微波消解–ICP–OES法测定难分解不锈钢和中低合金钢中7种元素

Determination of Seven Elements in Difficultly Decomposed Stainless Steel and Middle-Low Alloy Steel with Microwave Digestion and ICP–OES

以微波消解–ICP–OES法测定难分解不锈钢和中低合金钢中Cr，Ni，Mn，V，Ti，Cu，Mo的含量。样品经6 mL稀王水和0.5 mL HF微波消解处理后，用带有耐HF进样系统的ICP–OES仪测定试样中多种元素。在优化仪器分析参数和消除基体及共存元素的干扰后，各待测元素的检出限为0.0009%～0.0099%，校准工作曲线的线性相关系数均大于0.999，相对标准偏差为0.27%～1.50%（n=6）。该方法适用于难分解不锈钢和中低合金钢中7种元素含量的日常检测。

A method for the determination of Cr, Ni, Mn, V, Ti, Cu, Mo in difficultly decomposed stainless steel and middle-low alloy steel based on microwave digestion and ICP–OES was established. Samples were digested by microwave with 6 mL dilute aqua regia and 0.5 mL HF, and the digestion solution was determined by ICP–OES with hydrofluoric acid corrosion resistant injection systems. After optimizing the instrument parameters, and eliminating the interference of matrix and coexistence elements, detection results showed that the detection limit of the elements to be measured were 0.000 9%–0.009 9%, the linear correlation coefficients of the calibration curve were all more than 0.999, the relative standard deviations were 0.27%–1.50%（n=6）. The method can be used in the decomposition of 7 elements in stainless steel and low alloy steel in daily inspection with satisfactory results.