Cadmium determination water

In addition to systems of the above type, i.e. involving adduct formation, various other types of synergistic extraction systems are recognised and have been reviewed.4 An example is the synergistic influence of zinc in the extraction and A AS determination of trace cadmium in water.5... 

The first prototype of a technologically improved IWAO was developed and tested with a membrane based on a new H+-selective ketocyanine dye and a commercial cadmium ionophore [39]. Its incorporation in an IWAO allows a highly sensitive and portable optical system to be obtained for an situ chemical analysis as well. The authors propose a flow injection analysis (FIA) system for the determination of cadmium in water samples using a cadmium-selective IWAO, as an alternative method to the ones generally used in analytical control laboratories. It permits enhanced sensitive signals in short response times by taking advantage of the very thin membranes deposited over the circuit. 

The APDC—MIBK extraction system is widely used to determine a variety of metals in water. In both the U.K. [6, 7] and the U.S.A. [8] it is the standard method for the determination of lead and cadmium in water. It is also used as a standard method [8] in the determination of hexavalent chromium. In order to determine total chromium, trivalent chromium is oxidised to hexavalent chromium by bringing the sample to the boil and adding sufficient potassium permanganate solution (0.1 N) dropwise to give a persistent pink colour while the solution is boiled for 10 min. 

Potassium iodide solution, 0.1 M for cadmium determination Dissolve 1.66 g of KI in water and dilute to 100 ml prepare fresh daily. 

Pommery, J., Ebenga, J. P., Imbenotte, M., Palavitt, G., and Erb, F. (1988). Determination of the complexing ability of a standard humic acid with cadmium ions. Water Res. 22, 185-189. 

Chirila E. and Carazeanu I., 2001 Cadmium determination in water, fish and sediment of Tabacarie lake, Ovidius University Annals of Chemistry, 12,17-19. 

Fig. 8.2 Total concentrations and partitioning of Cd in a tidal flat sediment profile in the Heuckenlock areas near Hamburg. Sedimentation rates were determined using the Cs-method. Cadmium pore water profile was determined at low tide (Kersten 1989).

In view of the high toxicity of cadmium it is necessary to be able to determine very small concentrations in water. AAS techniques (Sections 3.4.7.1 and 3.4.7.2) are particularly suitable for determining cadmium in water. Where no AAS facilities are available, it is still possible to use the classical spectrophotometric technique (Section 3.4.7.3) with dithizone and extraction in chloroform. 

C. Henriquez, L.M. Laglera, M.J. Alpizar, J. Calvo, F. Arduini, V. Cerd Cadmium determination in natural water samples with an automatic multisyringe flow injection system coupled to a flow-through screen printed electrode, Talanta 96 (2012) 140—146. 

Brombenztiazo (BBT) is known to be one of the best reagents for extraction-photometric determination of cadmium(II). The reagent also fonus complexes with Co(II), Cu(II), Fe(II), Ni(II), Zn(II). The aim of this work was to develop a solid-phase reagent on the base of BBT immobilized on silica gel for sorption-spectroscopic and visual test determination of Cadmium, and also for soi ption-atomic-adsoi ption determination of total heavy metals contents in natural waters. 

Theory. Conventional anion and cation exchange resins appear to be of limited use for concentrating trace metals from saline solutions such as sea water. The introduction of chelating resins, particularly those based on iminodiacetic acid, makes it possible to concentrate trace metals from brine solutions and separate them from the major components of the solution. Thus the elements cadmium, copper, cobalt, nickel and zinc are selectively retained by the resin Chelex-100 and can be recovered subsequently for determination by atomic absorption spectrophotometry.45 To enhance the sensitivity of the AAS procedure the eluate is evaporated to dryness and the residue dissolved in 90 per cent aqueous acetone. The use of the chelating resin offers the advantage over concentration by solvent extraction that, in principle, there is no limit to the volume of sample which can be used. 

Insoluble fluorosilicates are brought into solution by fusion with four times the bulk of fusion mixture, and extracting the melt with water. In either case, the solution is treated with a considerable excess of ammonium carbonate, warmed to 40 °C, and, after standing for 12 hours, the precipitated silicic acid is filtered off, and washed with 2 per cent ammonium carbonate solution. The filtrate contains a little silicic acid, which may be removed by shaking with a little freshly precipitated cadmium oxide. The fluoride in the filtrate is determined as described in Section 11.59. 

This procedure has been utihzed to determine metal cations and anions in water sample [48,50,51], titanium in high-speed steel at a concentration level of 25 3 mg/g [22], heavy metals (20 to 400 mg/1) in electroplating waste waters [25], copper and nickel (5 mg/1) in metal electroplating baths on wedge-shaped plates [44], copper, lead, cadmium, or mercury in vegetable juices [29], and nickel (1 to 3.8 mg/1) in electroplating waste water of lock industries [42,47]. 

Quevauviller Ph, Kramer KJM, Vinhas T (1996) Certified reference material for the quality control of cadmium, copper, nickel and zinc determination in estuarine water (CRM 505). Fresenius J Anal Chem 354 397-404. 

