Nazari Saeid
Department of Chemistry, Faculty of Science, Tarbiat Moallem University of Sabzevar, Sabzevar, Iran.
J Hazard Mater. 2009 Jun 15;165(1-3):200-5. doi: 10.1016/j.jhazmat.2008.09.099. Epub 2008 Oct 2.
A powerful microextraction technique was used for determination of cadmium in water samples using liquid phase microextraction (LPME) followed by graphite furnace atomic absorption spectrometry (GF-AAS). In a preconcentration step, cadmium was extracted from a 2 ml of its aqueous sample in the pH 7 as 5,7-dibromoquinoline-8-ol (DBQ) complex into a 4 microl drop of benzyl alcohol. After extraction, the micro drop was retracted and directly transferred into a graphite tube modified by W.Rh.Pd. Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent, extraction time and stirring rate were optimized. Under the optimum conditions, the enrichment factor and recovery were 450% and 90%, respectively. The calibration graph was linear in the range of 0.008-1 microg L(-1) with correlation coefficient of 0.9961 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0035 microg L(-1) and relative standard deviation (RSD) for eight replicate measurement of 0.1 microg L(-1) and 0.4 microg L(-1) cadmium was 5.2% and 4.5%, respectively. The characteristic concentration was 0.0032 microg L(-1) equivalent to a characteristic mass of 12.8 fg. In order to evaluate the accuracy and recovery of the presented method the procedure was applied to the analysis of reference materials and seawater.
采用一种强大的微萃取技术,通过液相微萃取(LPME)结合石墨炉原子吸收光谱法(GF-AAS)测定水样中的镉。在预浓缩步骤中,镉在pH值为7时以5,7-二溴喹啉-8-醇(DBQ)络合物的形式从2 ml水样中萃取到4 μl苄醇微滴中。萃取后,将微滴缩回并直接转移到由W.Rh.Pd修饰的石墨管中。对萃取和络合物形成的一些有效参数,如有机溶剂的类型和体积、pH值、螯合剂浓度、萃取时间和搅拌速率进行了优化。在最佳条件下,富集因子和回收率分别为450%和90%。在推荐方法的最佳条件下,校准曲线在0.008 - 1 μg L⁻¹范围内呈线性,相关系数为0.9961。基于3Sb标准的检测限为0.0035 μg L⁻¹,对0.1 μg L⁻¹和0.4 μg L⁻¹镉进行八次重复测量的相对标准偏差(RSD)分别为5.2%和4.5%。特征浓度为0.0032 μg L⁻¹,相当于特征质量为12.8 fg。为了评估所提出方法的准确性和回收率,该方法应用于参考物质和海水的分析。