液液萃取电感耦合等离子体光谱法测定碳酸盐岩中的单质硫  

Liquid-Liquid extraction inductively coupled plasma atomic emission spectrometer (ICP-AES) for determination of elemental sulfur in carbonate rock

作　　者：全洗强 陶鑫[1] 杜文越[1] 秦愫妮[1] 俞建国[1] QUAN Xiqiang TAO Xin DU Wenyue QIN Suni YU Jianguo(Institute of Karst Geology, CAGS/Key Laboratory of Karst Dyna mics, MLR＆GZAR,Guilin, Guangxi 541004, China)

机构地区：[1]中国地质科学院岩溶地质研究所/国土资源部广西岩溶动力学重点实验室,广西桂林541004

出　　处：《中国岩溶》2017年第3期415-418,共4页Carsologica Sinica

基　　金：中国地质科学院岩溶地质研究所基本科研业务费项目(2015009)

摘　　要：建立了碳酸盐岩样品中单质硫的分析方法,此法以正己烷为萃取剂,在180.7nm和182.0nm波长下用电感耦合等离子体光谱法(ICP-AES)测定国家标准物质GBW(E)07108和碳酸盐岩样品。正己烷萃取碳酸盐岩中单质硫的回收率在90%~110%之间;每个样品测定7次,相对标准偏差(RSD)<5.0%。结果表明,此法满足实验要求,可用于大批量碳酸盐岩样品中单质硫的测定。Under condition of hypoxia,sulfate sulfur is reduced to sulfide sulfur in the process of carbonate deposition.Part of the sulfide is combined with organic to generate complicated organic sulfur while the majority of sulfide with metal ions to form sulfide precipitation.However,the sulfide precipitation is so unstable that can be converted to a stable pyrite through hydrogen sulfide,iron sulfide polysulfide and ferrous sulfide paths.Under the oxygen-rich condition,the sulfur-oxidizing bacteria will oxidate sulfide into elemental sulfur and the disproportionation of elemental sulfur will lead to the formation of various sulfurs which are stored in carbonate deposition.At present,a variety of methods are available for the measurement of elemental sulfur and its species.Unfortunately,only a few are useful at mg/L levels,which offer the possibility of applying them in different matrices.There are methods for the determination of elemental sulfur at trace levels,but they are often complicated and/or time-consuming.As a new analytical technique,inductively coupled plasma atomic emission spectrometry（ICP-AES）has many advantages such as high sensitivity,small matrix effects,wide linear range,good precision and a variety of elements can be measured simultaneously.In this paper,a method is proposed to analyze elemental sulfur in carbonate rock,which is determined with ICP-AES at the wave length of 180.7nm and 182.0nm,respectively.The linear correlation is 0.999and the relative standard deviation（RSD）is lower than 5.0%.In this work,the pre-treatment method of the elemental sulfur in carbonate is established.We made efforts to reduce the impacts of extraction volume,ultrasonic time and digestion time on the recovery of elemental sulfur to obtain the optimal solution for elemental sulfur extraction.The optimal scheme is as follow,firstly,a 0.5g carbonate standard sample was weighed in a 20mL glass tube,followed by adding 5mL hexane rapidly,10min of ultrasonic,intermittent 5min,repeating two times and 30min of cumulativ

关 键 词：碳酸盐岩 单质硫 电感耦合等离子体光谱法 

分 类 号：P575.4[天文地球—矿物学]