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液体推进剂混胺燃料中作为主要组分存在的三乙胺使其显示较高的碱性,对用卡尔费休滴定法测定其水分含量时产生干扰。提出了在试样的甲醇滴定介质中加入一定量的乙酸,保持液体混胺试样和乙酸的体积比小于或等于3比5,达到使滴定介质的酸度控制在最佳pH范围5~6之间。经此操作,由三乙胺的高碱度引起的干扰可消除。对已知水分含量的混胺试样按方法进行分析,算得其水分测定值的相对标准偏差(n=12)为2.1%。取不同批号的混胺试样7件,按方法进行分析并用标准气量法对结果进行校核。两种方法测定结果的相对偏差在-0.023%~0.033%之间。又根据t-检验法的结果认定,两方法所得测定值之间不存在显著差异。
The presence of triethylamine in the liquid propellant mixture amine fuel as a major component renders it more alkaline and interferes in the determination of its moisture content by Karl Fischer titration. It is proposed that a certain amount of acetic acid is added to the methanol titration medium of the sample so as to keep the volume ratio of the liquid mixed amine sample and acetic acid less than or equal to 3 to 5 so that the acidity of the titration medium is controlled within the optimum pH range of 5 to 6 between. With this operation, the interference caused by the high basicity of triethylamine can be eliminated. The method for the analysis of mixed amine samples of known moisture content was calculated to have a relative standard deviation (n = 12) of 2.1% for the measured value of moisture. Take different batches of seven samples of mixed amine, according to the method of analysis and the results of the standard gas volume method of checking. The relative deviation between the two methods was -0.023% ~ 0.033%. According to the results of the t-test, it is concluded that there is no significant difference between the measured values obtained by the two methods.