Raychaudhuri A, Roy S K, Chakraburtty A K
Analytical Chemistry Division, Central Glass & Ceramic Research Institute, Calcutta 700 032, India.
Talanta. 1992 Oct;39(10):1377-82. doi: 10.1016/0039-9140(92)80253-a.
A simple procedure for selective sorption of tungsten is described. The method involves reduction of W(VI) to W(V) with tin(II) chloride (2%, w/v) at 8-9M hydrochloric acid, formation of the W(V)-SCN complex with 0.2M KSCN and its sorption on polyurethane foam within 20 min. The sorbed complex is then eluted with acidified acetone (1 ml of 1M hydrochloric acid and 8 ml of acetone) followed by addition of 1 ml of 0.1M KSCN to the eluent. The method has been applied to the spectrophotometric determination of tungsten in steels and silicates by measuring the absorbance of the eluted solution at 400 nm. Beer's law is obeyed for the range 0.1-12 mug W/ml. Other elements, e.g., Co(III) (50 mug/ml), Cu(II) (10 mug/ml), Ti(IV) (20 mug/ml), V(V) (10 mug/ml) and Mo(VI) (0.5 mug/ml) have no effect on the method. Interference of copper, up to 100 mug/ml has been eliminated by masking with thiourea and that due to molybdenum by prior separation with thioglycollic acid on PUF. The method has been verified with standard samples.
描述了一种钨的选择性吸附的简单方法。该方法包括在8 - 9M盐酸中用氯化亚锡(2%,w/v)将W(VI)还原为W(V),与0.2M硫氰酸钾形成W(V)-SCN络合物,并在20分钟内将其吸附在聚氨酯泡沫上。然后用酸化丙酮(1毫升1M盐酸和8毫升丙酮)洗脱吸附的络合物,随后向洗脱液中加入1毫升0.1M硫氰酸钾。该方法已应用于通过测量洗脱液在400nm处的吸光度对钢和硅酸盐中钨的分光光度测定。在0.1 - 12μg W/ml范围内符合比尔定律。其他元素,例如Co(III)(50μg/ml)、Cu(II)(10μg/ml)、Ti(IV)(20μg/ml)、V(V)(10μg/ml)和Mo(VI)(0.5μg/ml)对该方法无影响。通过用硫脲掩蔽消除了高达100μg/ml的铜的干扰,通过在聚氨酯泡沫上用巯基乙酸预先分离消除了钼的干扰。该方法已用标准样品进行了验证。