Jiang Hongmei, Qin Yongchao, Hu Bin
Department of Chemistry, Wuhan University, Wuhan 430072, China.
Talanta. 2008 Feb 15;74(5):1160-5. doi: 10.1016/j.talanta.2007.08.022. Epub 2007 Aug 25.
A new method of dispersive liquid phase microextraction (DLPME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of trace Co and Ni using 1-(2-pyridylazo) 2-naphthol (PAN) as chelating reagent. Several factors influencing the microextraction efficiency of Co and Ni and their subsequent determinations, such as pH, extraction and disperser solvent type and their volume, concentration of the chelating agent, extraction time and ashing temperature and atomization temperature were studied, and the optimized experimental conditions were established. After extraction, the enrichment factors were 101 and 200 for Co and Ni, respectively. The detection limits of the method were 21 and 33pg/mL for Co and Ni, and the relative standard deviations (R.S.Ds.) for five determinations of 0.5ng/mL Co and Ni were 7.5% and 8.2%, respectively. The results for the determination of Co and Ni in East Lake water, Yangtse River water, Dongbei rice and spiked samples have demonstrated the accuracy, recovery and applicability of the proposed method. To validate the proposed method, two certified reference materials of Environment Water (GSBZ50009-88) and NIES No.10-b rice flour were analyzed, and the determined values were in good agreement with the certified values.
提出了一种分散液相微萃取(DLPME)与石墨炉原子吸收光谱法(GFAAS)相结合的新方法,以1-(2-吡啶偶氮)-2-萘酚(PAN)作为螯合剂测定痕量钴和镍。研究了影响钴和镍微萃取效率及其后续测定的几个因素,如pH值、萃取剂和分散剂溶剂类型及其体积、螯合剂浓度、萃取时间、灰化温度和原子化温度,并建立了优化的实验条件。萃取后,钴和镍的富集因子分别为101和200。该方法对钴和镍的检出限分别为21和33pg/mL,对0.5ng/mL钴和镍进行五次测定的相对标准偏差(R.S.Ds.)分别为7.5%和8.2%。对东湖水样、长江水样、东北大米和加标样品中钴和镍的测定结果表明了该方法的准确性、回收率和适用性。为验证该方法,分析了两种环境水标准物质(GSBZ50009-88)和NIES No.10-b米粉,测定值与认定值吻合良好。