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    8 views20 pages

    D 2272 2011

    Uploaded by

    Navneet Yadav

    Copyright:

    © All Rights Reserved
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    Designation: D2272 - 11 Standard Test Method for Oxidation Stal Pressure Vessel’ ity of Steam Turbine Oils by Rotating ‘This standard is issued under the fixed designation D2272; the umber immediately folowing the designation indicates the year of ‘rignal adoption on he ce of revision the year ola revision. A namber in premeses ince the year of Is eapproval. A Supesript epson (e) adkeates an editorial change since the last revision of approval ‘This standand hasbeen approved for use by agencies ofthe Department of Defense 1. Seope* 1.1 This test method? utilizes an oxygen-pressured vessel to evaluate the oxidation stability of new and in-service turbine oils having the same composition (base stock and additives) in the presence of water and a copper catalyst coil at 150°C. 1.2 Appendix XI describes a new optional wrbine oil (unused) sample nitrogen purge pretreatment procedure for determining the percent residual ratio of RPVOT value for the pretreated sample divided by RPVOT value of the new (untreated) oil, sometimes referred to as a ““e RPVOT Reten- tion.” This nitrogen purge pretreatment approach was designed to detect volatile antioxidant inkibitors 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 Exception—Other units are provided in parentheses (psi, grams, and inches), because they are either the industry accepted standard 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 responsibility 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 specific ‘warning statements, see 6.2, 6.4, 6.5, 6.6, and 6.10. "his wat method i under the jursition of ASTM Comaniuee DO2 ox eroleum Prods and Lubricant and is the dec esponsbiy of Subcom: 'Dn2.0.0C on Oxidition of Turbine Oil Cure edition approved: May 1, 2011, Published May 2011. Originally approved in 1964, Lat previous edition approved in 2009 es D2272-09. DOI 111S20vD2272-1 on Fucks. G. HL, Claige, EL and Zudema, H. HL. “The Rotary Bom Oxidation Test for Inhibited Turbine Gis" Mateiats Research and Standards, MRSA (formerly ASTM Bulletin), No” 186, December 1982, pp. 43-46; von Fuchs, G. H, "Rotary Bomb Oxidation Test” Lubrication Engluerng, Val 16, No, January 1960, pp 22-3 2, Referenced Documents 2.1 ASTM Standards:? BI Specification for Hard-Drawn Copper Wi D943 Test Method for Oxidation Characteristics of Inhib- ited Mineral Oils, 1193 Specification for Reagent Water 1D4057 Practice for Manual Sampling of Petroleum and Petroleum Products| 14742 Test Method for Oxidation Stability of Gasoline ‘Automotive Engine Oils by Thin-Film Oxygen Uptake (IFOUT) 16299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance 2.2. Energy Institute Standard IP 229 Determination of the relative oxidation stability by rotating bomb of mineral turbine oil Summary of Test Method 3.1 The test oil, water, and copper catalyst coil, contained in a covered glass container, ate placed in a vessel equipped with 4 pressure gauge. The vessel is charged with oxygen to a gauge pressure of 620 kPa (90 psi, 6.2 bar) (see Eq 1), placed in a ‘constant-temperature oil bath set at 150°C or dry block taken to 150°C (Fig. | and Fig. 2), and rotated axially at 100 rpm at an angle of 30° from the horizontal 2 The number of minutes required to reach a specific drop in gauge pressure is the oxidation stability of the test sample. 100 KPa = 1.00 bar = 14.5 psi o > For rferenced ASTM standais, visit the ASTAE website, wor astm. of ‘contact ASTM Customer Service at service @astnrg. For Annual Book of ASTM ‘Standards volume infomation, rer othe standards Docement Summiry Page on the ASTM went “Available from Energy Init, 61 New Cavenlih St, London, WIG TAR, UK, bnpsiweneneyne org A Summary of Changes section appears at the end of this standard. ees. Conehoockn,Peneria 19428280, Uns State ly v2272-11 x FIG. 1 Schematic Drawing of the Rotary Vessel Test Apparatus: Pressure Chay Pressure Chamber Lid Magnetic Cup with Sample Beaker ber Drive magnet |_Besatipte Totation FIG. 2 RPVOT Metal Block Bath Instrument 4. Significance and Use 4.1 The estimate of oxidation stability is useful in control- ling the continuity of this property for batch acceptance of production lots having the same operation. It is not intended that this test method be a substitute for