火花源原子发射光谱法测定中低合金钢中酸溶铝

Determination of acid-soluble aluminium in middle-low alloy steel by spark source atomic emission spectrometry

用火花源原子发射光谱仪对中低合金钢中酸溶铝进行分析。讨论了不同制样方法(铣床、平磨机)及氩气状态对测定结果的影响,得出铣床制样为最佳选择,而平磨机制样时砂纸会带来同类元素的干扰,提出用铝质砂纸磨样后要用重叠点激发方式分析酸溶铝。修正了仪器自带分析程序中的响应曲线,采用经调整后的分析程序及其重叠点激发方式分析酸溶铝。方法用于低合金钢标准样品的分析,相对标准偏差为1.2%和2.9%;对于实际样品的分析,测定值与湿法结果一致。从分析的精度、本法与湿法分析对比后的结果看,完全能满足国标GB/T4336的要求(残余的氮化铝可忽略不计)。

The determination of acid-soluble aluminum in middle-low alloy steel by spark source atomic emission spectrometry was investigated.The effect of various sample preparation methods（milling machine and flat grinding machine） and argon state on determination results was discussed.It was found that the sample preparation by milling machine was the best selection,while sand paper may bring the interference of same-type elements if sample was prepared by flat grinding machine.After the sample was grinded with aluminum sand paper,the acid-soluble aluminum should be analyzed using overlapping-point excitation mode.The response curve of instrumental analysis program was modified.The acid-soluble aluminum was determined using the modified analysis program and overlapping-point excitation mode.The proposed method was applied to the analysis of low alloy steel standard sample.The relative standard deviations（RSD） were 1.2 % and 2.9 %,respectively.The found results of actual sample were consistent with those obtained by wet method.The analytical precision and comparison results between this method and wet analysis indicated that,the proposed method could fully meet the requirements of GB/T4336（the residual aluminum nitride could be ignored）.