火花源原子发射光谱法测定取向硅钢中碳硅锰磷硫

通过试验确定氩气分析流量为3.5 L/min，静态流量为0.75 L/min，冲洗时间为3 s，预燃时间为12 s，积分时间为5 s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。

Determination of carbon,silicon, manganese,phosphorus and sulfur in orientedsilicon steel by spark source atomic emission spectrometry

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 3.5 L/min, the static flow rate was 0.75 L/min, the flush time was 3 s, the precombustion time was 12 s and the integration time was 5 s. Two sample preparation methods, including milling machine and grinding wheel, were investigated. The precision test results showed that, the determination results were slightly affected by the sample preparation method. The effect of possible coexisting elements on the determination of carbon, silicon, manganese, phosphorus and sulfur in oriented silicon steel was discussed. It was found that, the interference of silicon on manganese could not be avoided. After correction by interference coefficient method, the correlation coefficients of calibration curves of all elements by fitting were higher than 0.999 0. Precision test was performed,and the relative standard deviations (RSD, n=10) were between 0.71 % and 9.4 %. Two oriented silicon steel production samples were analyzed by proposed method and Central Iron and Steel Research Institute (CISRI). The found results were consistent. Moreover, the deviation was within the allowance range.