基体未分离高分辨电感耦合等离子体质谱法测定钢中痕量元素

Determination of trace elements in steel by high resolution inductively coupled plasma mass spectrometry without matrix separation

为了满足钢铁产品日益严格的质量需求，将钢铁产品中痕量元素的测定下限降低至μg／g级也日显重要。本研究工作利用高分辨率的等离子质谱仪快速、准确测定了钢中μg／g级的B，Al，P，Cr，Pb，Sn，Sb，As，Bi等多种元素。钢铁样品用硝酸、盐酸、氢氟酸在电热板上加热或微波消解，溶液经稀释后未经基体分离，未加内标直接用电感耦合等离子体质谱法（ICP—MS）测定。该方法检测下限：P为0．145μg／g，其余元素低于0．1μg／g。精密度好，相对标准偏差（n=10）：Bi为10．5％，其余元素小于5％。回收率：As为81％～120％，其余元素86％～106％。标样的测定值与认定值吻合，方法非常适合测定钢铁产品中痕量元素。

necessary In to study, trace mined fast order to meet strict increasing reduce the determination low I elements like B, AI, P, Cr, Pb, S and accurately. Steel samples ly quanlity requirement imits of trace elements n, Sb, As, Bi in μg/g or were dissolved with in iron and steel production, it is in steel to the μg/g order. In this sub μg/g level in steel were deternitric acid, hydrochloric acid and hydrofluoric acid by electrothermal heating or microwave digestion. After diluted, the solution was measured by high resolution inductively couled plasma-mass spectrometry（HR-ICP-MS） without any matrix separation or internal standard. It had good precision giving RSDs（n=10） of below 5% except for 10.5~ of Bi. The detection limits of the method was lower than 0.1 μg/g,except for 0. 144 μg/g of P. The recoveries of 86%--10% were satisfied,except for 81%--120% of As. The measured values tally with the certified values. The method is extraordinary suitable for the determination of trace elements in steel.