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作 者:柴红梅[1] 高楼军[1] 孙雪花[1] 罗晓平[1]
机构地区:[1]延安大学化学与化工学院,陕西延安716000
出 处:《冶金分析》2008年第11期46-49,共4页Metallurgical Analysis
基 金:陕西省教育厅资助项目(SJG0503);延安大学科研基金资助项目(YD200656)
摘 要:研究了新显色剂2-[2’-(5-硝基-吡啶)-偶氮]-1,8-二羟基萘-3,6-二磺酸(简称为5-NO2-PACA)的合成路线和方法,并应用光度法对其与Ni抖的显色反应进行了研究。以5-硝基-2-氨基吡啶为原料制备5-硝基-2-氨基吡啶重氮酸盐中间体,再与变色酸偶联合成了5-NO2-PACA。在pH11.5的NH3·H2O—NH4Cl缓冲介质中Ni^2+与该试剂在室温下很快形成摩尔比为1:1的蓝色稳定络合物,其最大吸收波长为635nm,表观摩尔吸光系数为1.00×10^5L·mol^-1·cm^-1,Ni^2+浓度在0~500/mL范围内符合比尔定律,常见离子不干扰测定,该方法用于测定环境水样中微量镍,相对标准偏差为2.6%~3.2%(n=6)。A new sensitive chromogenic reagent, 2-[2'-(5-nitro-pyridylazo) ]-1,8- dihydroxynaphtha- lene-3,6-disulfonic acid (5-NO2-PACA), has been synthesized and used in the spectrophotometric determination of nickel. 5-nitro-2-aminopyridine is used as a crude mterial to prepare a intermediate 5-nitro-2-aminopyridine diazotate, which couples with chromotropic acid to give 5-NO2-PACA. In the buffer solution of NH3 ·H2O-NH4Cl at pHll. 5, 5-NO2-PACA can react with nickel (Ⅱ) immediately at room temperature to form a stable blue complex with mole ratio of 1: 1. The apparent molar absorptivity (ε) is 1.00× 10^5 L ·mol^-1 ·cm^-1 at the maximum absorption wavelength of 635nm. Beer's law is obeyed over the nickel concentration range 0-500μg/L. Common foreign ions do not interfere. The proposed method has been applied to the determination of nickel in environmental water samples with RSDs of 2.6 %- 3.2 %.
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