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出 处:《理化检验(化学分册)》2009年第4期410-412,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:江苏省海洋生物技术重点建设实验室基金项目(2005HS001,010、2006HS020);淮海工学院自然科学基金(Z2006001)
摘 要:对由溴化十六烷基吡啶(CPB)、辛基苯基聚氧乙烯醚(OP)、正丁醇、正庚烷和水组成的微乳溶液存在下,4-(6-甲氧基-8-喹啉偶氮)-间苯三酚与镓(Ⅲ)的显色反应,进行了研究并提出了分光光度法测定痕量镓(Ⅲ)的方法。结果表明:在pH9.80的硼砂-氢氧化钠缓冲溶液中,镓(Ⅲ)与试剂形成1:2的红色络合物,络合物的最大吸收峰在525nm波长处,表观摩尔吸光率为1.6×10^5L·mol^-1·cm^-1。镓(Ⅲ)量在7-800μg·L^-1范围内符合比耳定律,检出限(3S/N)为μg·L^-1。方法用于煤和矿石中微量镓的测定,测得结果与原子吸收光谱法的结果相符,测定值的相对标准偏差(n=6)均小于5%。在两实样的基础上用标准加入法做回收试验,测得其平均回收率为102.7%。A new spectrophotometric method for determination of trace amounts of gallium (Ⅲ) was proposed, base on its reaction with 4-(6-methoxy-8-quinolylazo)-phloroglucinol (MOQAPG) in a microemulsoid composed of CPB, OP, n-butanol, n-heptane and water. It was found that in the microemulsoid with its mass ratio of m(CPB/OP): m(n-butanol): m(n-heptane) : m(H2O)=0. 25 : 3.3 : 0. 8 :89.9, and buffered at pH 9. 80 with borate buffer solution, a red colored complex was formed by the reaction of Ga(Ⅲ) with MOQAPG in the mole ratio of 1 to 2, having its absorption maximum at the wavelength of 525 nm and its apparent molar absorptivity (ε525) of 1.6×10^5L·mol^-1·cm^-1. Beer's law was kept in the range of 7-800 μg of Ga(Ⅲ) per 1 L of solution. Detection limit (3S/N) of the method was found to be 1 μg ·L^-1. The proposed method was applied to determine contents of gallium in samples of coal and ore, giving results in consistency with the results obtained by AAS, and values of RSD's (n= 6) less than 5%. Test for recovery was made by standard addition method, and value of average recovery found was 102. 7%.
关 键 词:分光光度法 4-(6-甲氧基-8-喹啉偶氮)-间苯三酚 镓(Ⅲ) 微乳体
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