阴极溶出伏安法测定硫脲

本文报道了一种阴极溶出伏安法测定硫脲的新方法。在乙二胺介质中,于-0.76V处出现硫脲峰电流.在PH11的条件下可获得很高的灵敏度。电富集10分钟便可测出0.05PPb(6.57×10~(-10)mol/L)的硫脲.硫脲在1～1000PPb浓度范围内呈良好的线性关系.此法可用了废水中痕量硫脲的测定。     

Voltammetric and Spectroscopic Determination of Toxic Metals in Sediments and Sea Water of Salerno Gulf

In this present work the distribution of heavy metals in sea water and sediments of the Salerno Gulf is measured. The elements determined were Cu, Pb, Cd, Zn and Hg, employing, as instrumental techniques, either differential pulse anodic stripping voltammetry (DPASV) or graphite furnace atomic absorption spectroscopy (GFAAS). A comparison of the results of the two analytical techniques is also made. Mercury determination was carried out employing the cold vapour atomic absorption spectroscopy (CVAAS) technique, with SnCl₂ as the reducing agent. The sample digestion was performed by a new procedure using concentrated suprapure H₂SO₄–K₂Cr₂O₇ mixture. The accuracy and precision of the analytical procedure were evaluated employing Sea Water BCR-CRM 403 and Estuarine Sediment BCR-CRM 277 as reference materials. Accuracy, expressed as relative error e and precision, expressed as relative standard deviation s_r, were in order of 2 to 5%. For both matrices, the detection limits, for all the elements, were in the range g g_-1 to ng g_-1.     

示差脉冲阳极溶出伏安法测定中药川附子痕量铅镉

本文报道了以ＨＮＯ３－ＨＣｌＯ４湿法消化、醋酸盐介质法差脉冲阳极溶出伏安法测定中药川附子中的铅镉。样品中铅镉含量分别在０．２－０．４μｇ．ｇ＾－１、０．０３－０．１６μｇ．ｇ＾－１,回收率９０－１１０％。     

Electrochemical determination of methyl parathion using a modified electrode

Electrochemical studies of pesticides using various electrode systems attain prominence in recent years because of their application in trace determinations. Cyclic voltammetric studies of methyl parathion on a glassy carbon electrode at various pH in 50% aqueous ethanol medium were carried out. Influence of pH led to the selection of pH 1.0 as the best pH for the electroanalysis of methyl parathion. The number of electrons transferred was determined using controlled potential coulometry. On the basis of the results a probable reduction mechanism was proposed. Cyclic voltammetric studies of methyl parathion using polypyrrole deposited and sodium montmorillonite clay modified electrodes in the presence of cetyl trimethyl ammonium bromide were carried out. The clay-modified electrode and the reduction peak around ?0.2?V were selected for stripping analysis owing to their maximum current response. The experimental parameters were optimized using the differential pulse stripping mode. A calibration plot was made. The determination limit and standard deviations were arrived. The applicability of the method was also verified in a sample soil analysis.     

Analysis of heavy metals in ecstasy tablets by electrochemical methods

Trace amounts of heavy metals have been analysed by electrochemical techniques in ecstasy tablets obtained from different police seizures in Spain. Lead, cadmium, copper and zinc were determined by differential-pulse anodic stripping voltammetry at a hanging mercury drop electrode, whereas nickel and cobalt were determined by adsorptive differential-pulse cathodic stripping voltammetry from their dimethylglyoxime complexes, M(DMG)₂. The performance of the procedure was compared with electrothermal atomic absorption spectrometry. The procedure was applied to the determination of these elements in nine ecstasy samples, finding that Zn is the element present in the highest concentration, ranging from 0.3 to 200?mg?kg^?1, Ni, Cu appear below 15?mg?kg^?1 and Pb below 8?mg?kg^?1, while Cd and Co levels were always lower than 0.51?mg?kg^?1.     

微氧环境中电化学活性微生物的分离与鉴定

电化学活性微生物在金属、碳等元素的生物地球化学循环,以及生物能源合成中具有重要作用.与微生物燃料电池厌氧阳极相比,微氧阳极能够捕集更多电能.但是相比于厌氧阳极中功能微生物的广泛研究,微氧阳极中的功能微生物还未被分离和研究.本研究采用传统好氧分离技术从微生物燃料电池微氧阳极分离获得3株纯菌Aeromonas sp.WS-XY2、Citrobacter sp.WS-XY3和Bacterium strain WS-XY4,其中WS-XY2和WS-XY3属于变形菌门,WS-XY4初步鉴定为新种.循环伏安、计时电流结果表明3株菌均具有电化学活性,且具有相似的直接胞外电子传递机制.3株菌在微生物分类学和电化学性质上的异同,表明微氧阳极能够定向筛选具有相似电化学性质的电化学活性微生物.微生物燃料电池微氧阳极具有更高效多样的功能微生物,可能是微氧阳极性能优于厌氧阳极的一个原因.因此,进一步针对微生物燃料电池微氧阳极中功能微生物的研究,将有助于阐明微氧阳极提高微生物燃料电池电能捕集的微生物机制.     

