Comparison of masking agents for antimony speciation analysis using hydride generation atomic fluorescence spectrometry

A sensitive atomic spectrometric method for the redox speciation analysis of Sb in water is described. The proposed method is based on the selective generation of stibine from Sb(III) in a continuous flow system using non-dispersive atomic fluorescence spectrometry for detection. The effects of the HCl concentration on the fluorescence intensities of Sb(III) and Sb(V) were investigated. The results indicated that atomic fluorescence emission due to Sb(V) can constructively interfere with the determination of Sb(III). For the determination of Sb(III), four compounds were tested as masking agents to inhibit the generation of stibine from Sb(V). The effects of the concentrations of the masking agents and of HCl on the fluorescence signals from Sb(III) and Sb(V) were studied. The results indicated that citric acid and NaF can successfully suppress hydride generation from Sb(V). To evaluate the developed methodology and the influence of the matrix, the recovery of Sb(III) from natural water that was spiked with different Sb(III) and Sb(V) concentrations was tested.     

Determination of Au(III) and Pd(II) ions by flame atomic absorption spectrometry in some environmental samples after solid phase extraction

A simple and sensitive solid phase extraction method was developed for simultaneous separation and preconcentration of gold and palladium ions with N-(4-methylphenyl)-2-{[(4-phenyl-5-pyridine-4-yl-4H-1,2,4-triazol-3-yl)thio]acetyl}hydrazine carbo thioamide complex on Amberlite XAD-1180 resin before their determination by flame atomic absorption spectrometry. Some analytical parameters such as HNO₃ concentration of the sample solution, amount of complexing agent, sample volume, eluent type and volume, effects of foreign ions and adsorption capacity of the resin were investigated for quantitative recovery of gold and palladium ions. The effects of some anions and cations were also examined. Under optimum conditions, the detection limits for gold and palladium ions were found to be 0.29 and 0.19 μg L^?1, respectively. The preconcentration factor for gold and palladium was 250. After being validated by standard addition and analysis of standard reference material, the procedure was successfully applied to the analysis of sea and stream water, anodic slime, gold ore, soil and electronic waste.     

Ultrasound-assisted emulsification/microextraction based on solidification of trace amounts of thallium prior to graphite furnace atomic absorption spectrometry determination

In the present work, determination of ultratrace amounts of thallium in water samples was performed by ultrasound-assisted emulsification microextraction based on solidification of a floating organic drop as sample preparation method prior to furnace atomic absorption spectrometry. 1-(2-Pyridylazo)-2-naphthol was used as chelating agent. The factors influencing the complex formation and extraction, such as pH of the aqueous solution, the type and the volume of extraction solvent, the volume of chelating agent solution, and the extraction time were investigated. Under optimized conditions, the enrichment factor was 200. The calibration graph was linear from 0.2 to 10.0 μg L^?1 with a correlation coefficient of 0.9966, the detection limit was 0.03 μg L^?1 and reproducibility was ±3.3% (C = 5.0 μg L^?1, n = 8). The method was successfully applied for the determination of thallium in water samples.     

分散液液微萃取-石墨炉原子吸收光谱法测定环境水样中的痕量镉

建立了分散液液微萃取分离富集一石墨炉原子吸收光谱法测定环境水样中痕量镉的新方法。以二乙基二硫代氨基甲酸钠为螯合剂、四氯化碳为萃取剂、丙酮为分散剂,详细考察YpH值、螯合剂质量分数、萃取剂体积、萃取时间等因素的影响。在优化的实验条件下,方法对水样中镉的检出限为4．2ng-L^-1,线性范围是20-300ng-L^-1,测定结果的相对标准偏差为3．5％,富集倍数达103。将建立的方法应用于三种实际环境水样中镉的检测,加标回收率在92％-108％范围内。本方法具有灵敏、准确、快速、环保的特点,是一种分析水样中痕量镉的较好方法。     

Microwave-assisted acid extraction of the major metal elements in herbal extracts followed by flame atomic absorption spectrometric (FAAS) determination

The content of As, Cd, Cr, Cu, Fe, Hg, Mg, Mn, Pb, and Zn was determined in Rosa damascena, Vitis vinifera, Crocus sativus, and Olea europaea L. herbal extracts produced in different areas in Greece. Samples were mineralized in a closed microwave system using nitric acid, and the concentration of all metals was determined by flame atomic absorption spectrometry. The herbal extracts contained As, Cd, Cr, Hg, Mn, and Pb at concentrations below their respective limits of detection, whereas Cu, Fe, Mg, and Zn were determined in varying quantities. The proposed method is precise and accurate, thus it can be used for the determination of metals in Rosa damascena, Vitis vinifera, Crocus sativus, and Olea europaea L. herbal extracts.     