Spencer and Brewer [144] have reviewed methods for the determination of nitrite in seawater. Workers at WRc, UK [ 145] have described an automated procedure for the determination of oxidised nitrogen and nitrite in estuarine waters. The procedure determines nitrite by reaction with N-1 naphthyl-ethylene diamine hydrochloride under acidic conditions to form an azo dye which is measured spectrophotometrically. The reliability and precision of the procedure were tested and found to be satisfactory for routine analyses, provided that standards are prepared using water of an appropriate salinity. Samples taken at the mouth of an estuary require standards prepared in synthetic seawater, while samples taken at the tidal limit of the estuary require standards prepared using deionised water. At sampling points between these two extremes there will be an error of up to 10% unless the salinity of the standards is adjusted accordingly. In a modification of the method, nitrate is reduced to nitrite in a micro cadmium/copper reduction column and total nitrite estimated. The nitrate content is then obtained by difference. 

Pruszkowska et al. [135] described a simple and direct method for the determination of cadmium in coastal water utilizing a platform graphite furnace and Zeeman background correction. The furnace conditions are summarised in Table 5.1. These workers obtained a detection limit of 0.013 pg/1 in 12 pi samples, or about 0.16 pg cadmium in the coastal seawater sample. The characteristic integrated amount was 0.35 pg cadmium per 0.0044 A s. A matrix modifier containing di-ammonium hydrogen phosphate and nitric acid was used. Concentrations of cadmium in coastal seawater were calculated directly from a calibration curve. Standards contained sodium chloride and the same matrix modifier as the samples. No interference from the matrix was observed. 

Stolzberg [143] has reviewed the potential inaccuracies of anodic stripping voltammetry and differential pulse polarography in determining trace metal speciation, and thereby bio-availability and transport properties of trace metals in natural waters. In particular it is stressed that nonuniform distribution of metal-ligand species within the polarographic cell represents another limitation inherent in electrochemical measurement of speciation. Examples relate to the differential pulse polarographic behaviour of cadmium complexes of NTA and EDTA in seawater. 

Cabezon et al. [662] simultaneously separated copper, cadmium, and cobalt from seawater by coflotation with octadecylamine and ferric hydroxide as collectors prior to analysis of these elements by flame atomic absorption spectrometry. The substrates were dissolved in an acidified mixture of ethanol, water, and methyl isobutyl ketone to increase the sensitivity of the determination of these elements by flame atomic absorption spectrophotometry. The results were compared with those of the usual ammonium pyrrolidine dithiocarbamate/methyl isobutyl ketone extraction method. While the mean recoveries were lower, they were nevertheless considered satisfactory. 

Campbell and Ottaway [672] have described a simple and rapid method for the determination of cadmium and zinc in seawater, using atomic absorption spectrometry with carbon furnace atomisation. Samples, diluted 1 + 1 with deionised water, are injected into the carbon furnace and atomised in an HGA-72 furnace atomiser under gas-stop conditions. A low atomisation temperature... 

Stein et al. [673] have described a simplified, sensitive, and rapid method for determining low concentrations of cadmium, lead, and chromium in estuarine waters. To minimise matrix interferences, nitric acid and ammonium nitrate are added for cadmium and lead only nitric acid is added for chromium. Then 10,20, or 50 pi of the sample or standard (the amount depending on the sensitivity required) is injected into a heated graphite atomiser, and specific atomic absorbance is measured. Analyte concentrations are calculated from calibration curves for standard solutions in demineralised water for chromium, or an artificial seawater medium for lead and cadmium. 

Brugmann et al. [680] compared three methods for the determination of copper, cadmium, lead, nickel, and zinc in North Sea and northeast Atlantic waters. Two methods consisted of atomic absorption spectroscopy but with preconcentration using either freon or methyl isobutyl ketone, and anodic stripping voltammetry was used for cadmium, copper, and lead only. Inexplicable discrepancies were found in almost all cases. The exceptions were the cadmium results by the two atomic absorption spectrometric methods, and the lead results from the freon with atomic absorption spectrometry and anodic scanning voltammetric methods. 

De Kersabiec et al. [708] have described a Zeeman method for the determination of copper, lead, cadmium, cobalt, nickel, and strontium in brines and in the soil water adjacent to the Red Sea. 

Unlike halogenated solvents, it does not produce noxious substances in the inductively coupled plasma, has a very low aqueous solubility, and yields hundredfold concentration in one step. Detection limits ranged from 0.02 jtg/l (cadmium) to 0.6 pg/1 (lead). The results indicate that the proposed procedure should be useful for the precise determination of metals in oceanic water, although a higher sensitivity would be necessary for lead and cadmium. 

A comparison was carried out on the results obtained using ICP-AES and AAS for eight elements in coastal Pacific Ocean water. The results for cadmium, lead, copper, iron, zinc, and nickel are in good agreement. For iron, the data obtained by the solvent extraction ICP method are also in good agreement with those determined directly by ICP-AES. In most of the results the relative standard deviations were 4% for all elements except cadmium and lead, which had relative standard deviations of about 20% owing to the low concentrations determined. 

Berndt et al. [740] have shown that traces of bismuth, cadmium, copper, cobalt, indium, nickel, lead, thallium, and zinc could be separated from samples of seawater, mineral water, and drinking water by complexation with the ammonium salt of pyrrolidine- 1-dithiocarboxylic acid, followed by filtration through a filter covered with a layer of active carbon. Sample volumes could range from 100 ml to 10 litres. The elements were dissolved in nitric acid and then determined by atomic absorption or inductively coupled plasma optical emission spectrometry. 

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