Sorbent extraction of some metal ions on a gas chromatographic stationary phase prior to their flame atomic absorption determinations

An enrichment/separation system for atomic absorption spectrometric determinations of Cu(II), Fe(III), Ni(II) and Co(II) has been established. The procedure is based on the adsorption of the analytes as calmagite chelates on Chromosorb-102. The effects of some parameters including pH, amount of ligand, salt matrix, flow rates of sample and eluent solutions were investigated. Under optimized conditions, the relative standard deviation of the combined method of sample treatment, preconcentration and determination with FAAS (N=5) is generally lower than 5%. The limit of detection (3σ) was between 6.0-112. 9 μg/L. The results were used for preconcentration of analytes from some sodium and ammonium salt

Extractable trace metals content of dust from vehicle air filters as determined by sequential extraction and flame atomic absorption spectrometry

A modified four-step sequential extraction procedure developed within the Standards, Measurement, and Testing Program (formally the Community Bureau of Reference) of the European Commission was applied to determine the distribution of Cd, Cu, Fe, and Mn in air filter dust samples collected from vehicles. The four fractions were acid-soluble, reducible, oxidizable, and residual. These fractions have the advantage of providing better insight into the mechanism of association of metals in the dust. The determination of trace metals in dust samples was performed by flame atomic absorption spectrometry. The results obtained after applying the sequential extraction scheme indicated that Cu was the most abundant metal in the organic and residual fractions of the dust matrix. Fe was found mainly in the residual fraction, and the major amounts of Mn and Cd were present in the acidsoluble and bound-to-carbonate fraction. The mean values of Cd, Cu, Fe, and Mn were found to be 15.58, 33.54,1625, and 180 μg/g, respectively. The results obtained are in agreement with data reported in the literature

The Solid Phase Extraction of Some Metal Ions Using Palladium Nanoparticles Attached to Silica Gel Chemically Bonded by Silica-Bonded N-Propylmorpholine as New Sorbent prior to Their Determination by Flame Atomic Absorption Spectroscopy

In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4–2.7 ng mL−1. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL−1) in different natural food samples

Simultaneous preconcentration of trace metals in environmental samples using amberlite XAD-2010/8-hydroxyquinoline system

A simple and sensitive system for simultaneous preconcentration of Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Pb(II) and Cd(II) at trace level by flame atomic absorption spectrometry (FAAS) is proposed. Amberlite XAD-2010 packed in a column was used as sorbent. Analyte ions were sorbed in the column as their 8-hydroxyquinoline chelates; they could then be eluted by 1 mol L -1 HNO3 in acetone. The analytical conditions including pH, amounts of 8-hydroxyquinoline, sample volume etc. on the quantitative recoveries of the analytes were investigated. The effects of the concomitants ions on the recoveries of the analytes column were also studied. The detection limits, corresponding to three times the standard deviation of the blank, were found to be in the range of 0.10-0.40 μg L-1. The accuracy of the procedure was measured by analyte determinations in certified reference materials (CRM NIES No. 7 Tea Leaves and TMDW-500 Drinking Water). The applications of the presented system were performed by the analysis of some environmental samples including water samples

Salicylic acid functionalized silica-coated magnetite nanoparticles for solid phase extraction and preconcentration of some heavy metal ions from various real samples

A method for the preconcentration of trace heavy metal ions in environmental samples has been reported. The presented method is based on the sorption of Cu(II), Cd(II), Ni(II) and Cr(III) ions with salicylic acid as respective chelate on silica-coated magnetite nanoparticles. Prepared adsorbent was characterized by XRD, SEM, BET and FT-IR measurements. The metals content of the sorbed complexes are eluted using 4.0 mL of 1.0 mol L-1 nitric acid. The influences of the analytical parameters including pH, amount of solid phase and condition of eluting solution, the effects of matrix ions on the retention of the analytes were examined. The accuracy and precision of suggested method were tested by analyzing of certified reference materials. The detection limits (3Sb/m, N = 8) for Cu(II), Cd(II), Ni(II) and Cr(III) ions are 0.22, 0.11, 0.27 and 0.15 μg L-1, respectively, and the maximum preconcentration factor is 200. The method was successfully applied to the evaluation of these trace and toxic metals in various waters, foods and other samples

Sorption of platinum on immobilized microorganisms for its on-line preconcentration and chemiluminescent determination in water samples

Fungi of the type Aspergillus sp. were immobilized on a cellulosic resin and used as a biosorbent for the on-line preconcentration and separation of Pt(IV) ions prior to their chemiluminescent determination via flow injection analysis. Biosorption and elution conditions were optimized, and the results compared to biosorbents based on the use of Chlorella vulgaris algae and Saccharomyces cerevisiae yeast in terms of preconcentration and selective retention of Pt(IV). The immobilized fungi presented here have a high potential for use in platinum biosorption. The procedure exhibits the currently lowest limit of detection (0.02 ng mL−1 of Pt) and very high selectivity. The procedure was applied to the determination of Pt(IV) in river water, road run-off, and wastewater samples

Evaluation of cadmium, lead, nickel and zinc status in biological samples of smokers and nonsmokers hypertensive patients

The objective of this study was to evaluate the association between trace and toxic elements zinc (Zn), cadmium (Cd), nickel (Ni) and lead (Pb) in biological samples (scalp hair, blood and urine) of smoker and nonsmoker hypertensive patients (n=457), residents of Hyderabad, Pakistan. For the purpose of comparison, the biological samples of age-matched healthy controls were selected as referents. The concentrations of trace and toxic elements were measured by atomic absorption spectrophotometer prior to microwave-assisted acid digestion. The validity and accuracy of the methodology were checked using certified reference materials and by the conventional wet acid digestion method on the same certified reference materials and real samples. The recovery of all the studied elements was found to be in the range of 97.8–99.3% in certified reference materials. The results of this study showed that the mean values of Cd, Ni and Pb were significantly higher in scalp hair, blood and urine samples of both smoker and nonsmoker patients than in referents (P<0.001), whereas the concentration of Zn was lower in the scalp hair and blood, but higher in the urine samples of hypertensive patients. The deficiency of Zn and the high exposure of toxic metals as a result of tobacco smoking may be synergistic with risk factors associated with hypertension

Use of nanomaterials in the pretreatment of water samples for environmental analysis

The challenge of providing clean drinking water is of enormous relevance in today’s human civilization, being essential for human consumption, but also for agriculture, livestock and several industrial applications. In addition to remediation strategies, the accurate monitoring of pollutants in water sup-plies, which most of the times are present at low concentrations, is a critical challenge. The usual low concentration of target analytes, the presence of in-terferents and the incompatibility of the sample matrix with instrumental techniques and detectors are the main reasons that renders sample preparation a relevant part of environmental monitoring strategies. The discovery and ap-plication of new nanomaterials allowed improvements on the pretreatment of water samples, with benefits in terms of speed, reliability and sensitivity in analysis. In this chapter, the use of nanomaterials in solid-phase extraction (SPE) protocols for water samples pretreatment for environmental monitoring is addressed. The most used nanomaterials, including metallic nanoparticles, metal organic frameworks, molecularly imprinted polymers, carbon-based nanomaterials, silica-based nanoparticles and nanocomposites are described, and their applications and advantages overviewed. Main gaps are identified and new directions on the field are suggested.publishe