外标法中利用溶剂信号降低气相色谱定量的不确定度

Q4 Chemistry Analitika i Kontrol Pub Date : 2022-01-01 DOI:10.15826/analitika.2022.26.2.005
I. Zenkevich, S. V. Byvsheva, A. Gerasimov, S. Gladnev, M. V. Grigoriev, N. Gubina, E. Didenko, A. S. Kazantsev, T. D. Kalutskaia, E. V. Katernuk, A. Koblova, D. V. Krutin, K. P. Malkova, S. A. Metliaeva, V. S. Odegova, D. S. Smirnova, V. Spivakovskyi, P. Terno
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引用次数: 0

摘要

采用绝对峰面积法(包括外标法)的气相色谱定量测定结果的不确定度对注射剂的重现性相当“敏感”。补偿这种误差的有效方法是在样品中引入额外的标准品,然后用它们与标准品的峰面积之比代替绝对峰面积。需要强调的是,样品的任何成分都可以用作附加标准,包括溶剂。溶剂可以用于这些目的,即使当分析信号超过放大器限制时,其峰的高度受到限制。使用相对峰面积不需要任何额外的样品处理,除了登记溶剂的峰面积。比较常用的外标法和改进后的外标法,用相对峰面积代替绝对峰面积不影响测定的整体精密度(按“引入-测定”标准),但可将重现性提高2-3倍。讨论了如何提高这类结果的统计评价的可靠性问题,并提出了改变实验“设计”的建议。而不是一系列的连续分析类似的来源样品,使用平行测定是可取的。例如,在学生实践作业的完成过程中可以实现这一点。
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Decreasing the uncertainty of gas chromatographic quantification using the solvent’s signal in the method of external standard
Uncertainties of the results of quantitative determinations in gas chromatography using the methods based on the absolute peak areas (including the external standard method) are rather “sensitive” to the reproducibility of injections. The effective way to compensate for such errors is to introduce the additional standards into the samples, followed by replacing the absolute peak areas by their ratios to peak areas of the standards. It is important to underline that any constituents of the samples can be used as additional standards, including the solvents. Solvents can be used for these purposes even if the heights of their peaks are restric­ted when the analytical signals exceed the amplifier limits. Using the relative peak areas does not require any extra sample processing besides the registration of peak areas for solvents. Comparing the commonly known and modified methods of external stan­dard demonstrates that using the relative peak areas instead of the absolute ones does not influence the overall precision of determinations (according to the criterion “intro­duced-determined”) but improve the reproducibility by 2-3 times. The problem of increasing the reliability of such statistical evaluations of results is discussed and to solve it, it is proposed to change the “design” of the experiments. Instead of series of successive analyses of similar origin samples, the use of parallel determinations is preferable. This can be realized, for example, during the fulfillment of student’s practical works.
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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).
期刊最新文献
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