Development of a flotation method for preconcentration-separation of trace amounts of some metal ions in plant tissues prior to their FAAS determinations

An efficient flotation method based on the combination of flame atomic absorption spectrometry (FAAS) and separation and preconcentration step for determination of Cr3+, Cu 2+, Co2+, Ni2+, Zn2+, Cd 2+, Fe3+ and Pb2+ ions in various real samples by the possibility of applying bis(2-hydroxyacetophenone)-1,4-butanediimine (BHABDI) as a new collector was studied. The influence of pH, amount of BHABDI as collector, sample matrix, type and amount of eluting agent, type and amount of surfactant as floating agent, ionic strength and air flow rates i.e. variables affecting the efficiency of the extraction system was evaluated. It is ascertained that metal ions such as iron can be separated simultaneously from matrix in the presence of 0.012 mM ligand, 0.025% (w/v) of CTAB to a test sample of 750 mL at pH 6.5. These ions can be eluted quantitatively with 6 mL of 1.0 mol L-1 HNO3 in methanol which lead to the enrichment factor of 125. The detection limits for analyte ions were in the range of 1.3-2.4 ng mL-1. The method has been successfully applied for determination of trace amounts of ions in various real samples.

Separation and preconcentration trace amounts of gold by using modified organo nanoclay closite 15A

The application of organo nanoclay 5-(4-dimethylamino-benzylidene) rhodanine-immobilized as a new, easily prepared, and stable solid sorbent for preconcentration trace amounts of Au(III) ions in aqueous solution is presented. The sorption of Au(III) ions was quantitative in the pH range of 2-4, and quantitative desorption occurred instantaneously with 10.0 mL of a mixture containing 0.5 mol L-1 Na2S2O3 and KSCN. Various parameters, such as the effect of pH, breakthrough volume, extraction time, and interference of a large number of anions and cations have been studied. The proposed method has been applied for determination of trace amount of gold in water samples.

Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination

In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results.

Ligandless cloud point extraction of trace amounts of palladium and rhodium in road dust samples using Span 80 prior to their determination by flame atomic absorption spectrometry

In this study, a procedure is developed for cloud point extraction of Pd(II) and Rh(III) ions in aqueous solution using Span 80 (non-ionic surfactant) prior to their determination by flame atomic absorption spectroscopy. This method is based on the extraction of Pd(II) and Rh(III) ions at a pH of 10 using Span 80 with no chelating agent. We investigated the effect of various parameters on the recovery of the analyte ions, including pH, equilibration temperature and time, concentration of Span 80, and ionic strength. Under the best experimental conditions, the limits of detection based on 3Sb for Pd(II) and Rh(III) ions were 1.3 and 1.2 ng mL-1, respectively. Seven replicate determinations of a mixture of 0.5 µg mL-1 palladium and rhodium ions gave a mean absorbance of 0.058 and 0.053 with relative standard deviations of 1.8 and 1.6%, respectively. The developed method was successfully applied to the extraction and determination of the palladium and rhodium ions in road dust and standard samples and satisfactory results were obtained.

Coprecipitation of trace amounts of silicon with aluminum hydroxide and the determination by flame atomic absorption spectrometry

A simple preconcentration method of silicon based on coprecipitation with aluminum hydroxide prior to its flame atomic absorption (FAAS) determination was established. The recovery values of analyte ion was higher than 95%. The parameters including types of hydroxide ion source for precipitation, acid type for dissolution step, amount of aluminum ion as collector, pH, temperature, standing and centrifuge time, and sample volume were optimized for the quantitative recovery of the analyte. The influences of matrix ions were also examined. The relative standard deviation was found to be 3.2%. The limit of detection was calculated as (0.1 mg L-1). The preconcentration factor is 100 for (200 mL) solution. The proposed method was successfully applied for the determination of silicon in some water and alloy samples.

Magnetic coupled electrochemistry: Exploring the use of superparamagnetic nanoparticles for capturing, transporting and concentrating trace amounts of analytes

We propose the use of functionalized superparamagnetic nanoparticles for capturing, and transporting analytes, in association with an external miniature magnet to deposit such nanocarrier species at the electrode surface. This approach can be employed for the electroanalytical determination of chemical species capable of interacting with the nanoparticles, or in the opposite case, to block their response at the electrode surface. The concept was successfully demonstrated by using aminofunctionalized nanoparticles to block the discharge of hexacyanoferrate(II) ions, and to enhance the signals of aquapentacyanoferrate(II) ions via coordination to the surface amino groups. Selective analysis was also performed for silver ions, surpassing the stripping methods in terms of versatility and usefulness. (C) 2010 Elsevier B.V. All rights reserved.

Electrochemical method for quantitative determination of trace amounts of disperse dye in wastewater

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effects of Deicing Salt Trace Compounds on Deterioration of Portland Cement Concrete, HR-271, 1987

A study was made of the detrimental effects of trace amounts of calcium sulfate (occurring naturally in halite deposits used for deicing) on portland cement concrete pavements. It was found that sulfate introduced as gypsum with sodium chloride in deicing brines can have detrimental effects on portland cement mortar. Concentrations of sulfate as low as 0.5% of the solute rendered the brine destructive. Conditions of brine application were critical to specimen durability. The mechanisms of deterioration were found to be due to pore filling resulting from compound formation and deposition. A field evaluation of deteriorating joints suggests that the sulfate phenomena demonstrated in the laboratory also operates in the field. A preliminary evaluation was made of remedies: limits on sulfates, fly ash admixtures, treatment of existing pavement, and salt treatments. This report gives details of the research objectives, experimental design, field testing, and possible solutions. Recommendations for further study are presented.

Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Ion pair-dispersive liquid-liquid microextraction of trace amount of rhodium ion in water and road dust samples prior to flame atomic absorption spectrometry determination

A simple ion pair-dispersive liquid-liquid microextraction method was proposed for preconcentration trace amounts of rhodium. An ion association complex of RhCl4- and tetradecyldimetylbenzylamonium was extracted into cholorobenzene. The volume and the type of extractive and dispersive solvents, the extraction time and the pH of the aqueous solutions were optimized. The calibration curve was linear in the range of 0.6-500 ng mL-1 of rhodium. The limit of detection was 0.10 ng mL-1 in initial solution and preconcentration factor was 40. The proposed method was successfully applied to the extraction and determination of rhodium in road dust and water samples.

Evanescent Wave Fibre Optic Sensors for Trace Analysis of Fe3+ in Water

In this communication, we discuss the details of fabricating an off-line fibre optic sensor (FOS) based on evanescent wave absorption for detecting trace amounts of Fe3+ in water. Two types of FOS are developed; one type uses the unclad portion of a multimode silica fibre as the sensing region whereas the other employs the microbent portion of a multimode plastic fibre as the sensing region. Sensing is performed by measuring the absorption of the evanescent wave in a reagent medium surrounding the sensing region. To evaluate the relative merits of the two types of FOS in Fe3+ sensing, a comparative study of the sensors is made, which reveals the superiority of the latter in many respects, such as smaller sensing length, use of a double detection scheme (for detecting both core and cladding modes) and higher sensitivity of cladding mode detection at an intermediate range of concentration along with the added advantage that plastic fibres are inexpensive. A detection limit of 1 ppb is observed in both types of fibre and the range of detection can be as large as 1 ppb–50 ppm. All the measurements are carried out using a LabVIEW set-up.

Evanescent wave fibre optic sensors for trace analysis of Fe3+ in water

In this communication, we discuss the details of fabricating an off-line fibre optic sensor (FOS) based on evanescent wave absorption for detecting trace amounts of Fe3+ in water. Two types of FOS are developed; one type uses the unclad portion of a multimode silica fibre as the sensing region whereas the other employs the microbent portion of a multimode plastic fibre as the sensing region. Sensing is performed by measuring the absorption of the evanescent wave in a reagent medium surrounding the sensing region. To evaluate the relative merits of the two types of FOS in Fe3+ sensing, a comparative study of the sensors is made, which reveals the superiority of the latter in many respects, such as smaller sensing length, use of a double detection scheme (for detecting both core and cladding modes) and higher sensitivity of cladding mode detection at an intermediate range of concentration along with the added advantage that plastic fibres are inexpensive. A detection limit of 1 ppb is observed in both types of fibre and the range of detection can be as large as 1 ppb–50 ppm. All the measurements are carried out using a LabVIEW set-up.

Evanescent wave fibre optic sensors for trace analysis of Fe3+ in water

In this communication, we discuss the details of fabricating an off-line fibre optic sensor (FOS) based on evanescent wave absorption for detecting trace amounts of Fe3+ in water. Two types of FOS are developed; one type uses the unclad portion of a multimode silica fibre as the sensing region whereas the other employs the microbent portion of a multimode plastic fibre as the sensing region. Sensing is performed by measuring the absorption of the evanescent wave in a reagent medium surrounding the sensing region. To evaluate the relative merits of the two types of FOS in Fe3+ sensing, a comparative study of the sensors is made, which reveals the superiority of the latter in many respects, such as smaller sensing length, use of a double detection scheme (for detecting both core and cladding modes) and higher sensitivity of cladding mode detection at an intermediate range of concentration along with the added advantage that plastic fibres are inexpensive. A detection limit of 1 ppb is observed in both types of fibre and the range of detection can be as large as 1 ppb–50 ppm. All the measurements are carried out using a LabVIEW set-up.

Evanescent wave fibre optic sensors for trace analysis of Fe3+ in water

In this communication, we discuss the details of fabricating an off-line fibre optic sensor (FOS) based on evanescent wave absorption for detecting trace amounts of Fe3+ in water. Two types of FOS are developed; one type uses the unclad portion of a multimode silica fibre as the sensing region whereas the other employs the microbent portion of a multimode plastic fibre as the sensing region. Sensing is performed by measuring the absorption of the evanescent wave in a reagent medium surrounding the sensing region. To evaluate the relative merits of the two types of FOS in Fe3+ sensing, a comparative study of the sensors is made, which reveals the superiority of the latter in many respects, such as smaller sensing length, use of a double detection scheme (for detecting both core and cladding modes) and higher sensitivity of cladding mode detection at an intermediate range of concentration along with the added advantage that plastic fibres are inexpensive. A detection limit of 1 ppb is observed in both types of fibre and the range of detection can be as large as 1 ppb–50 ppm. All the measurements are carried out using a LabVIEW set-up.

A fibre optic evanescent wave sensor used for the detection of trace nitrites in water

A fibre optic technique for detecting trace amounts of nitrite compounds in water is described. The off-line fibre optic sensor outlined here is based on evanescent field absorption in a test solution formed by the reaction of nitrite compounds in water with suitable chemical reagents. A short unclad portion of a plastic clad silica fibre acts as the sensing region. The experimental results clearly establish the usefulness of the present technique for detecting very low concentrations of the order of 1 ppb (parts per billion) of nitrite compounds with a large dynamic range of 1–1000 ppb. Such a high sensitivity enables the present device to be used for measuring the nitrite content in drinking water.