The Simultaneous Determination of Cu Pb Cd and Sb by Derivative Adsorption Chronopotentiometry

The behaviour of the complexes of copper,lead,cadmium and antimony with salicylfluorone(SAF)adsorbed on HMDE has been investigated by derivative chrono potentiometry in NH3/NH4C1.The dependence of the peak height on the dt/dE vs E curve on preconcentration time,the pH of solution and the constant reducing current are discussed.This method achieved the simultaneous determination of copper,lead,cadmium and antimony in human hair.     

Individual and Simultaneous Voltammetric Determination of Cd(II), Cu(II) and Pb(II) Applying Amino Functionalized Fe3O4@Carbon Microspheres Modified Electrode

Amino‐functionalized Fe₃O₄@carbon microspheres (NH₂?Fe₃O₄@C) were prepared and the electrochemical sensor was constructed using NH₂?Fe₃O₄@C modified glassy carbon electrodes (GCE) to determine toxic heavy metals in aqueous solution. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the structure and phase of NH₂?Fe₃O₄@C. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) results indicate that NH₂?Fe₃O₄@C modified GCE possesses large active area and excellent electron transfer. Under optimized electrochemical condition, Cd(II), Pb(II) and Cu(II) were determined using NH₂?Fe₃O₄@C modified GCE. The electrode through amino functionalization exhibits higher sensitivity and lower detection limit toward Cd(II) and Cu(II) due to the acid‐base pairing interaction between the electron‐rich ?NH₂ ligand and the electron‐deficient heavy metal ions. Compared with other similar results reported in the literature, the NH₂?Fe₃O₄@C modified electrode exhibits wider linear response range while with comparable lower detection limit. It also exhibits excellent stability, reproducibility and anti‐interference ability.     

改性磁性壳聚糖微球对Cu2+、Cd2+和Ni2+的吸附性能

Fe3O4/ chitosan magnetic microspheres of 50 to 80 滋m were prepared using the inverse phase emulsion dispersion and chemical crosslinking technology, and then modified with ethylenediamine for use in the adsorption of heavy metal ions. The adsorption properties of the modified Fe3O4/chitosan toward Cu2+, Cd2+ and Ni2+ were investigated. It was found that the adsorption capacities of Cu2+ and Ni2+ increased with pH, and a maximum adsorption for Cd2+ occurred at pH=3. The saturated adsorption capacities calculated by Langmuir isotherms were 54.3 mg·g-1 for Cu2+, 20.4 mg·g-1 for Cd2+, and 12.4 mg·g-1 for Ni2+, respectively. The adsorption kinetics were well described by pseudo-second-order equation models. The experimental results showed that the Fe3O4/chitosan modified with ethylenediamine presented higher adsorption selectivity for Cu2+ than for Cd2+ and Ni2+ in all studied pH ranges.     

反相高效液相色谱法同时测定镉、铅、铜和锌

 研究了meso-四（对羟基苯基）卟啉为柱前衍生化试剂与Cd2+,Pb2+,Cu2+和Zn2+离子的配合反应条件及配合物在C18色谱柱上的分离条件,建立了反相高效液相色谱快速分离光度检测Cd2+,Pb2+,Cu2+和Zn2+的新方法。配合物和试剂在15 min内出峰完毕。4种离子的检出限为: Cd2+0.02 ng,Pb2+0.02 ng, Cu2+0.02 ng,Zn2+0.12 ng;线性范围为:Cd2+0.8 μg/L～150 μg/L,Pb2+0.8 μg/L～300 μg/L,Cu2+0.8 μg/L～500 μg/L,Zn2+5.0 μg/L～1 000 μg/L;方法的日内相对标准偏差为:2.8%～4.8%,测定低、中、高3个浓度的日间相对标准偏差为3.7%～9.7%。     

Simultaneous determination of Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+ by using second-derivative spectrophotometry method

