1、Designation: D2272 11D2272 14Standard 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, th
2、e year 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 U.S. Department of Defense.1. Scope*1.1 This test method2 uti
3、lizes an oxygen-pressured vessel to evaluate the oxidation stability of new and in-service turbine oilshaving the same composition (base stock and additives) in the presence of water and a copper catalyst coil at 150C.1.2 Appendix X1 describes a new optional turbine oil (unused) sample nitrogen purg
4、e pretreatment procedure for determiningthe percent residual ratio of RPVOTvalue for the pretreated sample divided by RPVOTvalue of the new (untreated) oil, sometimesreferred to as a “% RPVOT Retention.” This nitrogen purge pretreatment approach was designed to detect volatile antioxidantinhibitors
5、that are not desirable for use in high temperature gas turbines.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3.1 ExceptionOther units are provided in parentheses (psi, grams, and inches), because they are either the i
6、ndustry acceptedstandard or the apparatus is built according the figures in this standard, or both.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and healt
7、h practices and determine the applicability of regulatorylimitations prior to use. For specific warning 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 Inhibited Miner
8、al OilsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4742 Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake (TFOUT)D6299 Practice for Applying Statistical Quality Assurance and Control Chart
9、ing Techniques to Evaluate Analytical Measure-ment System Performance2.2 Energy Institute Standard:4IP 229 Determination of the relative oxidation stability by rotating bomb of mineral turbine oilRelative Oxidation Stability byRotating Bomb of Mineral Turbine Oil2.3 ISO Standard:5ISO 3170 Petroleum
10、LiquidsManual Sampling1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.09.0C on Oxidation of Turbine Oils.Current edition approved May 1, 2011July 1, 2014. Published May
11、 2011August 2014. Originally approved in 1964. Last previous edition approved in 20092011 asD2272D2272 11.09. DOI: 10.1520/D2272-11.10.1520/D2272-14.2 von Fuchs, G. H., Claridge, E. L., and Zuidema, H. H., “The Rotary Bomb Oxidation Test for Inhibited Turbine Oils,” Materials Research and Standards,
12、 MTRSA(formerlyASTM Bulletin), No. 186, December 1952, pp. 43-46;46; von Fuchs, G. H., “Rotary Bomb Oxidation Test,” Lubrication Engineering, Vol 16, No.1, January 1960,pp. 22-31.31.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.or
13、g. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.4 Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.5 Available from American National Standards Institute (ANSI), 25 W. 43
14、rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all change
15、s accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr
16、Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Summary of Test Method3.1 The test oil, water, and copper catalyst coil, contained in a covered glass container, are placed in a vessel equipped with apressure gauge. The vessel is charged with oxygen to a gauge pressure o
17、f 620 kPa (90 psi, 6.2 bar) (see Eq 1), placed in aconstant-temperature oil bath set at 150C or dry block taken to 150C (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 drop in gauge pressure is the oxidat
18、ion stability of the test sample.100 kPa51.00 bar514.5 psi (1)4. Significance and Use4.1 The estimate of oxidation stability is useful in controlling the continuity of this property for batch acceptance of productionlots having the same operation. It is not intended that this test method be a substi
19、tute for Test Method D943 or be used to comparethe service lives of new oils of different compositions.4.2 This test method is also used to assess the remaining oxidation test life of in-service oils.Method A5. Apparatus5.1 MethodA, Liquid Bath RPVOTOxidationVessel, Glass Sample Container with Four-
20、Hole PTFE Disk, Hold-Down Spring,Catalyst-Coil, Pressure Gauge, Thermometer, and Test Bath as described in Annex A1. The assembled apparatus is shownschematically in Fig. 1 and Fig. A1.6.5.2 Method B, Dry Block Bath RPVOTSee Section 13 for this additional option.5.3 Temperature DisplayThe temperatur
