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本文应用单纯形(Simplex)优化方法研究了钨—连苯三酚红(PR)—溴化十六烷基三甲铵(CTMAB)分光光度测定微量钨的方法,通过初步试验和析因试验,确定出影响显色反应的主要因素,继而应用改进的单纯形优化方法进行优化试验,得到了钨显色反应的最佳条件:溶液的pH为4.70,PR和CTMAB的浓度中分别为6.0×10~(-5)M和6.0×10~(-4)M。经测定络合物中W:PR=1:2,钨量在0—92μg/25ml范围内服从比耳定律。试验了钼的干扰和掩蔽,选择以NH_2OH—DTPA体系为钼的掩蔽剂,0.5毫克以下的钼不干扰钨的测定。
In this paper, the simplex method was used to study the spectrophotometric determination of trace tungsten with tungsten-pyrogallol (PR) -cetyltrimethylammonium bromide (CTMAB). Through preliminary experiments and factorial experiments, The main factors that affect the color reaction were determined. Then the optimized simplex method was used to optimize the color reaction. The optimal conditions for the color reaction of tungsten were obtained: the pH of the solution was 4.70, the concentration of PR and CTMAB was 6.0 × 10 ~ (-5) M and 6.0 × 10 ~ (-4) M. The molar ratio of W to PR in the complex was 1: 2, and the amount of tungsten was in the range of 0-92μg / 25ml. The interference and masking of molybdenum were tested. The molybdenum masking agent with NH_2OH-DTPA system was selected. The molybdenum less than 0.5 mg did not interfere with the determination of tungsten.