A new method of simultaneous determination of Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+ is proposed here by using the second-derivative spectrophotometry method. In pH=10.35 Borax-NaOH buffer, using meso-tetra (3-methoxyl-4-hydroxylphenyl) porphyrin ([T-(3-MO-4-HP)P]) as chromomeric reagent, micelle solution was formed after Tween-80 surfactant was added into the solution containing Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+ ions. The original absorption spectrum of the above complexes was obtained after heating in the boiling water for 25 min. The second-derivative absorption peaks of five metal-porphyrin complexes can be separated from the original absorption spectrum by using chemometric tool. In this way, Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+ ions can be determined simultaneously. Under the optimal conditions, the linear ranges of the calibration curve were 0-0.60, 0-0.60, 0-0.40, 0-0.80 and 0-0.48 μg mL(-1) for Cu2+, Zn2+, Cd2+, Hg2+ and Pb2+, respectively. The molar absorptivity of these color systems were 1.38×10(5), 1.01×10(5), 3.24×10(5), 1.07×10(5) and 1.29×10(5)Lmol(-1)cm(-1). The method developed in this paper has advantages in selectivity, sensitivity, operation and can effectively resolve spectra overlapping problem. This method has been applied to determine the real samples with satisfactory results.     

Enhancing Removal of Cr(VI), Pb2+, and Cu2+ from Aqueous Solutions Using Amino-Functionalized Cellulose Nanocrystal

In this work, the amino-functionalized cellulose nanocrystal (ACNC) was prepared using a green route and applied as a biosorbent for adsorption of Cr(VI), Pb²⁺, and Cu²⁺ from aqueous solutions. CNC was firstly oxidized by sodium periodate to yield the dialdehyde nanocellulose (DACNC). Then, DACNC reacted with diethylenetriamine (DETA) to obtain amino-functionalized nanocellulose (ACNC) through a Schiff base reaction. The properties of DACNC and ACNC were characterized by using elemental analysis, Fourier transform infrared spectroscopy (FT-IR), Kaiser test, atomic force microscopy (AFM), X-ray diffraction (XRD), and zeta potential measurement. The presence of free amino groups was evidenced by the FT-IR results and Kaiser test. ACNCs exhibited an amphoteric nature with isoelectric points between pH 8 and 9. After the chemical modification, the cellulose I polymorph of nanocellulose remained, while the crystallinity decreased. The adsorption behavior of ACNC was investigated for the removal of Cr(VI), Pb²⁺, and Cu²⁺ in aqueous solutions. The maximum adsorption capacities were obtained at pH 2 for Cr(VI) and pH 6 for Cu²⁺ and Pb²⁺, respectively. The adsorption all followed pseudo second-order kinetics and Sips adsorption isotherms. The estimated adsorption capacities for Cr(VI), Pb²⁺, and Cu²⁺ were 70.503, 54.115, and 49.600 mg/g, respectively.     

Fabrication of SPR Nanosensor Using Gold Nanoparticles and Self-Assembled Monolayer Technique for Detection of Cu2+ in an Aqueous Solution

In this work, we investigated the fabrication of surface plasmon resonance (SPR) nanosensor using gold nanoparticles (AuNPs) chemisorbed onto self assembled monolayer of 10-(3-amino phenoxy) decane-1-thiol on gold substrate. The fabrication process of SPR nanosensor was characterized using different techniques such as infrared reflection-absorption spectra (IRRAS), xX-ray photoelectron spectroscopy (XPS), and atomic force microscope (AFM). The fabricated SPR nanosensor was used for detection of Cu²⁺ in an aqueous solution using surface plasmon resonance refractometer. The results confirm the fabrication of new SPR nanosensor. The fabricated SPR nanosensor showed a good activity toward the detection of Cu²⁺. The detection of Cu²⁺ in an aqueous solution using the fabricated SPR nansensor was enhanced in the presence of gold nanoparticles.     

Simultaneous determination of speciation parameters of Cu,Pb, Cd and Zn in model solutions of Suwannee River fulvic acid by pseudopolarography