21、e shall have a displayed resolution to 0.1C or better and be calibrated as describedin Annex A1 on an annual basis.5.4 Pressure DisplayThe pressure readout, whether analog or digital, shall be calibrated as described in Annex A1.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals
22、shall be used in all tests in the final cleaning stages. Unless otherwiseindicated, it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the AmericanChemical Society where such specifications are available.6 Other grades may be used, provided it i
23、s first ascertained that thereagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.6 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed byt
24、he American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.FIG. 1 Schematic Drawing of the Rotary Vessel Test ApparatusD2272 1426.2 Iso
25、propyl 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 (90 psi, 6.2 bar). ( WarningVigorously accelerates combustion.)6.6 Potassium
26、 Hydroxide, Alcohol Solution (1 %)Dissolve 12 g of potassium hydroxide (KOH) pellets in 1 L of the isopropylalcohol. (WarningFlammable. Health hazard.)6.7 Silicone Carbide Abrasive Cloth, 100-grit with cloth backing.6.8 Silicone Stopcock Grease.6.9 Wire Catalyst, Electrolytic Copper Wire, 1.63 6 1 %
27、 mm (0.064 6 1 % in.) in diameter (No. 16 Imperial Standard WireGauge or No. 14 American Wire Gauge, 99.9 % purity, conforming to Specification B1. Soft copper wire of an equivalent grademay also be used.6.10 Acetone, reagent grade. (WarningFlammable. Health hazard.)6.11 Reagent Water, conforming to
28、 Specification D1193, Type II.7. Sampling7.1 Samples for this test method can come from tanks, drums, small containers, or even operating equipment. Therefore, usethe applicable apparatus and techniques described in PracticeAs the results obtained by this method are readily affected by tracesof impu
29、rities, avoid contamination during sampling and subsequent handling; especially for used fluids. Samples shall be preparedand decanted in accordance D4057.with the procedures given in ISO 3170 and stored away from light in dark colored bottles.8. Preparation of Apparatus8.1 Catalyst PreparationBefor
30、e use, polish approximately 3 m of the copper wire with a silicon carbide abrasive cloth andwipe free from abrasives with a clean, dry cloth. Wind the wire into a coil having an outside diameter 44 to 48 mm and weightof 55.6 6 0.3 g and stretched to a height of 40 to 42 mm. Clean the coil thoroughly
31、 with isopropyl alcohol, air-dry, and insert insidethe glass sample container by a turning motion, if necessary.Anew coil is used for each sample. For extended storage, the preparedcoil may be packaged in a dry, inert atmosphere. For overnight storage (less than 24 h), the coils may be stored in n-H
32、eptane.NOTE 1Commercially available and prepackaged coils prepared as described in 8.1 can also be used for the test.77 Prepackaged coils were provided for RR:D02-1409.FIG. 2 RPVOT Metal Block Bath InstrumentD2272 1438.2 Cleaning of VesselWash the vessel body, cap, and inside of vessel stem with a s
33、uitable solvent (for example, petroleumspirit, heptane, or acetone.) Wash with hot detergent solution and rinse thoroughly with water. Rinse the inside of the stem withisopropyl alcohol and blow dry with clean compressed air. Keep the plastic valve out of the hot detergent to prevent itsdeterioratio
34、n. Failure to remove oxidation residue can adversely affect test results.8.3 Cleaning of Glass Container ContainerDrain and rinse with a suitable solvent (for example, non-reagent petroleumspirit, heptane, or acetone). Soak or scrub in an aqueous detergent solution. Brush thoroughly and flush thorou
35、ghly with tap water.Rinse with isopropyl alcohol, followed by distilled water and air dry. If any insolubles remain, soak overnight in an acid-typecleaning solution and repeat the above procedure starting from the tap water flush. Do not use chipped or cracked glassware.8.4 Cleaning of Polytetrafluo
