Slurry analysis after lead collection on a sorbent and its determination by electrothermal atomic absorption spectrometry

In this study, in order to eliminate the drawbacks of elution step and to reach higher enrichment factors, a novel preconcentration/separation technique for the slurry analysis of sorbent loaded with lead prior to its determination by electrothermal atomic absorption spectrometry was described. For this purpose, at first, lead was collected on ethylene glycol dimethacrylate methacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrolidine dithiocarbamate (APDC) by conventional batch technique. After separation of liquid phase, slurry of the sorbent was prepared and directly pipetted into graphite furnace of atomic absorption spectrophotometer. Optimum conditions for quantitative sorption and preparation of the slurry were investigated. A 100-fold enrichment factor could be easily reached.

The analyte element in certified sea-water and Bovine-liver samples was determined in the range of 95% confidence level. The proposed technique was fast and simple and the risks of contamination and analyte loss were low. Detection limit (3δ) for Pb was 1.67 μg l⁻¹.     

Mechanisms of the removal of hexavalent chromium by biomaterials or biomaterial-based activated carbons

Three papers published during recent 2 years in Journal of Hazardous Materials made a mistake in analyzing chromium species in aqueous solution, resulting in incorrect elucidation of Cr(VI) biosorption; the Cr(VI) was removed from aqueous solution systems by 'anionic adsorption'. However, it has been proved that Cr(VI) is easily reduced to Cr(III) by contact with organic materials under acidic conditions because of its high redox potential value (above +1.3 V at standard condition). Therefore, it is strongly possible that the mechanism of Cr(VI) removal by biomaterials or biomaterial-based activated carbons is not "anionic adsorption" but "adsorption-coupled reduction". Thus, for researches of Cr(VI) biosorption, researchers have to analyze not only Cr(VI) but also total Cr in aqueous solution and to check the oxidation state of chromium bound on the biomaterials or activated carbons.     

Electrothermal atomic absorption spectrometric determination of Cr(VI) during ferrochrome production

The level of the generation of hexavalent chromium during ferrochrome production was checked. The concentration of Cr(VI) increases with each stage of ferrochrome production, 7070microgg(-1) being the highest concentration encountered in the last stage of production (dust). This concentration exceeds the maximum acceptable total Cr concentration per 8h by a factor of more than 1000. It was further observed that there is a higher contamination of soil by this pollutant closer to the plant than further away. The highest concentrations of Cr(VI) in soil and grass were found to be 12.7 and 4.2microgg(-1), respectively. The results of the investigation indicate that the consumption of such grass by animals do not pose any health hazard, for concentrations of the toxic Cr species are very low. Therefore, the release of emissions, including dust, during ferrochrome production, is a major contributor to occupational diseases and death to people working in ferrochrome production plant or mine.     

Application of dolochar in the removal of cadmium and hexavalent chromium ions from aqueous solutions

Dolochar, a waste material generated in sponge iron industry, is processed and put to test as an adsorbent for removal of Cd(II) and Cr(VI) ions from aqueous solutions. The dolochar samples were characterised to determine the different phases and their distribution by reflection microscopy. The analysis indicated that the sample consists of metallic iron, fused carbon, and Ca-Mg bearing phases (Ca-Mg-silicate-oxide) along with lots of voids and pores. The fixed carbon (FC) content of the material is 13.8% with a Langmuir surface area of 81.6 m²/g and micropore area of 34.1 m²/g. Batch adsorption experiments have been conducted to study the sorption behaviour of Cd(II) and Cr(VI) ions on dolochar as a function of particle size, contact time, adsorbent dosages, pH and temperature. It is observed that higher pH and temperature enhances sorption of Cd(II) ions. In contrast, the adsorption for Cr(VI) is found to be better in acidic pH in comparison to alkaline media. The equilibrium adsorption isotherm data are tested by applying both Langmuir and Freundlich isotherm models. It is observed that Langmuir isotherm model fitted better compared to the Freundlich model indicating monolayer adsorption. The thermodynamic parameters such as ΔG°, ΔH° and ΔS° indicate the effectiveness of dolochar to remove Cd(II) and Cr(VI) ions from aqueous solution. The kinetics of adsorption is found to better fit to pseudo second order reaction.     

