Zhu Xiashi, Hu Bin, Jiang Zucheng, Li Mingfang
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Water Res. 2005 Feb;39(4):589-95. doi: 10.1016/j.watres.2004.11.006. Epub 2004 Dec 24.
A new method based on the cloud point extraction (CPE) separation and electrothermal atomic absorption spectrometry (ETAAS) detection was proposed for the determination of chromium species. When the system temperature is higher than the cloud point extraction temperature (CPT) of selected surfactant p-octyl polyethyleneglycolphenyether (Triton X-100), the complex of Cr(VI) with dibromophenylfluorone (Br-PF) could enter surfactant-rich phase, whereas the Cr(III) remained in aqueous phase. Thus, an in situ separation of Cr(VI) and Cr(III) could be realized. Cr(VI) in surfactant-rich phase was analyzed by ETAAS and Cr(III) was calculated by subtracting of Cr(VI) from the total chromium which was directly determined by ETAAS. The main factors affecting the cloud point extraction, such as pH, concentration of Br-PF and Triton X-100, equilibration temperature and time, were investigated systematically. Under the optimized conditions, the quantitation limit for Cr(VI) as low as 0.01 microg/L was obtained by preconcentrating a 10 mL sample solution, and the relative standard deviation (n=6, c=2.0 microg/L) was 2.6%. The proposed method was applied to the speciation of chromium in different water samples and the recoveries in the range of 98.9-105.3% were obtained by spiking the real samples. In order to verify the accuracy of the method, a certified reference water sample was analyzed and the results obtained were in good agreement with the certified values.
提出了一种基于浊点萃取(CPE)分离和电热原子吸收光谱法(ETAAS)检测的测定铬形态的新方法。当系统温度高于所选表面活性剂对辛基聚乙二醇苯基醚(Triton X - 100)的浊点萃取温度(CPT)时,六价铬(Cr(VI))与二溴苯基荧光酮(Br - PF)的络合物可进入富含表面活性剂的相,而三价铬(Cr(III))则保留在水相中。因此,可以实现Cr(VI)和Cr(III)的原位分离。通过ETAAS分析富含表面活性剂相中的Cr(VI),并通过从直接由ETAAS测定的总铬中减去Cr(VI)来计算Cr(III)。系统研究了影响浊点萃取的主要因素,如pH值、Br - PF和Triton X - 100的浓度、平衡温度和时间。在优化条件下,通过对10 mL样品溶液进行预浓缩,获得了低至0.01 μg/L的Cr(VI)定量限,相对标准偏差(n = 6,c = 2.0 μg/L)为2.6%。该方法应用于不同水样中铬的形态分析,通过对实际样品加标获得了98.9 - 105.3%的回收率。为了验证该方法的准确性,分析了一个有证参考水样,所得结果与认证值吻合良好。