36、roethylene (PTFE) DiskRemove any residual oil with a suitable solvent and clean by brushingwith detergent solution. Rinse thoroughly with tap water, followed by distilled water rinse and air dry.9. Procedure9.1 ChargingWeigh the glass sample container with a freshly cleaned catalyst coil. Weigh 50 6
37、 0.5 g of oil sample into thecontainer; also add 5 mL of reagent water. Add another 5 mL of reagent water to the vessel body and slide the sample containerinto the vessel body (see Note 2). Cover the glass container with a 57.2mm (2 14 in.) PTFE disk and place a hold-down spring8on top of the PTFE d
38、isk. Apply a thin coating of silicone stopcock grease to the O-ring vessel seal located in the gasket grooveof the vessel cap to provide lubrication, and insert the cap into the vessel body.NOTE 2The water between the vessel wall and the sample container aids heat transfer.9.1.1 Tighten the closure
39、ring by hand. Cover the threads of the gauge-nipple with a thin coating of stopcock grease (PTFE pipetape is a suitable alternative to the use of stopcock grease) and screw the gauge into the top center of the vessel stem. Attach theoxygen line with an inline pressure gauge to the inlet valve on the
40、 vessel stem. Slowly turn on the oxygen supply valve until thepressure has reached 620 kPa (90 psi, 6.2 bar). Turn off the oxygen supply valve. Slowly release pressure by loosening the fittingor by using an inline bleeder valve. Repeat purging process two more times; purge step should take approxima
41、tely 3 min. Adjustthe regulating valve on the oxygen supply tank to 620 6 1.4 kPa (90 psi, 6.2 bar) at a room temperature of 25C (77F). For each2.0C (3.6F) above or below this temperature, 5 kPa (0.7 psi, 0.05 bar) shall be added or subtracted to attain the required initialpressure. Fill the vessel
42、to this required pressure and close the inlet valve securely by hand. Open the pressure valve one more timeand watch the pressure gauge to make certain it is not decreasing. If not, then close the valve. If desired, test the vessel for leaksby immersing in water (see Note 3).NOTE 3If the vessel was
43、immersed in water to check for leaks, dry the outside of the wet vessel by any convenient means such as airblast or a towel.Such drying is advisable to prevent subsequent introduction of free water into the hot oil bath which would cause sputtering. For safety purposes, a faceshield is recommended d
44、uring the charging process.9.2 OxidationBring the heating bath to the test temperature while the stirrer is in operation. Switch off stirrer, insert the vesselinto the carriages, and note the time. Restart the stirrer. If an auxiliary heater is used, keep it on for the first 5 min of the run andthen
45、 turn it off (see Note 4). The bath temperature shall stabilize at the test temperature within 15 min after the vessel is inserted.Maintain the test temperature within 60.1C (see Note 5).NOTE 4The time for the bath to reach the operating temperature after insertion of the vessel may differ for diffe
46、rent apparatus assemblies and shouldbe observed for each unit. The objective is to find a set of conditions that does not permit a drop of more than 2C after insertion of the vessel and allowsthe vessel pressure to reach a plateau within 30 min as shown in Curve A of Fig. 3.NOTE 5Maintaining the cor
47、rect temperature within the specified limits of 6 0.1C during the entire test run is an important factor assuring bothrepeatability and reproducibility of test results.9.3 Keep the vessel completely submerged and maintain continuous and uniform rotation throughout the test. A standardrotational spee
48、d of 100 6 5 rpm is required; any appreciable variations in this speed could cause erratic results.9.4 The test is complete after the pressure drops more than 175 kPa (25.4 psi, 1.75 bar) below the maximum pressure (see Note6). The 175 kPa pressure drop usually, but not always, coincides with an ind
49、uction-type period of rapid pressure drop. When itdoes not, the operator may question whether he has produced 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 stop thetest at lesser pressure drops or to observe the condition of the oil after a predetermined test period of perhaps 100 min; that is, well within the normalinduction period of new inhibited oils.NOTE 7A typical experiment is shown in Fig. 3 as Curve A.
