Wuilloud R G, González A H, Marchevsky E J, Olsina R A, Martinez L D
National University of San Luis, Faculty of Chemistry, Department of Analytical Chemistry, Argentina.
J AOAC Int. 2001 Sep-Oct;84(5):1555-60.
An on-line lead preconcentration and determination system implemented with inductively coupled plasma-atomic emission spectrometry (ICP-AES) with ultrasonic nebulization (USN) in association with flow injection was studied. For the preconcentration of lead, a Pb-quinolin-8-ol complex was formed on-line at pH 6.8 and retained on Amberlite XAD-16 resin. The lead was removed from the microcolumn by countercurrent elution with nitric acid. A total enhancement factor of 225 was obtained with respect to ICP-AES with pneumatic nebulization (15.0 for USN and 15.0 for the column). The detection limit for Pb for the preconcentration of a 10 mL wine sample was 0.15 microg/L. The precision for 10 replicate determinations at a Pb level of 25 microg/L was a relative standard deviation of 2.5%, calculated from the peak heights obtained. The calibration graph obtained by using the preconcentration system for lead was linear with a correlation coefficient of 0.9995 for levels near the detection limit up to > or = 1000 microg/L. The method was successfully applied to the determination of lead in wine samples.
研究了一种在线铅预富集和测定系统,该系统采用电感耦合等离子体原子发射光谱法(ICP - AES)结合超声雾化(USN)与流动注射技术。对于铅的预富集,在pH 6.8条件下在线形成Pb - 8 - 羟基喹啉络合物,并保留在Amberlite XAD - 16树脂上。通过用硝酸逆流洗脱将铅从微柱上洗脱下来。相对于气动雾化的ICP - AES(超声雾化的增强因子为15.0,柱富集的增强因子为15.0),总增强因子为225。对于10 mL葡萄酒样品预富集后的铅检测限为0.15 μg/L。在25 μg/L的铅水平下进行10次重复测定的精密度,根据获得的峰高计算,相对标准偏差为2.5%。使用铅预富集系统获得的校准曲线在接近检测限直至≥1000 μg/L的水平范围内呈线性,相关系数为0.9995。该方法成功应用于葡萄酒样品中铅的测定。