火花源原子发射光谱法测定钢中氮

以火花源原子发射光谱法测定钢中氮，对样品制备、冲氩时间、预燃时间等分析条件进行讨论，发现砂纸磨样、铣床铣样两种样品制备方式对精度影响不大，考虑圆柱样品铣床制样不易控制，因此实验采用砂纸制样，同时确定冲氩时间和预燃时间均为5　s。为消除共存元素干扰，采用共存元素硅进行干扰校正，校正后校准曲线线性良好，元素的测定范围为0000 5%～0023 0%，氮的检出限为0000 5 %。对生产样和标样进行精密度考察，相对标准偏差（n=11）均小于5%；采用本法及惰气熔融热导法同时对样品进行分析，测定值基本一致，t检验的结果证明两种方法没有显著性差异。方法已应用于实际生产。

Analysis of nitrogen in steel by spark atomic emission spectrometry

The method of determining nitrogen in steel by spark source atomic emission spectrometry was used,and the sample preparation,the argon flushing time and the pre-sparking time were discussed.It was found two sample preparation methods: the sand paper grinding sample and the mill milling sample does hot affect the precision.It was not easy to control the milling machine milled the column sample,so the experiment adopted sand paper ground sample.At the same time the argon flushing time and the pre-sparking time was set at 5 second.To eliminate interference of coexisting elements,silicon of coexisting element was used as interference correction,and the corrected calibration curves linear were satisfactory,the determination range of nitrogen was 0.000 5%-0.023 0%,the detection limit of nitrogen was 0.000 5%,this method was applied in determining the production sample and standard sample that the precisions were investigated,the relative standard deviations(n=11) were all less than 5%;it was adopted that this method and the inert gas fusion thermal conductivity of t test method determined sample at the same time,the results obtained consistent basically,The results proved that no significant difference were observed.The method has been applied to the actual production.