There is a growing awareness of the importance of quantitative determinations of speciation parameters of the trace metals Cu, Zn, Cd and Pb in aqueous samples containing chemically heterogeneous humic substances, especially when they are present together, interacting with one another and competing for specific binding sites of the humic substances. Such determinations require fundamental knowledge and understanding of these complex interactions, gained through basic laboratory-based studies of well-characterized humic substances in model solutions. Since the chemical heterogeneity of humic substances plays an important role in the thermodynamics (stability) and kinetics (lability) of trace metal competition for humic substances, a metal speciation technique such as pseudopolarography that can reveal the special, distinctive nature of metal complexation is required, and it was therefore used in this study. A comparison of the heterogeneity parameters (Gamma) for Zn(II), Cd(II), Pb(II) and Cu(II) complexes in model solutions of Suwannee River fulvic acid (SRFA) shows that GammaCd>GammaZn>GammaPb>GammaCu, suggesting that SRFA behaves as a relatively homogeneous complexant for Zn(II) and Cd(II), whereas it behaves as a relatively heterogeneous complexant for Pb(II) and an even more heterogeneous complexant for Cu(II) under the experimental conditions used. The order of values of log K* (from the differential equilibrium function, DEF) for the trace metals at pH 5.0 follow the sequence: log K*Cu>log K*Pb>log K*Zn>log K*Cd. These results are in good agreement with the literature values. The results of this work suggest the possibility of simultaneously determining several metals in a sample in a single experiment, and hence in a shorter time than required for multiple experiments.     

Thiourea Based Dipodal Receptor Development for Electrochemical Detection of Br− Ion in an Aqueous Medium

Thiourea based dipodal receptor ( R1 ) was developed and characterised using ¹H NMR, ¹³C NMR and mass spectroscopy. Using re‐precipitation method, R1 was processed into organic nanoparticles ( N1 ), evaluated its sensor activity in aqueous medium. The prepared N1 were characterized using Transmission Electron Microscopy (TEM) which shows 30 nm size. Dynamic Light Scattering (DLS) was employed for calculating average particle size. To imply N1 as sensor, its interaction with various anions was studied and found reasonable selectively for Br^? ions with detection limit of 3.79 nM. For real life analysis, involving determining Br^? from environmental samples, proposed sensor works successfully with accuracy more than 95 %.     

双硫腙修饰玻碳电极阳极溶出伏安法测定痕量镉和铅

报道了双硫腙修饰玻碳电极同时测定痕量镉和铅的电分析方法。镉和铅离子通过与电极表面的双硫腙发生螯合作用而富集在电极表面 ,同时在 -1 .2 0V(vs.SCE)还原成零价镉和铅 ,当电极电势从 -1 .2 0V向 -0 .3 0V扫描时 ,被还原的镉和铅从电极表面溶出 ,分别于 -0 .78V和 -0 .4 8V左右形成灵敏的阳极溶出峰。优化了支持电解质及pH值、双硫腙用量、富集电位及时间等实验参数。利用该修饰电极测定镉、铅的线性范围分别为 1 .0×1 0 - 8～ 2 .5× 1 0 - 6 mol L和 5 .0× 1 0 - 9～ 2 .5× 1 0 - 6 mol L。检测限分别为 5 .0× 1 0 - 9mol L和7.0× 1 0 - 1 0 mol L。该法用于实际水样中镉和铅的测定 ,平均回收率分别为 99.3 0 %和 99.5 4 %。     

The Simultaneous Determination of Cu Ph Cd and Sb by Derivative Adsorption Chronopotentiometry

Anodic stripping voltammetry (ASV) is an effective electroanalytical technique for themeasurement of trace metal ions. But there are serious interferences due to overlappingstripping peaks and forming of intermetallic complex in complicated system. The peak ofcopper (ASV) is close to that of mercury. So the result of determination of copper is notsatisfactory. Adsorption chronopotentiometry was reported by H.Eskilsson et al i. In thismethod, instead of electrolytic accumulation of metal io…     

Voltammetric Determination of Pb(II) and Cd(II) Ions in Well Water Using a Sputtered Bismuth Screen‐Printed Electrode

A method using commercially available sputtered bismuth screen‐printed electrodes (Bi_spSPE), as substitute to mercury electrodes, for the determination of trace Pb(II) and Cd(II) ions in drinking well water samples collected in a contaminated area in The Republic of El Salvador by means of differential pulse anodic stripping voltammetry (DPASV) has been proposed. The comparable detection and quantification limits obtained for both Bi_spSPE and hanging mercury drop electrode (HMDE), together with the similar results with a high reproducibility obtained in these water samples analyses recommend the applicability of Bi_spSPE for the determination of low level of metal concentrations in natural samples.     

