碳纳米管-离子液体-木质素磺酸钠复合物修饰电极同位镀铋膜测定水中铅和镉

采用涂覆法制备多壁碳纳米管(MWCNTs)-离子液体([BMIM]PF6)-木质素磺酸钠(LSS)修饰玻碳电极(GCE),然后在其表面同位镀铋膜,研究Pb(Ⅱ)和Cd(Ⅱ)在该修饰电极上的阳极溶出伏安行为。实验表明,Pb、Cd在该修饰电极上分别于-0.44V、-0.73V产生灵敏的溶出峰,Pb(Ⅱ)和Cd(Ⅱ)分别在3.0×10-8～1.0×10-6mol·L-1和2.0×10-8～8.0×10-7mol·L-1浓度范围内与其溶出峰电流呈良好的线性关系,检出限分别为4.1×10-9mol·L-1、6.9×10-9mol·L-1。该修饰电极制备简单,重现性好,用于河水中铅和镉的测定,效果良好。     

对乙酰氨基酚在多壁碳纳米管修饰电极上的电化学行为

制备了多壁碳纳米管修饰玻碳电极,研究了对乙酰氨基酚在多壁碳纳米管修饰电极上的循环伏安行为,并建立了测定对乙酰氨基酚含量的电化学分析方法。在pH为6.89的磷酸盐缓冲液中,多壁碳纳米管修饰电极对对乙酰氨基酚有明显的电催化作用,其氧化峰电流与对乙酰氨基酚浓度在1.0×10-6～1.0×10-4mol·L-1范围内呈良好的线性关系,检测限为2.0×10-7mol·L-1。     

多壁碳纳米管修饰玻碳电极测定铜离子

以多壁碳纳米管(MWCNTs)修饰玻碳电极为工作电极,采用阳极溶出线性扫描法研究了铜离子的电化学测定方法。探讨了MWCNTs修饰层数、富集电位、富集时间、溶液pH、支持电解质对峰电流的影响。实验表明,铜离子浓度在1.0×10-8~1.0×10-5mol·L-1范围内与峰电流呈良好的线性关系,检测限为2.0×10-9mol·L-1,且该电极具有良好的稳定性和抗干扰能力。     

盐酸左氧氟沙星在聚L-精氨酸/多壁碳纳米管修饰电极上的电化学行为

运用循环伏安法、线性扫描伏安法、计时电量法等研究了盐酸左氧氟沙星在聚L-精氨酸/多壁碳纳米管修饰电极上的电化学行为。实验表明:盐酸左氧氟沙星在聚L-精氨酸/多壁碳纳米管修饰电极上的电极反应过程为等电子等质子吸附控制的不可逆过程,在pH=6.0的Na2HPO4-NaH2PO4支持电解质中,其氧化峰电流与浓度在7.0×10-6~1.0×10-4mol·L-1范围内呈良好的线性关系,相关系数R为-0.9992,检出限为5.0×10-6mol·L-1,样品测定回收率为98.26%~101.70%。     

聚L-半胱氨酸/多壁碳纳米管复合修饰电极同时测定邻苯二酚和对苯二酚

将羧基化多壁碳纳米管分散在L-半胱氨酸溶液中并滴涂在玻碳电极表面.将上述电极在pH 6.9的B-R缓冲溶液中,于-1.0～2.5 V的电位范围内进行电聚合,制备了聚L-半胱氨酸/多壁碳纳米管复合修饰电极(Pol-L-Cys/MWCNTs/GCE).研究发现,邻苯二酚和对苯二酚在聚L-半胱氨酸/多壁碳纳米管复合修饰电极上分别出现了一对氧化还原峰,且两者的氧化峰电位差达101 mV,提出了用微分脉冲伏安法同时测定邻苯二酚和对苯二酚的方法.氧化峰电流与邻苯二酚和对苯二酚的浓度在1.0×10-5～1.0×10-3mol·L-1呈线性关系,检出限(3S/N)均达1.0×10-5mol·L-1.修饰电极用于模拟样品中邻苯二酚和对苯二酚的测定,回收率在82.0%～107.0%之间.     

