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作 者:徐国想[1] 马卫兴[1] 许兴友[1] 洪晴[1]
机构地区:[1]淮海工学院化学工程系,江苏连云港222005
出 处:《冶金分析》2007年第8期19-22,共4页Metallurgical Analysis
基 金:江苏省海洋生物技术重点建设实验室基金项目(2006HS020)与江苏省应用化学重点建设学科项目(2005)
摘 要:研究了由十六烷基三甲基溴化铵(CTMAB)、正丁醇、正庚烷和水自制微乳溶液存在下,二溴对甲偶氮羧(DBpMCA)与Sn(Ⅳ)的显色反应,建立了分光光度法测定微量锡的新方法。结果表明,在pH10.4的NH4Cl—NH3·H2O缓冲溶液中,Sn(Ⅳ)与试剂形成组成比为1:3的紫红色络合物,该络合物的最大吸收峰在542nm波长处,表观摩尔吸光系数ε为1.04×10^5L·mol^-1·cm^-1。在10mL显色液中,Sn(Ⅳ)量在0.02~12μg范围内符合比尔定律,检出限为6.0×10^-4μg/mL。方法已用于粉煤灰中微量锡的测定,回收率为99.4%~101.6%,相对标准偏差为0.59%~1.06%。The color reaction of the reagent dibromo- p -methyl carboxyzo(DBpMCA) with Sn(Ⅳ) in the presence of CTMAB microemulsiom was studied,and a new spectrophotometric method for the determination of micro tin has been established. Resuhs show that the new color reagent reacts with Sn(Ⅳ)to form a stable purple-red complex(mole ratio 1 : 3)in the presence of NH3·H2O-NH4Cl buffer solution at pill0.4. The maximum absorption wavelength and apparent molar absorptivity are 544 nm and 1.04×10^5 L·mol^-1·cm^-1 respectively. Beerrs law is obeyed in the range of 0.02-12μg in 10 mL experimental liquor. The detection limit is 6 × 10^-4 μg/ mL. The method has been applied to the direct determination of tin in fly ash with the recovery of 99.40%-101.6 % and the relative standard deviation of O. 59%-1.06%
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