摘要
建立了电感耦合等离子质谱仪(ICP-MS)同时测定土壤和沉积物中硼、磷、锗、砷、铌、钼、锡、锑、钨的方法.实验确定了用2.75g过氧化钠于725 ℃熔融8 min,确保样品熔解完全,采用732型强酸性阳离子交换树脂交换消除溶液中的钠的基体干扰,最后在氦气流量为4.0 mL/min碰撞模式下进行测定.实验得到硼、磷、锗、砷、铌、钼、锡、锑、钨检出限分别为:0.47、2.65、0.06、0.41、0.86、0.17、0.43、0.03、0.29 μg/g;标准物质各元素测定结果与认定值的对数差△LgC小于0.035;相对标准偏差(RSD)小于8.06％;与多目标区域地球化学调查方法验证实验RD结果小于24％,方法检出限、正确度、精密度及RD都满足DZ/T 0258-2014 要求.
Abstract
A method of inductively coupled plasma mass spectrometry(ICP-MS)for the simultaneous determination of boron,phosphorus,ger-manium,arsenic,niobium,molybdenum,tin,antimony and tungsten in soil and sediments was established.It was determined that 2.75 g of sodium peroxide was melted at 725 ℃ for 8min to ensure the complete melting of the sample,and the strong acidic cation exchange resin type 732 was used to exchange to eliminate the matrix interference of sodium in the solution,and finally the determination was carried out under the collision mode with helium flow rate of 4.0 ml/min.The detection limits of boron,phosphorus,germanium,arsenic,niobium,molybdenum,tin,antimony and tungsten were 0.47,2.65,0.06,0.41,0.86,0.17,0.43,0.03 and 0.29 µg/g,respectively;the logarithmic difference between the results of the determination of the standard substance and the recognized value of the standard substance △LgC was less than 0.035;the relative standard deviation(RSD)was less than 8.06％;The RD result of the method validation experiment is less than 24％,and the method detection limit,correctness,precision and RD meet the requirements of DZ/T 0258-2014.
维普
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