Voltammetric Determination of Hesperidin on the Electrode Modified with SnO2 Nanoparticles and Surfactants

Highly sensitive voltammetric method for hesperidin determination is developed using glassy carbon electrode modified with SnO₂ nanoparticles (SnO₂ NPs) and surfactants. The highest oxidation currents of hesperidin are observed in the case of cationic 0.50 mM cetylpyridinium bromide (CPB). Parameters of hesperidin electrooxidation have been calculated. Adsorptive anodic differential pulse voltammetry (AdADPV) in phosphate buffer pH 7.0 after 120 s accumulation provides linear dynamic ranges of 0.10–10 and 10–75 μM with the detection limit of 0.077 μM. The selectivity of hesperidin response is proved in the presence of inorganic ions, saccharides, ascorbic acid and other natural phenolics.     

Simultaneous determination of Co, Ni, Cu and Zn ions in foodstuffs and vegetables with a new Schiff base using artificial neural networks

New complexes of Co²⁺, Ni²⁺, Cu²⁺ and Zn²⁺ with a recently synthesized Schiff base derived from 3,6-bis((aminoethyl)thio)pyridazine were applied for their simultaneous determination with artificial neural networks. The analytical data show the ratio of metal to ligand in all metal complexes is 1:1. The absorption spectra were evaluated with respect to Schiff base concentration, pH and time of the color formation reactions. It was found that at pH 10.0 and 60 min after mixing, the complexation reactions are completed and the colored complexes exhibited absorption bands in the wavelength range 300-500 nm. Spectral data was reduced using principal component analysis and subjected to artificial neural networks. The data obtained from synthetic mixtures of four metal ions were processed by principal component-feed forward neural networks (PCFFNNs) and principal component-radial basis function networks (PCRBFNs). Performances of the proposed methods were tested with regard to root mean square errors of prediction (RMSEP%), using synthetic solutions. Under the working conditions, the proposed methods were successfully applied to simultaneous determination of Co²⁺, Ni²⁺, Cu²⁺ and Zn²⁺ in different vegetable, foodstuff and pharmaceutical product samples.     

基于未修饰纳米金及无标记单链DNA的Pb~(2+)比色测定

根据纳米金对ss DNA和G-四联体结构的DNA的不同吸附能力,设计了一种简单的Pb2+比色传感器。富含G的无标记ss DNA可以通过静电作用吸附于Au NPs表面,保护Au NPs在高盐浓度溶液中仍呈分散态;当Pb2+存在时,DNA与Pb2+结合形成Pb2+-G-四联体结构,使得Au NPs失去DNA的保护而发生聚集,溶液颜色由红色变成蓝色,最大吸收峰发生红移。通过优化条件,得到溶液吸光度比值(A630/A520)与Pb2+浓度在0.1~10μmol/L范围内呈良好的线性关系,检出限可达50 nmol/L。其他金属离子对Pb2+的检测几乎无干扰。该方法灵敏度高,选择性好,且无需复杂的Au NPs表面修饰过程及DNA标记,制备和操作简便、成本低、响应快(1 min),非常适合于现场实时应用。     

Preparation of Activated Carbon From Olive Stone Waste: Optimization Study on the Removal of Cu2+, Cd2+, Ni2+, Pb2+, Fe2+, and Zn2+ from Aqueous Solution Using Response Surface Methodology

The removal efficiencies of Cu²⁺, Cd²⁺, Ni²⁺, Pb²⁺, Fe²⁺, and Zn²⁺ from aqueous solution with olive stone activated carbon (OSAC) were investigated in this paper. Central composite design method was used to optimize the preparation of OSAC by chemical activation using potassium hydroxide (KOH) as chemical agent. The optimum conditions obtained were 715°C activation temperature, 2 hours activation time, and 1.53 impregnation ratio. This resulted in removal of 99.25% Cu²⁺, 94.98% Cd²⁺, 99.08% Ni²⁺, 99.33% Pb²⁺, 99.41% Fe²⁺, and 99.17% Zn²⁺, as well as 73.94% OSAC yield. The surface characteristics of the activated carbon (AC) prepared under optimized condition were examined by pore structure analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy. The Brunauer–Emmett–Teller (BET) surface area, total pore volume, and average pore diameter of the prepared activated carbon were 886.72 m²/g, 0.507 cm³/g, and 4.22 nm, respectively. The equilibrium data of the adsorption was well fitted to the Langmuir and the highest value of adsorption capacity (Q) on the OSAC was found for Fe²⁺ (57.47 mg/g), followed by Pb²⁺ (22.37 mg/g), Cu²⁺ (17.83 mg/g), Zn²⁺ (11.14 mg/g), Ni²⁺ (8.42 mg/g), and Cd²⁺ (7.80 mg/g). The prepared OSAC can be used for efficient removal of metals from contaminated wastewater.     

