1、Designation: D 2272 02An American National StandardStandard 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 t
2、he case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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. Scope1.1 Thi
3、s test method2utilizes an oxygen-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 as thestandard
4、.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 regulatory limitations prior to use. For specificw
5、arning statements, see 6.2, 6.4, 6.5, 6.6, 6.10, and 6.11.2. Referenced Documents2.1 ASTM Standards:B1 Specification for Hard-Drawn Copper Wire3D 235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Cleaning Solvent)4D 943 Test Method for Oxidation Characteristics of Inhib-ited
6、Mineral Oils5D 1193 Specification for Reagent Water6D2112 Test Method for Oxidation Stability of InhibitedMineral Insulating Oil by Pressure Vessel7D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products8D 4742 Test Method for Oxidation Stability of GasolineAutomotive Engine Oils by T
7、hin-Film Oxygen Uptake(TFOUT)82.2 British Standard:9B2 2000 Part 0: Section 0.1,IP 37C Thermometer2.3 Institute of Petroleum Standard:10IP 2293. 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 press
8、ure gage. The vessel is charged with oxygen to a gagepressure of 620 kPa (90 psi, 6.2 bar) (see Eq 1), placed in aconstant-temperature oil bath set at 150C, and rotated axiallyat 100 rpm at an angel of 30 from the horizontal. The numberof minutes required to reach a specific drop in gage pressure is
9、the oxidation stability of the test sample.100 kPa 5 1.00 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 intendedthat this test meth
10、od be a substitute for Test Method D 943or 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.NOTE 1A modification of the rotating vessel method has beenpublished as Test Method D211
11、2, which uses a similar procedure andapparatus but a lower (140C) bath temperature. Test Method D2112requires duplicate testing and Test Method D 2272 conducted duplicatetesting in the past.5. Apparatus5.1 Oxidation Vessel, Glass Sample Container with Four-Hole PTFE Disk, Hold-Down Spring, Catalyst-
12、Coil, Pressure1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.09 on Oxidation.Current edition approved August 10, 2002. Published October 2002. Originallypublished as D 2272-64 T. Last previous
13、edition D 2272-98.2von Fuchs, G. H., Claridge, E. L., and Zuidema, 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 Enginee
14、ring, Vol 16, No.1, January 1960, pp. 22-31.3Annual Book of ASTM Standards, Vol 02.03.4Annual Book of ASTM Standards, Vol 06.04.5Annual Book of ASTM Standards, Vol 05.01.6Annual Book of ASTM Standards, Vol 11.01.7Annual Book of ASTM Standards, Vol 10.03.8Annual Book of ASTM Standards, Vol 05.02.9Ava
15、ilable from British Standards Institute, 389 Chiswick High Rd., London,W4 4AL, United Kingdom.10Available from Institute of Petroleum, 61 New Cavendish St., London,W1G 7AR, United Kingdom.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Stat
16、es.Gage, Thermometer, and Test Bath, as described in Annex A1.The assembled apparatus is shown schematically in Fig. 1 andFig. A1.6.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to
17、 the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.11Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determi
18、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 (90psi, 6.2 bar). (WarningVigorously accelerates combustion.)6.
19、6 Potassium Hydroxide, Alcohol Solution (1 %)Dissolve 12 g of potassium hydroxide (KOH) pellets 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,
20、1.63 6 1%mm (0.064 6 1 % in.) in diameter (No. 16 Imperial StandardWire Gage or No. 14 American Wire Gage, 99.9 % purity,conforming to Specification B1. Soft copper wire of anequivalent grade may also be used.6.10 Petroleum Spirit, conforming to Specification D 235for petroleum spirit (mineral spiri
21、ts). (WarningCombustible. Health hazard.)6.11 Acetone, reagent grade. (WarningFlammable.Health hazard.)6.12 Reagent Water, conforming to Specification D 1193,Type II.7. Sampling7.1 Samples for this test method can come from tanks,drums, small containers, or even operating equipment. There-fore, use
22、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 free from abrasives with a clean, dry cloth.Wind the wire into a coil having an out
23、side 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 necessary. A new coil is used for eachsample. For extended storage, the prepared
24、coil may bepackaged in a dry, inert atmosphere. For overnight storage (lessthan 24 h), the coils may be stored in n-Heptane.NOTE 2Commercially available and prepackaged coils prepared asdescribed in 8.1 can also be used for the test.128.2 Cleaning of VesselWash the vessel body, cap, andinside of ves
25、sel stem with hot detergent solution and rinsethoroughly with water. Rinse the inside of the stem with11Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see An
26、alar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U. S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.12Prepackaged coils were provided for Spring 1995 round robin.FIG. 1 Schematic Drawing of the Rotary Vessel Test
