Hátle M
Department of Analytical Chemistry, Charles University, Albertov 2030, 128 40 Prague 2, Czechoslovakia.
Talanta. 1987 Dec;34(12):1001-7. doi: 10.1016/0039-9140(87)80148-0.
Four types of working electrode (glassy-carbon and gold rotating-disk electrodes and two types of gold-film electrode) have been used in determination of traces of mercury by differential-pulse anodic-stripping voltammetry, and the analytical parameters of the procedures compared. The technique has been applied to the analysis of river sediments. The lowest limit of detection (0.02 mug/l.) was obtained with the gold rotating-disk electrode. Two procedures have been found optimal for analyses of sediment samples; determination with the gold rotating-disk electrode and solution-exchange after the preelectrolysis, and determination with the gold-film electrode prepared in situ in the sample extract. The sample pretreatment involved a separation of the 0.45-63 mum fraction, mineralization with a mixture of hydrochloric and nitric acids (3:1 or 1:3) under atmospheric pressure in a fused silica vessel, followed by irradiation with ultraviolet light, after addition of hydrogen peroxide (to destroy organic matter). The most serious interference is from iron; this can be prevented by adding fluoride or pyrophosphate. The procedure is an alternative to the AAS determination of the total mercury content in sediments, especially with heavily polluted samples (mercury concentrations up to 0.01%).
采用四种工作电极（玻碳旋转圆盘电极、金旋转圆盘电极和两种金膜电极），通过差分脉冲阳极溶出伏安法测定痕量汞，并比较了各方法的分析参数。该技术已应用于河流沉积物分析。使用金旋转圆盘电极时检测限最低（0.02μg/l）。已发现两种方法最适合沉积物样品分析：使用金旋转圆盘电极并在预电解后进行溶液交换，以及使用在样品提取物中原位制备的金膜电极进行测定。样品预处理包括分离0.45 - 63μm的部分，在常压下于熔融石英容器中用盐酸和硝酸（3:1或1:3）的混合物进行矿化，加入过氧化氢（以破坏有机物）后再用紫外光照射。最严重的干扰来自铁；可通过添加氟化物或焦磷酸盐来防止。该方法是原子吸收光谱法测定沉积物中总汞含量的替代方法，尤其适用于污染严重的样品（汞浓度高达0.01%）。
