峰值积分-火花源原子发射光谱法测定低合金钢中酸溶铝

应用分光光度法、电感耦合等离子体原子发射光谱法测定钢中的酸溶铝不能满足炉前快速分析要求。通过正交实验确定冲洗时间5 s、预燃时间4 s、曝光时间16 s、氩气流量180 L/h的最佳分析条件;以Fe 2:281.329 nm为内标线,Al_sol 396.2 nm为分析线,实现了峰值积分-火花源原子发射光谱法对低合金钢中酸溶铝的分析。采用具有浓度梯度的标准样品绘制校准曲线,对曲线进行线性回归,并进行元素间的干扰校正,方法适用于低合金钢中质量分数为0.000 1%～0.50%的酸溶铝的测定。选择4个低合金钢标准样品进行精密度考察,测定结果的相对标准偏差(RSD,n=10)在0.78%~4.9%范围内;采用方法对4个中低合金钢标准样品和1个自制标样09Cr2AlMoRE进行分析,结果同认定值或滴定法测定结果基本一致,且测量误差满足国标GB/T222-2006的要求。方法适用于炉前快速分析。

Determination of acid-soluble aluminum in low alloy steel by peak integration-spark source atomic emission spectrometry

Determination of acid-soluble aluminum in steel by spectrophotometry and inductively coupled plasma atomic emission spectrometry could not satisfy pre-furnace rapid analysis requirements. Through orthogonal experiment, the optimal analytical conditions were established as follows: flush time of 5 s, preburn time of 4 s, exposure time of 16 s, argon flow of 180 L/h; the peak integration-spark source atomic emission spectrometric determination of acid-soluble aluminum in low alloy steel was realized with Fe 2: 281.329 nm as internal standard line and Al_sol 396.2 nm as analytical line. Certified reference materials with concentration gradient were used for plotting the calibration curve. Through linear regression of the curve, the interference between elements was corrected. The method was applicable to the determination of 0.000 1%-0.50% acid-soluble aluminum in low alloy steel. Four low alloy steel certified reference materials were selected for precision test, and the relative standard deviation (RSD, n=10) was in the range of 0.78%-4.9%. Four middle-low alloy steel certified reference materials and one self-made reference materials 09Cr2aLMoRE were determined by proposed method, and the results were basically consistent with the certified values or that obtained by titrimetry method, whose determination error satisfying the requirements of National standard method GB/T222-2006. The method was suitable for pre-furnace rapid analysis.