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磷钼蓝体系薄层树脂相吸光光度法测定痕量钼的研究
THIN-LAYER RESIN-PHASE-PHOTOMETRIC DETERMINATION OF TRACE-AMOUNTS OF MOLYBDENUM WITH PHOSPHO-MOLYBDENUM-BLUE METHOD
【摘要】 提出了在酸性条件下,以磷钼蓝反应为基础的薄层树脂相吸光光度法测定钼。此方法灵敏度较高(ε705=8.1×104L·mol-1·cm-1),比液相光度法提高10倍,精密度理想(钼浓度为20μg/25ml,n=6),RSD为2.8%。应用此法测定天然水中钼,线性范围为0~18μg·ml-1,回收率为97%~102%。
【Abstract】 0.5g of phosphate-form anion exchange resin is added to 25ml of test solution containing an appropriate amount of Mo(Ⅵ) and having an acidity of 0.2mol·L-1 of HCl, that is 2.5ml of 2mol·L-1 HCl in 25ml of solution. After mixing for 20min with a magnetic stirrer, heteropoly acid is formed between Mo(Ⅵ) ion and phosphate ion on the resin, which is further reduced to "molybdenum blue" with a reducing solution containing ascorbic acid, sodium potassium tartrate and sulfuric acid. The absorbance of the resin adsorbed with the "molybdenum blue" is then measured at 705nm ( λ max of molybdenum blue) against resin blank prepared in the same way but containing no molybdenum(Ⅵ). The resin-phase photometric method gives a molar absorptivity of ( ε 705) 8.1×104L·mol-1·cm-1, which is about 10 times higher than that in water phase [ ε 705 (in H2O solń)=7.8×103L·mol-1·cm-1]. RSD ( n =6) tested at the concentration level of 20μg per 25ml achieve to a value of 2.8%. Recoveries obtained are in the range of 97%~102%.
【Key words】 Thin-layer resin-phase photometry; Phospho-molybdenum blue; Molybdenum(Ⅵ);
- 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis Part B Chemical Analysis , 编辑部邮箱 ,2003年12期
- 【分类号】O657.3
- 【被引频次】3
- 【下载频次】44