N,N′-双(苯偶氮水杨叉)肼的合成与方波伏安法测定微量镉
Synthesis of N,N′-Bis (Phenylazosalicylidene) Hydrazine and Its Use in the Square Wave Polarographic Determination of Micro Amounts of Cadmium
摘 要
合成了新试剂N,N′-双(苯偶氮水杨叉)肼(PASHZ),研究了试剂与镉的方波伏安法新体系的最佳条件.在氨水-NH4Cl缓冲溶液(pH 9.1)中,于-0.867 V(vs.SCE)出现一灵敏的方波伏安峰.Cd(Ⅱ)浓度在1.0×10-6~1.0×10-4mol·L-1范围与峰电流(Ip)呈线性关系,线性方程为Ip=9.745×106c+2.270,相关系数为0.999 4,检出限为0.5×10-6mol·L-1.该法应用于测定矿泉水中微量Cd(Ⅱ),测定结果与已知值相符,测定结果的平均RSD值及平均回收率依次为2.72%及98.6%.
N,N′-双(苯偶氮水杨叉)肼
镉
水样
Square wave voltammetry
N,N′-bis (phenylazosalicylidene) hydrazine
Cadmium(Ⅱ)
Water sample
Abstract
A new reagent,N,N′-bis (phenylazosalicylidene)-hydrazine (abbreviated as PASHZ) was synthesized and its molecular structure was identified by IR spectroscopy and elementary analysis.A binary complex was formed between PASHZ and Cd(Ⅱ) in an ammoniacal buffer medium of pH 9.1.Square wave voltammetric behavior of the new system containing PASHZ and Cd(Ⅱ) in the buffer medium of pH 9.1 was studied and a sensitive square wave voltammetric peak was observed at -0.867 V (vs.SCE).Linear relationship between the peak current (Ip) and the concentration of cadmium was obtained in the range of 1.0×10-6-1.0×10-4mol·L-1,giving the linear regression equation of Ip=9.745×106c+2.270 (r=0.999 4) with a detection limit of 0.5×10-6mol·L-1.In the application of the proposed method to the determination of microamounts of Cd(Ⅱ) in samples of mineral water and pure water,the results obtained were in consistency with the known values,and average values of RSD′s and recovery found were 2.72% and 98.6% respectively.
中图分类号 O657.14
所属栏目 试验与研究
基金项目 甘肃省教育厅基金资助项目(049B-06)和陇东学院科研基金资助项目(XYLG0411)
收稿日期 2006/4/13
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备注仵博万(1970-),男,甘肃庆阳人,副教授,从事新型偶氮试剂的合成与应用研究.
引用该论文: WU Bo-wan,ZHANG Bing,YU Xin-qiao,LIU Jian-ning. Synthesis of N,N′-Bis (Phenylazosalicylidene) Hydrazine and Its Use in the Square Wave Polarographic Determination of Micro Amounts of Cadmium[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(2): 102～104
仵博万,张兵,于新桥,刘建宁. N,N′-双(苯偶氮水杨叉)肼的合成与方波伏安法测定微量镉[J]. 理化检验－化学分册, 2007, 43(2): 102～104
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