Solid phase extraction of gold(III) on silica gel modified with benzoylthiourea prior to its determination by flame atomic absorption spectrometry

A new method has been developed for the determination of gold based on separation and preconcentration using silica gel modified with benzoylthiourea. The optimum experimental parameters for preconcentration of gold, such as acid concentration, sample flow rate, eluent and matrix ions, have been investigated. Gold could be quantitatively retained in the 0.25-2.0 mol L(-1) HCl and HNO(3) concentrations, and then eluted completely with 0.5 mol L(-1) thiourea in 1.0 mol L(-1) HCl. The sorption capacity of gold(III) is 0.92 +/- 0.04 mmol g(-1) with a high enrichment factor of 267. The relative standard deviation of the method, RSD%, was found as 1.2% for 0.1 microg mL(-1). The detection limit for gold was 1.4 microg L(-1). The validation of the proposed method was checked by the analysis of certified reference soil materials. The presented procedure was applied to the determination of gold in some environmental samples.     

Sensitive determination of cadmium using solidified floating organic drop microextraction-slotted quartz tube-flame atomic absorption spectroscopy

In this study, solidified floating organic drop microextraction (SFODME) by 1-undecanol was combined with slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) for the determination of cadmium at trace levels. Formation of a complex with 4,4′-dimethyl-2,2′-bipyridine facilitated the extraction of cadmium from aqueous solutions. Several chemical variables were optimized in order to obtain high extraction outputs. Parameters such as concentration of the ligand, pH, and amount of buffer solution were optimized to enhance the formation of cadmium complex. The SFODME method was assisted by dispersion of extractor solvent into aqueous solutions using 2-propanol. Under the optimum extraction and instrumental conditions, the limit of detection and limit of quantitation values obtained for cadmium using the combined methods (SFODME-SQT-FAAS) were found to be 0.4 and 1.3 μg L^?1, respectively. Matrix effects on the method were also examined for tap water and wastewater, and spiked recovery results were found to be very satisfactory.

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Graphical Abstract SFODME-SQT-FAAS system for sensitive determination of cadmium

     

Solid phase extraction of gold(III) on Amberlite XAD-2000 prior to its flame atomic absorption spectrometric determination

A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer (FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III) from 1.5 mol l⁻¹ HCl solution and the recovery of gold with 0.07 mol l⁻¹ NH₃ solution were quantitative (≥95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 μg l⁻¹. The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples.     

The effect of oxygen addition on the determination of cadmium and lead in blood and foods by graphite furnace atomic absorption spectrometry

It is well known that in the analysis of low temperature vaporized metal elements such as cadmium and lead, a high ashing temperature causes a loss of the target atoms at the ashing stage, while low ashing temperature causes incomplete decomposition of organic components in the sample. In order to solve these problems, the effect of oxygen addition on determination of cadmium and lead in blood and foods was studied. Oxygen was introduced into the atmosphere in the graphite furnace at the beginning of ashing stage for 20 seconds at 0.5 l/min. Relation between ashing temperature and sensitivity was examined, and the oxygen addition minimized signal depression by the sample matrix. It can be concluded that the addition of oxygen at the ashing stage not only reduces the background absorption, but also suppress the volatilization of target atoms at the ashing stage by the formation of their oxides.     

微波消解平台石墨炉原子吸收法测定活性污泥中重金属

以铜和铅为例建立了一种微波消解样品,平台石墨炉原子吸收法测定活性污泥中重金属含量的方法,该方法的样品加标回收率Cu为91 0%～97 3%,Pb为93 1%～98 0%,相对标准偏差RSD(%):Cu为1 38%～1 61%,Pb为1 28%～1 94%,检验限Cu为0 0052ng g,Pb为0 0073ng g,该方法应用于活性污泥中重金属的分析,实验所需时间短,取样量少,空白值低,实验过程中样品损失小,准确度和灵敏度高,结果令人满意。     

无火焰原子吸收石墨炉法测定海水中的总铬

研究了使用无火焰原子吸收石墨炉法测定海水中总铬的分析方法。在氧化过程后采用络合 -萃取技术使共存元素与待测元素分离 ,既消除了基体干扰 ,又达到了富集作用 ,使测定结果准确可靠。方法的相对标准偏差 6.34 % ,回收率85.2 %。     

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS)

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L^-1 HNO₃ and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L^?1 and 3.91 μg L^?1, respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.     

Solid-phase extraction of Mn(II) and slurry analysis of the sorbent by electrothermal atomic absorption spectrometry

In this study, a challenging preconcentration/separation method based on the sorption of manganese on ethylene glycol dimethacrylatemethacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrrolidine dithiocarbamate (APDC) and its slurry analysis by electrothermal atomic absorption spectrometry was described. Optimum conditions for quantitative sorption, as well as for preparing a homogeneous and stable slurry were investigated. A 100-fold enrichment factor could be reached. The analyte element in certified sea-water and bovine-liver samples were determined in the range of 95% confidence level. The proposed technique is fast, simple, and the risk of contamination is low. The limit of detection of the method for manganese in the slurry of the blank subjected to the proposed procedure was 0.07 μg L^?1 (3δ, N:10) corresponding to 0.56 μg kg^?1 slurry.     

