Pancras J Patrick, Puri Bal Krishan
Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi-110 016, India.
Anal Bioanal Chem. 2002 Dec;374(7-8):1306-11. doi: 10.1007/s00216-002-1630-2. Epub 2002 Nov 19.
A solid co-precipitated material obtained from an ion-pair of 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) and tetraphenylborate (TPB), and microcrystals of naphthalene has been tried as an adsorbent for the column preconcentration of copper(I), iron(II), nickel(II) and Zn(II). The retention of the metal ions was found to be maximum and constant in the pH range 3.0-8.0 for Cu, 3.8-7.5 for Fe, 4.5-7.5 for Ni and 8.5-11.0 for Zn. The elements were determined by FAAS after dissolving the metal along with the adsorbent in an organic solvent (10 mL of DMF). The characteristic concentration for 1% absorption was found to be 0.0332, 0.0536, 0.0537 and 0.0142 (aqueous medium 0.0512, 0.0638, 0.1294 and 0.0216) microg mL(-1) for Cu, Fe, Ni and Zn, respectively. The calibration plot was linear in the range 1.5-20.0, 2.0-38.0, 2.5-25.0 and 0.5-15.0 micro g in the final 10 mL of DMF solution for Cu, Fe, Ni and Zn, respectively. Various parameters such as pH, volume of buffer, amount of adsorbent, flow rate, preconcentration factor and effect of diverse salts and cations were studied. The optimised conditions were utilized for the determination of Cu, Fe, Ni and Zn in various water, beverage and human hair samples.
由2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚（5-Br-PADAP）与四苯基硼酸盐（TPB）形成的离子对以及萘微晶所得到的一种固体共沉淀材料，已被尝试用作柱预富集铜(I)、铁(II)、镍(II)和锌(II)的吸附剂。发现对于铜，在pH值3.0 - 8.0范围内金属离子的保留量最大且恒定；对于铁，在pH值3.8 - 7.5范围内；对于镍，在pH值4.5 - 7.5范围内；对于锌，在pH值8.5 - 11.0范围内。将金属与吸附剂一起溶解在有机溶剂（10 mL二甲基甲酰胺）中后，通过火焰原子吸收光谱法（FAAS）测定这些元素。发现对于1%吸收的特征浓度，铜、铁、镍和锌分别为0.0332、0.0536、0.0537和0.0142（水介质中分别为0.0512、0.0638、0.1294和0.0216）μg mL⁻¹。在最终10 mL二甲基甲酰胺溶液中，铜、铁、镍和锌的校准曲线分别在1.5 - 20.0、2.0 - 38.0、2.5 - 25.0和0.5 - 15.0 μg范围内呈线性。研究了各种参数，如pH值、缓冲液体积、吸附剂用量、流速、预富集因子以及不同盐类和阳离子的影响。利用优化后的条件测定了各种水样、饮料和人发样品中的铜、铁、镍和锌。