27、ApparatusD2272022isopropyl alcohol and blow dry with clean compressed air. Ifthe vessel body, cap, or inside of the stem smells sour aftersimple cleaning, wash with 1 % alcoholic KOH solution andrepeat as before. (WarningFailure to remove oxidationresidue can adversely affect test results.)8.3 Clean
28、ing of Glass ContainerDrain and rinse with asuitable solvent (for example, petroleum spirit or acetone).Soak or scrub in an aqueous detergent solution. Brush thor-oughly and flush thoroughly with tap water. Rinse withisopropyl alcohol, followed by distilled water and air dry. Ifany insolubles remain
29、, soak overnight in an acid-type cleaningsolution and repeat the above procedure starting from the tapwater flush.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
30、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.Add another5 mL of reagent water to the vessel body and slide the samplecontainer into t
31、he vessel body (see Note 3). Cover the glasscontainer with a 57.2mm (214 in.) PTFE disk and place ahold-down spring13on 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
32、cap into the vessel body.NOTE 3The water between the vessel wall and the sample containeraids heat transfer.9.1.1 Tighten the closure ring by hand. Cover the threads ofthe gage-nipple with a thin coating of stopcock grease (PTFEpipe tape is a suitable alternative to the use of stopcock grease)and sc
33、rew the gage into the top center of the vessel stem.Attach the oxygen line with an inline pressure gage to the inletvalve on the vessel stem. Slowly turn on the oxygen supplyvalve until the pressure has reached 620 kPa (90 psi, 6.2 bar).Turn off the oxygen supply valve. Slowly release pressure byloo
34、sening the fitting or by using an inline bleeder valve. Repeatpurging process two more times; purge step should takeapproximately 3 min. Adjust the regulating valve on theoxygen supply tank to 620 kPa (90 psi, 6.2 bar) at a roomtemperature of 25C (77F). For each 2.0C (3.6F) above orbelow this temper
35、ature, 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. If desired, test the vessel for leaks byimmersing in water (see Note 4).NOTE 4If the vessel was immersed in water
36、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 sputtering.9.2 OxidationBring the heating bath to the test tempera-ture while the
37、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 5). The bath temperatureshall stabilize at the test temperature within 15 m
38、in after thevessel is inserted. Maintain the test temperature within 60.1C (see Note 6).NOTE 5The 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 ofcond
39、itions 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. 2.NOTE 6Maintaining the correct temperature within the specifiedlimits of 6 0.1C during the entire test run is an important facto
40、r assuringboth repeatability and reproducibility of test results.13PTFE disk with 4-holes and hold down spring were provided for Spring 1995round robin.FIG. 2 Pressure Versus Times Plot of Two Rotary Vessel Oxidation Test RunsD22720239.3 Keep the vessel completely submerged and maintaincontinuous an
41、d 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) below the maximum pressure (seeNote 7). The 175 kPa
42、 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 8).NOTE 7While termination of the test at a 175 kPa (25.4 psi, 1.75 bar)pressure drop is the standard
43、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 8A typical experiment is shown in Fig. 2 as Curve A. The
44、maximum 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 difficult to evaluate. The gradualdecrease in pressure
45、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 valid.9.5 After termination of the test, the vessel sha
46、ll 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 water toquickly bring it to room temperature. Altern
47、ately, the vesselcan be cooled to room temperature in air. The excess oxygenpressure is bled off and the vessel opened.10. Report10.1 Interpretation of Results:10.1.1 In reference to Fig. 2, Curve A, observe the plot ofthe recorded pressure versus time and establish the plateau (seeNote 8). Record t
48、he time at the point on the falling part of thecurve where the pressure is 175 kPa (25.4 psi, 1.75 bar) lessthan the established plateau pressure. If the test is repeated, theplateau pressures in repeat tests should not differ by more than35 kPa (5.1 psi, 0.35 bar).10.1.2 In reference to Fig. 2, Cur
49、ve B, observe the plot ofthe recorded pressure versus time and establish the maximumpressure obtained during the initial 30 min of the experiment(see Note 8). Record the time on the falling part of the curvewhere the pressure is 175 kPa (25.4 psi, 1.75 bar) less than theestablished maximum pressure. If the test is repeated, maxi-mum pressures in repeat tests should not differ by more than 35kPa (5.1 psi, 0.35 bar).10.2 Report the Results:10.2.1 In reference to Fig. 2, Curve A, the vessel life of thesample is the time in minutes from the start of the t
