纳米金修饰分子印迹聚合膜电极检测双酚A

以纳米金修饰玻碳电极为基础电极,以双酚A为模板分子,以邻氨基苯硫酚为聚合单体,采用循环伏安法电聚合制备分子印迹聚合膜,利用循环伏安和交流阻抗法研究电极的电化学特性。结果表明,双酚A在修饰电极表面的反应是一个受吸附控制的等电子、质子转移的不可逆反应。采用差分脉冲伏安法检测双酚A,线性范围为5. 0×10~(-6)mol/L～4. 0×10~(-4)mol/L,检出限为2. 3×10~(-7)mol/L。将该电极用于自来水和牛奶样品的测定,结果均为未检出,加标回收率分别为93. 5%和95. 4%,3次测定结果的RSD分别为4. 0%和5. 7%。     

多壁碳纳米管修饰的分子印迹电极测定双酚A

将分子印迹技术与电化学传感器相结合,以双酚A(BPA)为模板分子,吡咯为功能单体,在基于多壁碳纳米管修饰的玻碳电极表面制备了一种对BPA具有选择性识别的分子印迹聚合物,并进行相关试验条件的优化。在最优条件下构建了BPA-MWCNTs-COOH分子印迹电化学传感器,以铁氰化钾K₃[Fe(CN)₆]为电化学探针,测得BPA在0.01μmol/L～17μmol/L范围内线性良好,检出限为0.006μmol/L。将该方法用于湖水样品测定,结果为未检出,加标回收率为97.8%～115%,RSD <5%。     

纳米TiO 2 -碳纳米管复合膜修饰电极伏安法测定水中α -萘酚和β -萘酚

摘要：制备了一种新型的纳米TiO2-碳纳米管复合膜修饰电极,在pH值为5.57的NaAc-HAc缓冲溶液中,研究了α-萘酚和β-萘酚在该修饰电极上的电化学行为,据此建立了纳米TiO2-碳纳米管复合膜修饰电极伏安法测定水中α-萘酚和β-萘酚的方法。优化了试验条件,α-萘酚和β-萘酚分别在8.3×10^-7mol／L—1.0×10^-5mol／L和7.8×10^-7mol／L—1.0×10^-5mol／L范围内,浓度与氧化峰电流呈良好的线性关系,开路富集3min,检出限分别为3.5××10^-7mol／L和2.3×10^-7mol／L,模拟水样测定的回收率为97.6％—101％。     

过氧化聚吡咯/聚乙烯吡咯烷酮修饰碳糊电极测定废水中苯酚

建立了过氧化聚吡咯(OPPy)和聚乙烯吡咯烷酮(PVP)修饰碳糊电极测定废水中苯酚的方法.优化了试验条件,苯酚的氧化峰电流在1.0×10-5 mol/L～1.0×10-3 mol/L之间线性关系良好,检出限为1.0×10-6 mol/L.该电极制作简单,选择性好,测定灵敏度高,精密度与准确度均符合要求.     

铅离子印迹电化学传感器的制备及检测性能研究

重金属因其具有高毒性、致癌性和潜在的生物积累性，引发的环境问题受到广泛关注。为精确监测环境中的重金属污染，结合电化学分析和离子印迹技术的优势，构筑了对铅离子的高灵敏电化学传感器。利用铅离子作为模板，采用3-（γ-氨基乙氨基）-丙基-三甲基硅烷作为功能单体，在介孔硅表面，通过共缩聚法制备了离子印迹聚合物，并将其作为电化学传感器的核心识别元件。经过优化碳糊电极的组成，制备了一系列高选择性的离子印迹电化学传感器，并对其电化学行为进行了分析。测试结果表明，所制传感器对铅离子的检测线性范围为10^-9～10^-6 mol/L，且检出限达到1.3×10^-11mol/L（信噪比=3）。在对河水和大米等实际样品的检测中，传感器展现了高灵敏性（相对标准偏差为2.5%～7.4%）和高准确性（回收率为98.8%～102.9%），表明其在环境监测和食品安全检测方面具有应用潜力。     

Nafion修饰汞膜电极微分脉冲阳极溶出伏安法测定蔬菜中的铅

采用Nafion修饰汞膜电极微分脉冲阳极溶出伏安法测定蔬菜中的铅,选择0.1 mol/L NH4NO3作为支持电解质,富集时间420 s,搅拌速度300 r/min,Nafion修饰体积10 μL,考察了共存离子的干扰.方法在0.01 μg/L～ 14.0 μg/L范围内线性良好,检出限为0.2 μg/L,铅酸电池厂附近蔬菜样品的测定结果与石墨炉原子吸收光谱法相吻合,加标回收率为89.5％～106％.     

