简易修正卡尔-费休滴定法测定甲醇中的水分含量
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摘要
最常用的水含量测定技术是卡尔-菲舍尔滴定法,它需要专门的设备。当没有适当的设备时,该方法可以通过目测滴定终点来实现,这不允许对有色样品进行分析。在这里,选择东方中海油生产的优级甲醇,通过分光度法检测。滴定终点,适用于甲醇样品的水分测定。反应发生在密封的4 mL容器中。检测波长为520nm。滴定终点根据标准ASTM E1064-16制定,根据滴定体积绘制吸光度图。该方法具有较好的重现性(RSD=4.3%)、准确度和线性(R~2=0.997)。
The most commonly used technique for the determination of water content is Karl Fischer titration,which requires specialized equipments.In the absence of proper equipment,the method can be used by visual titration endpoint,but it is not used for the analysis of colored samples.In this paper,the superior methanol produced by CNOOC was selected and detected by spectrophotometry.Titration end point was suitable for methanol sample moisture determination.The reaction occurred in a sealed 4 mL container.Detection wavelength was 520 nm.The titration end point was determined according to the standard ASTM E 1064-16,and the absorbance chart was drawn according to the titration volume.The method showed good reproducibility(RSD=4.3%),accuracy and linearity(R~2=0.997).
The most commonly used technique for the determination of water content is Karl Fischer titration,which requires specialized equipments.In the absence of proper equipment,the method can be used by visual titration endpoint,but it is not used for the analysis of colored samples.In this paper,the superior methanol produced by CNOOC was selected and detected by spectrophotometry.Titration end point was suitable for methanol sample moisture determination.The reaction occurred in a sealed 4 mL container.Detection wavelength was 520 nm.The titration end point was determined according to the standard ASTM E 1064-16,and the absorbance chart was drawn according to the titration volume.The method showed good reproducibility(RSD=4.3%),accuracy and linearity(R~2=0.997).
引文
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[9]孙海燕,王保玉,王向丽,李亚情.卡尔费休法测定尼龙66切片的含水量[J].工程塑料应用,2013,41(05):75-77.
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[2]何志惠.卡尔-费休法在油脂产品水分测定中的应用简介[J].泸天化科技,2017(04):185-188.
[3]井文杰,张航,王洋,刘冉,李海平,翁薇.空气湿度对卡尔费休法测定化工产品水分的影响[J].化学推进剂与高分子材料,2016,14(02):83-86.
[4]王爱萍,龚维,刘新,姚旭霞,李承荣,张符.卡尔·费休法测定水分的样品处理方法[J].理化检验(化学分册),2016,52(03):369-372.
[5]张健健,胡建强,杨士钊.石油产品水分检测技术研究现状及进展[J].当代化工,2016,45(01):210-212.
[6]张战军,温丽瑗,吴世逵,王志明.卡尔·费休法测定石油产品水分的影响因素分析[J].当代化工,2015,44(12):2936-2938.
[7]王大壮.助溶剂对甲醇汽油耐水性的影响[J].当代化工, 2013, 42(05):537-539+553.
[8]郭洪波.卡尔费休法微量水分测定仪测量结果不确定度评定[J].黑龙江科技信息,2013(23):136.
[9]孙海燕,王保玉,王向丽,李亚情.卡尔费休法测定尼龙66切片的含水量[J].工程塑料应用,2013,41(05):75-77.
[10]齐景杰.醛、酮类有机溶剂中水分的测定[J].山东化工,2011,40(07):52+69.