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乙二胺四乙酸二钠用于沉积物酸溶相中高精度硼同位素测定方法研究 被引量:3

Application of Ethylenediaminetetraacetic Acid Disodium Salt to High Precision Measurement of Isotope of Boron in Acid-soluble Fraction of Sediments
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摘要 采用传统的酸溶法进行沉积物样品(包括粘土样品或碳酸盐等样品)硼同位素测定的前处理过程中,酸通常会溶解出样品中大量Ca^2+、Fe^3+、Mg^2+、Al^3+等金属离子以及稀土元素。由于前处理过程中溶出的硼只有在碱性环境中才能被硼特效树脂有效地吸附,而大量共存的Ca^2+、Fe^3+、Mg^2+、Al^3+等金属离子在碱性条件下会产生难溶于水的氢氧化物沉淀,进而会造成硼的丢失和同位素分馏。本研究在沉积物酸溶相样品中加入适量EDTA-2Na饱和溶液,再将样品溶液调成碱性,能有效抑制沉淀的产生。用氨水淋洗吸附后的硼特效树脂,并延长样品电离时间,能有效降低EDTA-2Na对硼同位素测定的干扰,从而达到样品中硼元素的高效提取和硼同位素组成的准确测定。结果表明,样品加入EDTA-2Na饱和溶液后硼的回收率可达到95%以上。同时,经过处理后的NIST SRM 951硼酸标准样品的11B/10B比值在4.05146~4.05628之间;三亚沉积物、大柴旦湖心沉积物和大柴旦湖心晶间卤水沉积物的硼同位素组成(δ11 B)分别为+17.64‰、-5.74‰和+1.8‰。本方法可满足沉积物样品(如粘土沉积物、碳酸盐沉积物、黄土、古土壤等样品)酸溶相中硼同位素组成高精度测定的要求,为此类样品的高精度硼同位素测定提供了一种简单、低干扰的前处理方法。 When nature sediments(e.g. clay/carbonate sediments) are dissolved by hydrochloric acid, a large number of metallic ions such as Ca, Mg, Fe, Al and rare earth elements are released. These metal ions make large amount of water-insoluble hydroxide precipitate under alkaline condition which can easily absorb and affect the extraction of boron(B) along with boron isotope composition(δ11B) determination. In this work, it was proved that when the solution was adjusted to alkalescent, adding an appropriate EDTA-2 Na could effectively avoid insoluble hydroxide precipitation. The interference of EDTA-2 Na to boron isotope determination was effectively reduced by rinsing the resin with ammonia after the alkalescent solution passing through the boron specific resin and extending the ionization time of simples in the measurement process. After the entire process, the recovery rate of boron was more than 95%, and the boron isotopic ratio of NIST SRM 951 ranged from 4.05146 to 4.05628. The boron isotopic composition(δ11B) of sediment of Sanya, Dachaidan lacustrine and Dachaidan intercrystalline were +17.64‰,-5.74‰ and +1.8‰, respectively. This method could meet the need of the high-precision determination of boron isotope of sediments such as clay sediments, carbonate sediments, loess and paleosol. In addition, this study provided a simple and low interference pretreatment method for high-precision determination of boron isotope.
作者 杨剑 马云麒 李兴意 刘玉秀 韩风清 张艳灵 Syed Asim Hussain 李海军 YANG Jian;MA Yun-Qi*;LI Xing-Yi;LIU Yu-Xiu;HAN Feng-Qing;ZHANG Yan-Ling;Syed Asim Hussain;LI Hai-Jun(Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources,Chinese Academy of Sciences,Xining 810008,China;Qinghai Provincial Key Laboratory of Geology and Environment of Salt Lakes,Chinese Academy of Sciences,Xining 810008,China;Salt Lake Chemical Analyzing and Testing Center,Qinghai Institute of Salt Lakes,Chinese Academy of Sciences,Xining 810008,China;University of Chinese Academy of Sciences,Beijing 100049,China)
出处 《分析化学》 SCIE EI CAS CSCD 北大核心 2019年第9期1433-1439,共7页 Chinese Journal of Analytical Chemistry
基金 国家自然科学基金项目(No.41473117) 中国科学院仪器设备功能开发技术创新项目(No.2020g102)资助~~
关键词 沉积物酸溶相 氢氧化物沉淀 乙二胺四乙酸二钠 硼同位素 热电离质谱 Acid-soluble fraction of sediment Hydroxide precipitation Ethylenediaminetetraacetic acid disodium salt Boron isotope Thermoelectric ionization mass spectrometry
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