直流辉光放电原子发射光谱法测定中低合金钢中锆

Determination of zirconium in middle-low alloy steel by direct current glow discharge atomic emission spectrometry

采取9种不同梯度锆量中低合金钢标准样品绘制曲线,建立了测定中低合金钢中锆的直流辉光放电原子发射光谱法。以单因素法考察了直流辉光光谱仪实验参数对测定中低合金钢中锆的影响,确定激发电压为1 250V、激发电流为45mA、预燃时间为60s、积分时间为10s。以锆元素光谱强度为横坐标,锆元素质量分数为纵坐标绘制校准曲线,其校准曲线线性相关系数为0.996 1,线性范围为0.004 4%~0.35%。采用实验方法对中低合金钢标准样品中锆进行测定,测定值与认定值基本一致,相对标准偏差(RSD,n=11)为0.72%~1.7%,测定结果的相对标准偏差都符合仪器推荐测量要求(相对标准偏差小于3%)。将实验方法应用于中低合金钢实际样品分析,测得结果与国标方法 GB/T 223.30—1994基本一致。

The calibration curve was prepared using nine certified reference materials of middle-low alloy steel with various gradients of zirconium content.The determination method of zirconium in middle-low alloy steel by direct current glow discharge atomic emission spectrometry was established.The effect of experimental parameters of direct current glow discharge spectrometer on the determination of zirconium in middle low alloy steel was investigated by single factor method.The following conditions were obtained as follow：the excitation voltage was 1 250 V,the excitation current was 45 mA,the pre-combustion time was60 s,and the integration time was 10 s.The calibration curve was plotted using the spectral intensity of zirconium as horizontal ordinate and the corresponding mass fraction as the vertical coordinate.The linear correlation coefficient of calibration curve was 0.996 1,and the linear range was 0.004 4%-0.35%.The proposed method was applied to the determination of zirconium in standard samples of middle-low alloy steel.The found results were consistent with the certified values.The relative standard deviations（RSD,n=11）were between 0.72%and 1.7%,which could meet the recommended measurement requirements of instrument（RSD was less than 3%）.The proposed method was applied to the determination of zirconium in actual samples of middle-low alloy steel.The found results were in good agreement with those obtained by national standard method（GB/T 223.30-1994）.