以丁酮为衍生剂的气相色谱法测定盐湖水中碘
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摘要
建立了一种快速、批量测定盐湖水中碘含量的气相色谱法。碘离子与丁酮通过卤代衍生反应生成碘丁酮,由气相色谱(GC)-电子捕获检测器(ECD)进行定量测定。通过气相色谱-质谱法(GC-MS)确认了3-碘-2-丁酮和1-碘-2-丁酮两种异构体产物。采用两种异构体峰面积之和进行定量计算,标准曲线线性相关系数r2>0.999,方法的检出限为0.2 ng·L-1,10次重复测定RSD小于2%,加标回收率为94.7%~102%。方法可满足盐湖卤水中微量碘的测定,经验证该方法也可推广至海水、油田卤水、沉积物压榨水和孔隙水等水体中碘离子的快速测定。
This paper established a fast determination method of iodine in salt lake water. I-can be derived to iodine butanone which can be detected by gas chromatography(GC). GC-MS has confirmed that there are two iodine butanone isomers in the process which are 3-iodine-2-butanone and 1-iodine-2-butanone. This method adds two isomers peak area together to preform quantitative analysis. The liner correlation coefficient r2>0.999 and the detection limit was 0.2 ng · L~(-1). RSD was less than 2% in 10 parallel analysis and the recovery rates was 94.7%—102%. This method can not only determine iodine in salt lake water, but also determine iodine in seawater, oil field brine, sediment water and pore water.
This paper established a fast determination method of iodine in salt lake water. I-can be derived to iodine butanone which can be detected by gas chromatography(GC). GC-MS has confirmed that there are two iodine butanone isomers in the process which are 3-iodine-2-butanone and 1-iodine-2-butanone. This method adds two isomers peak area together to preform quantitative analysis. The liner correlation coefficient r2>0.999 and the detection limit was 0.2 ng · L~(-1). RSD was less than 2% in 10 parallel analysis and the recovery rates was 94.7%—102%. This method can not only determine iodine in salt lake water, but also determine iodine in seawater, oil field brine, sediment water and pore water.
引文
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[2]孙大鹏.我国高碘卤水分布规律及其形成(续完)——高碘卤水的形成条件和找碘方向[J].盐湖研究,2007,15(1):11-23.
[3]陈力.油田水中的碘、溴元素及其地球化学意义[J].石油实验地质,1983,5(1):85-86.
[4]宋彭生,李武,孙柏,等.盐湖资源开发利用进展[J].无机化学学报,2011,27(5):801-815.
[5]马培华.中国盐湖资源的开发利用与科技问题[J].地球科学进展,2000,15(4):365-375.
[6]Fehn U,Snyder G.129I in the Southern Hemisphere:Global redistribution of an anthropogenic isotope[J].Nuclear Instruments&Methods in Physics Research,2000,172(1–4):366-371.
[7]顾晓梅,王顺荣.以酮类为衍生剂气相色谱法测定碘的研究[J].中国科学院大学学报,1995,12(2):171-177.
[8]朱红霞,杨艳娥,许秀艳.气相色谱法测定水中碘化物前处理方法的比较[J].环境化学,2015,34(11):2142-2145.
[9]崔仙舟,王中柱.胶州湾近岸水中碘离子的气相色谱测定[J].海洋通报,1995,14(6):72-77.
[10]GB/T 5009.1-2003,食品卫生检验方法理化部分总则[S].
[11]DZ/T 0130.6-2006,地质矿产实验室测试质量管理规范第6部分:水样分析[S].
[2]孙大鹏.我国高碘卤水分布规律及其形成(续完)——高碘卤水的形成条件和找碘方向[J].盐湖研究,2007,15(1):11-23.
[3]陈力.油田水中的碘、溴元素及其地球化学意义[J].石油实验地质,1983,5(1):85-86.
[4]宋彭生,李武,孙柏,等.盐湖资源开发利用进展[J].无机化学学报,2011,27(5):801-815.
[5]马培华.中国盐湖资源的开发利用与科技问题[J].地球科学进展,2000,15(4):365-375.
[6]Fehn U,Snyder G.129I in the Southern Hemisphere:Global redistribution of an anthropogenic isotope[J].Nuclear Instruments&Methods in Physics Research,2000,172(1–4):366-371.
[7]顾晓梅,王顺荣.以酮类为衍生剂气相色谱法测定碘的研究[J].中国科学院大学学报,1995,12(2):171-177.
[8]朱红霞,杨艳娥,许秀艳.气相色谱法测定水中碘化物前处理方法的比较[J].环境化学,2015,34(11):2142-2145.
[9]崔仙舟,王中柱.胶州湾近岸水中碘离子的气相色谱测定[J].海洋通报,1995,14(6):72-77.
[10]GB/T 5009.1-2003,食品卫生检验方法理化部分总则[S].
[11]DZ/T 0130.6-2006,地质矿产实验室测试质量管理规范第6部分:水样分析[S].