论文部分内容阅读
建立了碱消解-高效液相色谱(HPLC)同时测定土壤中无机汞和甲基汞的分析方法。试验研究了KOH/甲醇提取液浓度、消解时间以及反萃取剂Na2S2O3浓度对碱消解过程中甲基汞提取率的影响,当KOH/甲醇提取液浓度为25%、消解时间为12 min、Na2S2O3浓度为0.01 mol/L时,KOH/甲醇溶液对土壤甲基汞的提取率最高。提取出的无机汞和甲基汞,经衍生后HPLC法测定,流动相最佳选择为0.01 mol/LTBABr和0.025 mol/L NaCl的水溶液:甲醇=45:55(v:v)。在优化检测条件下,土壤样品中无机汞和甲基汞的检出限分别为1 ng/g和10 ng/g。该方法样品前处理简单、线性范围宽、精密度高、准确性好,适用于土壤中汞化合物的形态分析。
An analytical method for simultaneous determination of inorganic mercury and methylmercury in soil by alkaline digestion - high performance liquid chromatography (HPLC) was established. The effects of concentration of KOH / methanol extract, digestion time and concentration of stripping agent Na2S2O3 on the extraction rate of methylmercury were studied experimentally. When the concentration of KOH / methanol extract was 25%, the digestion time was 12 min, the concentration of Na2S2O3 At 0.01 mol / L, KOH / methanol solution had the highest methylmercury extraction rate. The extracted inorganic mercury and methylmercury were determined by HPLC after derivatization. The best choice of mobile phase was 0.01 mol / L LTBABr and 0.025 mol / L NaCl aqueous solution: methanol = 45:55 (v: v). Under optimal conditions, the detection limits of inorganic mercury and methylmercury in soil samples were 1 ng / g and 10 ng / g, respectively. The method has the advantages of simple pre-treatment, wide linear range, high precision and good accuracy, and is suitable for the morphological analysis of mercury compounds in soil.