Simultaneous Voltammetric Determination of Cd2+ and Pb2+ in Gasoline Samples Employing a Chemically Modified Acrylonitrile-Butadiene-Styrene (ABS) Composite Electrode

A composite electrode based on acrylonitrile-butadiene-styrene and graphite chemically modified with a bismuth film (AGCE-BiF) was applied for the simultaneous determination of Cd²⁺ and Pb²⁺ in gasoline samples. Extraction induced by microemulsion breaking (EIMB) was used for the first time in the preparation of the samples for electroanalysis. AGCE-BiF was characterized by SEM, AFM, CV, and SWASV. The sensor showed an increase in sensitivity via in situ modification with bismuth film. The LOD was 4 μg L⁻¹ for Cd²⁺ and 2 μg L⁻¹ for Pb²⁺. The results showed satisfactory recoveries and precision, being statistically compatible to those obtained with FAAS.     

Voltammetric Determination of Pb,Cu and Hg in Biodiesel Using Gold Screen‐printed Electrode: Comparison of Batch‐injection Analysis with Conventional Electrochemical Systems

This article compares the use of batch‐injection analysis (BIA) with a conventional batch system for the anodic stripping voltammetric (ASV) determination of Pb, Cu and Hg in biodiesel using screen‐printed gold electrode (SPGE). The optimized BIA conditions were 200 µL of injection volume of the digested samples at 5 µL s^?1 directly on the working electrode of the SPGE immersed in 0.1 mol L^?1 HCl solution. Therefore, BIA‐ASV presented the advantages of low sample consumption, which extended the SPGE lifetime to a whole working day of analyses, and potential for on‐site analysis using battery‐powered micropipettes and potentiostats. Although presenting lower sensitivity than conventional systems, the BIA‐ASV presented detection limit values of 1.0, 0.5 and 0.7 µg L^?1, respectively for Pb, Cu and Hg, a linear range between 20 and 280 µg L^?1, and adequate recovery values (90–110 %) for spiked biodiesel samples.     

Preparation of PbS Nanoparticles by Phase-Transfer Method and Application to Pb2+-Selective Electrode Based on PVC Membrane

Abstract

A novel approach to prepare homogeneous PbS nanoparticles by phase-transfer method was developed. The preparatory conditions were studied in detail, and the nanoparticles were characterized by transmission electron microscopy (TEM) and UV-vis spectroscopy. Then a novel lead ion-selective electrode of polyvinyl chloride (PVC) membrane based on these lead sulfide nanoparticles was prepared, and the optimum ratio of components in the membrane was determined. The results indicated that the sensor exhibited a wide concentration range of 1.0 × 10^?5 to 1.0 × 10^?2 mol·L^?1. The response time of the electrode was about 10 s, and the optimal pH in which the electrode could be used was from 3.0 to 7.0. Selectivity coefficients indicated that the electrode was selective to the primary ion over the interfering ion. The electrode can be used for at least 3 months without any divergence in potential. It was successfully applied to directly determine lead ions in solution and used as an indicator electrode in potentiometric titration of lead ions with EDTA.     

杨树嫩茎质外体微透析液中K+,Na+,Ca2+的分析

采用微透析法获取3种杨树嫩茎质外体汁液的灌流液,流速1μL/min,探针截留分子量为30 kDa,无须处理直接通过原子吸收光谱(石墨炉法)测定样品中Na+,K+,Ca2+浓度,通过建立实时、无损检测离子浓度变化的实验技术,进行杨树生理生化的研究。此方法加标回收率在95.8%~103.1%之间。研究表明,吴屯杨、小胡杨和小美旱的Na+含量分别为1034~1156μg/L,1493~1611μg/L和1586~1703μg/L;K+含量分别为1012~1237μg/L,941~964μg/L和1095~1201μg/L;Ca2+含量分别为4976~5237μg/L,4786~5042μg/L和5893~6142μg/L,本方法为在植物应激反应中通过离子浓度变化来适应外界环境的研究提供可靠数据。