Characterization of TBP containing polysiloxane membrane/insulator/semiconductor structures for hexavalent chromium detection

A hexavalent chromium-sensitive EMIS sensor (electrolyte membrane insulator semiconductor sensor) is prepared by deposition of a tributylphosphate (TBP) ionophore-containing siloprene membrane on a Si/SiO₂/Si₃N₄ structure. The developed EMIS sensor was studied by means of impedance spectroscopy, capacitance–voltage, X-ray photoelectron spectrometry and FT-IR spectroscopy. From the flat-band shift of the EMIS structure, the nersntian response to the anionic species Cr₂O₇⁻ was demonstrated. The linear range of detection is 10^− 4 M to 10^− 1 M and the detection limit is 10^− 5 M. Sulfate and chloride anions are shown not to be interfering whereas carbonate ions present a pK^pot equal to 0.19.     

Modeling and evaluation on removal of hexavalent chromium from aqueous systems using fixed bed column

Removal of hexavalent chromium by xanthated chitosan was investigated in a packed bed up-flow column. The experiments were conducted to study the effect of important design parameters such as bed height and flow rate. At a bed height of 20 cm and flow rate of 5 mL min(-1), the metal-uptake capacity of xanthated chitosan and plain chitosan flakes for hexavalent chromium was found to be 202.5 and 130.12 mg g(-1) respectively. The bed depth service time (BDST) model was used to analyze the experimental data. The computed sorption capacity per unit bed volume (N(0)) was 4.6 ± 0.3 and 78.3 ± 2.9 g L(-1) for plain and xanthated flakes respectively at 10% breakthrough concentration. The rate constant (K(a)) was recorded as 0.0507 and 0.0194 L mg(-1)h(-1) for plain and xanthated chitosan respectively. In flow rate experiments, the results confirmed that the metal uptake capacity and the metal removal efficiency of plain and xanthated chitosan decreased with increasing flow rate. The Thomas model was used to fit the column sorption data at different flow rates and model constants were evaluated. The column was successfully applied for the removal of hexavalent chromium from electroplating wastewater. Five hundred bed volumes of electroplating wastewater were treated in column experiments using this adsorbent, reducing the concentrations of hexavalent chromium from 10 mg L(-1) to 0.1 mg L(-1).     

原子吸收光谱法间接测定樟树叶片中叶绿素总量

探讨了樟树叶片中叶绿素提取的条件,优化了原子吸收光谱仪的测定参数,建立了用无水乙醇作提取剂在研磨条件下提取叶绿素、用石油醚萃取以分离出有机镁、用0.8mol/L盐酸反萃取,使镁进入水溶液。采用火焰原子吸收分光光度法测定萃取液中的镁含量,从而间接测定樟树叶片中叶绿素的含量的分析方法。结果表明,方法的回收率为103~116%,相对标准偏差为4.8%。     

Electrothermal atomic absorption spectrometric determination of gold by vapor formation and in situ trapping in graphite tubes

Gold was determined in ore samples following generation, separation, collection on a graphite cuvette inner wall, and atomization of its volatile species formed by combining an acidified sample solution with an aqueous sodium tetrahydroborate solution at room temperature. A detection limit of 2.6 microg L(-1) (3sigma) was obtained with a 5.0 mL sample volume. Precision of replicate measurements was typically 10% RSD. The overall efficiency of the volatile species generation, transport, and trapping process was 0.4%. Atomization of gold from Pd, Ir, Cu, Ag, and W coated graphite cuvettes, following by trapping of the gaseous volatile gold species on these surfaces, has been investigated. Pd coating was found to decrease the sensitivity. Five microg of Ir, 20 microg of Cu, 20 microg of Ag, and 5 microg of W were chosen as optimum masses. W treatment was the best one for sensitivity enhancement, having an improvement factor of 2.4. Silanization of glass surfaces significantly decreased memory effects; improved peak shapes were thus obtained for flow injection vapor generation atomic absorption spectrometry (FI-VGAAS). The method described in this study was used for the determination of gold in an ore reference material, Gold Ore (MA-1b), Canadian Reference Materials Program.     

Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 molL(-1) HNO3 in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 microgL(-1), respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g(-1). The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.     

