X射线荧光光谱法测定锌合金中铜和铁

Determination of copper and iron in zinc alloy by X-ray fluorescence spectrometry

通过用未校正UniQuant软件对样品进行定性分析,找出样品中可能含有的元素,并对其逐一进行分析线扫描,确定样品中元素种类及大概含量,然后在最佳的仪器分析条件下,采用单点校正曲线,对锌合金中铜、铁元素进行了测试,从而实现X射线荧光光谱法(XRF)对锌合金中铜和铁的检测。考察了分析时间、探测器、分析线及制样方法对分析结果的影响。结果表明:分析时间为60s,选择FPC探测器,以Kα线作为分析线时,待测元素的灵敏度和精密度较高。对铣成的块状锌合金样品、屑状样品的粉末与硼酸通过压制成片状样品进行直接分析,测定结果与电解法和ICP-AES法基本一致,相对标准偏差分别为0.29%和1.9%(n=6),极差分别为0.016%和0.000 8%,小于现有国家标准方法中规定的重复性限。

In oder to find posible elements in sample, the sample was qualitatively analyzed using the UniQuant software without correction. The scanning of analytical lines for all elements was conducted to determine the type and approximate content of elements in sample. Then, copper and iron in zinc alloy were determined using single-point calibration curve under the optimal instrumental conditions, realizing the determination of copper and iron in zinc alloy by X-ray fluorescence spectrometry （XRF）. The effect of analytical time, detector, analytical line and sample preparation method on the determination results was investigated. The results indicated that the sensitivity and precision of testing elements were high under the following conditions： the analytical time was 60 s, the FPC detector was used, and the Kα line was selected as the analytical line. The milled block samples of zinc alloy and slice samples which were prepared by pressing the powder of ship shape samples and boric acid for direct analysis. The determination results were basically consistent with those obtained by electrolytic method and ICP-AES. The relative standard deviation （RSD, n=6） was 0.29% and 1.9%, respectively. The range was 0. 016% and 0. 0008%, which was lower than the repeatability limit specified in current national standard method.