Synthesis of 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 resin: Applications for the separation and preconcentration of trace metal ions prior to their determination by inductively coupled plasma atomic emission spectrometry

A simple, sensitive column solid-phase extraction procedure for separation and preconcentration of Cu(II), Ni(II), Co(II), and Cd(II) in spiked and natural water samples using 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 (XAD-4-DHN) chelating resin prior to their determination by inductively coupled plasma atomic emission spectrometry was discussed. The optimum experimental parameters such as pH, volume of sample and eluent, flow-rates of uptake and stripping, and sorption capacity of the chelating resin, were evaluated. The effect of the electrolytes and the cations on the preconcentration of metal ions was also investigated. The chelating resin could be reused for more than 20 cycles of sorption–desorption without any significant change (<1.0%). Recoveries obtained from this method range from 96 to 102% with R.S.D of 2.50 (n = 4). The detection limits for Cu(II), Ni(II), Co(II), and Cd(II) were found to be 1.9, 0.9, 1.2 µg, and 1.4 µg L^?1, respectively. The proposed method was applied for the determination of Cu(II), Ni(II), Co(II), and Cd(II) in spiked, tap water, and river water samples.     

Cadmium and nickel determinations in some food and water samples by the combination of carrier element-free coprecipitation and flame atomic absorption spectrometry

A procedure for separation and enrichment of Cd(II) and Ni(II) ions based upon carrier element-free coprecipitation by using an organic coprecipitant, 2-{4-[2-(1H-Indol-3-yl)ethyl]-3-(4-methylbenzyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl}-N′-(3-fluoro-phenylmethyliden) acetohydrazide, prior to their flame atomic absorption spectrometric detections has been developed. The effects of varied experimental conditions on the performance of the developed method such as pH, sample volume, amount of coprecipitating agent, etc. were evaluated in detail on the recovery of analyte ions, and the influences of some anions and cations were investigated. The limits of detection for Cd(II) and Ni(II) ions based on three times the standard deviation of the blanks (N: 10) were obtained as 0.70 μg L^?1 and 1.21 μg L^?1, respectively. The accuracy of the method was tested by analyzing a certified reference material and by spike tests. The method was applied to determine the levels of cadmium and nickel in stream and sea water, rice, red lentil, and wheat samples.     

微波消解-原子荧光法测定染毒小鼠体内汞的分布

小鼠经腹腔注射氯化汞(HgCl2)染毒后,采用微波消解-原子荧光法研究汞在小鼠全血、脑、睾丸、脾、肝脏以及肾脏的分布情况.结果表明,方法的检出限为0.002μg.L-1,加标回收率为92.12%—108.46%.该方法操作简便,灵敏度高,检出限低,线性范围宽,可作为生物体内汞含量的测定方法.汞在染毒小鼠血和各脏器中含量随染汞剂量的增加而明显增加,与对照组相比差异有统计学意义(P<0.05);小鼠体内总汞绝大部分蓄积在肾脏内,其次是肝脏,然后是脾、睾丸、脑;全血的总汞含量与肾脏、肝脏、脾、睾丸、脑的总汞含量有相关性.     

干法灰化和微波消解-火焰原子吸收法测定铅锌冶炼厂废旧除尘布袋中重金属

采用干法灰化和微波消解两种样品分解方法处理广东省某铅锌冶炼厂布袋试样,用火焰原子吸收光谱法测定样品中Cu、Zn、Pb、Cr、Ni、Cd 6种重金属元素含量.同时用两种前处理方法对国家一级标准物质进行测定,与标准值比对,验证两种方法的准确度和精密度.结果表明,不同的样品分解方法对各重金属元素的测定结果会产生不同程度的影响.微波消解法相对于干法灰化法的准确度高,试剂利用率高,有利于元素的分析.干法灰化和微波消解两种前处理方法的精密度（RSD,n=11）均小于5%.     

