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出 处:《分析化学》1992年第10期1126-1130,共5页Chinese Journal of Analytical Chemistry
基 金:国家自然科学基金资助课题
摘 要:铋(Ⅱ)在碱性介质(pH10.60~11.38)中,当有8-羟基喹哪啶和十二烷基苯磺酸钠存在时,在-0.60V(对SCE)处得到一个极为灵敏的二次导数示波极谱电流峰(p),较在纯碱性介质中,铋(Ⅱ)的测定灵敏度提高近100倍。铋(Ⅱ)浓度在0.8ng/ml~0.16μg/ml范围内,峰高(i_p)和浓度成正比,检出限为0.4ng/ml(1.9×10^(-9)mol/L),达迄今测铋同类方法的最高灵敏度。用于高温合金中痕量(10^(-5)%~10^(-4)%)铋的测定,结果满意。试验表明,铋(Ⅱ)与8-羟基喹哪啶形成摩尔比为1:2的络合物,其条件稳定常数(K)为2.1×10^(11)(等摩尔变化法)或2.77×10^(11)(摩尔比法)。In an alkaline medium(pH 10.60~11.38)containing 8-hydroxyquinaldine (8-OXQ) and sodium dodecyl benzene sulfonate, an extremely sensitive peak current of Bi(Ⅲ)(in second derivative oscillopolarography)was observed at -0.60V(νs. SCE), the sensitivity has been increased about a hundred times higher than that obtained in the alkaline medium alone. The peak height was proportional directly to the concentration of Bi in the range of 0.8ng/ml~0.16μg/ml, the detection limit was 0.4ng/ml(1.9×10^(-9)mol/ml)Bi(Ⅲ)with the sensitivity of 19.24μA/(μg/ml). The proposed method has been applied to the determination of trace Bi(10^(-5)~10^(-4)%)in superalloys after separation with sulfhydryl cotton, the results were reliable and satisfactory. It was shown that Bi(Ⅲ)formed a complex with 8-OXQ with the mole ratio of 1:2, the conditional stability constant was calculated to be 2.1×10^(11) (method changing in equal mole) and 2.77×10^(11) (mole ratio method), respectively. The complex of Bi(Ⅲ)-8-OXQ has been demonstrated as 〔Bi(Ⅲ)-L_2〕^+(L^-the dissociated form of 8-OXQ) existing in mentioned medium.
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