超声提取、气体在线稀释电感耦合等离子体质谱法测定土壤中有效钼  

Determination of available molybdenum in soil by inductively coupled plasma mass spectrometry with ultrasonic extraction and gas online dilution

作　　者：鄢飞燕[1,2,3] 袁玉玲 刘朝 张鑫[1,2,3] 王瑾 范鹏飞[1] 梁少霞 YAN Feiyan;YUAN Yuling;LIU Chao;ZHANG Xin;WANG Jin;FAN Pengfei;LIANG Shaoxia(Research Institute No.230,CNNC,Changsha 410007,China;CNNC Geological Exploration Environment Protection Technology Co.,Ltd.,Changsha 410017,China;Hunan Engineering Technology Research Center for Evaluation and Comprehensive Utilization of Associated Radioactive Mineral Resources,Changsha 410007,China;Perkinelmer Enterprise Management Co.,Ltd.,Guangzhou Branch,Guangzhou 510370,China)

机构地区：[1]核工业二三〇研究所,长沙410007 [2]湖南中核环保科技有限公司,长沙410007 [3]湖南省伴生放射性矿产资源评价与综合利用工程技术研究中心,长沙410007 [4]珀金埃尔默企业管理有限公司广州分公司,广州510370

出　　处：《化学分析计量》2025年第2期89-93,共5页Chemical Analysis And Meterage

摘　　要：建立基于超声波辅助提取、结合在线稀释气技术与电感耦合等离子体质谱法测定土壤中有效钼。利用国家标准物质GBW(E) 070333作为参考进行超声提取时间试验,确定了最佳超声提取时间为20 min。选择铟元素及氧化产率(以CeO/Ce计)作为观察对象,调节稀释气流量,在同时满足铟元素强度达到最高且氧化产率低于0.025条件下,确定最佳稀释气流量为0.32 L/min。在优化后的仪器条件下,有效态钼在质量浓度0~100μg/L内与钼及内标质谱强度比值线性关系良好,方法检出限为0.001 9 mg/kg,测定结果的相对标准偏差小于10%(n=8)。用国家有效态土壤标准物质进行方法准确度验证,相对误差在±5%之内(n=8),测定结果与推荐值相吻合,经t检验表明两种方法测量值无显著性差异。该方法具有快速、准确和检出限低的特点,可满足大量全国土壤普查样品中有效钼的分析要求。A method for the determination of available molybdenum in soil was established based on ultrasonic-assisted extraction,combined with on-line dilution gas technology and inductively coupled plasma mass spectrometry.The ultrasonic extraction time test was carried out by using the national standard material GBW(E)070333 as a reference,and the optimum ultrasonic extraction time was determined to be 20 min.The indium element and oxidation yield(calculated as CeO/Ce)were selected as the observation objects,and the dilution gas flow rate was adjusted.Under the condition that the indium element strength reached the highest and the oxidation yield was lower than 0.025,the optimal dilution gas flow rate was determined to be 0.32 L/min.Under the optimized instrument conditions,the effective molybdenum had a good linear relationship with the ratio of mass spectrometry intensity to internal standard intensity in the concentration range of 0-100μg/L.The detection limit of the method was 0.0019 mg/kg,and the relative standard deviation of the test results was less than 10%(n=8).The accuracy of the method were verified by the national available soil standard material.The relative error was within±5%(n=8).The results were consistent with the recommended values.The t test results showed that there was no significant difference between the two methods.The method is rapid and accurate with low detection limit,which can be applied to determine available forms of molybdenum in a large number of soil survey samples in China.

关 键 词：超声提取 电感耦合等离子体质谱 有效钼 在线稀释 

分 类 号：O657.6[理学—分析化学]