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作 者:李利军[1] 钟亮[2] 程昊[1] 李彦青[1] 喻来波[2]
机构地区:[1]广西工学院生物与化学工程系,柳州545006 [2]广西大学化学与化学工程学院,南宁530004
出 处:《化学通报》2011年第11期1053-1057,共5页Chemistry
基 金:广西自然科学基金项目(桂科自0832062);国家自然科学基金项目(20665001)资助
摘 要:在玻碳电极上成功制备了多壁碳纳米管(MWNTs)修饰玻碳电极(GCE),并对其进行显微表征。研究表明,该修饰电极(MWNTs/GCE)对Fe3+具有明显的电催化还原作用。将其用于流动注射不可逆双安培(FI-IB)体系的构建,即:利用Fe3+在MWNTs/GCE上的还原和硫酸羟胺((NH2OH)2.H2SO4)在另一支金电极上的氧化,构建了双安培检测新体系,建立了在外加电压为0 V条件下流动注射双安培法直接测定Fe3+的新方法。在0 V外加电位差下,在6×10-2 mol/L HCl载液中,该还原峰峰电流与Fe3+浓度在4.0×10-3~10-1mg/mL范围内呈良好的线性关系,其线性回归方程为i(nA)=1.4456×105C-582.97(r=0.9992,n=7),方法检出限为8.0×10-4mg/mL(S/N=3)。连续测定1.00×10-2mg/mL的Fe3+标准溶液20次,电流值RSD为2.99%,进样频率为90样/h。该方法具有较高的选择性和灵敏度。对模拟样品中Fe3+含量的测定,结果比较满意。The multi-walled carbon nanotubes(MWNTs) modified glassy-carbon electrode(MWNTs/GCE) was prepared and the micrographs of the MWNTs/GCE were obtained by scanning electron microscopy.The modified electrode showed an excellent electro-catalytic effect on the reduction of iron(Ⅲ).Based on the reduction of iron(Ⅲ) at MWNTs/GCE and oxidation of(NH2OH)2·H2SO4 at the Au electrode,a novel flow injection irreversible biamperometric method was developed for the determination of iron(Ⅲ) under the potential difference of 0 V imposed between two electrodes.In 6×10-2 mol/L HCl,the reduction peak current increased linearly with the concentration of iron(Ⅲ) in the range of 4.0×10-3~10-1 mg/mL,the linear regression equation was i(nA)=1.4456×105C-582.97(r=0.9992,n=7)with a sampling frequency of 90 samples per hour.The detection limit for iron(Ⅲ) was 8.0×10-4 mg/mL and the RSD was 2.99 %.The presented method has the advantage of high selectivity and sensitivity.The analysis of iron(Ⅲ) was performed with satisfactory results.
关 键 词:玻碳电极 MWNTs/GCE 不可逆双安培法Fe3+
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