Sawant Shakuntala S
Post-Graduate and Research Center, Department of Chemistry, R. B. N. B. College, Shrirampur, District-Ahmednagar, Maharashtra State 413709, India.
Anal Sci. 2009 Jun;25(6):813-8. doi: 10.2116/analsci.25.813.
Osmium was determined spectrophotometrically after coprecipitation with 5-chloro-2-hydroxythiobenzhydrazide at room temperature in the pH range 2.5-5.0 and collection on microcrystalline naphthalene. Beer's law was obeyed in the concentration range 1.8-14.4 ppm of osmium in a chloroform solution at 510 nm. The molar absorptivity and Sandell sensitivity were 1.056 x 10(4) l mol(-1) cm(-1) and 0.018 ppm, respectively. Six replicate analyses of a solution containing 7.2 ppm of osmium gave a mean absorbance of 0.405 with a standard deviation of 0.013 and a relative standard deviation of 0.92%. The complex was stable for over 72 h. The metal-to-ligand ratio in the complex was 1:2. Interference from various ions was studied, and the method was applied to the determination of osmium in various synthetic mixtures containing commonly associated metals and corresponding to the alloy composition. The sequential separation and determination of osmium and platinum is reported.
在室温下,于pH值2.5 - 5.0的范围内,锇与5 - 氯 - 2 - 羟基硫代苯甲酰肼共沉淀,然后收集在微晶萘上,用分光光度法测定锇。在510nm波长下,氯仿溶液中锇的浓度在1.8 - 14.4ppm范围内符合比尔定律。摩尔吸光系数和桑德尔灵敏度分别为1.056×10⁴ l·mol⁻¹·cm⁻¹和0.018ppm。对含7.2ppm锇的溶液进行六次重复分析,平均吸光度为0.405,标准偏差为0.013,相对标准偏差为0.92%。该配合物在72小时以上稳定。配合物中金属与配体的比例为1:2。研究了各种离子的干扰情况,并将该方法应用于测定含有常见伴生金属且符合合金组成的各种合成混合物中的锇。本文还报道了锇和铂的顺序分离与测定。