6 PdNPs /MWNTs 595 Cr VI CHI-660B SCE PS-20A JBZ- 12H Veeco Nano III a Multimode S-4800 FE-SEM Hitachi phs-3c ph 1 2 MWNTs 40 ~ 60 nm N-N DMF PB

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1 4 3 6 Vol 43 No Journal of Shanghai Normal University Natural Sciences Dec DOI /J ISSN PdNPs / MWNTs 用钯纳米粒子多壁碳纳米管修饰玻碳电极, 并用于对六价铬 ( Cr( VI) ) 的电化学测定采用场发射扫描电子显微镜循环伏安法交流阻抗法差分脉冲伏安法等方法对修饰电极进行了表征研究发现多种其他金属离子如 Cr 3 + Pd 2 + Zn 2 + Pb 2 + Cu 2 + Al 3 + Ba 2 + Ca 2 + Mg 2 + 等对六价铬离子的测定没有明显干扰, 且六价铬的还原峰电流与 Cr( VI) 的浓度在 ~ mol /L 范围内呈良好线性关系, 检测限达 mol /L 该法具有简便快速, 选择性好, 灵敏度高等特点六价铬 Cr( VI) ; 钯纳米粒子 ; 多壁碳纳米管 ; 电化学 ; 修饰电极 O A Cr VI Cr 14 - VI DXL zhunn@ shnu edu cn

2 + Ca 2 + Mg 2 + 等对六价铬离子的测定没有明显干扰, 且六价铬的还原峰电流与 Cr( VI) 的浓度在 8 10-7 ~ 5 10-8 mol /L 范围内呈良好线性关系, 检测限达 2 7 10-8 mol /L 该法具有简便快速, 选择性好, 灵敏度高等特

2 6 PdNPs /MWNTs 595 Cr VI CHI-660B SCE PS-20A JBZ- 12H Veeco Nano III a Multimode S-4800 FE-SEM Hitachi phs-3c ph 1 2 MWNTs 40 ~ 60 nm N-N DMF PBS ph = mol L mol L mol L mol L mol L - 1 / mol L - 1 Milli-Q 18 2 MΩ GCE 0 3 μm 0 05 μm Al 2 O min Al 2 O 3 1 mg MWNTs 1 ml N-N DMF 2 h 1 mg /ml 5 μl MWNTs MWNTs /GCE MWNTs /GCE mol L - 1 PdCl mol L - 1 KCl - 0 2V 100 s PdNPs / MWNTs /GCE Cr VI CV GCE MWNTs /GCE PdNPs / MWNTs /GCE mol L - 1 Cr VI ~ 1 0 V 100 mv s - 1 EIS mol L - 1 K 3 Fe CN 6 /K 4 Fe CN mol L - 1 KCl DPV mol L - 1 ~ mol L - 1 Cr VI FE-SEM PdNPs /MWNTs FE-SEM 2 2

/ml 5 μl MWNTs MWNTs /GCE MWNTs /GCE 2 5 10 3 mol L - 1 PdCl 2 + 0 1 10 6 mol L - 1 KCl - 0 2V 100 s PdNPs / MWNTs /GCE 1 1 4 Cr VI CV GCE MWNTs /GCE PdNPs / MWNTs /GCE 0 5 10 3 mol L - 1 Cr

3 PdNPs /MWNTs 2 20 ~ 40 nm PdNPs MWNTs 2 PdNPs /MWNTs /GCE FE-SEM CV 3 a GCE b MWNT /GCE c PdNPs-MWNT /GCE mol L - 1 3c PdNPs-MWNT 4 a GCE b MWNT / GCE c PdNPs /MWNT /GCE / 4 a b PdNPs 4c PdNPs 3 a GCE b MWNTs /GCE c PdNPs /MWNTs /GCE 4 a GCE b MWNTs /GCE c PdNPs /MWNTs /GCE mol L - 1 K3Fe CN mol L - 1 Fe CN / mol L - 1 KCl 5 a GCE b MWNTs /GCE d PdNPs /MWNTs /GCE mol L - 1 Cr VI mol L - 1 PBS ph a b MWNTs /GCE - 0 7V vs SCE Cr VI d PdNPs /MWNTs /GCE- 0 7V vs SCE Cr VI