Determination of total chromium by flame atomic absorption spectrometry after coprecipitation by cerium (IV) hydroxide

A method for the preconcentration of the total chromium based on coprecipitation with cerium (IV) hydroxide is proposed for determination of chromium by flame atomic absorption spectrometry. Different factors including carrier element amount, pH, sample volume and matrix ion effects for the precipitation were examined. The detection limit of the total chromium (k = 3, N = 15) was 0.18 μg l⁻¹. The presented method was applied for the determination of chromium in the wastewater samples from Kayseri and Nigde Organized Industrial Region-Turkey and in drinking water from our laboratory, Kayseri with satisfactory results (relative standard deviations below 8%, recoveries 95%). The analytical results obtained by the proposed method for certified copper sample was in good agreement with the certified value.     

Application of laser-based ion mobility (IM) spectrometry for the analysis of polycyclic aromatic compounds (PAC) and petroleum products in soils

The capability of laser-based IM spectrometry to detect PAC and petroleum products (oils) in model matrices, laboratory reference (LR) materials and in real-world contaminated soil samples was demonstrated. Quantitative IM investigations of PAC-doped PVC films yielded detection limits in the ppm range for single PAC. The potential of IM spectrometry for in situ analysis was demonstrated by the analysis of PAC-containing certified reference (CR) material, and of petroleum product-containing LR materials and real-world soil samples. The calibration of IM signals obtained from oil-doped LR materials was also possible, and detection of oils with concentrations below 100 mg kg(-1) was achieved. The in situ analysis of real-world contaminated soils with the IM and LIF techniques was in good accordance with ex situ reference investigations.     

Heavy metals assessment and identification of their sources in agricultural soils of Southern Tehran, Iran

A detailed investigation was conducted to evaluate heavy metal sources and their spatial distribution in agricultural fields in the south of Tehran using statistics, geostatistics, and a geographic information system. The content of Cd, Cu, Co, Pb, Zn, Cr, and Ni were determined in 106 samples. The results showed that the primary inputs of Cr, Co, and Ni were due to pedogenic factors, while the inputs of Zn, Pb, and Cu were due to anthropogenic sources. Cd was associated with distinct sources, such as agricultural and industrial pollution. Ordinary kriging was carried out to map the spatial patters of heavy metals, and disjunctive kriging was used to quantify the probability of heavy metal concentrations higher than their recommended threshold values. The results show that Cd, Cu, Ni, and Zn exhibit pollution risk in the study area. The sources of the high pollution levels evaluated were related to the use of urban and industrial wastewater and agricultural practices. These results are useful for the development of proper management strategies for remediation practices in the polluted area.     

Seasonal variation of different microorganisms with nickel and cadmium in the industrial wastewater and agricultural soils

Wastewater and soil samples were collected from the industrial area of Ghaziabad City, India from January 2005 to December 2007 and were analyzed for the presence of heavy metals by atomic absorption spectrophotometry. Test samples revealed high levels of Fe, Cr, Cu, Ni, Zn, and Cd as 967.03, 34.63, 27.97, 19.7, 16.70, and 3.20 mg/L of wastewater, respectively. The concentrations of inorganic minerals were higher in the soil samples irrigated with wastewater. Total coliforms were found to be maximum (1,133 × 10⁴ most probable number per 100 mL) during spring and summer followed by winter and postmonsoon in the wastewater samples. The microbial count in soil as well as in wastewater decreases as the metal concentration increases. The concentration 200 μg/mL of nickel and cadmium inhibits majority of the population, while, at some points, it inhibits 100% of the population. The exponential decay model for microbial count at the increasing metal concentrations indicate that asymbiotic N₂ fixers were best fitted to the model. In all the seasons, the order of decline in terms of exponential decay of the population of different microbial groups in soil was asymbiotic N₂ fixers > actinomycetes > fungi > aerobic heterotrophic bacteria. The different microbial groups that have different values of slope in different seasons indicate that the resistant population of microorganisms was variable with seasons.     

Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers

Persistence behavior of insecticides chlorpyriphos, profenofos, triazophos, cypermethrin, and deltamethrin following the use of three combination formulations Action 505 (chlorpyriphos?+?cypermethrin), Roket 44EC (profenofos?+?cypermethrin), and Anaconda Plus (triazophos?+?deltamethrin) was studied in cabbage following the spray application at the recommended and double doses. Bio-efficacy of these formulations was also evaluated against mustard aphids (Lipaphis erysimi Kaltenbach) and diamondback moth (Plutella xylostella L.). The residues of different insecticides persisted for 5–8 days at low dose and 8–12 days at high dose. The residues dissipated with time and 87–100 % dissipation was recorded on the 8th day. The half-life values varied from 0.4 to 1.6 days. Based on the acceptable daily intake (ADI) values, a safe waiting period of 1 day has been suggested for the formulations Action 505 and Roket 44EC and 3 days for Anaconda Plus at the recommended dose of application. Action (1.6 L/ha) treatment was found to be the best as it significantly reduced the diamondback moth (DBM) (~60 %) and aphid population (~70 %) besides giving the highest yield (170 % increase over control).     

