Liang Pei, Liu Rui
Key Laboratory of Pesticide & Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079, PR China.
Anal Chim Acta. 2007 Oct 17;602(1):32-6. doi: 10.1016/j.aca.2007.09.012. Epub 2007 Sep 14.
A novel solid phase extraction sorbent, nanometer titanium dioxide immobilized on silica gel (immobilized nanometer TiO2), was prepared by sol-gel method, and the adsorptive potential of immobilized nanometer TiO2 for inorganic arsenic species (As(III) and As(V)) was assessed. It was found that both As (III) and As(V) could be adsorbed quantitatively on immobilized TiO2 within a pH range of 5.0-7.5, and only As(III) could be quantitatively retained on the sorbent within a pH range of 9.5-10.5 while As(V) was passed through the microcolumn without the retention. Based on this fact, a new speciation scheme for inorganic arsenic was established, which involved determining total As at pH 6.0 and As(III) at pH 10, with As(V) obtained by difference. The adsorption capacity of immobilized nanometer TiO2 for As(III) was found to be 4.22 mg g(-1). Under the optimized conditions, the detection limits of this method for As(III) were 24 ng L(-1) with an enrichment factor of 50, and the relative standard deviation (R.S.D.%) was 4.8% (n=11, c=5 ng mL(-1)). The proposed method has been applied to the speciation of inorganic arsenic in natural water samples with satisfactory results.
通过溶胶 - 凝胶法制备了一种新型固相萃取吸附剂——硅胶负载纳米二氧化钛(负载型纳米TiO₂),并评估了负载型纳米TiO₂对无机砷形态(As(III)和As(V))的吸附潜力。研究发现,在pH值为5.0 - 7.5范围内,As(III)和As(V)均可被定量吸附在负载型TiO₂上;而在pH值为9.5 - 10.5范围内,只有As(III)能被定量保留在吸附剂上,As(V)则会通过微柱而不被保留。基于这一事实,建立了一种新的无机砷形态分析方法,即通过在pH 6.0时测定总砷含量,在pH 10时测定As(III)含量,通过差值计算得到As(V)含量。负载型纳米TiO₂对As(III)的吸附容量为4.22 mg g⁻¹。在优化条件下,该方法对As(III)的检测限为24 ng L⁻¹,富集倍数为50,相对标准偏差(R.S.D.%)为4.8%(n = 11,c = 5 ng mL⁻¹)。该方法已应用于天然水样中无机砷的形态分析,结果令人满意。