{"title":"容器顶空液相微萃取-分光光度法测定碘酸盐","authors":"Aimad-Eddine Tamen, A. Vishnikin","doi":"10.17721/moca.2021.137-146","DOIUrl":null,"url":null,"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 After that, the triiodide complex formed in the acceptor phase is withdrawn with a microsyringe and transferred to a 50 μL quartz micro cell with a 10 mm path length, where the absorbance is measured at 288 or 350 nm.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.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7000,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"3","resultStr":"{\"title\":\"In-Vessel Headspace Liquid Phase Microextraction Coupled to Spectrophotometry for Iodate Determination\",\"authors\":\"Aimad-Eddine Tamen, A. Vishnikin\",\"doi\":\"10.17721/moca.2021.137-146\",\"DOIUrl\":null,\"url\":null,\"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.\",\"PeriodicalId\":18626,\"journal\":{\"name\":\"Methods and Objects of Chemical Analysis\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.7000,\"publicationDate\":\"2021-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"3\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Methods and Objects of Chemical Analysis\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.17721/moca.2021.137-146\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Methods and Objects of Chemical Analysis","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.17721/moca.2021.137-146","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
In-Vessel Headspace Liquid Phase Microextraction Coupled to Spectrophotometry for Iodate Determination
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.
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.