Determination of some heavy metal levels in soft drinks on the Ghanaian market using atomic absorption spectrometry method

Twenty-three soft drink samples (i.e., four pineapple-based fruit drinks, eight citrus-based fruit juices, one soya-based drink, three cola carbonated drinks, one apple-based fruit drink, and six cocktail fruit drinks) were randomly purchased from retail outlets in an urban market in Accra and analyzed for the concentrations of iron, cobalt, cadmium, zinc, lead, and copper using flame atomic absorption spectrometry. The mean concentration of iron and cadmium were 0.723?±?0.448 mg/L and 0.032?±?0.012 mg/L, respectively. The mean cobalt concentration was 0.071?±?0.049 mg/L, while the mean Zn concentration in the samples was 0.060?±?0.097 mg/L. The mean concentrations of Pb and Cu in the fruit juice samples were 0.178?±?0.091 mg/L and 0.053?±?0.063 mg/L respectively. About 78 % of the samples exceeded the United States Environmental Protection Agency (USEPA) maximum contaminant level of 0.3 mg/L prescribed for iron, whereas all the samples exceeded the USEPA maximum contaminant level of 0.005 mg/L prescribed for cadmium. About 91 % of the samples exceeded the EU maximum contaminant level prescribed for lead insoft drinks.     

强酸型离子交换纤维富集-火焰原子吸收测定水中痕量铜、铅、镉、镍

通过强酸型离子交换纤维柱,在同一水样中同时富集和洗脱了铜、铅、镉、镍,采用火焰原子吸收光谱法测定,并对富集条件及洗脱条件、干扰因素进行了探讨。该方法简便易行,回收率在96.1%~105.5%之间,测定的相对标准偏差小于5.0%。     

The use of rapidly synergistic cloud point extraction for the separation and preconcentration of trace amounts of Ni (II) ions from food and water samples coupling with flame atomic absorption spectrometry determination

A novel improved preconcentration method known as rapidly synergistic cloud point extraction (RS-CPE) was established for nickel preconcentration and determination prior to its determination by flame atomic absorption spectrometry. In this work, the traditional CPE pattern was changed and greatly simplified in order to be applicable in metal extraction and detection. This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. The various parameters affecting the extraction and preconcentration of nickel such as sample pH, 2,2′-Furildioxime concentration, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time, and ionic strength were investigated and optimized. Under optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 2–200 μg L^?1, and the limit of detection was 0.6 μg L^?1 for nickel. The developed method was successfully applied for the determination of nickel in food and water samples. The results showed that, the proposed method can be used as a cheap, rapid, and efficient method for the extraction and preconcentration of nickel from real samples.     

Copper fractionation with dissolved organic matter in natural waters and wastewater--a mixed micelle mediated methodology (cloud point extraction) employing flame atomic absorption spectrometry

A cloud point extraction-preconcentration methodology for the speciation analysis of free and organically complexed metal species in natural waters is presented. The method is based on the neutralization of the electrostatic charge of the humate-metal complexes with a positively charged surfactant in a high ionic strength solution environment. The resulting complexes are conveniently solubilized in the micelles of a non-ionic surfactant medium and are thus separated from the bulk aqueous phase. Free metal species are also determined by complexation with a conventional chelating agent under mild conditions. The overall procedure is easy, rapid and allows for a high sample throughput in terms of massive analysis of many samples in the same time period. The method offers substantially low detection limits of 8.5 and 0.9 micrograms l-1 for bound and labile species respectively, with a calibration curve rectilinear in the wide range 40-150 micrograms l-1 for the humate associated and 4-40 micrograms l-1 for the free metal species. The method is free from interferences yielding recoveries in the range 97-102% for various samples of different matrixes.     

Chemical speciation studies on DU contaminated soils using flow field flow fractionation linked to inductively coupled plasma mass spectrometry (FlFFF-ICP-MS)

Flow field flow fractionation (FlFFF) in combination with inductively coupled plasma mass spectrometry (ICP-MS) was used to study the chemical speciation of U and trace metals in depleted uranium (DU) contaminated soils. A chemical extraction procedure using sodium pyrophosphate, followed by isolation of humic and fulvic substances was applied to two dissimilar DU contaminated sample types (a sandy soil and a clay-rich soil), in addition to a control soil. The sodium pyrophosphate fractions of the firing range soils (Eskmeals and Kirkcudbright) were found to contain over 50% of the total U (measured after aqua regia digestion), compared to approximately 10% for the control soil. This implies that the soils from the contaminated sites contained a large proportion of the U within more easily mobile soil fractions. Humic and fulvic acid fractions each gave characteristic peak maxima for analytes of interest (Mn, Fe, Cu, Zn, Pb and U), with the fulvic acid fraction eluting at a smaller diameter (approximately 2.1 nm on average) than the humic fraction (approximately 2.4 nm on average). DU in the fulvic acid fraction gave a bimodal peak, not apparent for other trace elements investigated, including natural U. This implies that DU interacts with the fulvic acid fraction in a different way to all other elements studied.