1.1 本试验方法旨在作为卡尔·费歇尔（KF）容量滴定法应用的通用指南，用于测定大多数固体或液体有机和无机化合物中的游离水和水合水。本试验方法设计用于自动滴定系统，该系统能够电位测定KF滴定终点；然而，包括一种手动滴定法，用于直观地确定终点 附录X1 .室温下为气态的样品不包括在内（参见 附录X4 ).本试验方法包括使用不含吡啶的KF试剂通过容量滴定法测定水。没有讨论使用KF库仑滴定法测定水。 通过适当选择样品大小、KF试剂浓度和仪器，该测试方法适用于测量宽浓度范围内的水，即纯水的百万分之一。 1.2 以国际单位制表示的数值应视为标准。 1.3 本标准并不旨在解决与其使用相关的所有安全问题（如有）。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践，并确定监管限制的适用性。 中给出了具体警告 3.1 . 1.4 查阅当前的安全数据表（SDS），了解有关本试验程序中使用的化学品的毒性、急救程序和安全预防措施的详细信息。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 4.1 使用KF试剂的滴定技术是最广泛用于测定水的技术之一。 4.2 尽管容量KF滴定法可以测定低水平的水，但通常接受库仑KF滴定（见试验方法 E1064 )对于非常低水位的常规测定来说更准确。一般来说，如果样品通常含有500 mg/kg或更低的水浓度，则应考虑库仑法。 4.3 应用程序可细分为两个部分:( 1. )有机和无机化合物，其中可以直接测定水，以及( 2. )化合物，其中的水不能直接测定，但其中的干扰可以通过适当的化学反应或程序的修改来消除。有关干扰的进一步讨论，请参见第节 5. 和 附录X2 . 4.4 水可以在以下类型的化合物存在下直接测定: 有机化合物 缩醛 醚类 酸( 注1 ) 卤化物 酰卤 碳氢化合物（饱和和不饱和） 酒精类 酮类，稳定( 注4 ) 醛类，稳定( 注2 ) 腈类 Amides 正交酯 胺，弱( 注3 ) 过氧化物（氢、二烷基） 酸酐 硫化物 二硫化物 硫氰酸盐 酯类 硫酯类 无机化合物 酸( 注5 ) 氧化铜 酸性氧化物( 注6 ) 干燥剂 氧化铝 硫酸肼 酸酐 有机酸和无机酸的盐( 注6 ) 二氧化钡 碳酸钙 注1: 一些酸，如甲酸、乙酸和己二酸，是缓慢酯化的。当使用不含吡啶的试剂时，可在滴定前将市售缓冲溶液加入样品中。对于甲酸，可能需要使用不含甲醇的溶剂和滴定剂 ( 1. ) . 4. 注2: 稳定醛的例子是甲醛、糖、氯醛等。甲醛聚合物含有作为羟甲基的水。 这种合并的水不会被滴定。添加过量的NaOCH 3. 在甲醇中，在用乙酸大致中和过量的碱后，可以释放和滴定这种合并的水（参见 注释9 ). 注3: 弱胺被认为是那些具有 K b 值<2.4 × 10 −5 . 注4: 稳定酮的实例是二异丙基酮、樟脑、二苯甲酮、联苯胺、二苯甲酮等。 注5: 浓度高达92的硫酸 % 可以直接滴定；有关更高的浓度，请参阅 注释13 . 注6: 在碘-碘体系中发生氧化还原反应的化合物会产生干扰。

1.1 This test method is intended as a general guide for the application of the volumetric Karl Fischer (KF) titration for determining free water and water of hydration in most solid or liquid organic and inorganic compounds. This test method is designed for use with automatic titration systems capable of determining the KF titration end point potentiometrically; however, a manual titration method for determining the end point visually is included as Appendix X1 . Samples that are gaseous at room temperature are not covered (see Appendix X4 ). This test method covers the use of pyridine-free KF reagents for determining water by the volumetric titration. Determination of water using KF coulometric titration is not discussed. By proper choice of the sample size, KF reagent concentration and apparatus, this test method is suitable for measurement of water over a wide concentration range, that is, parts per million to pure water. 1.2 The values stated in SI units are to be regarded as standard. 1.3 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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warnings are given in 3.1 . 1.4 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions for chemicals used in this test procedure. 1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 4.1 Titration techniques using KF reagent are one of the most widely used for the determination of water. 4.2 Although the volumetric KF titration can determine low levels of water, it is generally accepted that coulometric KF titrations (see Test Method E1064 ) are more accurate for routine determination of very low levels of water. As a general rule, if samples routinely contain water concentrations of 500 mg/kg or less, the coulometric technique should be considered. 4.3 Applications can be subdivided into two sections: ( 1 ) organic and inorganic compounds, in which water may be determined directly, and ( 2 ) compounds, in which water cannot be determined directly, but in which interferences may be eliminated by suitable chemical reactions or modifications of the procedure. Further discussion of interferences is included in Section 5 and Appendix X2 . 4.4 Water can be determined directly in the presence of the following types of compounds: Organic Compounds Acetals Ethers Acids ( Note 1 ) Halides Acyl halides Hydrocarbons (saturated and unsaturated) Alcohols Ketones, stable ( Note 4 ) Aldehydes, stable ( Note 2 ) Nitriles Amides Orthoesters Amines, weak ( Note 3 ) Peroxides (hydro, dialkyl) Anhydrides Sulfides Disulfides Thiocyanates Esters Thioesters Inorganic Compounds Acids ( Note 5 ) Cupric oxide Acid oxides ( Note 6 ) Desiccants Aluminum oxides Hydrazine sulfate Anhydrides Salts of organic and inorganic acids ( Note 6 ) Barium dioxide Calcium carbonate Note 1: Some acids, such as formic, acetic, and adipic acid, are slowly esterified. When using pyridine-free reagents, commercially available buffer solutions can be added to the sample prior to titration. With formic acid, it may be necessary to use methanol-free solvents and titrants ( 1 ) . 4 Note 2: Examples of stable aldehydes are formaldehyde, sugars, chloral, etc. Formaldehyde polymers contain water as methylol groups. This combined water is not titrated. Addition of an excess of NaOCH 3 in methanol permits release and titration of this combined water, after approximate neutralization of excess base with acetic acid (see Note 9 ). Note 3: Weak amines are considered to be those with K b value <2.4 × 10 −5 . Note 4: Examples of stable ketones are diisopropyl ketone, camphor, benzophenone, benzil, dibenzolacetone, etc. Note 5: Sulfuric acid up to a concentration of 92 % may be titrated directly; for higher concentrations see Note 13 . Note 6: Compounds subject to oxidation-reduction reactions in an iodine-iodide system interfere.