摘要
高岭土作为重要的铝硅酸盐,其微量元素的含量决定着高岭土产品的性能指标。高岭土的三种国家标准物质成分GBW03121、GBW03122、GBW03122a中均未含有As、Sb等10种微量元素的标准值,在高岭土的检测中只能采用近似的岩石标准物质作为监控物质,对高岭土组分的准确分析有一定影响。本文通过微波消解技术,对比了硝酸-氢氟酸二酸及硝酸-氢氟酸-过氧化氢三酸溶样体系,讨论了微波消解的程序升温条件及消解时间等影响因素,并对电感耦合等离子体质谱法(ICP-MS)的干扰因素进行了探讨,建立了微波消解硝酸-氢氟酸-过氧化氢三酸溶样体系,ICP-MS法测定高岭土中As、Sb等10种微量元素的分析方法。方法检出限在0.01~0.09mg/kg之间,测定下限在0.03~0.30mg/kg之间。利用岩石标准物质直接验证了方法的准确度和精密度,元素回收率在90.9%~103.2%之间,相对标准偏差(RSD)在1.2%~5.8%之间。同时对方法的不确定度进行了综合评估,证实方法准确可靠。本方法酸类用量少,缩短了测定时间,减少了对环境及人体的影响,适用于高岭土样品中As、Sb等10种微量元素的批量分析,对高岭土国家标准物质成分中As、Sb等10种微量元素的标准值测定提供了参考。
BACKGROUND:As an important aluminosilicate,trace element contents affect the performance of the product.The kaolin standard substances GBW03121,GBW03122,GBW03122a lack the recommended values of ten elements such as arsenic and antimony.Similar rock standard materials were used for monitoring the determination procedure,but the accurate results of the kaolin samples may be affected.OBJECTIVES:To establish a method for accurate determination of 10 trace elements in kaolin sample such as arsenic and antimony.METHODS:With microwave digestion technology,the nitrate-hydrofluoric acid system and nitrate-hydrofluoric-peroxide system were compared for the procedural heating conditions and dissolution time of microwave digestion.Interference factors of the inductively coupled plasma mass spectrum were also investigated.RESULTS:The detection limits of 10 elements were 0.01-0.09mg/kg,and measurement limits were 0.03-0.30 mg/kg.The accuracy and precision of the method were directly verified by using rock reference materials.The element recovery was between 90.9%and 103.2%,and the relative standard deviation(RSD)was between 1.2%and 5.8%.At the same time,a comprehensive evaluation of the uncertainty of the method was carried out,and the method was proved to be accurate and reliable.CONCLUSIONS:This method has little acid dosage,shortens the measurement time,and reduces the damage on the environment and human,making it suitable for the batch analysis of 10 trace elements in kaolin samples.The method also provides a reference for the determination of the certified values of 10 trace elements such as As and Sb in the national standard material of kaolin.
作者
李丽君
薛静
LI Li-jun;XUE Jing(Shenyang Centre of Geological Survey,China Geological Survey,Key Laboratory for Evolution and Ecological Effect in Black Soil,Ministry of Natural Resources,Shenyang 110032,China)
出处
《岩矿测试》
CSCD
北大核心
2022年第1期22-31,共10页
Rock and Mineral Analysis
基金
中国地质调查局地质调查项目“兴凯湖平原及松辽平原西部土地质量地球化学调查”(DD20190520)。
关键词
高岭土
微量元素
硝酸-氢氟酸-过氧化氢酸溶
微波消解
电感耦合等离子体质谱法
动能歧视模式
kaolin
trace elements
nitrate-hydrofluoric-peroxide acid dissolution
microwave digestion
inductively coupled plasma-mass spectrometry
kinetic energy discrimination model
