微萃取浮选剂微萃取浮选浓度及水中氯乙酸浓度的测定

Q4 Chemistry Analitika i Kontrol Pub Date : 2021-01-01 DOI:10.15826/analitika.2021.25.2.002
V. Krylov, R. Mosyagin
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引用次数: 0

摘要

研究了一氯乙酸、二氯乙酸和三氯乙酸的浮选辅助液液微萃取方法。以甲基叔丁基醚(MTBE)为萃取剂。采用超声辐照进行乳化。微萃取过程在27 ml专用管中进行。它配备了用于提取样品的毛细血管和一个出风口。采用盐析添加剂Na2SO4降低MTBE在水中的溶解度,提高CAAs的萃取效率。采用八通道毛细管起泡器进行萃取剂乳液的空气通道。将有机基质置换法应用于离子色谱法测定CAAs的电导率检测。目前的研究表明,浮选辅助破乳优于离心破乳。氯化乙酸的浓度因子提高了2 ~ 3倍。水中CAAs的检出限降至(5·10-4 ~ 4·10-3 mg/l)。提取时间缩短3倍以上。采用加成法对HUC杂质的测定结果进行了验证。与随机误差相比,系统误差在统计上不显著。所建立的预富集与离子色谱相结合的方法可以测定比标准化的SanPiN和WHO低40-1250倍的CAAs浓度。这使得在临界生态状态开始之前就可以对水中的CAAs进行高度敏感的测定。
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Microextraction flotamicroextraction flotation concentration and determination of chloroacetic acids in watertion concentration and determination of chloroacetic acids in water
The flotation-assisted liquid-liquid microextraction method of mono-, di -, and trichloroacetic acids (CAAs) has been developed. Methyl tert-butyl ether (MTBE) was used as an extractant. The emulsification was performed by the ultrasonic irradiation. The microextraction procedure was carried out in a 27 ml special tube. It was equipped with the capillaries for sampling the extract and an air outlet. A salting-out additive (Na2SO4) was used to reduce the solubility of MTBE in water and to increase the extraction efficiency of CAAs. The air passage through the emulsion of the extractant was carried out using the eight-channel capillary bubbler. The organic matrix replacement was applied for ion chromatographic determination of CAAs with the conductivity detection. Current study showed the advantages of the flotation-assisted demulsification over the centrifugal one. The concentration factors of chlorinated acetic acids were 2-3 times higher. The detection limits of CAAs in water were reduced to (5·10-4 - 4·10-3 mg/l). The extraction time was reduced by more than three times. The trueness of the determination of HUC impurities was confirmed by the addition method. The statistical insignificance of the systematic error in comparison with the random error was shown. The developed method of preconcentration in combination with ion chromatography made it possible to determine the concentrations of CAAs 40-1250 times lower than the normalized SanPiN and WHO. This allowed conducting a highly sensitive determination of CAAs in water long before the onset of the critical ecological state.
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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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