Electrocatalytic reduction of ortho nitrobenzaldehyde using modified aluminum electrode and its determination

A simple, cost effective and rapid electrochemical method has been developed for the determination of micro level ortho nitrobenzaldehyde（ONB） based on outstanding properties of modified aluminum electrode tin nanorods/anodic aluminum oxide/aluminum（SnNR/AAO/Al） for the first time. The SnNR/AAO/Al electrode was fabricated by a second step anodization, followed by electrodeposition and its electrochemical behavior was investigated in detail. The cyclic voltammetry results indicated that the SnNR/AAO/Al electrode exhibited efficient electrocatalytic activity toward reduction of ONB in the acidic solution. It provides an appreciable improvement of reduction peak for ONB at-0.721 V.Furthermore, various kinetic parameters such as transfer electron number, transfer proton number and standard heterogeneous rate constant were calculated from the scan rates.The electrocatalytic behavior was further exploited as a sensitive detection scheme for the ONB determination by differential pulse voltammetry. Under the optimized conditions, the concentration range and detection limit are 0.1-100 μmol/L and 0.05 μmol/L, respectively,for ONB. The analytical performance of this modified sensor has been evaluated for detection of real sample such as river water and recovery of ONB was achieved all-out up to102.3% under standard addition method.     

基于电聚合作用的脂质体免疫传感器检测水体中毒莠定的实验研究

利用脂质体包埋亚铁氰化钾,通过戊二醛交联毒莠定兔抗制成免疫脂质体,开发快速检测水中毒莠定的夹心型免疫传感器.在修饰电极的成分等方面优化传感器的工作参数,确定了Nation、多壁碳纳米管(multiwalled carbon nanotubes, MWCNTs)和毒莠定兔抗浓度的最优值分别为0.5%、10mg·mL-1、50μg·mL-1.免疫传感器的制作及测定过程如下:采用循环伏安法促使3,4-乙烯二氧噻吩(3,4-ethylendioxythiophene, EDOT)发生电聚合作用,将毒莠定兔抗直接固定到被修饰的玻碳电极上,电极再依次与待测水样和毒莠定兔抗修饰的免疫脂质体培育一定时间,最后利用TfitonX-100溶解与抗原结合的免疫脂质体,采用方波伏安法检测还原电流以反映毒莠定浓度,整个检测过程可以在70rain内完成.在0.1 mol·-1,的H3PO4中浸泡5 rain,可实现该传感器的良好再生.结果表明,毒莠定的检测下限达到了10-10mol·L-1,线性区间为10-10～10-4mol·L-1,适合饮用水中毒莠定浓度的检测要求.     

水环境中溶解态腐殖酸对锌抗甲状腺激素干扰效应的影响

本文以重金属锌为研究对象,应用重组人甲状腺激素受体(h TR)基因酵母快速测试方法,检测溶解态腐殖酸对锌抗甲状腺激素干扰效应的影响,利用阳极溶出伏安法(ASV)检测溶解态腐殖酸与锌作用后,生物有效态锌含量的变化,同时利用三维荧光光谱中的激发-发射矩阵(3DEEM)技术初步考察腐殖酸与锌的作用机制.结果表明,氯化锌具有显著的抗甲状腺激素干扰效应,其RIC20(抑制率为20%时氯化锌的浓度)值为1.70×10-5mol·L~(-1),当腐殖酸与氯化锌作用后,其抗甲状腺激素干扰效应降低了30%~50%,ASV测试结果表明当腐殖酸和氯化锌溶液混合后,生物有效态锌含量明显降低,与生物测试结果相似;紫外照射腐殖酸与氯化锌的混合体系后,其抗甲状腺激素干扰效应上升,但仍低于未加腐殖酸氯化锌溶液的抗甲状腺激素干扰效应值;3DEEM的测试结果表明氯化锌能够降低腐殖酸荧光峰的荧光强度,能够直观地表征腐殖酸与氯化锌相互作用.上述结果可为研究环境水体中锌的生物毒性及锌水质基准的制定提供基础数据和理论支持.     

三维粒子电极处理染料废水的效能及机制

以自制的负载Sb掺杂SnO2的陶瓷颗粒为粒子电极,构建三维电极体系,对其处理活性艳红X-3B废水的效能进行研究,并借助于循环伏安曲线、羟基自由基的荧光光谱检测技术对三维粒子电极体系的电催化氧化机制进行研究。结果表明,优化槽电压为13 V,处理时间为60 min时,三维电极体系对活性艳红X-3B废水的COD去除率和相应能耗分别为85.6%与16.8 kW·h/(kg COD),与二维电极体系相比COD去除率提高了32.9%,能耗降低了33.3%。UV-Vis吸收光谱分析表明电催化氧化技术可以破坏活性艳红X-3B分子中的偶氮键、苯环和萘环,将大分子降解为小分子。电催化氧化机制研究表明,在本实验条件下三维电极主要通过间接氧化而不是直接氧化提高电催化氧化效能,即在三维粒子电极体系中羟基自由基的产生量多于二维电极体系,从而实现高效低耗处理活性艳红X-3B废水。