Solvent extraction separation of iron(III) and aluminium(III) from other elements with Cyanex 302

A rapid method was developed for the solvent extraction separation of iron(III) and aluminium(III) from other elements with Cyanex 302 in chloroform as the diluent. Iron(III) was quantitatively extracted at pH 2.0-2.5 with 5 x 10(-3) M Cyanex 302 in chloroform whereas the extraction of aluminium(III) was quantitative in the pH range 3.0-4.0 with 10 x 10(-3) M Cyanex 302 in chloroform. Iron(III) was stripped from the organic phase with 1.0 M and aluminium(III) with 2.0 M hydrochloric acid. Both metals were separated from multicomponent mixtures. The method was applied to the separation of iron and aluminium from real samples.     

Separation of large amounts of iron(III) from cobalt,nickel, and aliminum by combined ion exchange-solvent extraction

A method is described for the cation-exchange separation of large amounts of iron(III) from cobalt, nickel, and aluminium. On the strongly acidic Dowex 50-X8, iron(III) is not adsorbed from an 80% tetrahydrofuran-20% 3 M hydrochloric acid mixture, while cobalt, nickel, and aluminium are retained; a quantitative separation is thus possible. Cobalt and nickel or aluminium are then separated by elution with 90% tetrahydrofuran-10% 6 M hydrochloric acid. In these mixtures combined ion exchange-solvent extraction appears to occur; both ion exchange and liquid-liquid extraction are. effective simultaneously.     

Extraction chromatographic study of aluminium(III) and mutual separation of aluminium(III), gallium(III), indium(III) and thallium(III) with N-n-octylaniline

A selective method has been developed for extraction chromatographic studies of aluminium(III) and its separation from several metal ions with a chromatographic column containing N-n-octylaniline (liquid anion exchanger) coated on silanized silica gel as a stationary phase. The aluminium(III) was quantitatively extracted with the 0.065 mol/L N-n-octylaninine from 0.013 to 0.05 mol/L sodium succinate at a flow rate of 1.0 mL/min. The extracted metal ion has been recovered by eluting with 25.0 mL of 0.05 mol/L hydrochloric acid and estimated spectrophotometrically with aurintricarboxylic acid. The effects of the acid concentration, the reagent concentration, the flow rate and the eluting agents have been investigated. The log-log plots of distribution coefficient (KdAl(III)) versus N-n-octylaniline concentrationin 0.005 and 0.007 mol/L sodium succinate gave theslopes 0.5 and 0.7 respectively and showed theprobable composition of theextracted species was 1:1 (metal to amine ratio) and the nature of extracted species is [RR''NH2+ Al succinate2-] org. .The extraction of aluminium(III) was carried out in the presence of various ions to ascertain the tolerance limit of individual ions. Aluminium(III) has been separated from multicomponent mixtures, pharmaceutical samples and synthetic mixtures corresponding to alloys. A scheme for mutual separation of aluminium(III), indium(III), gallium(III) and thallium(III) has been developed by using suitable masking agents. The method is fast, accurate and precise.     

Chemical determination of some major constituents in rocks and minerals

Macro-analytical schemes are described for the determination of aluminium, total iron and iron(II), as part of the complete analysis of silicate rocks and minerals Solvent extraction eliminates interferences before titration of aluminium with DCTA Iron(III) is extracted with MIBK and determined indirectly with EDTA Iron(II) is determined by potentiometric titration under an inert atmosphere. Interferences are removed with 2,4-pentanedione and carbon tetrachloride before the determination of calcium and magnesium.     

Universelles Verfahren zur Bestimmung des Aluminiums in natürlichen Materialien und technischen Produkten

The paper outlines what may be considered a universally applicable procedure for the determination of aluminium. It is based on a complexometric titration according to the NaF demasking technique employing voltametric indication. This is normally preceeded by chloroform extraction of elements which react with cupferron in strongly acidic solutions [e.g. Ti, Zr, Nb Fe(III), rare earth elements] and extraction of the aluminium itself (in the form of its cupferron complex) from acetic acid solution, chloroform again being employed as solvent, to effect separation from the alkaline earths. This latter extraction is necessary only where alkaline earths, in particular Ca, are present in excess of aluminium. Examples of application and detailed instructions are given for the determination of aluminium in rocks, limestone, iron ores, complex nickel basis alloys and titanium alloys. Although additions to the standard procedure may become necessary for certain sample compositions the standard process itself remains unchanged regarding the titration step. A high grade of accuracy (standard deviation of 0,03 for 10% of Al) and a wide range of application (0.005% of Al in limestone to 45% Al in Bauxite) are the advantages of the method proposed.     