石墨炉原子吸收法直接测定饮用水中的铍

采用石墨炉原子吸收法,使用热解涂层石墨管,加上硝酸镁作基体改进剂,直接测定水中的铍。     

Flame atomic absorption spectrometric determination of trace quantities of cadmium in water samples after cloud point extraction in Triton X-114 without added chelating agents

A new micell-mediated phase separation method for preconcentration of ultra-trace quantities of cadmium as a prior step to its determination by flame atomic absorption spectrometry has been developed. The method is based on the cloud point extraction (CPE) of cadmium in iodide media with Triton X-114 in the absence of any chelating agent. The optimal extraction and reaction conditions (e.g., acid concentration, iodide concentration, effect of time) were studied, and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 3-300 ng mL(-1) of cadmium. The detection limit of the method is 1.0 ng mL(-1) of cadmium. The interference effect of some anions and cations was also tested. The method was applied to the determination of cadmium in tap water, waste water, and sea water samples.     

火焰原子吸收分光光度法测定碳素钢中铜含量的测量不确定度评定

对火焰原子吸收分光光度法测定碳素钢中铜含量的测量不确定度进行了分析,分析了测量不确定度的主要来源,并对各不确定度分量进行了评定,求得合成标准不确定度和扩展不确定度分别为0.00071%和0.0014%.     

Activated carbons and low cost adsorbents for remediation of tri- and hexavalent chromium from water

Hexavalent chromium is a well-known highly toxic metal, considered a priority pollutant. Industrial sources of Cr(VI) include leather tanning, cooling tower blowdown, plating, electroplating, anodizing baths, rinse waters, etc. The most common method applied for chromate control is reduction of Cr(VI) to its trivalent form in acid (pH approximately 2.0) and subsequent hydroxide precipitation of Cr(III) by increasing the pH to approximately 9.0-10.0 using lime. Existing overviews of chromium removal only cover selected technologies that have traditionally been used in chromium removal. Far less attention has been paid to adsorption. Herein, we provide the first review article that provides readers an overview of the sorption capacities of commercial developed carbons and other low cost sorbents for chromium remediation. After an overview of chromium contamination is provided, more than 300 papers on chromium remediation using adsorption are discussed to provide recent information about the most widely used adsorbents applied for chromium remediation. Efforts to establish the adsorption mechanisms of Cr(III) and Cr(VI) on various adsorbents are reviewed. Chromium's impact environmental quality, sources of chromium pollution and toxicological/health effects is also briefly introduced. Interpretations of the surface interactions are offered. Particular attention is paid to comparing the sorption efficiency and capacities of commercially available activated carbons to other low cost alternatives, including an extensive table.     

Biosorption of hexavalent chromium by raw and acid-treated green alga Oedogonium hatei from aqueous solutions

The hexavalent chromium, Cr(VI), biosorption by raw and acid-treated Oedogonium hatei were studied from aqueous solutions. Batch experiments were conducted to determine the biosorption properties of the biomass. The optimum conditions of biosorption were found to be: a biomass dose of 0.8 g/L, contact time of 110 min, pH and temperature 2.0 and 318 K respectively. Both Langmuir and Freundlich isotherm equations could fit the equilibrium data. Under the optimal conditions, the biosorption capacities of the raw and acid-treated algae were 31 and 35.2 mg Cr(VI) per g of dry adsorbent, respectively. Thermodynamic parameters showed that the adsorption of Cr(VI) onto algal biomass was feasible, spontaneous and endothermic under studied conditions. The pseudo-first-order kinetic model adequately describe the kinetic data in comparison to second-order model and the process involving rate-controlling step is much complex involving both boundary layer and intra-particle diffusion processes. The physical and chemical properties of the biosorbent were determined and the nature of biomass-metal ions interactions were evaluated by FTIR analysis, which showed the participation of -COOH, -OH and -NH(2) groups in the biosorption process. Biosorbents could be regenerated using 0.1 M NaOH solution, with up to 75% recovery. Thus, the biomass used in this work proved to be effective materials for the treatment of chromium bearing aqueous solutions.     

