气相色谱系统惰性测试的改进

Q4 Chemistry Analitika i Kontrol Pub Date : 2020-01-01 DOI:10.15826/analitika.2020.24.2.004
I. Zenkevich, A. I. Desyatova
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引用次数: 0

摘要

先前提出的控制气相色谱(GC)系统惰性的方法是基于对随后稀释(10倍稀释的样品数量为5)获得的一系列样品的测试溶液中极性和非极性成分的峰面积比(S rel = S极性/ S非极性)的测定。为了提高评估分析物最小量(m lim)的可靠性,可以忽略气相色谱系统的惰性不足,对该方法进行了修改。除此之外,还实现了实验操作的简化和并行决策的最小化,以及数据处理的更加合理的算法。改进方法的实质是用三次多项式近似S rel = f (p m)数据集,然后将这些数据与平均S rel(带有标准偏差)值进行比较,以获得具有最高浓度测试化合物的三种测试方法的最具重复性的S rel值。结果表明,wcot色谱柱(标准非极性聚二甲基硅氧烷固定相)的惰性范围从纳克级到几纳克级。测试样品的结果中含有一些极性成分(如苯丙醇),这表明惰性不足的整体表现不仅可能是由于色谱系统的影响,而且还可能是由于用于稀释测试样品的小瓶表面吸附了极性分析物。在相同的分析条件下,当在玻璃或聚丙烯小瓶中进行稀释时,揭示了相同极性组分的m值的差异。
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Modification of inertness test for gas chromatographic systems
The previously proposed approach for controlling the inertness of gas chroma to graphic (GC) systems was based on the determination of peak area ratios for polar and non-polar constituents of test-solutions ( S rel = S polar / S non-polar ) for the series of samples obtained by the consequent dilutions (for the 10-times dilutions the number of samp les was five). This appro ach was modified with the purpose of increasing the relia bi lity of evaluating the minimal quantities of analytes ( m lim ), for which one can neglect the insufficient inertness of GC systems. In addition to that, the simplification of experimental opera tions and minimizing the number of parallel determina ti ons as well as more rational algorithm of data processing was achieved. The essence of the modified appro ach was the approximation of S rel = f (p m ) data sets with the 3 rd degree polynomials, following by comparing these data with the averaged S rel (with standard deviations) values for the most reproducible S rel values of three test-so lu tions with the highest concentrations of test-compounds. It was shown that the limits of the inertness for the WCOT-column (with the standard non-polar polydimethylsiloxane stationary phase) were from the fractions of nano gram to several nanograms of polar analytes in the chromatographic zone. The results for the test-samples contained some polar constituents (e.g., benzyl alco hol) which lead to suggesting that the integral manifestations of the insufficient inertness could be caused not only by the influence of chromatographic systems, but also by the sorp tion of polar analytes on the surfaces of vials used for the dilution of test-samples. The differences in m lim values for the same polar components at the same analytical conditions, when the dilutions were carried out in the glass or polypropylene vials, were revealed.
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来源期刊
Analitika i Kontrol
Analitika i Kontrol Chemistry-Analytical Chemistry
CiteScore
0.90
自引率
0.00%
发文量
15
期刊介绍: Analitika i Kontrol is a scientific journal covering theoretical and applied aspects of analytical chemistry and analytical control, published since autumn 1997. Founder and publisher of the journal is the Ural Federal University named after the first President of Russia Boris Yeltsin (UrFU, Ekaterinburg).
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