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旨在提出一种微波酸溶/石墨炉原子吸收分光光度法测定土壤和沉积物中铍的方法。文中优化了仪器工作条件、阐述了校准曲线的绘制情况、讨论了土壤和沉积物的前处理过程(包括微波升温程序及消解体系的选择)以及考察了共存元素的干扰情况。实验表明,采用硝酸/氢氟酸/盐酸体系-微波消解进行样品前处理,应用塞曼扣背景-石墨炉原子吸收光谱法测定土壤/沉积物中铍,具有操作简单、无需基体改进剂、共存离子无干扰、再现性和重复性好等优点。在最优的实验条件下,当取样量为0.200 0g,定容体积为25mL,该方法测定土壤铍的方法检出限为0.004 9mg·kg-1,方法测定下限为0.020mg·kg-1。该法用于测定土壤标样和实际样品,不管是实验室内的方法比对,还是实验室间的方法验证,都获得较好的准确度和精密度。
Aiming to present a method for the determination of beryllium in soil and sediment by microwave acidolysis / graphite furnace atomic absorption spectrophotometry. In this paper, the working conditions of the instrument are optimized. The drawing of the calibration curve is described. The pretreatment process of soil and sediment (including the selection of microwave heating program and digestion system) and the interference of coexisting elements are discussed. Experiments show that the sample preparation by nitric acid / hydrofluoric acid / hydrochloric acid system - microwave digestion, the determination of beryllium in soil / sediment by using Zeeman buckle background - graphite furnace atomic absorption spectrometry, has the advantages of simple operation, no matrix modifier and coexistence Ion interference, reproducibility and repeatability and so on. Under the optimal experimental conditions, the detection limit of beryllium was 0.004 9 mg · kg-1 and the lower limit of determination was 0.020 mg · kg-1 when the sample volume was 0.200 g and the constant volume was 25 mL. The method is used to determine soil samples and actual samples, whether in the laboratory method comparison, or laboratory method validation, get better accuracy and precision.