Determination of aluminium in molybdenum and tungsten metals, iron, steel and ferrous and non-ferrous alloys with pyrocatechol violet

A method for determining 0.001-0.10% of aluminium in molybdenum and tungsten metals is described. After sample dissolution, aluminium is separated from the matrix materials by chloroform extraction of its acetylacetone complex, at pH 6.5, from an ammonium acetate-hydrogen peroxide medium, then back-extracted into 12M hydrochloric add. Following separation of most co-extracted elements, except for beryllium and small amounts of chroinium(III) and copper(II), by a combined ammonium pyrrolidincdithiocarbamate-cupfen-on-chlorofonn extraction, aluminium is determined spectrophotometrically with Pyrocatechol Violet at 578 nm. Chromium interferes during colour development but beryllium, in amounts equivalent to the aluminium concentration, does not cause significant error in the results. Interference from copper(II) is eliminated by reduction with ascorbic acid. The proposed method is also applicable to iron, steel, ferrovanadium, and copper-base alloys after preliminary removal of the matrix elements by a mercury cathode separation.     

On-line aluminium preconcentration on chelating resin and its FIA-spectrofluorimetric determination in foods and dialysis concentrates

A new, sensitive and rapid spectrofluorimetric flow-injection method, is presented for the determination of trace levels of aluminium based on the formation of a fluorescent complex between aluminium and 5,7-dibromo-8-quinolinol (DBQ) and its extraction into diethylether (λ_exc = 400 nm, λ_em = 525 nm). Experimental conditions such as pH, reagent concentration, flow-rates, sample volume, extraction coil length, etc., have been optimized for on-line and batch procedures. The detection limits are 1 ppb and 0.3 ppb for batch and on-line systems respectively. The coeflicient of variation is 3.0% at the 4 ppb level for the FIA system. To remove interferences and to preconcentrate aluminium, a chelating resin microcolumn which was able to selectively complex A1(III) and was obtained by immobilizing Chromotrope 2B on AG1-X8 ion-exchange resin, was incorporated into the FIA system. The proposed method was successfully applied to determine aluminium in tap water, food samples and dialysis solutions.     

Spectrophotometric determination of trace amounts of iron(III) by extraction of the mixed-ligand iron-fluoride-purpurin complex

The characteristics of the mixed-ligand iron(III)-fluoride-purpurin complex, including optimum conditions of formation and extraction into methyl isobutyl ketone are described. A procedure for determination of trace amounts of iron in fluoride medium (0.5M) with purpurin (1,2,4,-trihydroxy-anthraquinone) in methyl isobutyl ketone is given. The method is suitable for determining iron in the presence of large amounts of aluminium, cyanide, phosphate and nickel.     

Determination of gallium in an iron-aluminium matrix by solvent extraction and flame emission spectroscopy

Solvent extraction of gallium(III) into methyl isobutyl ketone from hydrochloric acid solutions containing titanium (III) sulphate provides a rapid method for separation of gallium from an iron/aluminium matrix and may be employed to eliminate the interference of these elements in the flame emission spectrometric determination of gallium.     

Analytical applications of ternary complexes-VIII An improved reagent system for the spectrophotometric determination of aluminium

Aluminium ions form a ternary complex with Catechol Violet (CV) and cetyltrimethylammonium bromide (CTAB) in which an Al(3)+:CV:CTAB ratio of 1:2:5 is observed. The sensitivity of the binary complex between aluminium and Catechol Violet (615nm) = 1.50 x 10(3) l. mole (-1). mm(-1) is enhanced on ternary complex formation to (670nm) = 5.30 x 10(3) l. mole(-1). mm(-1). The colour is formed instantaneously, stabilizes within 20 min, and may be used for the detection of aluminium in the range O.27-54 pm in the presence of EDTA which prevents the interference of most ions. A benzoate extraction procedure for aluminium is used to prevent interference from hundredfold amounts of Cr(VI), Fe(II), Fe(III), Hg(II), Sb(III), Ti(IV) and acetate, but Be, Cr(III), rare earths, V(V), Zr and tartrate must be absent, as must high concentrations of phosphate and fluoride ions.     

