微波消解-电感耦合等离子体质谱法同时测定肥料中9种有毒有害元素  

Simultaneous determination of 9 toxic and harmful elements in fertilizers by microwave digestion inductively coupled plasma mass spectrometry

作　　者：姚春毅 陈佳悦 王国兴 李玉朴 刘晨雨 YAO Chun-yi;CHEN Jia-yue;WANG Guo-xing;LI Yu-pu;LIU Chen-yu(Shijiazhuang Customs Technology Center,Shijiazhuang Hebei 050051)

机构地区：[1]石家庄海关技术中心,河北石家庄050051

出　　处：《中国土壤与肥料》2024年第11期264-270,共7页Soil and Fertilizer Sciences in China

摘　　要：由于钒(V)、铬(Cr)、镍(Ni)、钴(Co)、砷(As)、镉(Cd)、锑(Sb)、铊(Tl)、铅(Pb)9种元素已被列为肥料中有毒有害物质,被强制要求不得高于限量,现有的国家标准检测方法对肥料中有毒有害元素的检测方法复杂,建立微波消解结合电感耦合等离子体质谱(ICP-MS)测定肥料中9种有毒有害元素的方法,以完善肥料检测的需求。选用河北省市场上销售的不同种类肥料作为实验样品,采用微波消解前处理技术消解样品,优化仪器工作参数,以73锗(Ge)、103铑(Rh)、209铋(Bi)为内标元素,使用ICP-MS测定肥料中9种元素。结果表明,9种元素在线性范围内关系良好,加标回收率为91.09%~105.43%,相对标准偏差(n=6)为1.28%~7.40%,检出限分别为1.76、10.64、35.87、3.17、0.43、1.50、3.78、4.28、180.47μg/L。所测肥料均符合国标要求,同时该方法灵敏度高、简便快捷,适用于肥料中9种有毒有害元素的测定。Due to the fact that nine elements,vanadium(V),chromium(Cr),nickel(Ni),cobalt(Co),arsenic(As),cadmium(Cd),antimony(Sb),thallium(Tl),and lead(Pb),have been listed as toxic and harmful substances in fertilizers and are required to not exceed their limits,the existing national standard testing methods for toxic and harmful element in fertilizers are complex,this article established a method of microwave digestion combined with inductively coupled plasma mass spectrometry(ICP-MS)to determine the nine toxic and harmful elements in fertilizers,in order to improve the requirements of fertilizer detection methods.Different types of fertilizers sold in the market in Hebei Province were selected as experimental samples,microwave digestion pre-treatment technology was used to digest the samples,instrument operating parameters were optimized,and 73 germanium(Ge),103 rhodium(Rh),and 209 bismuth(Bi)were used as internal standard elements to determine 9 elements in fertilizers using ICP-MS.The results showed that the 9 toxic and harmful elements had a good linear relationship,with a recovery rate of 91.09%-105.43%and a relative standard deviation(n=6)of 1.28%-7.40%.The detection limits were 1.76,10.64,35.87,3.17,0.43,1.50,3.78,4.28 and 180.47μg/L.In conclusion,the tested fertilizers all met the requirements of national standards,and this method was highly sensitive,simple,and fast,suitable for the determination of 9 toxic and harmful element in fertilizers.

关 键 词：肥料 微波消解 电感耦合等离子体质谱 有毒有害元素 

分 类 号：O657.63[理学—分析化学] TQ440.72[理学—化学]