In-Vessel Headspace Liquid Phase Microextraction Coupled to Spectrophotometry for Iodate Determination

IF 0.7 Q4 CHEMISTRY, ANALYTICAL Methods and Objects of Chemical Analysis Pub Date : 2021-01-01 DOI:10.17721/moca.2021.137-146
Aimad-Eddine Tamen, A. Vishnikin
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引用次数: 3

Abstract

A new, highly sensitive and selective method for the spectrophotometric determination of iodate is developed based on the in-vessel mode of headspace liquid phase microextraction (IV-HS-LPME). The approach involves converting iodate to vapor iodine with excess of iodide and extracting it into a 50 μL of 1 % potassium iodide, which exposed to the headspace in a specially designed vessel. The extraction proceeds from 8 mL of aqueous solution containing 0.24 mmol L-1 of iodide and 0.5 mol L-1 of Na2SO4 after injection of 2 mL of 25 % H2SO4. The complete equilibrium is established after the aqueous solution stirred at 1200 rpm for 20 minutes. After that, the triiodide complex formed in the acceptor phase is withdrawn with a microsyringe and transferred to a 50 μL quartz micro cell with a 10 mm path length, where the absorbance is measured at 288 or 350 nm. The calibration graph is linear (r2 = 0.9998) in the range of 4 to 180 μg L-1 (as IO3-) with a detection limit of 1.5 μg L-1. The developed method has a high precision of 0.5 – 1.4 %. It was successfully applied to the determination of iodate in table salt, sea, and mineral water samples.
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容器顶空液相微萃取-分光光度法测定碘酸盐
建立了一种基于顶空液相微萃取(IV-HS-LPME)的高灵敏度、高选择性分光光度法测定碘酸盐的新方法。该方法包括将碘酸盐与过量的碘化物一起转化为蒸汽碘,并将其提取到50 μL的1%碘化钾中,将其暴露在一个特殊设计的容器中。在8ml含0.24 mmol L-1碘化物和0.5 mol L-1 Na2SO4的水溶液中,注入2ml 25% H2SO4进行萃取。溶液以1200rpm搅拌20分钟后达到完全平衡。然后,用微注射器取出受体相形成的三碘化物配合物,转移到50 μL的石英微池中,通道长度为10 mm,在288或350 nm处测量吸光度。在4 ~ 180 μg L-1(以IO3-为单位)范围内,标定图呈线性关系(r2 = 0.9998),检出限为1.5 μg L-1。该方法的精密度为0.5 ~ 1.4%。该法成功地应用于食盐、海水和矿泉水样品中碘酸盐的测定。
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来源期刊
CiteScore
1.00
自引率
14.30%
发文量
12
期刊介绍: The journal "Methods and objects of chemical analysis" is peer-review journal and publishes original articles of theoretical and experimental analysis on topical issues and bio-analytical chemistry, chemical and pharmaceutical analysis, as well as chemical metrology. Submitted works shall cover the results of completed studies and shall make scientific contributions to the relevant area of expertise. The journal publishes review articles, research articles and articles related to latest developments of analytical instrumentations.
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