Test Method D943 or be used to compare the 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. ‘inetd eam jethod A 5. Apparatus 5.1 Method A, Liquid Bath RPVOT—Oxidation Vessel, Glass Sample Container with Four-Hole PTFE Disk, Hold- Down Spring, Catalyst-Coil, Pressure Gauge, Thermometer, and ‘Test Bath as described in Annex Al. The assembled apparatus is shown schematically in Fig. 1 and Fig. A1.6, 5.2 Method B, Dry Block Bath RPVOT—See Section 13 for this additional option. ly v2272-11 6, Reagents and Materials 6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests in the final cleaning stages. Unless otherwise indicated, it is imtended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available.’ Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determi- nation. 6.2 Isopropyl Alcohol, Flammable. Health hazard.) 63 Liquid Detergent. 6.4 n-Heptane, 99.0 minimum mol % (pure grade). (Warning—Flammable. Health hazard.) 65 Oxygen, 99.5 %, with pressure regulation to 620 kPa (90 psi, 6.2 bar). (Warning—Vigorously accelerates combustion.) 6.6 Potassium Hydroxide, Alcohol Solution (1 %)—Dis- solve 12 g of potassium hydroxide (KOH) pellets in 1 L.of the isopropyl alcohol. (Warning—Flammable. Health hazard.) 6.1 Silicone Carbide Abrasive Cloth, \00-grit with cloth backing, 68 Silicone Stopcock Grease. 69 Wire Catalyst, Electrolytic Copper Wire, 1.63 = 1 % mm (0.064 + 1 % in.) in diameter (No. 16 Imperial Standard Wire Gauge or No. 14 American Wire Gauge, 99.9 % purity, conforming to Specification BI. Soft copper wire of an equivalent grade may also be used. 6.10 Acetone, reagent grade. Health hazard.) G11 Reagent Water, conforming to Specificati ‘Type I. 7. Sampling, 7.1 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 in Practice D4057. reagent grade. (Warning— (Warning—Flammable. 1193, 8, Preparation of Apparatus 8.1 Catalyst Preparation—Before use, polish approxi- mately 3 m of the copper wire with a silicon carbide abrasive cloth and wipe free from abrasives with a clean, dry cloth Wind the wire into a coil having an outside diameter 44 to 48 mm and weight of 55.6 + 0.3 g and stretched to a height of 40 to 42 mm, Clean the coil thoroughly with isopropyl alcohol, air-dry, and insert inside the glass sample container by a turing motion, if necessary. A new coil is used for each sample. For extended storage, the prepared coil may be packaged in a dry, inert atmosphere. For overnight storage (less than 24 h), the coils may be stored in n-Heptane. 5 Reagent Chemicals. American Chemical Society Specifications, American (Cuomicl Society. Washington, DC. Foe Suggestions on the testing of teagents Bot listed by the American Chemical Society. see Annual Stans for Laboratory Chemicals, BDH Li, Poole, Dorset, UK. and the United Sater Phamacopess ‘and National Formulary, US. Phamcopeial Convention, In. (USPC), Rockville, Mp, ‘inetd eRe. Nore 1—Commercialy available and prepackaged coils prepared as described in 8.1 can also be used forthe tes 8.2 Cleaning of Vessel—Wash the vessel body, cap, and inside of vessel stem with a suitable solvent (for example, petroleum spirit, heptane, or acetone.) Wash with hot detergent solution and rinse thoroughly with water. Rinse the inside of the stem with isopropyl alcohol and blow dry with clean compressed air. Keep the plastic valve out of the hot detergent to prevent its deterioration. Failure to remove oxidation residue can adversely affect test results. 8.3 Cleaning of Glass Container—Drain and rinse with a suitable solvent (for example, non-reagent petroleum spirit, heptane, or acetone). Soak or scrub in an aqueous detergent solution. Brush thoroughly and flush thoroughly with tap water. Rinse with isopropyl alcohol, followed by distilled water and air dry If any insolubles remain, soak overnight in an acid-type cleaning solution and repeat the above procedure starting from the tap water flush. Do not use chipped or cracked glassware. 