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采用与带超声雾化的电感耦合等离子体发射光谱仪联用的打结反应器在线预富集法测定葡萄酒中的低镉浓度。

Determination of low cadmium concentrations in wine by on-line preconcentration in a knotted reactor coupled to an inductively coupled plasma optical emission spectrometer with ultrasonic nebulization.

作者信息

Lara R F, Wuilloud R G, Salonia J A, Olsina R A, Martinez L D

机构信息

Instituto de Investigaciones Mineras, Facultad de Ingeniería, Universidad Nacional de San Juan, Argentina.

出版信息

Fresenius J Anal Chem. 2001 Dec;371(7):989-93. doi: 10.1007/s00216-001-1096-7.

Abstract

An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 microg/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1,000 microg/L. The method was successfully applied to the determination of cadmium in wine samples.

摘要

研究了一种在线镉预富集与测定系统,该系统采用电感耦合等离子体发射光谱法(ICP - OES),与流动注射(FI)以及超声雾化系统(USN)联用。镉在pH 9.5条件下以镉 - 2 -(5 - 溴 - 2 - 吡啶偶氮)- 5 - 二乙氨基苯酚(Cd -(5 - Br - PADAP))络合物的形式被保留。用3.0 mol/L硝酸从打结反应器(KR)中洗脱镉络合物。相对于使用气动雾化的ICP - OES(超声雾化增强12倍,打结反应器增强18倍),在60 s预富集时间下获得了216的总增强因子。5 mL样品溶液预富集的检测限为5 ng/L。在5 μg/L镉水平下进行10次重复测定的精密度为2.9%相对标准偏差(RSD),由所得峰高计算得出。使用镉预富集系统的校准曲线在接近检测限直至至少1000 μg/L的水平范围内呈线性,相关系数为0.9998。该方法成功应用于葡萄酒样品中镉的测定。

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