Determination of copper

Discussion. Copper(II) ions are quantitatively reduced in 2M hydrochloric acid solution by means of the silver reductor (Section 10.140) to the copper(I) state. The solution, after reduction, is collected in a solution of ammonium iron(III) sulphate, and the Fe2+ ion formed is titrated with standard cerium(IV) sulphate solution using ferroin or AT-phenylanthranilic acid as indicator. 

Comparatively large amounts of nitric acid, and also zinc, cadmium, bismuth, tin, and arsenate have no effect upon the determination the method may therefore be applied to determine copper in brass. 

Procedure (copper in crystallised copper sulphate). Weigh out accurately about 3.1 g of copper sulphate crystals, dissolve in water, and make up to 250 mL in a graduated flask. Shake well. Pipette 50 mL of this solution into a small beaker, add an equal volume of ca AM hydrochloric acid. Pass this solution through a silver reductor at the rate of 25 mL min i, and collect the filtrate in a 500 mL conical flask charged with 20 mL 0.5M iron(III) ammonium sulphate solution (prepared by dissolving the appropriate quantity of the analytical grade iron(III) salt in 0.5M sulphuric acid). Wash the reductor column with six 25 mL portions of 2M hydrochloric acid. Add 1 drop of ferroin indicator or 0.5 mL N-phenylanthranilic acid, and titrate with 0.1 M cerium(IV) sulphate solution. The end point is sharp, and the colour imparted by the Cu2+ ions does not interfere with the detection of the equivalence point. 

Procedure (copper in copper(I) chloride). Prepare an ammonium iron(III) sulphate solution by dissolving 10.0 g of the salt in about 80 mL of 3 M sulphuric acid and dilute to 100 mL with acid of the same strength. Weigh out accurately about 0.3 g of the sample of copper(I) chloride into a dry 250 mL conical flask and add 25.0 mL of the iron(III) solution. Swirl the contents of the flask until the copper(I) chloride dissolves, add a drop or two of ferroin indicator, and titrate with standard 0.1 M cerium(IV) sulphate. 

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The electrodes have a wide linear response range to CrP" and Ni " ions concentration. For this reason, they are adequate for the potentiometric determinations of copper and nickel ions in diluted solutions (dilutions may go down to 10 M) as well as in checking the industrial waters. 

NEW FLUORESCENCE QUENCHING METHOD FOR DETERMINATION OF COPPER (II) IN WATER... 

In order to find optimal conditions for the soluble copper determination we examined the influence of electrolysis potential, electrolysis time, and the solution stirring rate on the accuracy and sensitivity of determination. We found that the optimal parameters for PSA determination of copper were electrolysis potential of -0.9 V vs. 3.5 mol/dm Ag/AgCl, electrolysis time of 300 s, and solution stirring rate of 4000 rpm. The soluble copper content in samples investigated in this study varied from 1.85 to 4.85 ppm. Very good correlation between the copper content determined by PSA and AAS indicated that PSA could be successfully applied for the soluble copper content determination in various dental materials. 

THE DETERMINATION OF COPPER MICROAMOUNTS ON THE TERBIUM LUMINESCENCE SENSITIZED BY IT IN HETEROBINUCLEAR COMPLEX... 

Discussion. Neo-cuproin (2,9-dimethyl-l,10-phenanthroline) can, under certain conditions, behave as an almost specific reagent for copper(I). The complex is soluble in chloroform and absorbs at 457 nm. It may be applied to the determination of copper in cast iron, alloy steels, lead-tin solder, and various metals. 

Determination of copper as copper(I) thiocyanate Discussion. This is an excellent method, since most thiocyanates of other metals are soluble. Separation may thus be effected from bismuth, cadmium, arsenic, antimony, tin, iron, nickel, cobalt, manganese, and zinc. The addition of 2-3 g of tartaric acid is desirable for the prevention of hydrolysis when bismuth, antimony, or tin is present. Excessive amounts of ammonium salts or of the thiocyanate precipitant should be absent, as should also oxidising agents the solution should only be slightly acidic, since the solubility of the precipitate increases with decreasing pH. Lead, mercury, the precious metals, selenium, and tellurium interfere and contaminate the precipitate. 

The effect of different ions upon the titration is similar to that given under iron(III) (Section 17.57). Iron(III) interferes (small amounts may be precipitated with sodium fluoride solution) tin(IV) should be masked with 20 per cent aqueous tartaric acid solution. The procedure may be employed for the determination of copper in brass, bronze, and bell metal without any previous separations except the removal of insoluble lead sulphate when present. 

J. "Determination of Copper In Serum With a Graphite Rod Atomizer for Atomic Absorption Spectrophotometry". Anal. Chlm. Acta (1971), 263-269. 

Stevens, B. J. "Biological Applications of the Carbon Rod Atomizer In Atomic Absorption Spectroscopy. 2. Determination of Copper In Small Samples of Tissue". Clin. Chem. (1972), 18, 1379-1384. 

Inoue, H. et al., Determination of copper(II) chlorophyllin by reversed-phase high-performance liquid chromatography, J. Ghromatogr. A, 679, 99, 1994. 

Carrion N, De Behzo ZA, Moreno B, Fernandez EJ, Flores D (1988) Determination of copper, chromium, iron and lead in pine needles by electrothermal atomisation spectrometry with slurry sample introduction. J Anal At Spectrom 3 479-483. 

Allen LB, Siitonen PH, Thompson HC Jr. 1998. Determination of copper, lead, and nickel in edible oils by plasma and furnace atomic spectroscopies. Journal of the American Oil Chemists Society 75(4) 477-481. 

Hardcastle JL, Compton RG (2001) The electroanalytical detection and determination of copper in heavily passivating media ultrasonically enhanced solvent extraction by N-benzoyl-N-phenyl-hydroxylamine in ethyl acetate coupled with electrochemical detection by sono-square wave stripping voltammetry analysis. Analyst 126 2025-2031... 

Freeman J.E., Childers A.G., Steele A.W., Hieftje G.M., A fiber-optic absorption cell for remote determination of copper in industrial electroplating baths, Anal. Chim. Acta 1985 177 21. 

A hanging mercury drop electrodeposition technique has been used [297] for a carbon filament flameless atomic absorption spectrometric method for the determination of copper in seawater. In this method, copper is transferred to the mercury drop in a simple three-electrode cell (including a counterelectrode) by electrolysis for 30 min at -0.35 V versus the SCE. After electrolysis, the drop is rinsed and transferred directly to a prepositioned water-cooled carbon-filament atomiser, and the mercury is volatilised by heating the filament to 425 °C. Copper is then atomised and determined by atomic absorption. The detection limit is 0.2 pg copper per litre simulated seawater. 

Marvin et al. [302] have discussed the effects of sample filtration on the determination of copper in seawater, and concluded that glass filters could seriously affect the reliability of subsequent analysis. 

Rodionova and Ivanov [667] used chelate extraction in the determination of copper, bismuth, lead, cadmium, and zinc in seawater. The metal complexes of diethyl and dithiophosphates are extracted in carbon tetrachloride prior to determination by atomic absorption spectrometry. 

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. 

The results demonstrate that cadmium can be determined directly the direct determination of copper, manganese, and chromium is also possible, but their application is more limited than cadmium. The lead and nickel determination proved to be the most difficult, since their determination is limited by their low sensitivity and by the overlap of their absorption profiles with the background absorbance generated by seawater matrix. The direct determination of lead and nickel by this technique can be used only for seawater samples taken in coastal or estuarine zones that are quite polluted. 

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