1、Designation: D 2272 09Standard Test Method forOxidation Stability of Steam Turbine Oils by RotatingPressure Vessel1This standard is issued under the fixed designation D 2272; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method2utilizes an oxy
3、gen-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 The values stated in SI units are to be regarded asstandard. No other units of measurement a
4、re included in thisstandard.1.2.1 ExceptionOther units are provided in parentheses(psi, grams, and inches), because they are either the industryaccepted standard or the apparatus is built according the figuresin this standard, or both.1.3 This standard does not purport to address all of thesafety co
5、ncerns, 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 regulatory limitations prior to use. For specificwarning statements, see 6.2, 6.4, 6.5, 6.6, and 6.10.2. Referenced
6、Documents2.1 ASTM Standards:3B1 Specification for Hard-Drawn Copper WireD 943 Test Method for Oxidation Characteristics of Inhib-ited Mineral OilsD 1193 Specification for Reagent WaterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4742 Test Method for Oxidation Stability of
7、GasolineAutomotive Engine Oils by Thin-Film Oxygen Uptake(TFOUT)D 6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance2.2 Energy Institute Standard:4IP 229 Determination of the relative oxidation stability byrota
8、ting 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 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), place
9、d 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 horizontal.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
10、 bar 5 14.5 psi (1)4. Significance and Use4.1 The estimate of oxidation stability is useful in control-ling the continuity of this property for batch acceptance ofproduction lots having the same operation. It is not intended1This test method is under the jurisdiction of ASTM Committee D02 onPetroleu
11、m Products and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved June 15, 2009. Published September 2009. Originallyapproved in 1964. Last previous edition approved in 2002 as D 227202.2von Fuchs, G. H., Claridge, E. L., and Zu
12、idema, H. H., “The Rotary BombOxidation Test for Inhibited 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
13、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 Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K.,
14、 http:/www.energyinst.org.uk.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.that this test method be a substitute for Test Method D 943 orbe used to compare the servi
15、ce 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 A5. Apparatus5.1 Method A, Liquid Bath RPVOTOxidation Vessel,Glass Sample Container with Four-Hole PTFE Disk, Hold-Down Spring, Catalyst-Coil, Pressure
16、 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 Block Bath RPVOTSee Section 13 forthis additional option.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all test
17、s in the final cleaning stages. Unless otherwiseindicated, it is intended that all reagents conform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society where such specifications areFIG. 1 Schematic Drawing of the Rotary Vessel Test ApparatusFIG. 2 RPVOT Metal
18、 Block Bath InstrumentD2272092available.5Other grades may be used, provided it is firstascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.6.2 Isopropyl Alcohol, reagent grade. (WarningFlammable. Health hazard.)6.3 Liquid
19、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 (90psi, 6.2 bar). (WarningVigorously accelerates combustion.)6.6 Potassium Hydroxide, Alcohol Solution (1 %)Dissolve 12 g of potassium hydroxide (KOH) pe
20、llets in 1 L ofthe isopropyl alcohol. (WarningFlammable. Health hazard.)6.7 Silicone Carbide Abrasive Cloth, 100-grit with clothbacking.6.8 Silicone 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 Am
21、erican Wire Gauge, 99.9 % purity,conforming to Specification B1. Soft copper wire of anequivalent grade may also be used.6.10 Acetone, reagent grade. (WarningFlammable.Health hazard.)6.11 Reagent Water, conforming to Specification D 1193,Type II.7. Sampling7.1 Samples for this test method can come f
22、rom tanks,drums, small containers, or even operating equipment. There-fore, use the applicable apparatus and techniques described inPractice D 4057.8. Preparation of Apparatus8.1 Catalyst PreparationBefore use, polish approxi-mately3mofthecopper wire with a silicon carbide abrasivecloth and wipe fre
23、e 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 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 n
24、ecessary. A new coil is used for eachsample. For extended storage, the prepared coil may bepackaged in a dry, inert atmosphere. For overnight storage (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
25、for the test.68.2 Cleaning of VesselWash the vessel body, cap, andinside of vessel stem with a suitable solvent (for example,petroleum spirit, heptane, or acetone.) Wash with hot detergentsolution and rinse thoroughly with water. Rinse the inside ofthe stem with isopropyl alcohol and blow dry with c
26、leancompressed air. Keep the plastic valve out of the hot detergentto prevent its deterioration. Failure to remove oxidation residuecan adversely affect test results.8.3 Cleaning of Glass ContainerDrain and rinse with asuitable solvent (for example, non-reagent petroleum spirit,heptane, or acetone).
27、 Soak or scrub in an aqueous detergentsolution. Brush thoroughly and flush thoroughly with tap water.Rinse with isopropyl alcohol, followed by distilled water andair dry. If any insolubles remain, soak overnight in an acid-typecleaning solution and repeat the above procedure starting fromthe tap wat
28、er flush. Do not use chipped or cracked glassware.8.4 Cleaning of Polytetrafluoroethylene (PTFE) DiskRemove any residual oil with a suitable solvent and clean bybrushing with detergent solution. Rinse thoroughly with tapwater, followed by distilled water rinse and air dry.9. Procedure9.1 ChargingWei
29、gh 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.Add 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.
30、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 seallocated 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
31、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 stopcock 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
32、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 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
33、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 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 subtra
34、cted to attain the required initial pressure. Fill thevessel to this required pressure and close the inlet valvesecurely by hand. Open the pressure valve one more time andwatch the pressure gauge to make certain it is not decreasing.If not, then close the valve. If desired, test the vessel for leaks
35、by 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 introduction of freewater into the hot oil bath which would cause sputt
36、ering. For safetypurposes, a face shield is recommended during the charging process.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.D227209
38、39.2 OxidationBring the heating bath to the test tempera-ture while the stirrer is in operation. Switch off stirrer, insert thevessel into the carriages, 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).
39、 The bath temperatureshall stabilize at the test temperature within 15 min after thevessel is inserted. Maintain the test temperature within 60.1C(see Note 5).NOTE 4The time for the bath to reach the operating temperature afterinsertion of the vessel may differ for different apparatus assemblies and
40、should 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 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 spe
41、cifiedlimits of 6 0.1C during the entire test run is an important factor assuringboth repeatability and reproducibility of test results.9.3 Keep the vessel completely submerged and maintaincontinuous and uniform rotation throughout the test.Astandardrotational speed of 100 6 5 rpm is required; any a
42、ppreciablevariations 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) below the maximum pressure (seeNote 6). The 175 kPa pressure drop usually, but not always,coincides with an induction-type period of rapid pressure d
43、rop.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 kPa (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 con
44、dition of the oil aftera predetermined test period of perhaps 100 min; that is, well within thenormal induction period of new inhibited oils.NOTE 7A typical 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
45、 induction-type pressure drop is observed.Curve B, in which there is a gradual decrease in pressure before theinduction break is recorded, is more difficult to evaluate. The gradualdecrease in pressure could be due to a vessel leak, although some syntheticfluids will generate this type of curve. If
46、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 valid.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 int
47、o 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 water toquickly bring it to room temperature. Alternately, the vesselcan be cooled to room temperature in air. The excess oxygenpressure is bled off a
48、nd 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 ana
49、lyze by control charts orother statistically equivalent techniques to ascertain the statis-tical control status of the total test process. Investigate any outof control data for root cause(s).10.4 The frequency of QC testing is dependent on thecriticality of the measurement, the demonstrated stability of thetesting process, and customer requirements. The QC sampletesting precision should be periodically checked against theexpected test precision to ensure data quality.10.5 It is recommended that, if possible, the type of QCsample that is regularly
