{"title":"用脂肪族硫醇进行现场衍生化和气相色谱鉴定","authors":"T. Rozsypal","doi":"10.2298/jsc221207025r","DOIUrl":null,"url":null,"abstract":"The report describes the development of methods for rapid and simple identification of Adamsite in mobile laboratory conditions using a field gas chromatograph coupled with mass spectrometer. Adamsite is a chemical warfare agent with unique properties that cannot be analyzed without conversion to a volatile derivative. Derivatization procedures with 5 aliphatic thiols (ethanethiol, 1-propanethiol, 2-propanethiol, 1-butanethiol and 1-hexanethiol) were developed and compared. The retention characteristics of the derivatization products, peak characteristics and the formation of unwanted artifacts in the chromatograms were monitored. The influence of the reaction media and the time dependence of the reaction were also objects of interest. Other investigated parameters were the optimal reaction temperature and the volume of the derivatization agent. Mass spectra of newly created substances that are not yet included in the chemical weapons related databases were recorded. With optimal reagents (1-butanethiol and 1-hexanethiol), calibration procedures for analyte determination were subsequently developed, and the methods were verified during the Adamsite identification test in selected environmental and urban matrices.","PeriodicalId":17489,"journal":{"name":"Journal of The Serbian Chemical Society","volume":"1 1","pages":""},"PeriodicalIF":1.0000,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Use of aliphatic thiols for on-site derivatization and gas chromatographic identification of Adamsite\",\"authors\":\"T. Rozsypal\",\"doi\":\"10.2298/jsc221207025r\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"The report describes the development of methods for rapid and simple identification of Adamsite in mobile laboratory conditions using a field gas chromatograph coupled with mass spectrometer. Adamsite is a chemical warfare agent with unique properties that cannot be analyzed without conversion to a volatile derivative. Derivatization procedures with 5 aliphatic thiols (ethanethiol, 1-propanethiol, 2-propanethiol, 1-butanethiol and 1-hexanethiol) were developed and compared. The retention characteristics of the derivatization products, peak characteristics and the formation of unwanted artifacts in the chromatograms were monitored. The influence of the reaction media and the time dependence of the reaction were also objects of interest. Other investigated parameters were the optimal reaction temperature and the volume of the derivatization agent. Mass spectra of newly created substances that are not yet included in the chemical weapons related databases were recorded. With optimal reagents (1-butanethiol and 1-hexanethiol), calibration procedures for analyte determination were subsequently developed, and the methods were verified during the Adamsite identification test in selected environmental and urban matrices.\",\"PeriodicalId\":17489,\"journal\":{\"name\":\"Journal of The Serbian Chemical Society\",\"volume\":\"1 1\",\"pages\":\"\"},\"PeriodicalIF\":1.0000,\"publicationDate\":\"2023-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of The Serbian Chemical Society\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.2298/jsc221207025r\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of The Serbian Chemical Society","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.2298/jsc221207025r","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Use of aliphatic thiols for on-site derivatization and gas chromatographic identification of Adamsite
The report describes the development of methods for rapid and simple identification of Adamsite in mobile laboratory conditions using a field gas chromatograph coupled with mass spectrometer. Adamsite is a chemical warfare agent with unique properties that cannot be analyzed without conversion to a volatile derivative. Derivatization procedures with 5 aliphatic thiols (ethanethiol, 1-propanethiol, 2-propanethiol, 1-butanethiol and 1-hexanethiol) were developed and compared. The retention characteristics of the derivatization products, peak characteristics and the formation of unwanted artifacts in the chromatograms were monitored. The influence of the reaction media and the time dependence of the reaction were also objects of interest. Other investigated parameters were the optimal reaction temperature and the volume of the derivatization agent. Mass spectra of newly created substances that are not yet included in the chemical weapons related databases were recorded. With optimal reagents (1-butanethiol and 1-hexanethiol), calibration procedures for analyte determination were subsequently developed, and the methods were verified during the Adamsite identification test in selected environmental and urban matrices.
期刊介绍:
The Journal of the Serbian Chemical Society -JSCS (formerly Glasnik Hemijskog društva Beograd) publishes articles original papers that have not been published previously, from the fields of fundamental and applied chemistry:
Theoretical Chemistry, Organic Chemistry, Biochemistry and Biotechnology, Food Chemistry, Technology and Engineering, Inorganic Chemistry, Polymers, Analytical Chemistry, Physical Chemistry, Spectroscopy, Electrochemistry, Thermodynamics, Chemical Engineering, Textile Engineering, Materials, Ceramics, Metallurgy, Geochemistry, Environmental Chemistry, History of and Education in Chemistry.