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发展了一种用于黑火药余烬中无机阴离子测定的毛细管电泳分析方法。对缓冲溶液的组成及pH值、电渗流改性剂的浓度以及分离电压等条件进行了研究。选定条件 :分离电压为 - 2 0kV ,缓冲溶液为 5 0mmol/L的Na2 CrO4(pH 8 2 0 ) ,电渗流改性剂为 0 5mmol/L的溴化十六烷基三甲基铵 (CTAB) ,检测波长为 2 5 4nm。在上述条件下 ,5种阴离子在 4min内可完全分离。各组分迁移时间和峰面积的相对标准偏差 (RSD)分别为 0 17%～1 4 0 %和 3 9%～ 5 0 % ,最低检测限为 5 0 μmol/L～ 10 0 μmol/L。用该法对某黑火药余烬中的无机阴离子进行分析 ,发现其中含有Cl-和NO2 -,测定其浓度的相对标准偏差分别为 6 0 %和 3 9% ,满足分析要求
A capillary electrophoresis method was developed for the determination of inorganic anions in black powder ember. The composition and pH of the buffer solution, the concentration of the electroosmotic flow modifier and the conditions of the separation voltage were studied. Selected conditions: the separation voltage of - 2 0kV buffer solution of 50mmol / L of Na2 CrO4 (pH 8 2 0), electroosmotic flow modifier 0 5mmol / L of cetyltrimethylammonium bromide ( CTAB), detection wavelength of 254nm. Under the above conditions, 5 kinds of anions can be completely separated in 4min. The relative standard deviations (RSDs) of migration time and peak area were 0 17% -140% and 39% ~ 50%, respectively. The lowest detection limits were 50 μmol / L and 100 μmol / L. Using this method to analyze the inorganic anions in a black gunpowder ember, it was found that the relative standard deviations for the determination of Cl - and NO2 - were 60% and 39%, respectively, which met the analytical requirements