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1 引 言 变色酸双偶氮试剂用于络合物极谱行为的研究并不鲜见,对镍的研究也有报道.本文设计合成并提纯了新试剂对羧基偶氮氯膦(CPApK),将其用于镍的络合物极谱行为的研究,拟定了镍的测定方法,该方法灵敏度高,线性范围宽,可直接测定铝合金中的镍.2 络合剂CPApK的合成及纯化2.1 络合剂的合成 称取1.0g对氨基苯甲酸于100 mL烧杯中,加入 3.5 mL水及 1.7 mL浓盐酸,搅匀,于冰盐浴上冷却至0℃,在剧烈搅拌下,不断滴入含0.5g亚硝酸钠的水溶液重氮化,保持0℃,备用.
1 Introduction It is not uncommon to study the polarographic behavior of complexes with bis-azo chromogenic reagents, and nickel has also been reported.In this paper, a new reagent, CPApK, was synthesized and purified, Nickel for the determination of polarographic behavior of nickel, developed a method for the determination of nickel, the method of high sensitivity, wide linear range, direct determination of nickel in aluminum alloy .2 Complexing agent CPApK synthesis and purification 2.1 complexation Weigh 1.0g of p-aminobenzoic acid in 100mL beaker, add 3.5mL water and 1.7mL of concentrated hydrochloric acid, stir, cooled to 0 ° C on an ice-salt bath, with vigorous stirring, constantly dropping 0.5 g aqueous solution of sodium nitrite diazotization, keep 0 ℃, spare.