微波消解-电感耦合等离子体质谱法同时测定有机肥料中9种有毒有害元素的含量  

Simultaneous Determination of 9 Toxic and Harmful Elements in Organic Fertilizer by Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion

作　　者：丁伟[1] 王文佳[1] 吴凡[1] 柳羽丰[1] DING Wei;WANG Wenjia;WU Fan;LIU Yufeng(The Academy of Quality Inspection and Research in Heilongjiang Province,Harbin 150028,China)

机构地区：[1]黑龙江省质量监督检测研究院,哈尔滨150028

出　　处：《理化检验（化学分册）》2024年第1期83-87,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：黑龙江省省属科研院所科研业务费项目(CZKYF2020C011)。

摘　　要：提出了微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定有机肥料中As、Cd、Co、Cr、Ni、Pb、Sb、Tl、V等9种有毒有害元素含量的方法。取0.10 g有机肥料样品于聚四氟乙烯微波消解罐中,以2.5 mL盐酸、7.5 mL硝酸和2.0 mL氢氟酸为混合酸进行微波消解。消解结束后,于140℃赶酸,然后加入1.0 mL 50%(体积分数)硝酸溶液,再用水定容至50 mL,摇匀,过滤,取滤液待测,在线加入混合内标溶液。结果表明:9种元素标准曲线的线性范围均为2~100μg·L^(-1),方法检出限(3s)为0.59~66.75μg·kg^(-1);按照标准加入法对典型有机肥料样品进行回收试验,9种元素测定值的相对标准偏差(n=7)为2.0%~3.5%,回收率为81.5%~112%。A method for the simultaneous determination of 9 toxic and harmful elements, including As, Cd, Co, Cr, Ni, Pb, Sb, Tl and V in organic fertilizer by inductively coupled plasma mass spectrometry(ICP-MS) with microwave digestion was proposed. The organic fertilizer sample(0.10 g) was placed into a polytetrafluoroethylene microwave digestion tank, and 2.5 mL of hydrochloric acid, 7.5 mL of nitric acid and 2.0 mL of hydrofluoric acid were used as the mixed acid for microwave digestion. After digestion finished, the acid was driven at 140 ℃. Then 1.0 mL of 50%(volume fraction) nitric acid solution was added, and the volume was made up to 50 mL with water. The mixed solution was shaken well and filtered, and the filtrate was taken to be determined with adding the mixed internal standard solution online. It was shown that the linear ranges of the standard curves for 9 elements were 2-100 μg·L^(-1), with detection limits(3s) of method in the range of 0.59-66.75 μg·kg^(-1). Test for recovery was made on the typical organic fertilizer sample according to the standard addition method, and RSDs(n=7) of the determined values for 9 elements were in the range of 2.0%-3.5%, with recoveries ranged from 81.5% to 112%.

关 键 词：有机肥料 微波消解 电感耦合等离子体质谱法(ICP-MS) 元素 

分 类 号：O657.63[理学—分析化学]