/GCE c PdNPs /MWNTs /GCE 2 2 1 10 3 mol L - 1 K3Fe CN 6 1 10 3 mol L - 1 Fe CN 6 4 - /3-0 1 10 6 mol L - 1 KCl 5 a GCE b MWNTs /GCE d

4 6 PdNPs /MWNTs 597 PdNP S Cr VI - 0 6V Cr VI c PdNPs /MWNTs /GCE Cr VI mol L - 1 PBS ph V vs SCE d - 0 7V Cr VI PdNPs /MWNTs /GCE Cr VI 2 3 ph ph 6 PdNPs /MWNTs /GCE ph mol L - 1 PBS mol L - 1 Cr VI ph 7 0 ph ph 7 0 ph 7 0 a GCE b MWNTs /GCE c Pd NPs /MWNTs /GCE without Cr VI d PdNPs / MWNTs /GCE mol L - 1 PBS 5 ph mv s mol L - 1 Cr VI mol L - 1 ph 4 0 ~ 9 0 Cr VI PdNPs /MWNTs / GCE mol L - 1 Cr VI mol L - 1 PBS ph = ~ 200 mv s - 1 Cr VI 20 ~ 100 mv s - 1 Ip μa = υ 1 /2 mv s R = PdNPs /MWNTs /GCE a ~ f mv s mol L - 1 Cr VI Cr VI 8A Pd NPs /MWNTs /GCE mol L - 1 PBS ph = 7 0

0 100 mv s - 1 0 5 10 3 mol L - 1 Cr VI 6 0 1 10 6 mol L - 1 ph 4 0 ~ 9 0 Cr VI 2 4 7 PdNPs /MWNTs / GCE 0 5 10 3 mol L - 1 Cr VI 0 1 10 6 mol L - 1 PBS ph = 7 0 7 20 ~ 200 mv s - 1 Cr VI 20 ~ 100

5 ~ mol L - 1 Cr VI 8 b ~ f V a PBS 8A Cr VI 8B ~ mol L - 1 I = c R = mol L - 1 S /N = mol L - 1 PBS ph 7 0 a blank b mol L - 1 c mol L - 1 d mol L - 1 e mol L - 1 f mol L - 1 A Pd NPs /MWNTs /GCE Cr VI B ph mol L - 1 PBS mol L - 1 Cr VI Zn 2 + Pb 2 + Cu 2 + Cr 3 + Al 3 + Ba 2 + Ca 2 + Mg 2 + Cr VI PEREZ A C RENEDO O D LOMILLO M A A et al Simultaneous determination of Cr III and Cr VI by differential pulse voltammetry using modified screen-printed carbon electrodes in array mode J Electroanalysis ANDRLE C M BROEKAERT J A C Speciation of Cr III and Cr VI by reversed phase high-performance liquid chromatography using UV-detection J Fresenius J Anal Chem POSTA J GASPAR A TOTH R et al Cr III and Cr VI on-line preconcentration and determination with high performance flow flame emission spectrometry in natural samples J Fresenius J Anal Chem ZAZOUA A MORAKCHI K KHERRAT R et al Electrochemical characterization of an EIS sensor functionalized with a TOPO doped polymeric layer for Cr VI detection J ITBM-RBM

2 + Cr 3 + Al 3 + Ba 2 + Ca 2 + Mg 2 + Cr VI 50 3 1 PEREZ A C RENEDO O D LOMILLO M A A et al Simultaneous determination of Cr III and Cr VI by differential pulse voltammetry using modified

