辉光放电发射光谱法测定钢板镀锌层中铅镉铬

发布时间：2019-04-09 12:31

【摘要】：通过条件试验,确定了辉光放电发射光谱仪(GD-OES)的最佳分析参数为:分析功率30 W、氩气气压620Pa、预溅射时间200s、积分时间10s。选用多种基体标准样品,通过溅射率校正建立校准曲线,定量分析镀锌板镀层中铅、镉、铬元素含量及分布状况,得到镀锌层中各元素随深度变化的分析谱图,方法定义了镀层中元素积分计算方法,从而得到镀层中铅、镉、铬元素含量。以纯锌标准样品进行检出限测定,各元素的检出限分别为3.65(铅)、1.33(镉)、0.21(铬)μg/g;以纯锌标准样品进行短期精密度考察,3个元素测定结果的相对标准偏差(RSD,n=15)分别为2.8%(铅)、1.3%(镉)、6.6%(铬)。制备了典型涂镀样板,采用实验方法进行测定,并采用电感耦合等离子体质谱法进行比对分析,结果一致性较好。实验方法适用于快速定量测定钢表面1~50μm厚度的镀锌板镀层中铅、镉、铬元素含量。
[Abstract]:The optimum analytical parameters of glow discharge emission spectrometer (GD-OES) are determined by conditional test: analysis power 30 W, argon pressure 620 Pa, pre-sputtering time 200 s, integral time 10 s. The calibration curves of various matrix standard samples were established by sputtering rate correction, and the content and distribution of lead, cadmium and chromium elements in the coating of galvanized sheet were quantitatively analyzed, and the analytical spectra of the elements in the plating layer varied with depth were obtained. Methods the integral calculation method of elements in the coating was defined, and the contents of lead, cadmium and chromium in the coating were obtained. The detection limits of each element were 3.65 (lead), 1.33 (cadmium) and 0.21 (chromium) 渭 g 路g-1 for pure zinc standard samples, respectively, and the detection limits for each element were 3.65 (lead), 1.33 (cadmium) and 0.21 (chromium) 渭 g respectively. The relative standard deviations (RSD,n=15) of the three elements were 2.8% (lead), 1.3% (cadmium) and 6.6% (chromium), respectively. The typical coating samples were prepared and determined by experimental method and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). The results were consistent with each other. The experimental method is suitable for the rapid quantitative determination of lead, cadmium and chromium in the coating of galvanized sheet with the thickness of 1 ~ 50 渭 m on the surface of steel.
【作者单位】：鞍钢集团公司钢铁研究院;
【基金】：国家质检公益性科研项目(200810595)
【分类号】：TG142.15

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