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采用全氟油为固定液,聚三氟氯乙烯为担体的色谱柱及吸收氟用银柱,用镍丝镍材热导池鉴定器和耐腐蚀平面六通阀的三柱串联流程可定量分析含有氢、氮、氧、氟、四氟化硅、氟化氢等混合物的气体组成。本文中对峰高定量归一化衰减法及重叠峰减扣定量法进行了理论分析,认为对分析误差为1%的峰高定量法所要求的分离度为K_1=1.91,相当R=1.17。即当色谱峰只要能分离(5%分离度)就能进行峰高定量。而重叠峰减扣定量因子是不随各峰浓度变化的一个常数,并可由分离度来预测。上述两种定量方法用实验证明对氢、氮、氟、氧等已知配样的分析误差一般在1%以内。对化学性极活泼的四氟化硅、氟化氢分析误差较大,最大可达3.5%。
Using perfluorinated oil as fixed liquid, polychlorotrifluoroethene as support column and absorption of fluorine silver column, with nickel wire nickel material thermal conductivity detector and corrosion resistance of the plane six-way valve three-column series process can be quantitative analysis Contains hydrogen, nitrogen, oxygen, fluorine, silicon tetrafluoride, hydrogen fluoride and other mixtures of gas composition. In this paper, the quantitative analysis of peak height quantitative normalization and overlapped peak subtraction deduction method is theoretically analyzed. It is considered that the resolution required by peak height quantitative method with analytical error of 1% is K_1 = 1.91 and equivalent R = 1.17. That is when the chromatographic peak as long as the separation (5% resolution) will be able to peak height quantitative. The overlapped peak deduction quantification factor is a constant that does not vary with each peak concentration and can be predicted by resolution. The above two quantitative methods experimentally prove that the analytical errors of known sample of hydrogen, nitrogen, fluorine and oxygen are generally within 1%. For chemical extremely active silicon tetrafluoride, hydrogen fluoride analysis error is large, up to 3.5%.