6 6 PdNPs /MWNTs CHOI Y W MOON S H Determination of Cr VI using a pulse amperometric method with an ionophore-immobilized membrane electrode J Electroanalysis GUELL R FONTAS C SALVADO V et al Development of a selective optical sensor for Cr VI monitoring in polluted waters J Analytica Chimica Acta MILACIC R SCANCAR J TUSEK J Determination of Cr VI in welding fumes by anion-exchange fast protein liquid chromatography with electrothermal atomic absorption spectrometric detection J Anal Bioanal Chem GRATE J W TAYLOR R H Sequential injection method with on-line soil extraction for determination of Cr VI J Field Analytical Chemistry And Technology WELCH C M NEKRASSOVA O COMPTON R G Reduction of hexavalent chromium at solid electrodes in acidic media reaction mechanism and analytical applications J Talanta RAJ C R ABDELRAHMAN A I OHSAKA T Gold nanoparticle-assisted electroreduction of oxygen J Electrochem Commun LIU S Q JU H X Nitrite reduction and detection at a carbon paste electrode containing hemoglobin and colloidal gold J Analyst LIU B Z LU L Y WANG M et al A study of nanostructured gold modified glassy carbon electrode for the determination of trace Cr VI J J Chem Sci XU H ZHENG Q L YANG P et al Electrochemical synthesis of silver nanoparticles-coated gold nanoporous film electrode and its application to amperometric detection for trace Cr VI J Sci China Chem ZHENG Z X DU Y L FENG Q L et al Facile method to prepare Pd / graphene-polyaniline nanocomposite and used as new electrode material for electrochemical sensing J Journal of Molecular Catalysis A Chemical YOU J M JEON S Electrocatalytic oxidation of NADH on a glassy carbon electrode modified with MWCNT-Pd nanoparticles and poly 3 4-ethylenedioxypyrrole J Electrochimica Acta Preparation of palladium nanoparticles and carboxylated MWNTs modified glassy carbon electrode and its application for the electrochemical determination of Cr VI YANG Shuai TANG Wanxin ZHANG Chao ZHU Ningning College of Life and Environmental Sciences Shanghai Normal University Shanghai China Abstract This study described a simple and rapid method for the electrochemical determination of Cr VI based on palladium nanoparticles and carboxylated multi-walled carbon nanotubes MWNTs modified glassy carbon electrode GCE written as PdNPs-MWNT /GCE The prepared PdNPs-MWNT /GCE was characterized by FE-SEM CV EIS and DPV It was found that many other metal ions such as Cr 3 + Pd 2 + Zn 2 + Pb 2 + Cu 2 + Al 3 + Ba 2 + Ca 2 + Mg 2 + had no influence on Cr VI determination Under the optimal conditions the reduction current of Cr VI increased linearly with increasing the concentration of Cr VI in the range of ~ mol /L with a correlation coefficient of and the detection limit of mol /L based on S /N = 3 The present method has the following advantages such as simple rapid good selectivity and sensitivity Key words Cr VI PdNPs MWNTs electrochemical modified electrode ( 责任编辑 : 顾浩然 )

welding fumes by anion-exchange fast protein liquid chromatography with electrothermal atomic absorption spectrometric detection J Anal Bioanal Chem 2002 372 549-553 8 GRATE J W TAYLOR R H Sequential

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<4D6963726F736F667420576F7264202D203435372D343631203230313230393135303033CEE2D0A1BEEA5F6E65775FCDACCEBBB6C6EEE9B7BDB2A8C8DCB3F6B7FCB0B2B7A8BCECB2E2A1AD> 3 5 Vol. 3 No. 5 2012 10 Journal of Food Safety and Quality Oct., 2012 吴小娟, 蔡健荣 *, 韩恩, 周立娜, 陈铭枫 (, 212013) 摘要 : 目的方法,, 结果, ph,,, 0.580 V, 5~100 μg/l(r=0.9965), 0.630 μg/l 结论关键词 : ; ;