亚硝酸盐氮对次溴酸钠氧化法氨氮测定的影响

次溴酸盐氧化法是一种海水或高盐度水质氨氮的常用检测方法,但实验发现该方法在亚硝酸盐氮存在时氨氮测定结果有较大误差。研究了次溴酸盐氧化法中亚硝酸盐氮对氨氮测定结果的影响。结果显示,氨氮的测量误差随着水样中亚硝酸盐氮含量的升高而变大,且具有明显的正相关性;探讨误差产生的机理发现,误差可能是次溴酸盐不能将氨氮完全氧化为亚硝酸盐氮导致的;研究了氧化率的影响因素发现,氧化时间对氧化率的影响可忽略,温度对氧化率有很大影响。在室温为(23±1)℃时,拟制出亚硝酸盐氮浓度对氨氮测量绝对误差的影响曲线,曲线方程为y=1.834x+0.018,r=0.996 7。利用修订的氨氮测定计算公式,可大大提高亚硝酸盐氮存在时水中氨氮的测量精度。     

农药废水中邻苯二胺的分光光度法测定

利用Fe3 催化氧化邻苯二胺(o-PDA),研究了分光光度法测定o-PDA的最佳实验条件和干扰去除方法.研究表明,在稀HCl介质中,显色体系最佳pH=3.0;λmax=450 nm;方法的线性范围0～8 mg/L,线性回归方程A = 0.011 4C 0.037 2,相关系数r= 0.999 6;体系的摩尔吸光系数ε=1.22×104 L·mol-1·cm-1;方法的检测下限为0.015 mg/L,动力学研究表明显色反应为一级,dA/dt=0.007 5A-0.011 67,r=0.999 5.用硫酸铜沉淀去除农药生产废水中的干扰后测定水中的o-PDA,结果满意.     

番红花红T紫外分光光度法测定微量亚硝酸盐氮

1实验方法 :于 2 5ml比色管中加 5μg亚硝酸盐氮标准使用液 ( 5.0 μg/ml)、2 .0 ml1 .0× 1 0 -3mol/L 番红花红 T、4 .0 ml2 .0 mol/L 缓冲溶液( H2 SO4) ,用水定容 ,摇匀。放置 1 0 min,用 1 cm比色皿以试剂空白为参比在 365nm处测吸光度 ,吸光值至少在 1 h内保持恒定。 2变异系数 0 .59%～ 1 .35% ,加标回收率 98.2 %～ 1 0 0 .4 %。 3亚硝酸盐氮在 0～ 1 0 .0 μg/2 5ml内符合比耳定律 ,表观摩尔吸光系数 3.1× 1 0 4L/mol· cm,回归方程y=0 .0 2 67c 0 .0 0 2 ,相关系数 r=0 .9992 ,结果满意。番红花红T紫外分光光度法测定微量亚…     

基于亨利定律的水中臭氧浓度检测方法研究

为提高水中臭氧(O3)浓度检测方法的普适性、准确性和便捷性,提出了一种新的非接触式的水中O3浓度检测方法.基于亨利定律(Henry's Law),采用电化学方法,建立空气中O3浓度与水中O3浓度的回归方程,从而推导出水中O3浓度.实验结果显示,水体O3传感器的检出限为0.02 mg/L,检测上限为0.40 mg/L,可...     

