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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
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引用本文:全洗强,陶 鑫,杜文越,秦愫妮,俞建国.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[J].中国岩溶,2017,36(3):415-418.
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全洗强 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 
陶 鑫 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 
杜文越 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 
秦愫妮 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 
俞建国 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 
基金项目:中国地质科学院岩溶地质研究所基本科研业务费项目(2015009)
中文摘要: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180.7 nm和182.0 nm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。
中文关键词:碳酸盐岩  单质硫  电感耦合等离子体光谱法
 
Liquid-Liquid extraction inductively coupled plasma atomic emission spectrometer (ICP-AES) for determination of elemental sulfur in carbonate rock
Abstract: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 180.7 nm and 182.0 nm, respectively. The linear correlation is 0.999 and 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 0.5 g carbonate standard sample was weighed in a 20 mL glass tube, followed by adding 5 mL hexane rapidly, 10 min of ultrasonic,intermittent 5 min, repeating two times and 30 min of cumulative ultrasonic, then stewing the filtrate for 10 min stratification. After centrifuging for 10 min, we got a supernatant and then transferred it to a Teflon crucible. They were repeated two times. Then hexane supernatant was collected and evaporated to dryness at a low temperature, 2 mL purity nitric acid was added to the Teflon crucible, then the lid cover was fixed to the cylinder barrel and then the solution was digested in an oven for 5 h at 150 ℃. Next we set the volume to 25 mL, shaking and measuring. We also conducted the blank experiments and standard addition method to obtain the recovery of elemental sulfur at 90%-110%. The results indicate that this method can meet the test requirements and can be used to determine elemental sulfur in carbonate rock.
keywords:carbonate rock, elemental sulfur, ICP-AES
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