卡尔费休法测定有机胺中水分含量的改进研究

Improvement of Karl Fischer method for determination of water content in organic amines

在现有方法的基础上进行改进,建立了新的卡尔费休法测定有机胺中水分含量的方法。向滴定容器中加入甲醇,平衡水分检测装置;加入稳定剂硫酸锌,调节pH,再次平衡水分检测装置;最后加入试样,利用卡尔费休试剂进行滴定,测定己二胺样品中的水分含量。利用此方法测定有机胺中的水分含量,样品的加标回收率达到95.51%~102.41%,相对标准偏差(RSD)在8%以内,且避免了现有酸类试剂与胺反应产生水导致测试结果不准确的问题。结果表明,该方法操作简单方便,准确度高,重复性好,适用于有机胺中水分含量的测定。

A Karl Fischer method for the determination of water content in organic amines is established based on the improvement of the existing method.Methanol is added into the titration vessel to balance the moisture detection device;Then,zinc sulfate,the stabilizer,is added to adjust the pH value and balance the moisture detection device again;Finally,the sample is added and titrated with Karl Fischer reagent to determine the moisture content in organic amine sample.When using this method to determine the moisture content in organic amines,the recoveries of the samples are 95.51%-102.41%,and the relative standard deviation(RSD)is less than 8%.The inaccurate test results problem that is caused by the reaction between existing acid reagents and amines to produce water is avoided.Results indicate that the method is simple,accurate and reproducible,and suitable for the determination of water content in organic amines.