Maize tassel-modified carbon paste electrode for voltammetric determination of Cu(II)

The preparation and application of a practical electrochemical sensor for environmental monitoring and assessment of heavy metal ions in samples is a subject of considerable interest. In this paper, a carbon paste electrode modified with maize tassel for the determination of Cu(II) has been proposed. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were used to study morphology and identify the functional groups on the modified electrode, respectively. First, Cu(II) was adsorbed on the carbon paste electrode surface at open circuit and voltammetric techniques were used to investigate the electrochemical performances of the sensor. The electrochemical sensor showed an excellent electrocatalytic activity towards Cu(II) at pH 5.0 and by increasing the amount of maize tassel biomass, a maximum response at 1:2.5 (maize tassel:carbon paste; w/w) was obtained. The electrocatalytic redox current of Cu(II) showed a linear response in the range (1.23 μM to 0.4 mM) with the correlation coefficient of 0.9980. The limit of detection and current–concentration sensitivity were calculated to be 0.13 (±0.01) μM and 0.012 (±0.001) μA/μM, respectively. The sensor gave good recovery of Cu(II) in the range from 96.0 to 98.0 % when applied to water samples.     

快速检测痕量铜的光电型传感器的研制

利用铜对葡萄糖氧化酶的抑制作用,以及葡萄糖氧化酶-辣根过氧化物酶-葡萄糖(Glu)-邻联甲苯胺(OT)偶联反应体系生成蓝色底物的原理,将Glu与OT固定化制成试纸条,插入自制的便携式单色光反射计,组装出检测铜的光电型传感器。当铜的质量浓度范围为1 mg/L～100 mg/L时,光反射强度值与铜的质量浓度呈良好的线性关系。在优化的试验条件下,该方法的检测限为0.064 mg/L,检测时间为5 min。     

A new catalytic-spectrophotometric method for quantification of trace amounts of nitrite in fruit juice samples

A new kinetic method has been developed for the determination of nitrite in fruit juice samples. The method is based on the catalytic effect of nitrite with the oxidation of Nile Blue A (NBA) by KBrO₃ in the sulfuric acid medium. The optimum conditions obtained are 1.2 mM sulfuric acid, 0.034 mM of NBA, 2.8?×?10^?3 M KBrO₃, reaction temperature of 20 °C, and reaction time of 100 s at 595.5 nm. Under the optimized conditions, the method allowed the quantification of nitrite in a range of 0.2–800 μg/mL with a detection limit of 0.02 μg/mL. The method was applied to the determination of nitrite in 15 brands of fruit juice samples.     

Detection of Lead in Vegetables with New Chromogenic Reagent by Spectrophotometry

A new simple, rapid selective and highly sensitive chromogenic reagent dibromo-p-methyl-carboxyazo (DBMCA) was synthesized and studied in detail for the spectrophotometric detection of lead. In 0.25 M phosphoric acid medium, which greatly increases the selectivity, Lead reacts with DBMCA to form a 1:2 blue complex having a sensitivity absorption peak at 646 nm. Under optimal conditions, Beer's Law is obeyed over the range from 0.09 to 0.8 microg mL(-1) Pb (II) and the apparent molar absorptivity is 1.03 x 10(5) mL(-1) cm(-1). The detection limit and the variation coefficient were found to be 2.12 microg mL(-1) and 1.0% respectively. It is found that, except for Ca (II) and Ba (II) all foreign ions studied do not interfere with detection. The interference caused by Ca (II) and Ba (II) can be easily eliminated by prior extraction with potassiumiodide-methylisobutylketone. The proposed method has been applied successfully for to the detection of Lead in vegetable leaves with good results.     

高效液相色谱法直接测定环境水体中直链烷基苯磺酸钠类阴离子表面活性剂

使用亚甲蓝分光光度法和流动注射法分析环境水体中的阴离子表面活性剂的过程中用到的三氯甲烷会带来次生环境污染问题,同时也会在一定程度上影响检测人员的健康。结合现有仪器设备,通过优化检测流程,建立了一种适用于高海拔条件下测定环境水体中直链烷基苯磺酸钠(LAS)类阴离子表面活性剂的方法。该方法以十二烷基苯磺酸钠(SDBS)为定量标准物质,采用高效液相色谱法测定,使用归一化法定量。经验证,在0.02~2.00 mg/L浓度范围内,所建立校准曲线的线性回归系数在0.999以上。该方法具有良好的检出能力(检出限为0.01 mg/L)和抗干扰能力,重复性范围为1.3%~6.2%,准确度范围为2.1%~4.0%,回收率范围为80.0%~116%,相关验证参数均能满足实际样品的分析要求。检测过程避免了二次污染物的产生,减少了对实验人员健康的影响。该方法具有操作简便、高效且对环境友好的特点。     

Detection of petroleum hydrocarbons at low ppb levels using quartz resonator sensors and instrumentation of a smart environmental monitoring system