84 Cleaning of Polytetraftuoroethylene (PTFE) Disk— Remove any residual oil with a suitable solvent and clean by ‘brushing with detergent solution. Rinse thoroughly with tap ‘water, followed by distilled water rinse and air dy. 9. Procedure 9.1 Charging—Weigh the glass sample container with a freshly cleaned catalyst coil. Weigh 50 + 0.5 g of oil sample into the container; also add 5 mL of reagent water. Add another ‘5 mL of reagent water to the vessel body and slide the sample container into the vessel body (see Note 2). Cover the glass container with a 57.2-mm (2 % in.) PTFE disk and place a hhold-down spring” on top of the PTFE disk. Apply a thin coating of silicone stopcock grease to the O-ring vessel seal located in the gasket groove of the vessel cap t0 provide lubrication, and insert the cap into the vessel body. Nore 2—The water between the vessel wall and the sample contsiner sid 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 Pipe 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 the inlet valve on the vessel stem. Slowly turn on the oxygen supply valve until the pressure has reached 620 kPa (90 psi, 6.2 bat). Turn off the oxygen supply valve. Slowly release pressure bby loosening the fitting or by using an inline bleeder valve. Repeat purging process two more times; purge step should take approximately 3 min, Adjust the regulating valve on the ‘oxygen supply tank to 620 * 1.4 kPa (90 psi, 6.2 bar) at a room temperature of 25°C (77°F), For each 2.0°C (3.6°F) above or ‘below this temperature, 5 kPa (0.7 psi 0.05 bar) shall be added ‘or subtracted to attain the required initial pressure. Fill the vessel to this required pressure and close the inlet valve securely by hand. Open the pressure valve one more time and watch the pressure gauge to make certain it is not decreasing. { Prepackaged coils were provided fr RR:DO2-1408, > PIE dik with oles an hold down sping were provided for RR:DO2. 409, oO 09 1 1m 80 vm {= 0 20 = se] { neo to Bus + col 1009 ¢ 100 i” wo #90 : Eve 4 wf oo B woe m0 7 Ne AL 0 so rr Te—ManTED FIG. 3 Pressure Versus Times Plot of Two Rotary Vessel Oxidation Test Runs If not, then close the valve. If desired, test the vessel for leaks by immersing in water (see Note 3) Nore 3—Ifthe vessel was immerse in water o check for leaks, dry the ‘outside ofthe wet vessel by any convenicat means such as arbast or a towel Such dying is advisable to prevent subsequent ineoducton office water into the hot oil bath which would cause sputtering. For safety purposes, a face shield is recommended during the charging process 9.2 Oxidation—Bring the heating bath to the test tempera- le the stirrer isin operation. Switch of stirrer, insert the vessel into 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 and then tur it off (see Note 4), The bath temperature shall stabilize atthe test temperature within 15 min after the vessel is inserted, Maintain the test temperature within 0.1°C (see Note 5). Nore 4—The tine forth baht each the operating temperature afer insertion of the vessel may difr for diferent apparatus assembles and should be observed for cach unit. The objective is to find a set of conditions that does ot permit a drop of more than 2°C after insetion of the vessel and allows the vessel presture to reach a plateau within 30 min as shown in Care A of Fig. 3 Nore $—Mainaning the comect temperature within the specified limits of = 0.1°C dung he ene est runs an important Fctor assuring bor repeatability and reproduibiiy of test results, 9.3 Keep the vessel completely submerged and maintain ‘continuous and uniform rotation throughout the test. A standard rotational speed of 100 * 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 Note 6). The 175 kPa pressure drop usually, but not always, coineides with an induction-type period of rapid pressure drop. When it does not, the operator may question whether he has produced a valid experiment (see Note 7). ‘Nore. 6—While termination of the test ta 175 KPa 25.4 pi, 1.75 bar) pressure drop is the standard procedure, some operators may elect to stop the testa lesser pressure drops orto observe the condition of the oil after Copyright by ASTM Int! (all rights reserved); Fei May 27 01:09:18 EDT 2011, 4 predetermined test period of perhaps 100 min; that i, well within the normal indetion period of new inhibited ois, Nore 7—A pial experiment is shown in Fig. 3 as Curve A. The maximum pressure is expected t be reached within 30 min, pressure plateau is established, and an indtion-type pressure drop is observed. ‘Carve By in which thee isa gradual decrease in pressure before the induction break is recorded, is more dificult to evaluate. The gradual THREADS (PTFE ~ PIPE TAPE) THREADS (tre = pire Tare) NEEDLE VALVE QUICK RELEASE COUPLING CLOSURE RING SPRING ~~ 0-RING GASKET PIFE DISC O-RING BOMB SEAL GLASS CONTAINER FIG. A1.7 Oxidation Vessel Assembly Copyright by ASTM Int! (al sights reserved); Fei May 27.01:09:18 EDT 2011, 4 2272-11 ty ph FIG, A1.8 