Ordered Mesoporous Carbon and Thiolated Polyaniline Modified Electrode for Simultaneous Determination of Cadmium(II) and Lead(II) by Anodic Stripping Voltammetry

The fabrication and evaluation of a glassy carbon electrode (GCE) modified with ordered mesoporous carbon (OMC), 2‐mercaptoethanesulfonate (MES)‐tethered polyaniline (PANI) and bismuth for simultaneous determination of trace Cd²⁺ and Pb²⁺ by differential pulse anodic stripping voltammetry (DPASV) are presented here. The morphology and electrochemical properties of the fabricated electrode were respectively characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). Experimental parameters such as PANI disposition, preconcentration potential, preconcentration time and bismuth concentration were optimized. Under optimum conditions, the fabricated electrode exhibited linear calibration curves ranged from 1 to 120 nM for Cd²⁺ and Pb²⁺. The limits of detection (LOD) were 0.26 nM for Cd²⁺ and 0.16 nM for Pb²⁺ (S/N=3), respectively. Additionally, repeatability, reproducibility, interference and application were also investigated, and the proposed electrode exhibited excellent performance. The proposed method could be extended for the development of other new sensors for heavy metal determination.     

铅镉重金属离子在铋膜电极上的相互影响

采用原位镀铋电极的方式,以玻碳电极为工作电极,通过改变Cd2+和Pb2+的比例,考察不同Pb2+和Cd2+浓度条件下,两者同时存在时的相互影响。实验发现,Cd2+和Pb2+同时存在时,存在相互的影响,特别是对于Cd2+的检测,由于Pb2+较正的析出电位,对于Cd2+的析出有一定的辅助作用。考察了Cd2+和Pb2+单独存在时的分析性能,Pb2+沉积时间为60 s时,在1~80μg/L范围内呈线性关系,检出限为0.5μg/L;Cd2+的沉积时间为120 s,在1~25μg/L和30~200μg/L范围内有良好的线性关系,检出限为1.0μg/L。考察了铋膜电极在不同实际水样中对Pb2+和Cd2+的分析,获得了较好的一致性。     

Controlled aging of PbS colloidal quantum dots under mild conditions

A new controlled aging methodology was developed for the synthesis of PbS colloidal quantum dots (QDs), applying larger PbS QDs as a starting material for smaller QDs by application of environmentally friendly oleic acid and oleylamine as reagents. This simple and mild procedure provides a possible strategy for tailoring the size-dependent properties of PbS QDs.     

Bioinspired synthesis of pure massicot phase lead oxide nanoparticles and assessment of their biocompatibility,cytotoxicity and in-vitro biological properties

Green and ecofriendly route for biosynthesis of lead oxide nanoparticles has been successfully demonstrated using aqueous leaf extracts of Sageretia thea (Osbeck.). Biosynthesized PbO (∼27 nm) nanoparticles were extensively characterized using XRD, FTIR, Raman, EDS etc. Morphology was studied through HR-TEM/SEM. As synthesized nanoparticles were investigated for their iv-vitro biological properties. Antibacterial activities revealed enhancement upon modulation by UV in a concentration dependent manner. Pseudomonas aeruginosa was found to be the most resistant strain (MIC = 250 µg/mL and MIC^uv = 31.25 µg/ml). MTT cytotoxicity on leishmania promastigotes and amastigotes revealed significant inhibition as indicated by their IC₅₀ values of 14.7 µg/mL and 11.95 µg/m respectively. Cytotoxicity was also confirmed using brine shrimp lethality (IC₅₀ = 27.7 µg/mL). Bio-compatibility evaluation indicated cytotoxicity to freshly isolated human macrophages (IC₅₀ = 57.1 µg/mL). Insignificant alpha-amylase inhibition and moderate protein kinase inhibition was revealed. Antioxidant activities indicated free radical scavenging activity (58 ± 2.45) at 200 µg/mL. Moderate total reducing power and total antioxidant activity was also indicated. Overall, we conclude lead oxide as a potential candidate for biological applications, however further studies are recommended on their in vitro and in vivo cytotoxicity.     

Electrochemical behavior of PbO2/PbSO4 electrode in the presence of surfactants in electrolyte

The electrochemical behavior of PbO₂/PbSO₄ electrode is investigated in 4.5 M H₂SO₄ in presence of three surfactants, Sodium Dodecyl Sulfate (SDS), Cetyltrimethylammonium bromide (CTAB) and Sodium tripolyphosphate (STPP), using cyclic voltametry, electrochemical spectroscopy impedance and galvanostatic discharge as techniques. The micro morphology of the surface of the modified PbO₂ electrodes is examined by scanning electron microscopy. The results show that SDS and CTAB when added in the electrolyte could refine the coating particles and change the roughness of the surface of the electrode leading to a thin film of PbO₂ with amorphous character. In addition, SDS and CTAB shift the hydrogen evolution potential towards more negative values, improve the discharge capacity of the anodic layer and accelerate the charge transfer. Under cathodic polarization, CTAB presents the lowest value of the charge transfer resistance R_ct. In the contrary, STPP shifts the oxygen evolution potential towards more positive values, passivates the surface of the electrode and inhibits completely the reaction of PbO₂ formation.     

