Multi-element speciation of trace metals in fresh water adapted to plasma source mass spectrometry (original) (raw)
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Microchemical Journal, 2014
This article describes the application of on-line isotope dilution mass spectrometry with inductively coupled plasma (OID-ICP-MS) to the field of trace metal analysis (B, Cd, Cr, Fe, Ni, Pb and Zn) in water samples by the certified reference material (CRM) characterization. Drinking, natural and waste water certified reference materials were analyzed. Emphasis is placed on OID-ICP-MS measurements of highest analytical quality and their validation against direct external calibration mass spectrometry with inductively coupled plasma analysis (ICP-MS). Differences in the calibration strategies such as single OID-ICP-MS versus direct external calibration ICP-MS were discussed. In general, it can be stated that OID-ICP-MS offers high accurate and precise results with small measurement uncertainties, when properly applied, compared to external calibration. Thus, OID-ICP-MS proved to be an ideal solution for routine water sample analysis, increasing sample throughput without any previous sample handling and improving the quality and reliability of the analytical results.
Hydrochemical balance studies require knowledge on the speciation of the elements concerned, i.e. the distribution between soluble and suspended forms and among different soluble species. The present paper is focused on the separation of truly soluble forms of trace elements from the fraction associated with the particulate phase in natural fresh waters. The commonly used filtration through a 0.45 pm membrane is not satisfactory in this respect. Improvements can be achieved by introducing alternative separation techniques such as ultrafiltration, centrifugation, dialysis in slta or in the laboratory, electrodialysis, free-liquid electrophoresis, or a combination of separation steps based on these techniques. In general separations that can be carried out at the sampling site are preferable. In this paper each of the above mentioned separation techniques will be critically discussed regarding their feasibility for speciation studies in natural waters, and examples from applications to groundwaters, lakes and rivers will be given, mainly from work carried out by the authors.
2001
A method has been developed for the determination of Cd (II), Cu (II), Mn (II), Ni (II), Pb (II) and Zn (II) in natural waters by ind uctively coupled plasma-atomic emission spectrometry after pre-concentration by solvent extraction with piperidine dithiocarbamate (pipDTC). The metals are complexed with pipDTC and the complexes extracted into isobutyl methyl ketone and subsequently back-extracted into nitric acid. Metals in nitric ac id have been determined by aspirating into argon plasma of lCP-AES. The method has been applied for the dete rmination of the tested metal ions in natural waters.
Journal of Analytical Atomic Spectrometry, 1988
The remarkable detection power of inductively coupled plasma mass spectrometry (ICP-MS) was demonstrated b y the analysis of an open ocean sea water reference material (with the acronym NASS-2). A 50-fold pre-concentration of several trace metals in the sea water was realised b y their adsorption o n t o silica-immobilised 8-hydroxyquinoline, which separates the elements of interest f r o m the bulk of the alkali and alkaline earth elements. The isotope dilution technique was used for the determination of seven elements (Ni, Cu, Zn, Mo, Cd, Pb and U). Accurate results were obtained for all of these elements except for Mo, with concentrations ranging between 0.027 and 11.5 pg 1-1.
Chemical Speciation of Heavy Metals in Ground and Surface Waters
The 2008 Annual Meeting, 2008
Metal speciation in natural waters is of increasing interest and importance because of toxicity, bioavailability, and environmental mobility. Biogeochemical behavior and potential risk in general are strongly dependent on the chemical species of metals. The present study aims to determine the distribution of chemical species of dissolved heavy metals in shallow and deep aquifers and surface waters from Buddha nala stream and Sutlej River of Punjab, north-west India. Attempt was also made to identify different possible minerals that may control the solubility of elements in these aqueous solutions. The study was performed at village Walipur in Ludhiana ( 30 0 55 / N, 75 0 54 / E) district of Punjab, north-west India, where Buddha nala surface water stream loaded with heavy metals from municipal waste and Industrial effluents contaminate underground water. A sutlej River also flowed a couple of Km from the village site. Ground water samples were collected at four different occasions from the same sites of shallow aquifer (45 feet deep) and deep aquifer (200 feet deep) by the already installed hand pump and tube well adjacent to Buddha nala stream. Before sampling the water was drawn for half an hour to empty the hand pump and tube well pipes in order to collect the fresh water from the shallow and deep aquifers, respectively. Surface water samples on four different occasions were also taken from Buddha nala stream and Sutlej River. Polyethylene bottles of 50 ml volumes were used for collection of water samples. These bottles were repeatedly washed with the water to be sampled. Bottles were fully filled with water and closed avoiding air bubbles. Field measurements of redox potential (Eh) were also made at the time of water sampling. The redox meter checked with Zobell's solution several times during the investigation period. Water samples were taken from each location and brought back to Laboratory at Punjab Agricultural University for further analyses. The samples were put in a cooled ice box during transportation and stored in refrigerator until analysis (at 5 0 C). The pH of water samples was determined using Elico model L 110 glass electrode in combination with calomel as reference electrode on pH meter. The electrical