Chart of Recording Pressure Gauge (Actual Size = 4% in.) A2. APPARATUS FOR ROTARY PRESSURE VESSEL OXIDATION TEST—METAL BLOCK BATH. A2.1 Pressure Chamber Access A2.1.1 The 2.5 in, stainless steel opening under the pressure ‘chamber lid (see Fig. A2.1 and Fig. A2.2) on the front of the unit provides access to the interior of the pressure chamber: ‘This is where the glass sample beaker carried by the magnetic cup (see Fig. A2.3) is placed during the test operation, A2.2 Pressure Chamber Lid 2.2.1 This is the cover to the pressure chamber that seals the test during operation. As shown, one (1) O-ring is placed on the underside of the lid to maintain a good seal. See Fig. A2.4. A2.3 Knurled Lid Nuts A2.3.1 Three finger-tightened lid nuts are used to hold the lid in contact with the pressure chamber to seal it during test. A24 Magnetic Cup A24.1 The magnetic cup shown in Fig. A2.3 and Fig. A2.5, holds the glass sample beaker during operation. This magnetic ‘cup is driven by the motor magnet located just adjacent to the pressure chamber bottom inside the cabinet. The underside of the cup has a pivot point (peek screw) designed to reduce friction of the cup on the bottom of the chamber. See operator's, ‘manual for replacement details Copyright by ASTM Int! (al sights reserved); Fei May 27 01:09:18 EDT 2011, < 42.5 Glass Sample Beaker A25.1 The beaker shown in Fig. A2.3 and Fig. A2.6 holds the test sample and the copper coil catalyst as well as 5 mL. of distilled water during the test. A26 Beaker Cover A2.6.1. The glass sample beaker is covered during the test as, in Fig. A23. A27 Copper Coil Catalyst A27.1 Catalyst is used to encourage oxidation of the sample, 28 Spring Clip A28.1 The spring clip shown in Fig. A23 is used to securely brace the glass sample beaker inside the magnetic cup to ensure proper rotational speed during the test. A29 Cup and Beaker Removal Tongs A29.1 Special tongs permit insertion and removal of the slass sample beaker and magnetic cup before and after a testis, ‘complete. A2.10 Lid Removal Tool A2.10.1 The lid removal tool is used to hold and remove the hot pressure chamber lid. This removal tool threads into the front port of the chamber lid shown in Fig, A2.1. ly v2272-11 A211 Oxygen (O,) Fill Valve A2ILI A toggle fill valve (see Fig. A2.1) is used to introduce the pressurized oxygen to the pressure chamber. A2.12 Oxygen (O,) Vent Valve ‘A2.12.1 needle valve used to purge the air in the pressure ‘chamber after itis sealed using pressurized oxygen and to also set the desired pressure level for test, See Fig. A2.1 A213 Anti-Frietion Band 2.13.1 A Lin, wide section of special heat-shrink plastic tubing placed around the circumference of the magnetic cup and shrunk to fit. It is designed to reduce friction and eliminate wear between the magnetic cup and the inner wall of the pressure chamber during the test, See operator’s manual for replacement of this band, A214 Lid Alignment Wire A2.14.1 A stiff metal wire that is inserted through the test port access hole in the lid (see Fig. A2.1) and then into the calibration test port in the pressure chamber wall. This posi- tions the lid properly and keeps the calibration test port clear of | debris. A2IS PTFE Lid Cover A2.15.1. This lid cover is positioned over the chamber lid for reducing heat loss from the lid during the test as well as protecting the operator from its hot surface, This lid cover is required during operation for proper results to be obtained. Pressurized ‘Oxygen (02) Fill Toggle Valve Knurled Lid Nuts) —— PrewureChmberLid Drip Tray — Heat Switch Switeh Drive Motor Safe-Opening Indicator Light Oxygen (03) — Vent Valve Calibration Test Port access hole }— Lid Removal Port Crater Vas, tide }—~ Realtime Pressure Monitor J —~pro Bara w/USB cry Qa = a Teflon Lid FIG. A2.1 Quantum Assembly Front ‘Cine eam Cooling Fan & Fan Switch Low Pressure Vent Hose Connection Oxygen (O,) Port q from High Pressure 3 Source Analog Output = Fuses Multi-unit Automation Inputs USB connection to Computer FIG. A2.2 Quantum Assembly Rear FIG, A2.3 Magnetic Cup Assembly Copyright by ASTM Int (all rights reserved); Fei May 27 01:09:18 EDT 2011 4 : (eer 2101 NO WNIG ‘33HM3S 00 'AHANI43H HOOD "AHSNIIIH IVENNIN "VOION H3LV3H9 OAHO LV ASN HOd TOdd HO4 WLS¥ OHS 3 eFl6'62 63,25+2 FIG. A2.5 Magnetic Cup Drawing 3 i i 3 a 2 Copyright by ASTM Int! (all rights reserved); Fei May 27 01:09:18 EDT 2011 4.

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