Petroleum hydrocarbon vapors at low ppb levels can be detected using a thickness shear mode resonator (TSMR) coated with a chemical-sensing overlayer, prepared by radiofrequency sputtering of porous sintered-polyethylene (PS-PE). The sensing capabilities of PS-PE sensors were profoundly affected by the sputtering methods; they were enhanced by the photo-excitation effect, and were reduced by carbonization and water treatment. The photo-assisted PS-PE sensor was extremely sensitive and could detect linear hydrocarbon (> C12) vapors below the ppb level. The time constant of the sorption curve, however, was large, indicating a slow sensing speed. Toward creating instrumentation for a smart environmental monitoring system, the TSMR sensors were arrayed on a circuit board equipped with a serial interface and signal processing chips of the oscillation drive and frequency counter. Co-sorption with water vapor at a relative humidity of about 10% has almost no effect on the sensing ability of PS-PE sensors for 1,2,4-trimethylbenzene. Conversely, it enhances the sensitivity of the TSMR sensor coated with a D-phenylalanine film. Upward shifts in the baseline are evident with elapsed time. However, a rigorous ten-cycle iteration test for 100 ppm toluene vapor demonstrated good reproducibility of the sensor's signals.     

Paramagnetic antibody-modified microparticles coupled with voltammetry as a tool for isolation and detection of metallothionen as a bioindicator of metal pollution

Low-molecular mass proteins rich in cysteines called metallothioneins (MT) can be considered as markers for the pollution of the environment by metals. Here, we report on suggestion for an automated procedure for the isolation of MT followed by voltammetric analysis. Primarily, we optimized the automated detection of MT using an electrochemical analyser. It was found that the most sensitive and repeatable analyses are obtained at a temperature of 4 °C for the supporting electrolyte. Further, we optimized experimental conditions for the isolation of MT by using antibody-linked paramagnetic microparticles. Under the optimal conditions (4 h long interaction between the microparticles and MT), the microparticles were tested on isolation of various amounts of MT. The lowest isolated amount of MT by antibody-linked paramagnetic microparticles was 5 μg ml(-1) of MT (50 ng). The automated procedure of MT isolation was further tested on isolation of MT from guppy fish (Poecilia reticulata) treated with silver(i) ions (50 μM AgNO(3)). The whole process lasted less than five hours and was fully automated. We attempted to correlate these results with the standard method for MT isolation. The correlation coefficient is 0.9901, which confirms that results are in good agreement. Moreover, the concentration of silver ions in tissues of fish treated with Ag(i) ions was determined by high performance liquid chromatography with electrochemical detection.     

Electrochemical Detection of Pathogen Infection Using Cell Chip

The immobilized cell using self-assembled synthetic oligopeptide was applied to the electrochemical detection of pathogen infection. Thin films based on cysteine-terminated synthetic oligopeptides were fabricated for the immobilization of HeLa cell on gold (Au) substrate. Layer formation and immobilization of the cell were investigated with surface plasmon resonance (SPR) and electrochemical impedance spectroscopy (EIS). Experimental results showed that the thin film of cysteine-terminated synthetic oligopeptide was successfully fabricated and it could be applied for the immobilization of HeLa cells. The adhered living cell was exposed to E. coli O157:H7, which induced the change of SPR angle and electrochemical impedance signal. The proposed cell immobilization method using self-assembly technique can be applied to construct the cell microarray for on-site pathogen monitoring.     

Electrochemical sensors for environmental monitoring: design, development and applications

The advancement in miniaturization and microfabrication technology has led to the development of sensitive and selective electrochemical devices for field-based and in situ environmental monitoring. Electrochemical sensing devices have a major impact upon the monitoring of priority pollutants by allowing the instrument to be taken to the sample (rather than the traditional way of bringing the sample to the laboratory). Such devices can perform automated chemical analyses in complex matrices and provide rapid, reliable and inexpensive measurements of a variety of inorganic and organic pollutants. Although not exhaustive due to the vast amounts of new and exciting electrochemical research, this review addresses many important advances in electrochemical sensor design and development for environmental monitoring purposes. Critical design factors and development issues including analytical improvements (e.g. detection limits), microfabrication and remote communication are presented. In addition, modern environmental applications will be discussed and future perspectives considered.