呋喃唑酮在多壁碳纳米管修饰电极上的电化学行为及分析应用

本文采用循环伏安法(CV)和差分脉冲伏安法(DPV),研究了呋喃唑酮(FZ)在多壁碳纳米管修饰玻碳电极(MWNTs/GCE)上的电化学行为。对影响该修饰电极电流大小的主要条件,如底液的pH值、富集电位和富集时间等进行了优化。结果表明:FZ在MWNTs/GCE上呈现不可逆的还原峰。与裸电极相比,FZ在修饰电极上的还原峰电流明显增大。在最佳的实验条件下,其峰电流随着FZ浓度的增加而增大,在4.9×10-7～5.9×10-5 mol.L-1范围内成线性关系,检测限低至8.0×10-8 mol.L-1。该修饰电极对FZ的测定表现出良好的重现性和稳定性,可用于药物制剂中FZ的定量测定。     

氧化石墨烯修饰碳糊电极的方波溶出伏安法测定锌

实验采用改进的Hummers法合成氧化石墨烯并将其修饰在碳糊电极(CPE)的表面制备了氧化石墨烯修饰碳糊电极(GO/CPE),以该修饰电极为工作电极,采用方波溶出伏安法对锌离子进行测定。结果表明:在十二烷基苯磺酸钠的增敏作用下,在0.1mol·L~(-1)KCl溶液中,该修饰电极对锌的氧化溶出有良好的催化作用,溶出峰电流与Zn~(2+)的浓度在4.0×10-8mol·L~(-1)~2.0×10-7mol·L~(-1)呈良好的线性关系,检出限为1.8×10~(-10)mol·L~(-1).该修饰电极用于实际样品中锌的含量分析,结果令人满意。     

聚拉莫三嗪修饰玻碳电极测定痕量铜(Ⅱ)的研究

在稀H2SO4介质中,采用循环伏安法制备了聚拉莫三嗪膜修饰玻碳电极(PLTG/GCE),将制得的膜修饰电极(PLTG/GCE)在一定电位下选择性预富集Cu(Ⅱ),并用差分脉冲溶出伏安法测定.结果表明,该膜修饰电极对Cu(Ⅱ)的富集作用明显强于裸玻碳电极.对电聚合条件、富集和溶出介质、富集时间及富集电位等实验参数进行了考察,在优化实验条件下,Cu(Ⅱ)的浓度在4.0×10-9～1.3×10-7mol· L-1范围内与溶出峰电流呈线性关系,相关系数为0.9999,检出限为1.5×10-9 mol·L-1.该修饰电极具有较高的灵敏度和选择性,用于实际水样的分析,平均回收率为98.7％.     

多壁碳纳米管修饰乙炔炭黑微电极测定碘

以多壁碳纳米管修饰乙炔炭黑微电极为工作电极,研究了碘离子在该修饰电极上的阳极溶出伏安特性。在0.1 mol/L KH2PO4 缓冲液(pH4.0)中,从200 mV以200 mV/s的速率正向扫描至1200 mV,碘离子在570 mV处出现一灵敏的阳极溶出峰。峰电流与碘离子的浓度在2.0×10-6～1.0×10-3 mol/L范围内呈良好的线性关系,检出限为8.0×10-7 mol/L。方法用于食盐中碘含量的测定,结果满意。     

基于多壁碳纳米管化学修饰电极直接测定饮料中的麦芽酚

采用循环伏安法和示差脉冲伏安法研究了麦芽酚在多壁碳纳米管修饰电极上的电化学行为,建立了一种直接测定饮料样品中麦芽酚含量的电分析测试方法. 在pH=8.5的NH3 ·H2 O-NH4 Cl 缓冲溶液中,麦芽酚在多壁碳纳米管修饰电极上于0.55 V(vs.SCE)产生不可逆的氧化峰. 该修饰电极对麦芽酚的电化学反应具有促进作用,阳极峰电流与溶液中麦芽酚的浓度成正比,线性范围为5.0×10-6～9.0×10-4mol/L,检出下限为2.0×10-6mol/L.对含5.0×10-5mol/L的麦芽酚溶液平行测定10次的相对标准偏差(RSD)为1.1%.多壁碳纳米管修饰电极具有良好的电极稳定性,可用于饮料样品中麦芽酚的直接测定,避免了繁复费时的样品前处理过程. 将该修饰电极用于啤酒、可乐和葡萄酒样品中麦芽酚测定,回收率为98%～103%.     

