ASTM E1064-2008 866 Standard Test Method for Water in Organic Liquids by Coulometric Karl Fischer Titration《用卡尔费歇尔库仑滴定法测定有机液体中水含量的标准试验方法》.pdf
《ASTM E1064-2008 866 Standard Test Method for Water in Organic Liquids by Coulometric Karl Fischer Titration《用卡尔费歇尔库仑滴定法测定有机液体中水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 E1064-2008 866 Standard Test Method for Water in Organic Liquids by Coulometric Karl Fischer Titration《用卡尔费歇尔库仑滴定法测定有机液体中水含量的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E 1064 08Standard Test Method forWater in Organic Liquids by Coulometric Karl FischerTitration1This standard is issued under the fixed designation E 1064; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t 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. Scope*1.1 This test method covers the determinat
3、ion of water from0 to 2.0 % mass in most liquid organic chemicals, with KarlFischer reagent, using an automated coulometric titrationprocedure. Use of this test method is not applicable forliquefied gas products such as Liquid Petroleum Gas (LPG),Butane, Propane, Liquid Natural Gas (LNG), etc.1.2 Th
4、e values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 Review the current material safety data sheets (MSDS)for detailed information concerning toxicity, first-aid proce-dures, handling, and safety precautions.1.4 This standard does
5、not purport to address all of thesafety problems, 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. Specific precau-tionary statements ar
6、e given in Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 203 Test Method for Water Using Volumetric Karl FischerTitration3. Summar
7、y of Test Method3.1 This test method is based on the Karl Fischer reactionfor determining waterthe reduction of iodine by sulfurdioxide in the presence of water to form sulfur trioxide andhydriodic acid. The reaction becomes quantitative only whenpyridine or other organic base and methanol or other
8、alcoholare present. Unlike the volumetric Karl Fischer reagents thatinclude iodine, the coulometric technique electrolytically gen-erates iodine, with 10.71 C of generating current correspondingto 1 mg of water in accordance with Faradays law.4. Significance and Use4.1 The coulometric technique is e
9、specially suited for de-termining low concentrations of water in organic liquids thatwould yield small titers by the Karl Fischer volumetricprocedure. The precision and accuracy of the coulometrictechnique decreases for concentrations of water much greaterthan 2.0 % because of the difficulty in meas
10、uring the small sizeof sample required. The test method assumes 100 % efficiencyof coulombs in iodine production. Provision is made forverifying this efficiency. (See Table 1 and Note 6.)5. Interferences5.1 Interfering substances are the same as are encounteredin the volumetric Karl Fischer titratio
11、n. A detailed discussionof interfering substances can be found in the treatise on“Aquametry.”35.2 Test Method E 203 discusses organic compounds inwhich water may be determined directly and compounds inwhich water cannot be determined directly, but in whichinterferences may be eliminated by suitable
12、chemical reactions.6. Apparatus6.1 Automatic Titrator,4consisting of a control unit, titrationvessel, dual platinum sensing electrode, generator assembly,and magnetic stirrer. The instrument is designed to coulometri-cally generate iodine that reacts stoichiometrically with the1This test method is u
13、nder the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.01 on General Standards.Current edition approved April 1, 2008. Published May 2008. Originallyapproved in 1985. Last previous edition approved in 2005 as E 1064 05.2Fo
14、r referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3J. Mitchell, Jr. and D. M. Smith, “Aquametry”A Treatise on Meth
15、ods for theDetermination of Water, Part IIIThe Karl Fischer Reagent, 2nd Ed., J. Wiley andSons, Inc., New York, NY 1990.4Basic references to the automatic coulometric titrator: M. T. Kelley, R. W.Stelzner, W. R. Laing, and D. J. Fisher, Analytical Chemistry 31, No. 2, 220 (1959)and A. W. Meyer, Jr.
16、and C. M. Boyd, Analytical Chemistry 31, No. 2, 215 (1959).1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.water present in the sample solution. The coulombs of elec-t
17、ricity required to generate the reagent are converted tomicrograms of water, which is obtained as a direct digitalreadout.6.2 Syringe, 50-mL, fitted with an 115-mm hypodermicneedle for removing excess solution from the titration chamber.NOTE 1Rinse all glass syringes and needles with anhydrous aceto
18、neafter cleaning, then dry in an oven at 100C for at least 1 h and store ina desiccator. Plastic syringes shall be disposed of following use.6.3 Syringe, 20-mL, fitted with an 115-mm hypodermicneedle for introduction of neutralizing solution into the titrationchamber (see Note 1).6.4 Syringes, 1- an
19、d 5-mL, fitted with 115-mm hypodermicneedles for introduction of samples into titration chamber (seeNote 1).6.5 Syringe, 5 L, fitted with 115-mm hypodermic needlefor standardization of instrument (see Note 1).6.6 Fluorocarbon Sealing Grease or TFE-Fluorocarbon,toseal the titration chamber against at
20、mospheric moisture.6.7 Septa, to seal sample port but allow introduction ofsamples by a needle with a minimum of moisture contamina-tion. Replace serum caps and septa as required to prevent airleakage as indicated by instrument drift.6.8 Serum Bottles.6.9 Oven, temperature 100 6 5C.6.10 Dessicator,
21、standard laboratory type with color changeindicator.6.11 Analytical Balance, capable of weighing to 60.0001 g.7. Reagents7.1 Purity of ReagentsUnless otherwise indicated, it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-ca
22、l Society, where such specifications are available.5Othergrades may be used, provided it is first ascertained that thereagent is of sufficiently high purity to permit its use withoutlessening the accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referenceto water shall be
23、understood to mean Type II or Type IIIreagent water, conforming to Specification D 1193.7.3 Karl Fischer ReagentsCommercial coulometric KFreagents and reagent systems of various types are available foruse with autotitrators for water determination. Traditionally,pyridine was the organic base used in
24、 KF reagents. Pyridine-free formulations are available and are preferred by most KFinstrument manufacturers for use with their equipment. Thepyridine-free reagents are less toxic, less odorous, and morestable than those containing pyridine. The use of pyridine-freereagents is recommended whenever po
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