Spectrophotometric determination of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection analysis

A cloud point preconcentration and flow injection (FI) analysis methodology for aluminium(III) determination has been developed. The analyte in the initial aqueous solution was complexed with Chrome Azurol S (CAS) in the presence of the cationic surfactant benzyldimethyltetradecylammonium chloride (BDTAC). The absorption spectroscopic characteristics of the ternary complex [Al(III)-CAS-BDTAC] were examined in detail. The preconcentration step was carried out by means of the non-ionic surfactant polyethylene glycol p-nonylphenyl ether (PONPE 7.5). The enriched analyte solution was injected into an FI system using an HPLC pump. The chemical variables affecting the analytical performance of the combined methodology were studied and optimised. The developed approach was successfully applied to the determination of trace amounts of aluminium in parenteral solutions without previous treatment. Under the optimum experimental conditions, 99.9% extraction was achieved for a preconcentration factor of 50. The limit of detection was 1.12 x 10(-7) mol(-1). The calibration plot was linear over at least two orders of magnitude of aluminium concentration. The developed coupled methodology, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate for monitoring the aluminium concentration in parenteral nutrition.     

Catalytic-kinetic absorptiostat technique with the indigo carmine—hydrogen peroxide reaction as the indicator reaction

The absorptiostat method previously described is used for the catalytic-kinetic determination of sulphur compounds (sulphide, thioacetamide. thiourea and thiosulphate) in the micromolar range by means of their catalytic action for the indigo carmine—hydrogen peroxide indicator reaction. The thiosulphate catalyst is activated by iron(III) or aluminium(III); aluminium(III) is deactivated by fluoride. On this basis, iron(III) is determined in the ng range, and aluminium(III) and fluoride in the μg range.     

Extraktion von Eisen mit Methyl?thylketon

Zusammenfassung Eisen(III) wird mit Methyläthylketon aus salzsauren Lösungen extrahiert und der optimale Bereich der für eine quantitative Extraktion erforderlichen Säurekonzentration bestimmt. Die meisten Elemente der III. analytischen Gruppe werden hinsichtlich ihrer Extrahierbarkeit mit dem Keton untersucht und die Vorteile dieser Verbindung aufgezeigt. Eine Trennung des Eisens von mehreren Metallen ist möglich. Beschrieben wird eine Eisen-Aluminium- und Eisen-Mangan-Trennung.

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Extraction of iron with methylethylketon

The extraction of iron(III) with methylethylketone as solvent from hydrochloric acid solution is described, and the maximum range of acid concentration for quantitative extraction determined. Most of the elements of the third analytical group were investigated according to their extractability with this ketone, and the advantages of this compound are illustrated. Separation of iron from several other elements is possible. The separation from aluminium and manganese is described.

     

Fluorimetric determination of aluminium in serum

A convenient fluorimetric method for the routine determination of aluminium in serum has been developed using lumogallion [4-chloro-3-(2,4-dihydroxyphenylazo)-2-hydroxybenzene-1-sulphonic acid]. Losses of aluminium during deproteinisation of the serum were prevented by treatment with a combination of 20 or 30% m/V trichloroacetic acid (TCA) and 5% m/VTCA. Iron(III) was removed by extraction into chloroform with capriquat (methyltrioctylammonium chloride) as an Fe3+-lumogallion-capriquat ternary complex. The interference from Cu2+ was eliminated by using thiosulphate as a masking agent. The detection limit was 3.6 ng ml-1 and the calibration graph was linear up to 1.4 micrograms ml-1 of aluminium. Using the proposed method, the average concentration of aluminium in the serum of healthy subjects was found to be 6.8 ng ml-1, in agreement with values reported in the literature.     