Efficiency of Acacia Gummifera powder as biosorbent for simultaneous decontamination of water polluted with metals

Biosorbent materials represent an interesting alternative to classic methods of metal removal from industrial effluents. Acacia biomass showed a higher absorption capacity for heavy metals than living biomass. This study aimed to evaluate the bioadsorption of Lead and Cadmium onto Acacia Gummifera gum, using batch experiment. The structural characterization of the biosorbent was carried out using FT-IR, SEM, BET, TGA and DSC analysis. The adsorption equilibrium was reached within 15 min. A maximum uptake of 18.3 mg.g⁻¹ Pb²⁺ and 9.57 mg.g⁻¹ Cd²⁺ was achieved at pH 6.5. The metal ions seemed to be removed exclusively by ion exchange, physical sorption and chelation. The biomass of A. Gummifera powder was found to be effective for lead and cadmium removal with respectively 97% and 86% sorption efficiency at a concentration of 100 mg/L, in aqueous media. Parameters affecting adsorption capacities such as biosorbent dosage, initial metal concentration, temperature, and pH are discussed in detail. Furthermore, adsorption thermodynamics, kinetics, and equilibrium were studied and fitted by different models. Langmuir, Freundlich, Temkin and Dubinin–Radushkevich isotherms were used to compare adsorption data at equilibrium. The adsorption kinetics data were found to be best fitted by the pseudo-second-order model, and the adsorption isotherm was well fitted with the Langmuir model. The calculated thermodynamic parameters (ΔG⁰, ΔS⁰ and ΔH⁰) indicated a spontaneous and exothermic biosorption of both metal ions onto Acacia Gummifera. Moreover, chromatograms obtained by size exclusion chromatography coupled with multi-angle laser light scattering detection system (SECMALLS) showed the formation of complexes between the arabinogalactan-peptide (AGP) and glycoprotein (GP) Acacia moieties and the two studied metal ions. The analysis of the FTIR spectra of dried Acacia and that of Acacia loaded with lead and cadmium in aqueous media suggests that the surface functional groups such as amides and carboxy groups might be involved in the metal removal process.The extent of adsorption for both metals increased along with an increase of the A. Gummifera biomass dosage. A. Gummifera biomass, which is safe, of low-cost, and highly selective, seems therefore to be a promising substrate for simultaneous trapping of Pd and Cd ions in aqueous solutions.     

微波辅助消解-原子荧光法测定玻璃中的镉砷铅

光学玻璃中的各种元素对玻璃的光学性能有不同的影响。如加入镉可以提高玻璃折射率;砷的引入能增加玻璃的透光度,含铅玻璃具有低成本、高折射性等优点。但是镉、砷、铅均为有毒元素,玻璃加工和处理过程以及毒废弃物的处理都可能引起水、土壤、大气的污染并给人体带来一定的危害     

铋膜电极微分电位溶出法测定生物材料中痕量铅

研究了镀铋膜电极替代镀汞膜电极痕量铅的微分电位溶出分析法(DPSA)。考察并优化了同位镀铋膜测定铅的条件。结果表明,在HAc-NaAc(pH=4.4)介质中,铅可在镀铋膜电极上得到灵敏的微分电位溶出峰;利用标准加入法对人尿及血中痕量铅进行了测定。本法避免了镀汞膜电极对人体健康及环境的危害。     

原子吸收光谱法测定铅蓄电池板栅中锡、钙和铝

通过先加酒石酸、硝酸溶解样品,用氧化镧、EDTA联合掩蔽铝来测定钙,盐酸沉淀铅后测锡、铝的试验,采用火焰原子吸收光谱法测定锡、钙和铝.     

石墨炉原子吸收光谱法测定鼠肝脏中的铅

采用2mg/mL磷酸二氢铵-1mg/mL硝酸镁作为混合基体改进剂,电热石墨炉原子化系统和氘灯扣背景校正的原子吸收光谱仪测定鼠肝脏中的痕量铅.结果表明铅在0-100ng/mL呈良好线性关系,r=0.9994,平均回收率为97.6%,RSD=2.6%,检出限为0.40ng/mL.方法操作简便,重现性好、灵敏度高且结果准确.