微波消解-电感耦合等离子质谱(ICP-MS)法测定肥料中8种重金属元素  

Determination of 8 Heavy Metal Elements in Fertilizers by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)with Microwave Digestion

作　　者：杨凯 欧阳燕 文典 刘成文 YANG Kai;OUYANG Yan;WEN Dian;LIU Chengwen(Shenzhen Institute of Quality&Safety Inspection and Research,Shenzhen,Guangdong 518055,China;Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences,Guangzhou,Guangdong 510640,China)

机构地区：[1]深圳市质量安全检验检测研究院,广东深圳518055 [2]广东省农业科学院农业质量标准与监测技术研究所,广州510640

出　　处：《中国无机分析化学》2024年第9期1204-1210,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：广东省农业标准化协会团体标准项目(粤农标协字﹝2023﹞19号)。

摘　　要：为有效监管肥料中重金属元素,样品经硝酸(HNO_(3))+盐酸(HCl)+高氯酸(HClO_(4))微波消解体系消解后,于150℃赶酸2 h,加入适量金元素作为汞稳定剂,采用电感耦合等离子体质谱法-氦气碰撞模式(KED)技术,以锗(Ge)、铟(In)、铋(Bi)元素作为内标,同时对样品中铅、镉、铬、砷、汞、铜、锌、镍等8种元素进行分析,建立了微波消解-电感耦合等离子质谱(ICP-MS)法同时测定肥料中8种重金属元素含量的方法。结果表明,各元素的相关系数均大于0.9993,检出限0.001~0.058 mg/kg,加标回收率83.0%~114%,平行样品相对标准偏差(RSD)0.70%~5.2%。方法简便快捷、灵敏度高、准确可靠,适合肥料中铅、镉、铬、砷、汞、铜、锌、镍等8种元素的同时测定。In order to effectively regulate heavy metal elements in fertilizers,inductively coupled plasma mass spectrometry(ICP-MS)with microwave digestion method was established to simultaneously determine the content of eight heavy metal elements in fertilizers.The sample was digested by a microwave digestion system consisting of nitric acid(HNO_(3)),hydrochloric acid(HCl),and perchloric acid(HClO_(4)).After being pickled at 150℃for 2 hours,an appropriate amount of gold was added as a mercury stabilizer.The helium collision mode(KED)of ICP-MS was used,with germanium(Ge),indium(In),and bismuth(Bi)as internal standards.Eight elements,including lead,cadmium,chromium,arsenic,mercury,copper,zinc,and nickel,were analyzed in the sample.The results showed that the correlation coefficients of each element were greater than 0.9993,the detection limit was 0.001—0.058 mg/kg,the recoveries of spiked samples was 83.0%—114%,and the relative standard deviation(RSD)of parallel samples was 0.70%—5.2%.This method is simple,fast,highly sensitive,accurate and reliable,suitable for the simultaneous determination of 8 elements in fertilizers,including lead,cadmium,chromium,arsenic,mercury,copper,zinc,and nickel.

关 键 词：微波消解 ICP-MS 肥料 重金属元素 

分 类 号：O657.63[理学—分析化学]