ASTM E203-2001 Standard Test Method for Water Using Volumetric Karl Fischer Titration《水的卡尔 弗歇尔容积滴定标准试验方法》.pdf
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1、Designation: E 203 01Standard Test Method forWater Using Volumetric Karl Fischer Titration1This standard is issued under the fixed designation E 203; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb
2、er 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. Scope1.1 This test method is intended as a general guide for theap
3、plication of the volumetric Karl Fischer (KF) titration fordetermining free water and water of hydration in most solid orliquid organic and inorganic compounds. This test method isdesigned for use with automatic titration systems capable ofdetermining the KF titration end point amperometrically;howe
4、ver, a manual titration method for determining the endpoint visually is included as Appendix X1. Samples that aregaseous at room temperature are not covered (see AppendixX4). This test method covers the use of both pyridine andpyridine-free KF reagents for determining water by the volu-metric titrat
5、ion. Determination of water using KF coulometrictitration is not discussed. By proper choice of the sample size,KF reagent concentration and apparatus, this test method issuitable for measurement of water over a wide concentrationrange, that is, parts per million to pure water.1.2 This standard does
6、 not purport to address all of thesafety concerns, 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 warningsare given in 3.1 an
7、d 7.3.3.1.3 Review the current Material Safety Data Sheets (MSDS)for detailed information concerning toxicity, first aid proce-dures, and safety precautions for chemicals used in this testprocedure.2. Referenced Documents2.1 A list of existing ASTM Karl Fischer methods, theirapplications to various
8、products, and the sponsoring commit-tees is given in Appendix X3.2.2 ASTM Standards:D 789 Test Methods for Determination of Relative Viscos-ity, and Moisture Content of Polyamide (PA)2D 803 Test Methods for Testing Tall Oil3D 890 Test Method for Water in Liquid Naval Stores3D 1123 Test Methods for W
9、ater in Engine Coolant Concen-trate by the Karl Fischer Reagent Method4D 1152 Specification for Methanol (Methyl Alcohol)5D 1193 Specification for Reagent Water6D 1348 Test Methods for Moisture in Cellulose3D 1364 Test Method for Water in Volatile Solvents (FischerReagent Titration Method)5D 1533 Te
10、st Method for Water in Insulating Liquids byCoulometric Karl Fischer Titration7D 1568 Test Methods for Sampling and Chemical Analysisof Alkylbenzene Sulfonates8D 1631 Test Method for Water in Phenol and RelatedMaterials by the Iodine Reagent Method5D 2072 Test Method for Water in Fatty Nitrogen Com-
11、pounds3D 2575 Method for Testing Polymerized Fatty Acids3D 3277 Test Methods for Moisture Content of Oil-Impregnated Cellulosic Insulation7D 3401 Test Methods for Water in Halogenated OrganicSolvents and Their Adixtures9D 4017 Test Method for Water in Paints and Paint Materialsby Karl Fischer Method
12、10D 4377 Test Method for Water in Crude Oils by Potentio-metric Karl Fischer Titration11D 4672 Test Methods for Polyurethane Raw Materials-Determination of Water Content of Polyols12D 4928 Test Methods for Water in Crude Oils by Coulom-etric Karl Fischer Titration131This test method is under the jur
13、isdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.01 on General Standards.Current edition approved Oct. 10, 2001. Published December 2001. Originallypublished as E 203 62 T. Last previous edition E 203 96.2Annual Book of ASTM Sta
14、ndards, Vol 08.01.3Annual Book of ASTM Standards, Vol 06.03.4Annual Book of ASTM Standards, Vol 15.05.5Annual Book of ASTM Standards, Vol 06.04.6Annual Book of ASTM Standards, Vol 11.01.7Annual Book of ASTM Standards, Vol 10.03.8Annual Book of ASTM Standards, Vol 15.04.9Annual Book of ASTM Standards
15、, Vol 15.05.10Annual Book of ASTM Standards, Vol 06.01.11Annual Book of ASTM Standards, Vol 05.02.12Annual Book of ASTM Standards, Vol 08.03.13Annual Book of ASTM Standards, Vol 05.03.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D
16、 5460 Test Method for Rubber Compounding Materials-Water in Rubber Additives14D 5530 Test Method for Total Moisture of Hazardous WasteFuel by Karl Fischer Titrimetry15D 6304 Test Method for Determination of Water in Petro-leum Products, Lubricating Oils, and Additives by Coulo-metric Karl Fisher Tit
17、ration8E 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial Chemicals9E 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis9E 1064 Test Method for Water in Organic Liquids byCoulometric Karl
18、Fischer Titration93. Summary of Test Method3.1 The sample, containing a maximum of 100 mg of water,is dissolved or dispersed in a suitable liquid and titrated withKF reagent, which consists of iodine, sulfur dioxide, organicbase, and a solvent (typically an alcohol, such as methanol,ethylene glycol,
19、 or 2-methoxyethanol). The titration end pointis determined amperometrically with a platinum electrodewhich senses a sharp change in cell resistance when the iodineis reduced by sulfur dioxide in the presence of water.(WarningKF reagent contains four toxic compounds,namely, iodine, sulfur dioxide, p
20、yridine or other organic bases,and methanol or glycol ether. The reagent should be dispensedin a well-ventilated area. Care must be exercised to avoidinhalation of the reagent or direct contact of the reagent withthe skin.)3.2 The general equation to this reaction is as follows:H2O 1 I21 SO21 R8OH 1
21、 3 RN . RNH!SO4R8 1 2RNH!I (1)where:RN = an organic base such as pyridine, andR8OH = alcohol.4. Significance and Use4.1 Titration techniques using KF reagent are one of themost widely used for the determination of water.4.2 Although the volumetric KF titration can determine lowlevels of water, it is
22、 generally accepted that coulometric KFtitrations (see Test Method E 1064) are more accurate forroutine determination of very low levels of water. As a generalrule, if samples routinely contain water concentrations of 500ppm or less, the coulometric technique should be considered.4.3 Applications ca
23、n be subdivided into two sections: (1)organic and inorganic compounds, in which water may bedetermined directly, and (2) compounds, in which water cannotbe determined directly, but in which interferences may beeliminated by suitable chemical reactions or modifications ofthe procedure. Further discus
24、sion of interferences is includedin Section 5 and Appendix X2.4.4 Water can be determined directly in the presence of thefollowing types of compounds:Organic CompoundsAcetals EthersAcids (Note 1) HalidesAcyl halides Hydrocarbons (saturated and unsaturated)Alcohols Ketones, stable (Note 4)Aldehydes,
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