Speciation and determination of ultra trace amounts of chromium by solidified floating organic drop microextraction (SFODME) and graphite furnace atomic absorption spectrometry

Solidified floating organic drop microextraction (SFODME) method in combination with graphite furnace atomic absorption spectrometry (GFAAS) has been used for the determination of chromium species in water and urine samples. 1-undecanol containing 2-thenoyltrifluoroacetone (TTA) was used as a selective chelating agent for the extraction of Cr(III). The total Cr was determined after the reduction of Cr(VI) to Cr(III) with hydroxylamine. The concentration of Cr(VI) was determined from the difference between the concentration of total chromium and the Cr(III). Several variables such as the sample pH, concentration of TTA, salt concentration, extraction time and the sample volume were investigated in detail. Under the optimum conditions, the limit of detection of the proposed method was 0.006 μg l(-1) for Cr(III) and the relative standard deviation for six replicate determinations at 0.1 μg l(-1) Cr(III) was 5.1%. The proposed method was successfully applied for the determination of chromium species in tap water, well water, mineral water, and urine samples.     

Monochromatization of resonance radiation in Zeeman atomic absorption spectrometry

Two methods of background correction in atomic absorption spectrometry with nonselective atomic effects are investigated: first, with a source possessing a continuous spectrum and, second, that of correction based on the Zeeman effect. The parameters of the monochromator, which was developed expressly for Zeeman atomic absorption spectrometry, are considered. __________ Translated from Izmeritel’naya Tekhnika, No. 9, pp. 20–24, September, 2007.     

次灵敏线火焰原子吸收光谱法测定磷酸铁锂中的锂含量

以锂的次灵敏线323．3nm为分析谱线,采用火焰原子吸收光谱法测定磷酸铁锂中的高含量锂。通过研究酸介质、消电离剂和基体离子对锂测定的影响,以及进行共存离子干扰实验发现：在2％的硝酸介质中方法的灵敏度最佳;在标准溶液中加入基体离子,可以消除基体对锂测定的干扰;常见共存离子不干扰锂的测定。在优化的实验条件下,锂的检测线性范围为4—140μg·mL-1,检出限（30-）为2．0肛g·mL-1,对20．0μg·mL-1的锂标准溶液连续测定11次,其RSD为0．05％。方法简便、快速、准确,检测线性范围广,避免了稀释操作带来的误差,可用于高含量锂的直接测定;方法用于磷酸铁锂样品测定,回收率在92PTe～103．7％之间,相对标准偏差（n=7）在1．04％～1．16％之间。     

Palladium nanoparticles supported on amine-functionalized glass fiber mat for fixed-bed reactors on the effective removal of hexavalent chromium by catalytic reduction

Palladium nanoparticles were deposited on the amine-grafted glass fiber mat (GFM-NH₂) catalyst support by a conventional impregnation process followed by the borohydride reduction in aqueous solution at room temperature to create the designed Pd/GFM-NH₂ catalyst. By the use of large size glass fiber mat without nano/mesopores as the catalyst support, the internal mass transfer limitations due to the existence of nano/mesopores on the catalyst support were eliminated and the Pd/GFM-NH₂ catalyst could be easily separated from treated water due to the large size of the catalyst support. Batch experiments demonstrate its good catalytic reduction performance of Cr(VI) with formic acid as the reducing agent. It also demonstrated an efficient Cr(VI) removal and stability in a lab-prepared, packed fixed-bed tube reactor for the continuous treatment of Cr(VI)-containing water. Thus, it has a good potential for the catalytic reduction of Cr(VI) in the water treatment practice.     

石墨炉原子吸收法测定头发中硒

利用优级纯硝酸浸润,放置过夜,适当水浴加热的方法,将头发样品制备成溶液,用石墨炉原子吸收法测定头发中硒,在选定的测定条件下检出限0．004mg／l,精密度3．7％,回收率在91．1％-98．2％之间。     

火焰原子吸收法测定百合中的微量元素

兰州百合含有丰富的营养物质和微量元素。为测定兰州百合中的微量元素（ca、Zn、Fe、Mn、Mg、K、Cu等）的含量，采用空气-乙炔火焰原子吸收法对经过4：1的硝酸一高氯酸消解处理消除相关干扰后的兰州百合进行测定。结果表明：七种元素的回收率在97．1％～102．3％范围内，结果准确可靠，方法简单、快速、重现性好。