摘要
从分析样品的制备、分析方法的检出限、精密度和准确度方面,对同时测定地球化学样品中的铜、铅、锌和镍的电感耦合等离子体原子发射光谱法(ICP-AES)、X射线荧光光谱法(XRF)和摄谱法进行了比较。其中ICP-AES采用王水溶样,各元素选用干扰较少的分析线进行测定;XRF采用岩石、土壤、水系沉积物和合成灰岩光谱分析标准物质等国家标准物质绘制校准曲线,使用铑靶Kα线的康普顿散射线作内标校正基体效应;摄谱法无需称样,采用碘酸钾饱和溶液作为缓冲剂进行摄谱,CTS计算机自动译谱仪进行定量译谱。经过比较后得出:ICP-AES测量范围宽,检出限低,精密度高,准确度好,适合大批量地球化学样品中铜、铅、锌、镍的测定;XRF检出限、精密度和准确度基本满足区域地球化学调查规范的要求,其分析效率取决于地球化学样品压制的成型率;摄谱法检出限、精密度和准确度基本符合要求,其分析流程长,操作繁琐,对于大批量地球化学样品测定,分析效率比较低。
A comparison between inductively coupled plasma atomic amission spectrometry（ICP-AES）, X- ray fluorescent spectrometry（XRF） and spectrographic method for the determination of copper, lead, zinc and nickel in geochemical samples was made from the preparation of analytical sample, the detection limit, precision and accuracy of analytical method aspects. In ICP-AES , the sample was dissolved in aqua regia and the elements were determined using analytical lines with low interference In XRF, the calibration curve was plotted using the national certified reference materials of rock, soil, stream sediment and synthesized limestone for spectral analysis. The Compton scattering line of Ka line from rhodium target was used as in- ternal standard to correct the matrix effect. In spectrographic method, the sample weighing was not re- quired. The potassium iodate saturated solution was used as buffer reagent. The quantitative spectra inter- pretation was automatically realized by CTS computer. The comparison indicated that the ICP-AES exhibited wide measurement range, low detection limit, high precision and good accuracy, and it was suitable for the determination of copper, lead, zinc and nickel in large amounts of geochemical samples. The detection limit, precision and accuracy of XRF could basically meet the requirements of regional geochemical investigation specifications. Its analytical efficiency was depended on the forming rate of pressed geochemical samples. The detection limit, precision and accuracy of spectrographic method could basically meet the requirements. However,the analytical procedures were long and the operation was complicated. Its analytical efficiency was low for the determination of geochemical samples in large amount.
出处
《冶金分析》
CAS
CSCD
北大核心
2015年第5期48-53,共6页
Metallurgical Analysis
关键词
电感耦合等离子体原子发射光谱法
X射线荧光光谱法
摄谱法
地球化学样品
铜
铅
锌
镍
inductively coupled plasma atomic emission spectrometry
X-ray fluorescence spectrometry
spectrographic method
geochemical sample
copper
lead
zinc
nickel
