.9.4 The test is complete after the pressure drops more than175 kPa (25.4 psi, 1.75 bar)
44、 below the maximum pressure (seeNote 6). The 175 kPa pressure drop usually, but not always,coincides with an induction-type period of rapid pressure drop.When it does not, the operator may question whether he hasproduced a valid experiment (see Note 7).NOTE 6While termination of the test at a 175 kP
45、a (25.4 psi, 1.75 bar)pressure drop is the standard procedure, some operators may elect to stopthe test at lesser pressure drops or to observe the condition of the oil aftera predetermined test period of perhaps 100 min; that is, well within thenormal induction period of new inhibited oils.NOTE 7A t
46、ypical experiment is shown in Fig. 3 as Curve A. Themaximum pressure is expected to be reached within 30 min, a pressureplateau is established, and an induction-type pressure drop is observed.Curve B, in which there is a gradual decrease in pressure before theinduction break is recorded, is more dif
47、ficult to evaluate. The gradualdecrease in pressure could be due to a vessel leak, although some syntheticfluids will generate this type of curve. If a leak is suspected, repeat the testin a different vessel. If the same type of curve is derived when the test isrepeated, the experiment is likely val
48、id.9.5 After termination of the test, the vessel shall be removedfrom the oil bath and cooled to room temperature. The vesselcan be briefly dipped into and swirled around in a bath of lightmineral oil to wash off the adhering bath oil. The vessel isrinsed off with hot water, then immersed into cold
49、water toquickly bring it to room temperature. Alternately, the vesselcan be cooled to room temperature in air. The excess oxygenpressure is bled off and the vessel opened.10. Quality Control Monitoring10.1 The performance of the equipment should be con-firmed by analyzing quality control (QC) sample(s).10.2 Prior to monitoring the measurement process, deter-mine the average value and control limits for the QC sample.10.3 Record QC results and analyze by control charts orother statistically equivalent techniques to ascertain the statis-tical cont
