ASTM D4047-2013 Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method《用喹啉磷钼酸盐法测定润滑油及添加剂中磷含量的标准试验方法》.pdf
《ASTM D4047-2013 Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method《用喹啉磷钼酸盐法测定润滑油及添加剂中磷含量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D4047-2013 Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method《用喹啉磷钼酸盐法测定润滑油及添加剂中磷含量的标准试验方法》.pdf(6页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D4047 00 (Reapproved 2011)D4047 13Designation: 149/93Standard Test Method forPhosphorus in Lubricating Oils and Additives by QuinolinePhosphomolybdate Method1This standard is issued under the fixed designation D4047; the number immediately following the designation indicates the year of
2、original adoption or, in the case of revision, the 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 Department o
3、f Defense.1. Scope Scope*1.1 This test method covers the determination of 0.005 to 10.0 mass % phosphorus in unused lubricating oil and additiveconcentrates. There is no reason to doubt its applicability to filtered, used lubricating oils, but no systematic study of thisapplication has been made.1.2
4、 The test method is applicable to samples containing any of the phosphorus compounds in normal use.NOTE 1This test method extends the scope of the previous version of IP 149 and replaces IP 148 and the previous version of IP 149 as a refereemethod.1.3 This test method is free from most interferences
5、 because the high insolubility of the quinoline phosphomolybdate precipitateleads to constant composition and freedom from most adsorbed or occluded impurities, especially from cations which wouldotherwise interfere in the subsequent titration of the precipitate.1.4 Barium, calcium, magnesium, zinc,
6、 iron, aluminum, alkali salts, citric acid and citrates, chromium up to 18 times thephosphorus content, and titanium up to 3.5 times do not interfere with the test method.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6
7、 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 health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard
8、 statements, see 6.9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System Performance2.2 IP Standard:IP 148 Test Method for Phosphorous in L
9、ubricating Oils and Additives33. Summary of Test Method3.1 Additive concentrates are diluted with phosphorus-free white oil to produce a working blend.3.2 The sample is ignited with excess of zinc oxide whereby phosphorus is converted to phosphate. The residue is dissolvedin hydrochloric acid and an
10、y sulfide formed is oxidized with potassium bromate. Phosphorus is then precipitated as quinolinephosphomolybdate and determined volumetrically by addition of excess standard alkali and back titration with standard acid.1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum
11、Products and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved May 1, 2011June 15, 2013. Published May 2011August 2013. Originally approved in 1981. Last previous edition approved in 20052011 asD4047 00 (2005).(2011). DOI: 10.1520/D4047-
12、00R11.10.1520/D4047-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from Energy Institute, 61
13、New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.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 depic
14、t all changes 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 Internationa
15、l, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Significance and Use4.1 Knowledge of the phosphorus content, and thus the phosphorus-containing additives, in a lubricating oil or additive can beused to predict performance characteristics.5. Apparatus5.1 Sili
16、ca Crucibles, 40-mm internal diameter at the top and 40 mm in height. The internal surface should be smooth and freefrom pitting.5.2 Muffle Furnace, capable of maintaining a temperature of approximately 700C, and fitted with ports to allow air circulation.5.3 Beakers, 25-mL capacity.5.4 Filtering Ap
17、paratus, a filter flask of capacity 500 mL, provided with a glass crucible adapter fitted in a rubber bung togetherwith a rubber sleeve.5.5 Gooch Crucible, porcelain, 35 mm diameter at the top, or a filter funnel fitted with a porcelain filter disk of approximately20 mm diameter.5.6 Filter Pad, appr
18、oximately 20 mm diameter.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheres
19、uch specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to
20、 mean reagent water as defined byType II or Type III of Specification D1193.6.3 Hydrochloric Acid, approximately 1 N reagent solution.6.4 Hydrochloric Acid (36 mass %)Concentrated hydrochloric acid (HCl).6.5 Hydrochloride Acid, (0.1N)Hydrochloric acid (HCl) accurately standardized.6.6 Mixed Indicato
21、rMix 2 volumes of phenolphthalein solution with 3 volumes of thymol blue solution.6.7 Phenolphthalein Solution, (1 g/L in 95 % volume ethanol).6.8 Potassium Bromate (KBrO3), solid.6.9 Quinoline (WarningQuinoline has a high toxic acute systemic rating.)Redistilled synthetic or, if this is unobtainabl
22、e,quinoline freshly distilled from the technical product. Collect the colorless distillate in the boiling range from 232 to 238C. Storethe quinoline in an amber bottle in the dark.6.10 Quinoline Hydrochloride SolutionDissolve 20 mL of quinoline in 800 mL of hot water acidified with 25 mL ofconcentra
23、ted HCl; add a little paper pulp, cool, filter, and make up to 1 L with water. This solution is stable for about 1 month.6.11 Sodium Hydroxide Solution (0.1 M)Sodium hydroxide (NaOH) accurately standardized.6.12 Sodium Molybdate SolutionDissolve 10 g of sodium hydroxide (NaOH) and 18 g of ammonia-fr
24、ee molybdenum trioxidein 200 mL of water and filter the solution.NOTE 2To avoid high blanks caused by silicate interference with alkaline reagents, including sodium molybdate solution, store in polythenecontainers.6.13 Thymol Blue Solution (1 g/L) in 95 % volume ethanol.6.14 Zinc Oxide (ZnO), finely
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