Synthesis,structural characterization and antimicrobial activity of nickel(II) tetrathiocyanato dicuperate(I) complexes with some acyl hydrazones

Heterobimetallic complexes of the type Ni[Cu(SCN)₂]₂ · L (where L = acetophenone benzoylhydrazone, acetophenone isonicotinoyl hydrazone, acetophenone salicyloylhydrazone (ash), acetophenone anthraniloylhydrazone, p-hydroxy acetophenone benzoylhydrazone, p-hydroxy acetophenone isonicotinoyl hydrazone p-hydroxy acetophenone salicyloylhydrazone (phash), p-hydroxy acetophenone anthraniloyl hydrazone), were synthesized and characterized. The complexes are polymeric, insoluble in common organic solvents and are nonelectrolytes. Magnetic moments and electronic spectral studies suggest a spin-free octahedral geometry for the complexes. IR spectra show the bidentate nature of all the ligands bonding through >C=O and >C=N–groups. The SCN group acts as a bridge between two metal centers. X-ray powder diffraction parameters for Ni[Cu(SCN)₂]₂ · ash and Ni[Cu(SCN)₂]₂ · phash correspond to orthorhombic and tetrahedral crystal lattices, respectively, for these complexes. The complexes show a significant antifungal activity against Rizoctonia, Stemphylium and Aspergillus sp. and antibacterial activity against Clostridium and Pseudomonas sp. The metal complexes are more active than the ligands.     

Determination of cadmium in water and herbal medicine by Penicillium chrysogenum immobilized on silica gel for flame atomic absorption spectroscopy

Penicillium chrysogenum was immobilized on silica to develop a simple and cost effective method for solid phase extraction of Cd(II) and determination using flame atomic absorption spectrometry (FAAS). The sorbent was characterized by Fourier transform infrared spectroscopy and packed into a column. The conditions for quantitative sorption and desorption of Cd(II) were optimized. The preconcentration factor was 100 while detection limit was 0.61 µg L^?1 with a relative standard deviation of 1.0%. The method was applied for determination of Cd in herbal medicine and tap water.     

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节...     

铜在日本青鳉体内的累积特征及其对肝脏组织结构的影响

为了解水体铜(Cu(Ⅱ))在日本青鳉(Oryzias latipes)脑、鳃、肝脏、性腺和肌肉组织中的累积特征,以及Cu(Ⅱ)对肝脏组织结构的影响,本文采用生态学单因子梯度实验,进行20 d的日本青鳉毒性暴露试验。结果显示,日本青鳉各个组织对Cu(Ⅱ)的累积量随着浓度的升高而增多,但不同组织对Cu(Ⅱ)的累积量有较大的差异,铜累积量由大到小依次为:肝脏脑鳃性腺肌肉。铜暴露后的日本青鳉肝细胞出现肿大、大小不一、排列混乱,静脉扩张淤血,部分肝细胞固缩和坏疽等现象。肝脏是日本青鳉蓄积铜的主要器官之一,实验发现高浓度的Cu(Ⅱ)对肝脏组织结构造成了明显的损伤,进而严重影响日本青鳉的存活率。     

Solid phase extraction of Cu (II), Ni (II), Co (II), and Fe (III) ions in water samples using salicylaldehyde benzoylhydrazone on Amberlite XAD-4 and their determinations by flame atomic absorption spectrometry

A multi element preconcentration procedure for solid phase extraction on Amberlite XAD-4 as their salicylaldehyde benzoylhydrazone chelates and flame atomic absorption spectrometric determination of some trace metal ions in water samples are proposed in this work. The influences of some analytical parameters, including pH of aqueous solution, amounts of reagent, flow rates of sample and eluent solutions, and sample volume on the quantitative recoveries of copper, nickel, cobalt, and iron were investigated. The effects of concomitant ions on the retentions of the analytes were also examined. The developed method has been successfully applied to the determination of metal ions in some real samples, including, tap water, river water, spring water, and waste water.     

