【摘要】 通过试验确定氩气分析流量为3.5L/min,静态流量为0.75L/min,冲洗时间为3s,预燃时间为12s,积分时间为5s的激发条件,采用火花源原子发射光谱法测定取向硅钢中碳、硅、锰、磷、硫。分别采用铣床铣样、砂轮磨样两种制样方式进行了精密度考察,发现制样方式对结果影响不大;讨论了取向硅钢样品中碳、硅、锰、磷、硫测定时可能存在的共存元素干扰,发现硅对锰元素的干扰不可忽略,采用干扰系数法进行了校正,据此拟合得到各元素校准曲线的相关系数均在0.999 0以上。精密度考察结果表明,碳、硅、锰、磷、硫的相对标准偏差(n=10)在0.71%~9.4%之间。对两块取向硅钢生产样品进行分析,并与钢铁研究总院进行比对分析,结果一致,且偏差均在允许范围内。
【Abstract】 Carbon,silicon,manganese,phosphorus and sulfur in oriented silicon steel were determined by spark source atomic emission spectrometry.The selected excitation conditions were as follows:the analytical flow rate of argon was 3.5L/min,the static flow rate was 0.75L/min,the flush time was3s,the precombustion time was 12sand the integration time was 5s.Two sample preparation methods,including milling machine and grinding wheel,were investigated.The precision test results showed that,the determination…
火花源原子发射光谱;
碳;
硅;
锰;
磷;
硫;
【Key words】 oriented silicon steel;
spark source atomic emission spectrometry;
carbon;
silicon;
manganese;
phosphorus;
sulfur;
原文发表于《冶金分析》2013年第10期