Hu Qiufen, Yang Guanyu, Yang Jihong, Yin Jiayuan
Department of Chemistry, Yuxi Teacher's College, Yuxi, P. R. China 653100.
J Environ Monit. 2002 Dec;4(6):956-9. doi: 10.1039/b204874b.
A new method for the determination of iron, cobalt, nickel, copper, zinc and manganese in drinking water by the reversed-phase high-performance liquid chromatography (RP-HPLC) with 2-(2-quinolinylazo)-5-diethylaminophenol (QADEAP) as precolumn derivatizing reagent was studied in this paper. The iron, cobalt, nickel, copper, zinc, and manganese ions react with QADEAP to form color chelates in the presence of cetyl trimethylammonium bromide (CTMAB) and acetic acid-sodium acetic buffer solution medium of pH 4.0. These chelates were enriched by solid-phase extraction with a Waters Nova-Pak C18 cartridge and eluted the retained chelates from the cartridge with tetrahydrofuran (THF). The enrichment factor of 100 was achieved. Then the chelates were separated on a Waters Nova-Pak C18 column (3.9 x 150 mm, 5 microm) by gradient elution with methanol (containing 0.2% of acetic acid and 0.1% of CTMAB) and 0.05 mol L(-1) acetic acid-sodium acetic buffer solution (containing 0.1% of CTMAB) (pH 4.0) as mobile phase at a flow rate of 0.5 ml min(-1), and monitored with a photodiode array detector from 450 approximately 700 nm. The detection limits (S/N = 3) of iron, cobalt, nickel, copper, zinc and manganese are 0.8, 1.1, 0.9, 1.1, 1.5 and 2.0 ng L(-1), respectively, in the original sample. This method can be applied to determination at the microg L(-1) level of iron, cobalt, nickel, copper, zinc and manganese in drinking water with good results.
本文研究了一种以2-(2-喹啉基偶氮)-5-二乙氨基苯酚(QADEAP)作为柱前衍生试剂,采用反相高效液相色谱(RP-HPLC)测定饮用水中铁、钴、镍、铜、锌和锰的新方法。在十六烷基三甲基溴化铵(CTMAB)和pH 4.0的乙酸-乙酸钠缓冲溶液介质存在下,铁、钴、镍、铜、锌和锰离子与QADEAP反应形成有色螯合物。这些螯合物用Waters Nova-Pak C18柱进行固相萃取富集,并用四氢呋喃(THF)从柱上洗脱保留的螯合物,实现了100倍的富集因子。然后,以甲醇(含0.2%乙酸和0.1% CTMAB)和0.05 mol L(-1)乙酸-乙酸钠缓冲溶液(含0.1% CTMAB)(pH 4.0)为流动相,流速为0.5 ml min(-1),在Waters Nova-Pak C18柱(3.9×150 mm,5μm)上进行梯度洗脱分离螯合物,并用光电二极管阵列检测器在450~700 nm波长范围内进行监测。原样品中铁、钴、镍、铜、锌和锰的检测限(S/N = 3)分别为0.8、1.1、0.9、1.1、1.5和2.0 ng L(-1)。该方法可用于饮用水中铁、钴、镍、铜、锌和锰的微克L(-1)水平的测定,结果良好。