Chen Dahui, Hu Bin, Huang Chaozhang
Department of Chemistry, Wuhan University, Wuhan 430072, China.
Talanta. 2009 Apr 30;78(2):491-7. doi: 10.1016/j.talanta.2008.11.046. Epub 2008 Dec 6.
A novel adsorbent of chitosan chemically modified ordered mesoporous silica was synthesized and employed as a solid phase extraction (SPE) material for flow injection (FI) micro-column preconcentration on-line coupled with inductively coupled plasma optical emission spectrometry (ICP-OES) determination of trace heavy metals V, Cu, Pb, Cd and Hg in environmental water samples. The factors affecting separation and preconcentration of target heavy metals such as pH, sample flow rate and volume, eluent concentration and volume, interfering ions were investigated. Under the optimized experimental conditions, an enrichment factor of 20 and sampling frequency of 10h(-1) were obtained. The detection limits of the method for V, Cu, Pb, Cd and Hg were 0.33, 0.30, 0.96, 0.05 and 0.93 ng mL(-1), and the relative standard deviations (RSDs) were 2.8%, 6.7%, 1.8%, 4.0% and 5.3% (n=7, C=10 ng mL(-1)), respectively. The adsorption capacities of chitosan modified ordered mesoporous silica for V, Cu, Pb, Cd, and Hg were found to be 16.3, 21.7, 22.9, 12.2 and 13.5 mg g(-1), respectively. In order to validate the developed method, a certified reference material of GSBZ50009-88 environmental water sample was analyzed and the determined values were in good agreement with the certified values. The proposed method has also been applied to the determination of trace heavy metals in natural water samples with satisfactory results.
合成了一种壳聚糖化学修饰的有序介孔二氧化硅新型吸附剂,并将其用作固相萃取(SPE)材料,用于流动注射(FI)微柱预富集在线联用电感耦合等离子体发射光谱法(ICP - OES)测定环境水样中的痕量重金属V、Cu、Pb、Cd和Hg。研究了影响目标重金属分离和预富集的因素,如pH值、样品流速和体积、洗脱液浓度和体积、干扰离子等。在优化的实验条件下,获得了20的富集因子和10 h⁻¹的采样频率。该方法对V、Cu、Pb、Cd和Hg的检出限分别为0.33、0.30、0.96、0.05和0.93 ng mL⁻¹,相对标准偏差(RSD)分别为2.8%、6.7%、1.8%、4.0%和5.3%(n = 7,C = 10 ng mL⁻¹)。壳聚糖修饰的有序介孔二氧化硅对V、Cu、Pb、Cd和Hg的吸附容量分别为16.3、21.7、22.9、12.2和13.5 mg g⁻¹。为验证所建立的方法,分析了GSBZ50009 - 88环境水样标准物质,测定值与认定值吻合良好。该方法还应用于天然水样中痕量重金属的测定,结果令人满意。