Determination of aluminium(III) in water samples in a microemulsion system by spectrofluorimetry

The sensitizing effect of cetyltrimetrylammonium bromide (CTAB) microemulsion media on the determination of aluminium(III) by spectrofluorimetry was developed. The main factors affecting the determination were investigated in detail. The results showed that 8-hydroxyquinoline (HQ) react with aluminium(III) forming a complex with fluorescence in the system of potassium acid phthalate-NaOH buffer solution at pH 6.0, the maximum excitation and emission wavelengths are at 380.0 and 502.6 nm, the sensitizing effect of CTAB microemulsion is higher than that of CTAB micelle. The proposed method has been applied to the determination of aluminium(III) in tap water and lake water samples with satisfactory results.     

Separation and analysis of aluminium(III) by cation exchange ion chromatography

A method for the determination of aluminium(III) ions based on separation by cation exchange column chromatography and detection by conductivity detector has been developed. It is fast and reliable, and can be used for the separation and analysis of aluminium(III) ions from other metal ions like Mg(II), Mn(II), Zn(II), Co(II), Ca(II), Sr(II), rare earth elements like Lu(III), Tm(III), and Gd(III), which are eluted at different times and so do not interfere. Effect of p-phenylene diamine concentration present in the eluent, presence of other metal ions and effect of various anions present in the injection sample on the separation and analysis of aluminium(III) ions have also been studied.     

Spectrophotometric and derivative spectrophotometric determination of aluminium with Hydroxynaphthol Blue

The reaction of aluminium(III) with Hydroxynaphtol Blue (HNB) in aqueous media at apparent pH 5.5 results in a red complex that is stable for at least 4 hr. Beer's Law is obeyed up to 1.6 microg/ml of aluminium(III) with an apparent molar absorptivity of 1.66 x 10(4) l.mol(-1). cm(-1) at 569 nm. This paper proposes procedures for aluminium(III) determination by ordinary and first-derivative spectrophotometry. The results demonstrated that the linear dynamic range is 0.03-1.60 microg/ml for ordinary spectrophotometry and 11.8-320.0 ng/ml for first derivative spectrophotometry. The HNB is not selectivity for aluminium, but the addition of EDTA allows the aluminium determination in the presence of accepted amounts of Ca(II), Mg(II), Mn(II), Ba(II), Sr(II), Cd(II), Pb(II), La(III), In(III), Bi(III) and Zn(II). The interference of Cu(II) and Hg(II) can be masked by thiosulphate. Ions such as UO(2)(II), Mo(VI), Co(II), Ti(IV) and PO(4)(III) do interfere seriously. This method was applied for aluminium determination in copper-base alloy, zinc-base alloy, magnesium-base alloy, iron ore, manganese ore, cement, dolomite, feldspar and limestone. The results indicated high accuracy and precision.     

The effect of combinations of aluminium(III) oxides and decabromobiphenyl on the flammability of and smoke production from acrylonitrile-butadiene-styrene terpolymer

Studies have been made of the flammability [expressed in terms of the limiting oxygen index (LOI)] and the smoke-forming tendency [expressed in terms of the maximum smoke density (D_s)] of systems containing widely varying proportions of an acrylonitrile-butadiene-styrene terpolymer (ABS), decabromobiphenyl (DBB) and (a) anhydrous aluminium(III) oxide, (b) aluminium(III) oxide monohydrate and (c) aluminium(III) oxide trihydrate. The values of LOI and D_s have been plotted by polynomials up to the fourth order and plotted in triangular diagrams. The optimum aluminium/halogen atomic ratios for flame retardance are different for the three oxides. Flame-retardant synergism has been observed, however, between all three oxides and DBB and is particularly marked with anhydrous alumina and the halogen compound. All the systems also give a significant degree of smoke-suppression. Simultaneous thermal analyses strongly suggest that the flame-retardant action of the aluminium compounds is not purely physical and is largely confined to the condensed phase.     

Fluorimetric determination of trace amounts of aluminium and gallium with salicylaldehyde-1-phthalazinohydrazone

Fluorimetric determinations of aluminium and gallium, based on the formation of fluorescence complexes between Al(III) or Ga(III) and salicylaldehyde-1-phthalazinohydrazone, SAPhH, are proposed. The Al(III)-SAPhH complex exhibits fluorescence with maximum emission at 475 nm when excited at 414 nm; the Ga(III)-SAPhH chelate has emission and excitation maxima at 480 and 410 nm, respectively. For both determinations the range of application is 10–100 ng/ml. Aluminium has been determined in waters, and gallium in aluminium and nickel alloys.