Bucky-gel coated glassy carbon electrodes, for voltammetric detection of femtomolar leveled lead ions

Femtomolar (fM) leveled lead ions were electrochemically detected using a bucky-gel coated glassy carbon electrode and differential pulse anodic stripping voltammetry. The bucky-gel was composed of dithizone, ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate), and multi-walled carbon nanotubes (MWCNTs). The fabrication of the bucky-gel coated electrode was optimized. The modified electrode was characterized with voltammetry, electrochemical impedance spectroscopy, and chronoamperometry. After the accumulation of lead ions into the bucky-gel modified electrode at −1.2 V vs. saturated calomel electrode (SCE) for 5 min in a pH 4.4 sodium acetate-acetate acid buffer solution, differential pulse anodic stripping voltammograms of the accumulated lead show an anodic wave at −0.58 V. The anodic peak current is detectable for lead ions in the concentration range from 1.0 μM down to 500 fM. The detection limit is calculated to be 100 fM. The proposed method was successfully applied for the detection of lead ions in lake water.     

Electrochemical Analysis of Antipsychotic Drug Quetiapine Fumarate Using Multi-walled Carbon Nanotube Modified Glassy Carbon Electrode

Electrochemical properties of quetiapine fumarate were examined on the anodic direction with multi-walled carbon nanotube modified glassy carbon electrode using voltammetric methods. The ratio of multi-walled carbon nanotube has been optimized using its various concentrations. The oxidation process was found to be irreversible, and adsorption controlled. The linear ranges were determined as 4×10⁻⁹–2×10⁻⁶ M for differential pulse stripping voltammetry and 2×10⁻⁹–2×10⁻⁶ M for square-wave stripping voltammetry with detection limits of 8.07×10⁻¹⁰ and 2.71×10⁻¹⁰ M, respectively. The methods were validated and successfully applied for the analysis of quetiapine fumarate tablets. The groups responsible for the oxidation reaction of quetiapine fumarate were investigated with model substances.     

Electrocatalytic Oxidation and Direct Determination of L-Tyrosine by Square Wave Voltammetry at Multi-wall Carbon Nanotubes Modified Glassy Carbon Electrodes

The electrochemical behavior of L-tyrosine was investigated at a multi-wall carbon nanotubes modified glassy carbon electrode. L-tyrosine itself showed a poor electrochemical response at the bare glassy carbon electrode; however, a multi-wall carbon nanotubes film fabricated on the glassy carbon electrode can directly enhance the electrochemical signal of L-tyrosine when applying cyclic voltammetry and square wave stripping voltammetry without any mediator. Cyclic voltammetry was carried out to study the electrochemical oxidation mechanism of L-tyrosine, which shows a totally irreversible process and an oxidation potential of 671 mV at the modified electrode and 728 mV at the bare electrode, ΔE_p = 57 mV. The anodic peak current linearly increases with the square root of scan rate in the low range, suggesting that the oxidation of L-tyrosine on the multi-wall carbon nanotubes modified electrode is a diffusion-controlled process. The square wave stripping voltammetry currents of L-tyrosine at the multi-wall carbon nanotubes modified electrodes increased linearly with the concentration in the range of 2.0 × 10⁻⁶–5.0 × 10⁻⁴ mol L⁻¹. The detection limit was 4.0 × 10⁻⁷ mol L⁻¹. The method is simple, quick, sensitive and accurate.     

还原氧化石墨烯-多壁碳纳米管复合膜负载金纳米粒子修饰玻碳电极检测双酚A

以水合肼为还原剂,采用均相还原法制备还原氧化石墨烯-多壁碳纳米管复合材料(rGO-MWCNTs),通过滴涂法将其修饰到玻碳电极(GCE)表面.以此复合材料为载体,采用电化学方法制备了金纳米粒子-还原氧化石墨烯-多壁碳纳米管复合膜修饰电极(AuNPs-rGO-MWCNTs/GCE).通过扫描电镜(SEM)、EDS能谱技术和电化学方法对此电极进行了表征.研究了双酚A在修饰电极上的电化学行为.结果表明,此电极对双酚A的电极过程具有良好的电化学活性,在0.10 mol/L PBS溶液(pH 7.0)中,微分脉冲伏安法测定双酚A的线性范围为5.0 × 10-9~1.0 × 10-7 mol/L和1.0 × 10-7~2.0 × 10-5 mol/L,检出限为1.0 ×10-9 mol/L(S/N=3). 将此电极用于模拟水样和超市购物小票样品中双酚A含量的测定,加标回收率分别为97%~110%和98%~104%.     

