摘要
基于在NaOH溶液中及45℃加热条件下，Ni（Ⅱ）对H2O2氧化2，3，7-三羟基-9-水杨基荧光酮溶液褪色反应具有灵敏的催化作用。研究了反应的最佳条件，建立了催化动力学光度法测定痕量Ni（Ⅱ）的光度分析方法。非催化反应与催化反应的吸光度差值△A与Ni（Ⅱ）的质量浓度ρ在0．00～0．15μg／mL范围内呈良好的线性关系，检出限为7．63×10^-10g／mL。测定了动力学参数，Ni（II）为一级反应，总反应为准一级反应。反应表观速率常数为4．943×10^-3／s，表观活化能为49．98kJ／mol。对0．1μgNi（Ⅱ）进行11次测定，求得相对标准偏差（RSD）为1．2％。该方法用于含钒生铁和低合金钢中痕量Ni（II）的测定，其回收率在100％～104％的范围，符合痕量分析的要求。
The fading reaction of 2,3,7-Trihydroxy-9-Salicyl Fluorone solution oxidized by H202can be greatly catalyzed by Nickel （ Ⅱ ） in sodium by droxide solution at 45 ~C. The optimum experimental condition of the reaction was studied and a new catalytic kinetic method of trace Ni（Ⅱ ） determination was proposed based on the upper mentioned phenomenon. The absorbency difference A A between non-catalytic reaction and catalytic reaction remained good linear relationship with the mass concentration p of Nickel （ Ⅱ ） in the range of 0.00 0. 15 μg/mL. The detection limit of this method was 7.63 x 10^-10 g/mL and kinetic parameters were determined, which showed that the catalytic reaction was the first order reaction to Nickel （ Ⅱ ） and pseudo first order to the total reaction. The apparent rate constant of the reaction was 4. 943 x 10^-4/s and the apparent activation energy was 49.98 kJ/tool. The relative standard deviation （RSD） of this method was calculated to be 1.2% according to the 11 times of determinations for 0. 1 txg Nickel （Ⅱ ） This method was also applied to the determination of trace Nickel （ Ⅱ） in vanadium iron and low alloy steel with recoveries rate between 100% and 104% , which fulfilled the trace analysis requirements.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第5期73-76,共4页
Chinese Journal of Analysis Laboratory