Oxidized multiwalled carbon nanotubes modified with 2-(2-hydroxy-5-nitrophenyl)-4,5-diphenyl imidazole for solid phase extraction and preconcentration of some metal ions

In this work, a new procedure for the enrichment of the trace amount of Cu²⁺, Ni²⁺, Co²⁺, Pb²⁺, Fe²⁺, and Zn²⁺ ions based on the utilization of multiwalled carbon nanotubes (MWCNT) modified with 2-(2-hydroxy-5-nitrophenyl)-4,5-diphenyl imidazole as chelating agent prior to their determination by flame atomic absorption spectrometry has been described. The influence of effective parameters including pH, amount of ligand and MWCNT, composition of eluent, and coexisting ions on recoveries of understudy metal ions was examined. At the optimum pH of 5.0, all metal ions were quantitatively sorbed onto the proposed solid phase and completely desorbed with 8?mL of 5.0?mol?L^?1 HNO₃. The detection limit of Cu²⁺, Co²⁺, Ni²⁺, Pb²⁺, Fe²⁺, and Zn²⁺ ions was 1.7, 2.4, 2.3, 2.9, 2.8, and 1.4?µg?L^?1, while the preconcentration factor was 63 for Cu²⁺ and 94 for the other metal ions and relative standard deviations between 1.8 less than 3.0%. The proposed procedure was applied for the analysis of various samples.     

Thallium(I) and thallium(III) induce apoptosis in isolated rat hepatocytes by alterations in mitochondrial function and generation of ROS

Environmental metal toxins, generated through diverse anthropogenic activities, constitute one of the major contaminants that have led to global dispersion of these toxic metals in the ecosystem. Thallium is one of these widely dispersed metals that produce severe adverse effects on human and biological systems. The influence of thallium(I) and thallium(III) on the early events that trigger apoptosis signaling were examined in freshly isolated rat hepatocytes. In addition, the role of oxidative stress, and mitochondria in the induction of apoptosis were also investigated. Incubation of thallium(I) and thallium(III) with isolated rat hepatocytes generated reactive oxygen species (ROS), collapse of mitochondrial membrane potential, activation of caspases cascade, and appearance of apoptosis phenotype. Mitochondrial permeability transition (MPT) pore sealing agents (cyclosporine A and carnitine) and ATP generators (L-glutamine, fructose, and xylitol) inhibited the activation of caspase-3 and apoptosis, indicating that both the cations activated apoptosis signaling via mitochondrial pathway. Pretreatment of hepatocytes with antioxidants (α-tocopherol or deferoxamine) also blocked caspase-3 activation induced by these cations, suggesting that oxidative stress may be directly involved in a mitochondrial MPT pore opening and activation of caspases cascade. These findings contribute to a better understanding of the mechanisms that mediate thallium-induced apoptosis in isolated rat hepatocytes.     

Effect Of pH on the complexation of U(II) with organic matter dissolved in resh waters

In the present work we study the effect of pH on the complexation of copper with organic matter dissolved in fresh surface waters. Samples collected in rivers of Galicia (NW of Spain) were titrated with copper solution at pH values in the range 5.5–7.5. Copper concentration was measured by DPASV technique. The complexation parameters were obtained from the simple model of 1 : 1 complex formation. The obtained values show a linear increase of the logarithm of the conditional stability constant as the pH increases.     

Enhanced degradation of trichloroethene by calcium peroxide activated with Fe(III) in the presence of citric acid

Trichloroethene (TCE) degradation by Fe(III)-activated calcium peroxide (CP) in the presence of citric acid (CA) in aqueous solution was investigated. The results demonstrated that the presence of CA enhanced TCE degradation significantly by increasing the concentration of soluble Fe(III) and promoting H₂O₂ generation. The generation of HO? and O₂^-? in both the CP/Fe(III) and CP/Fe(III)/CA systems was confirmed with chemical probes. The results of radical scavenging tests showed that TCE degradation was due predominantly to direct oxidation by HO?, while O₂^-? strengthened the generation of HO? by promoting Fe(III) transformation in the CP/Fe(III)/CA system. Acidic pH conditions were favorable for TCE degradation, and the TCE degradation rate decreased with increasing pH. The presence of Cl^-, HCO₃^-, and humic acid (HA) inhibited TCE degradation to different extents for the CP/Fe(III)/CA system. Analysis of Cl^- production suggested that TCE degradation in the CP/Fe(III)/CA system occurred through a dechlorination process. In summary, this study provided detailed information for the application of CA-enhanced Fe(III)-activated calcium peroxide for treating TCE contaminated groundwater.