1、Designation: D2272 14D2272 14aStandard 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, t
2、he 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 ut
3、ilizes 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 pur
4、ge 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
6、industry 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 heal
7、th 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 Mine
8、ral OilsD1193 Specification for Reagent WaterD4742 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 Charting Techniques to Evaluate Analytical Measure-ment System Performance
9、2.2 Energy Institute Standard:4IP 229 Determination of the Relative Oxidation Stability by Rotating Bomb of Mineral Turbine Oil2.3 ISO Standard:5ISO 3170 Petroleum LiquidsManual Sampling3. Summary of Test Method3.1 The test oil, water, and copper catalyst coil, contained in a covered glass container
10、, are placed in a vessel equipped with apressure gauge. The vessel is charged with oxygen to a gauge pressure of 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
11、from the horizontal.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.09.0C on Oxidation of Turbine Oils.Current edition approved July 1, 2014Oct. 1, 2014. Published August 2014Oct
12、ober 2014. Originally approved in 1964. Last previous edition approved in 20112014 asD2272 11.D2272 14. DOI: 10.1520/D2272-14.10.1520/D2272-14A.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, MTRS
13、A(formerly ASTM Bulletin), No. 186, December 1952, pp. 4346; von Fuchs, G. H., “Rotary Bomb Oxidation Test,” Lubrication Engineering, Vol 16, No.1, January 1960,pp. 2231.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annua
14、l 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. 43rd St., 4th
15、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 changes accurately
16、, 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 Harbor Drive
17、, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2 The number of minutes required to reach a specific drop in gauge pressure is the oxidation 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 controll
18、ing the continuity of this property for batch acceptance of productionlots having the same operation. It is not intended that this test method be a substitute 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
19、 the remaining oxidation test life of in-service oils.FIG. 1 Schematic Drawing of the Rotary Vessel Test ApparatusFIG. 2 RPVOT Metal Block Bath InstrumentD2272 14a2Method A5. Apparatus5.1 MethodA, Liquid Bath RPVOTOxidationVessel, Glass Sample Container with Four-Hole PTFE Disk, Hold-Down Spring,Cat
20、alyst-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 temperature shall have a displayed resolution
21、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 shall be used in all tests in the fi
22、nal 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 is first ascertained that thereagent
23、is of sufficiently high purity to permit its use without lessening the accuracy of the determination.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
24、 pressure regulation to 620 kPa (90 psi, 6.2 bar). ( WarningVigorously accelerates combustion.)6.6 Potassium 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-
25、grit with cloth backing.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 Standard WireGauge or No. 14 American Wire Gauge, 99.9 % purity, conforming to Specification B1. Soft copper wire of an equivalent grademay a
26、lso be used.6.10 Acetone, reagent grade. (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. As the resultsobtained by this method are r
27、eadily affected by traces of impurities, avoid contamination during sampling and subsequent handling;especially for used fluids. Samples shall be prepared and decanted in accordance with the procedures given in ISO 3170 and storedaway from light in dark colored bottles.8. Preparation of Apparatus8.1
28、 Catalyst PreparationBefore 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.
29、 Clean the coil thoroughly 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
30、coils may be stored in n-Heptane.NOTE 1Commercially available and prepackaged coils prepared as described in 8.1 can also be used for the test.78.2 Cleaning of VesselWash the vessel body, cap, and inside of vessel stem with a suitable solvent (for example, petroleumspirit, heptane, or acetone.) Wash
31、 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 itsdeterioration. Failure to remove oxidation residue can adversely affect test results.
32、6 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmac
33、opeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.7 Prepackaged coils were provided for RR:D02-1409.D2272 14a38.3 Cleaning of Glass ContainerDrain and rinse with a suitable solvent (for example, non-reagent petroleum spirit, heptane,or acetone). Soak or scrub in
34、an aqueous detergent solution. Brush thoroughly and flush thoroughly with tap water. Rinse withisopropyl alcohol, followed by distilled water and air dry. If any insolubles remain, soak overnight in an acid-type cleaning solutionand repeat the above procedure starting from the tap water flush. Do no
35、t use chipped or cracked glassware.8.4 Cleaning of Polytetrafluoroethylene (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 s
36、ample container with a freshly cleaned catalyst coil. Weigh 50 6 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
37、in.) PTFE disk and place a hold-down spring8on top of the PTFE disk. 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 th
38、e sample container aids heat transfer.9.1.1 Tighten the closure 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 theoxy
39、gen line with an inline pressure gauge to the inlet valve on the 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
40、purging process two more times; purge step should take approximately 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 sub
41、tracted to attain the required initialpressure. Fill the vessel 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
42、leaksby immersing in water (see Note 3).NOTE 3If the vessel was 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 caus
43、e sputtering. For safety purposes, a faceshield is recommended during 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 h
44、eater is used, keep it on for the first 5 min of the run andthen 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 operatin
45、g temperature after insertion of the vessel may differ for different 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 withi
46、n 30 min as shown in Curve A of Fig. 3.NOTE 5Maintaining the correct 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
47、 uniform rotation throughout the test. A standardrotational speed 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
48、kPa pressure drop usually, but not always, coincides with an induction-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 sta
49、ndard 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. The maximum pressure is expected to be reached by 30 min, a pressure plateau isestablished, and an induction-type pressure drop is observed. Curve B, in which there is a gradual decrease in pressure before the induction break isrecorde