芦丁碳纳米管修饰玻碳电极电催化氧化肼的研究

应用循环伏安法研究了芦丁碳纳米管修饰玻碳电极(Rt-MWNT/GC)的电化学行为及其对肼的电催化氧化.实验表明,该修饰电极能使肼的氧化电位降至260 mV附近,表现出良好的电催化作用.安培法测得催化电流与肼浓度在2.5×10-6～1.0×10-4 mol·L-1范围内呈线性关系,检出限5×10-7 mol.L-1.     

Anodic Stripping Voltammetric Determination of Lead（Ⅱ） Using Glassy Carbon Electrode Modified with Novel Calix[4] arene

A new glassy carbon electrode modified with novel calix[4]‐arene derivative was prepared and then applied to the selective recognition of lead ion in aqueous media by cyclic and square wave voltammetry. A new anodic stripping peak at ? 0.92 V (vs. Ag/Ag⁺) in square wave voltammogram can be obtained by scanning the potential from ? 1.5 to ? 0.6 V, of which the peak current is proportional to the concentration of Pb²⁺. The modified electrode in 0.1 mol/L HNO₃ solution showed a linear voltammetric response in the range of 2.0 × 10–⁸–1.0 × 10–⁶ mol/L and a detection limit of 6.1 × 10–⁹ mol/L. In the modified glassy carbon electrode no significant interference occurred from alkali, alkaline and transition metal ions except Hg²⁺, Ag⁺ and Cu²⁺ ions, which can be eliminated by the addition of KSCN. The proposed method was successfully applied to determine lead in aqueous samples.     

金纳米粒子/碳纳米管修饰电极对4 壬基酚的电催化氧化及检测研究

制备了金纳米粒子/碳纳米管修饰玻碳电极(AuNPs-CNTs/GCE),采用循环伏安法和线性扫描伏安法研究了4-壬基酚在修饰电极上的电化学行为,并建立了一种灵敏简便地检测4-壬基酚的电化学方法。优化了pH值、扫描速率、富集时间等测定参数,并计算出pH值与氧化峰电压、扫描速率与氧化峰电流之间的数量关系。在pH 10.0的BR缓冲溶液中,4-壬基酚在AuNPs-CNTs/GCE上出现灵敏的氧化峰,氧化电位为0.51 V。与裸玻碳电极(GCE)和单一碳纳米管修饰电极(CNTs/GCE)相比,AuNPs-CNTs/GCE明显提高了4-壬基酚的氧化电流。在优化实验条件下,4-壬基酚的浓度分别在0.05～4μmol/L和6～14μmol/L范围内与氧化峰电流呈良好的线性关系,检出限为0.023μmol/L,对于实际样品测定的回收率为95%～104%。该修饰电极具有良好的重现性和稳定性,可用于环境样品中4-壬基酚的直接检测。     

基于羧基化多壁碳纳米管修饰玻碳电极快速检测氨基脲的研究

基于羧基化多壁碳纳米管修饰的玻碳电极(CMWCNTs/GCE),构建了一种灵敏检测氨基脲(SEM)的电化学传感器.采用傅里叶变换红外光谱、透射电子显微镜、电化学阻抗谱对修饰材料进行表征.结果表明,羧基化的多壁碳纳米管出现羧基碳氧双键的红外特征峰,管径明显减小,长度变短,电化学阻抗值显著减小.在1 mol/L HAc-NaAc缓冲液中,利用循环伏安法和时间-电流曲线研究了SEM在CMWCNTs修饰电极上的电化学行为.SEM在修饰电极上呈现不可逆的氧化峰.与裸电极相比,氧化峰电流明显增大.在最佳实验条件(pH 7.0,扫描速度为0.1 V/s)下,测得SEM在5.00×10-6~1.09×10-3mol/L浓度范围内与氧化峰电流呈线性关系,线性方程为IP(μA)=-0.472+0.0599C(μmol/L),相关系数r=0.997,检出限为1.88×10-7 mol/L(S/N=3).在实际猪肝样品检测中加标回收率为92.8%~98.0%.