conductivity of water samples was measured by Elico model CM-84 Conductivity Bridge. The carbonates and bicarbonates concentrations were measured by titration a known volume of water against standard sulfuric acid using phenolphthalein and methyl red as indicators respectively. The chloride concentration in water samples were measured by titrating with a known volume against standard N/40 silver nitrate solution using potassium chromate as indicator. All samples were filtered and acidified prior to analysis. The acidified water samples were analyzed for Cadmium, Nickel, Lead, Zinc, copper, Iron, Manganese and sulfur on Inductively Coupled Argon Plasma of Thermo Electron corporation iCAP 6000 series. Mean of Metals and dominant anions composition of waters determined after four occasions for different sites are listed in . The higher concentration of Cd, Cu,Fe, Mn, Ni, and Pb in waste water of Buddha nala stream must be due to disposal of Industrial effluents. The ionic strength of waste water was also three times more than other water sources. Comparatively high concentration of Zinc (16.10 uM) was measured in water of shallow aquifer than water of deep aquifer and surface water of Buddha nala stream and Sutlej River. The geochemical speciation model Visual MINTEQA2 Version 3.11 was used to calculate the equilibrium concentrations of dissolved species for four solutions, representing the range of water compositions encountered in the shallow and deep aquifers as well as in surface waters of Buddha nala
Microchimica Acta, 2005
The strong cation exchanger Dowex 50W-x4 was used for the enrichment of traces of Cd, Co, Cu, Fe, Ni, Pb and Zn in mineral and mine waters as an alternative to the commonly applied procedures based on the application of chelating resins. The resin used was found suitable for complete retention of these metals both from the solutions of very low pH as well as those close to neutral, thus eliminating the need to buffer the samples. An analytical scheme based on filtration and solid phase extraction with Dowex 50W-x4 was proposed for partitioning Cd, Co, Cu, Fe, Ni and Pb in the examined waters. The fraction of metals associated with the suspended particles was determined after filtration through a 0.45 mm pore size filter and decomposition of the deposited matter. For the evaluation of fractions of the labile metal species and the total dissolved metals, the untreated filtrates and the solutions resulting from their digestion, respectively, were passed through Dowex 50W-x4 cation exchange columns. The retrieval of the metals was completed using a 4.0 mol L À1 solution of HCl. The described metal preconcentration and fractionation protocol offered the enrichment factor of 25 with detection limits equal to 22, 30, 92, 41, 70, 36 and 340 ng L À1 , respectively for Cd, Co, Cu, Fe, Ni and Pb. Reasonably good precision and accuracy were attained.
Analytical Relevance of Trace Metal Speciation in Environmental and Biophysicochemical Systems
American Journal of Analytical Chemistry, 2013
This article presents a review of the analytical relevance of trace metal speciation analysis, which must be considered in environmental and biophysicochemical systems for reliable and efficient assessment and monitoring of trace metals. Examples are given of methodological approaches used for speciation analysis. An overview of speciation analysis in sediments, aquatic ecosystems and agrosystems is also presented.
Water Air and Soil Pollution, 2020
A sensitive, specific, precise, accurate, and fast method Swas suitably developed for the determination of selected heavy metals including Cd, Cu, Fe, Pb, and Zn in tap water samples by inductivity coupled plasma-optical emission spectrometry (ICP-OES) after pre-concentration using Chelex-100 ion exchange resin. This method is based on studying several parameters including pH, weight of Chelex-100, HNO 3 concentration, flow rate, and column diameter. It was found that the suitable conditions used for pH, weight of Chelex-100, HNO 3 concentration, flow rate, and column diameter were 6, 4 g, 2 M, 1 mL/min, and 1 cm, respectively. Under these conditions, high recoveries were achieved with values of 95%, 106%, 77%, and 91% for Cu, Fe, Pb, and Zn, respectively. A total of 90 tap water samples were collected from five sampling zones of Irbid City, North Jordan, including (A: Barha zone; B: West and Zabda zone, C: South zone, D: East and city center zone, and E: North zone), and analyzed for Cd, Cu, Fe, Pb, and Zn; also the pH and electric conductivity (EC) values were measured. Moreover, the correlations between metals' concentrations and type of tanks (iron, plastic, or semantic), type of pipes (iron or plastic), age of tanks, and age of pipes were evaluated. The mean concentrations of tested metals in tap water samples collected from zone A, zone B, zone C, zone D, and zone E, respectively, were the following: Cu (9.
Speciation and Bioavailability of Trace Metals in Water: Progress Since 1982
Australian Journal of Chemistry, 2004
The advances in studies of trace metal speciation and bioavailability since Mark Florence’s 1982 review of the topic, published in Talanta, have been comprehensively reviewed. While the relative merits of kinetic and equilibrium approaches are still being determined, advances in the applications of stripping voltammetry, including the application of microelectrodes and an appreciation of detection windows in both CSV and ASV, have been matched by the introduction of new dynamic techniques including diffusive gradients in thin films (DGTs), permeation liquid membranes (PLMs), and improved applications of chelating resins. There have also been improvements in equilibrium techniques such as ion-selective electrodes and Donnan dialysis. The ability of geochemical speciation models to predict metal complexation by natural organic matter has greatly improved, yet the models still require validation against field measurements. More reliable and relevant bioassays have been developed using ...