电感耦合等离子体原子发射光谱法和电感耦合等离子体质谱法测定不同肥料产品中铊含量比对  

Comparison of Thallium Content in Different Fertilizer Products by ICP-AES and ICP-MS

作　　者：姚洵 卢志琴 顾强 秦立俊 徐海斌 YAO Xun;LU Zhiqin;GU Qiang;QIN Lijun;XU Haibin(Comprehensive Technology Center of Zhangjiagang Customs,Zhangjiagang,Jiangsu 215600,China;Zhangjiagang Inspection and Certification Co.,Ltd.,Zhangjiagang,Jiangsu 215600,China;Comprehensive Technology Center of Lianyungang Customs,Lianyungang,Jiangsu 222042,China)

机构地区：[1]张家港海关综合技术中心,江苏张家港215600 [2]张家港检验认证有限公司,江苏张家港215600 [3]连云港海关综合技术中心,江苏连云港222042

出　　处：《中国无机分析化学》2023年第12期1363-1369,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：南京海关科研项目(2023KJ31)。

摘　　要：铊是一种高毒性的微量元素,具有较强的富集能力,已被列为肥料的强制性检验项目。选择水溶性肥料、复混肥料、有机肥料3种代表性的肥料样品,通过比对微波消解和电热板敞口消解前处理方式,分析电感耦合等离子体原子发射光谱(ICP-AES)法和电感耦合等离子体质谱(ICP-MS)法主要干扰来源,建立各自的标准工作曲线、比对方法检出限、精密度、加标回收率,探讨肥料产品中铊含量的测定方法。结果表明:微波消解法和电热板敞口消解法各有优点,可以根据样品实际情况灵活选择;ICP-AES法主要干扰为光谱干扰,需要在前处理过程中除去Mn,而ICP-MS法主要干扰为基体效应,可以使用内标物加以校正;ICP-MS法的检出限低于ICP-AES法;由于微波消解-ICP-AES法无法除去消解液中的Mn带来的光谱干扰,因此不适合测定铊含量,而微波消解-ICP-MS法、电热板敞口消解-ICP-AES法和电热板敞口消解-ICP-MS法这三种方法测定结果无明显差异,测定标准化肥质控样品均在指定值范围内,加标回收率为86.0%~110%。实验室可以根据肥料样品的数量、组成、性质合理选择搭配前处理方式和测定方法。Thallium is a highly toxic trace element,with strong enrichment ability,and has been listed as a mandatory test item of fertilizer.In this study,three representative fertilizer samples of water-soluble fertilizer,compound fertilizer and organic fertilizer were selected to comparing the pretreatment method of microwave digestion and electric heating plate digestion.The main interference sources of the inductively coupled plasma atomic emission spectrum(ICP-AES)method and the inductively coupled plasma mass spectrometry(ICP-MS)method were analyzed.The determination method of thallium content was discussed by establishing standard working curve,detection limit,precision and recovery in fertilizer products.The results showed that microwave digestion method and electric heating plate digestion method had different advantages and could be selected flexibly according to the actual situation of samples.The main interference of ICP-AES method was spectral interference.It needed to remove Mn elements during pre-treatment.The main interference of ICP-MS method was matrix effect.It could be corrected by using internal standard.The detection limit of the ICP-MS method was lower than the ICP-AES method.The microwave digestion-ICP-AES method couldn′t remove the spectral interference of the Mn element in the digestion solution,so it was not suitable to determine the thallium content.There was no significant difference among microwave digestion-ICP-MS method,electric heating plate digestion-ICP-AES method and electric heating plate digestion-ICP-MS method.The standard fertilizer quality control samples were within the specified value range,and the recovery rates were 86.0%—110%.The pretreatment and determination methods can be selected according to the quantity,composition and property of samples.

关 键 词：电感耦合等离子体原子发射光谱法 电感耦合等离子质谱法 肥料 铊 微波消解 电热板敞口消解 

分 类 号：O657.31[理学—分析化学]