Dosage des traces de gallium dans les bauxites et produits dérivés

A method for the estimation of gallium in bauxites and derived products, has been described. The gallium is estimated fluorimetrically in chloroform solution as the oxmate. The interfering ions and the means of their removal have been studied.The method allows the estimation of 1.4–4.2 γ of gallium with an accuracy of about 10%.     

Dosage colorimetrique du zinc dans le gallium de haute purete

A method for the determination of traces of zinc in high-purity gallium is proposed. The sample is dissolved in hydrochloric acid, the reaction being catalysed by platinum, and gallium is extracted as its chloro complex with ether; losses of zinc during this operation are determined radiochemically with ⁶⁵Zn as tracer. Zinc is then separated from other impurities in gallium by two extractions with dithizone, and determined colorimetrically as the dithizonate after excess of reagent has been removed. The limit of sensitivity of the method is 0.04 p.p.m.     

衬钽管石墨炉原子吸收法测定痕量镓时基体改进剂的研究及应用

提出用钒和铜混合基体改进剂衬钽管石墨炉原子吸收测定镓的方法。衬钽管使镓的灵敏度提高6倍左右,钒和铜混合基体改进剂不仅能进一步提高灵敏度,而且能提高灰化温度,降低原子化温度,增强抗干扰能力。测定 GSD 标准样品中的镓时,不需对样品进行预分离即可直接进行测定,结果与参考值相符。     

Determination of gallium by square-wave voltammetry anodic stripping, based on the electrocatalytic action of 2,2'-bipyridine in dimethylsulphoxide: comparison with an aqueous NaSCN/NaClO(4) electrolyte

Deposition potential, deposition time, square-wave frequency, 2,2'-bipyridine concentration, and gallium concentration have been studied in detail, for the determination of trace concentration levels of the metal by square-wave voltammetry anodic stripping analysis, in dimethylsulphoxide. Optimum conditions have been found for gallium(III) determination and results compared to those obtained in 0.5M NaSCN + 4.2M NaClO(4) aqueous electrolyte by obtaining calibration graphs for the range 1 x 10(-8)M-1 x 10(-5)M gallium. Accuracy (+/- 3%) and precision (4-6% SD) of this method were assessed with both 4 x 10(-8)M and 4 x 10(-7)M gallium solutions used as synthetic samples. The efficiency of solvent extraction of gallium with di-isopropyl ether was found to be 99.98% at a 4 x 10(-7)M gallium concentration. The proposed method was applied to the determination of the gallium content in rock mineral samples (using the above mentioned solvent extraction procedure), are compared to those obtained with the NaSCNNaClO(4) based electrolyte. No statistically significant difference was observed. Analytical procedures followed are given in detail.     

Flame atomic absorption spectrometric determination of lead in waste water and effluent after preconcentration using a rapid coprecipitation technique with gallium phosphate

A determination method for lead in waste water and effluent was studied using flame atomic absorption spectrometry after preconcentration of lead by the rapid coprecipitation technique with gallium phosphate. Lead ranging from 0.5 to 50 microg was quantitatively coprecipitated with gallium phosphate from 100-150 mL sample solution (pH approximately 5). The presence of gallium phosphate did not affect the atomic absorbance of lead. Since the concentration of gallium in the final sample solution is also measurable by flame atomic absorption spectrometry at 250.0 nm without further dilution, the rapid coprecipitation technique, which does not require complete collection of the precipitate, becomes possible using a known amount of gallium and measuring the concentrations of both lead and gallium in the final sample solution by flame atomic absorption spectrometry. The 32 diverse ions tested gave no significant interferences in the lead determination. The method proposed here is rapid and has good reproducibility.     

A new principle of activation-analysis separations-X Substoichiometric determination of traces of gallium

A rapid method for the substoichiometric determination of gallium by neutron-activation analysis has been developed. After irradiation and dissolution of the test sample, gallium carrier is added and two preliminary separation steps are performed: the extraction into chloroform of cupferrates from 7N sulphuric acid and of diethyldithiocarbamates from 2-3N sulphuric acid. The pH of the remaining aqueous phase is then adjusted to 5.5, the solution extracted with a substoichiometric amount of 8-hydroxyquinoline in chloroform and the activity of the gallium hydroxyquinolate extract measured. A simultaneously irradiated gallium standard is treated in exactly the same way. From the activities of these two substoichiometric extracts the amount of gallium originally present in the test sample can be calculated. The method has been applied to the determination of 10(-6) to 10(-3)% of gallium in metallic aluminium and transistor-grade silicon.     

Electrothermal Vaporization of Trace Gallium via In SITU Alkylation for Inductively Coupled Plasma Atomic Emission Spectrometry

Abstract

A sample introduction method based on alkylation of the analyte was proposed for introducing trace gallium into inductively coupled plasma for atomic emission spectrometry. By using 10 μl of a sample solution with 15 μl of a 0.9 mol 1^-1 solution of ethylmagnesium bromide in tetrahydrofuran as alkylating reagent, a detection limit of 1.9 ng of gallium was obtained and the calibration graph was linear with the amount of gallium up to 100 ng. The relative standard deviation (n = 10) was 2.0% when 10 ng of gallium was present in the sample.     

Separation gallium-fer en presence d'edta

Macro- or microquantities of gallium can be separated from iron by precipitating the latter with sodium hydroxide in the presence of EDTA. Nearly all the gallium remains in solution. After the separation of iron, gallium is extracted with tributylphosphate from 3 N hydrochloric acid medium, and then re-extracted into water. Gallium is finally determined by precipitation with cupferron and ignition to the oxide, or for trace amounts of gallium, by colorimetric determination with rhodamine B. The method was checked with radioactive gallium and iron.     

Approaching bulk limit for three‐dimensional solids via the cyclic cluster approximation: Semiempirical INDO study

The cyclic cluster method has been examined for a number of solids using a recently developed computer code, Solid 98. Calculations are based on the quasirelativistic (QR) INDO/1 (intermediate neglect of differential overlap) method that is simple enough to allow for a saturation of the (cyclic) clusters. Convergence toward the bulk limit (INDO/1) charge density with respect to the size of the model cyclic cluster is shown for diamond, silicon, germanium, boron nitride, gallium phosphide, gallium arsenide, and gallium antimonide. Results show that, as soon as the initial cluster size reaches 5 to 6 nm, one can safely use the obtained density matrix as a good approximation to the bulk limit. ©1999 John Wiley & Sons, Inc. J Comput Chem 20: 253–261, 1999     

Preconcentration of gallium by coprecipitation with synthetic zeolites prior to determination by electrothermal atomic absorption spectrometry.

Synthetic zeolites were dissolved in nitric acid, and the resulting solution used as a coprecipitant for the preconcentration of trace amounts of gallium in water samples prior to determination by electrothermal atomic absorption spectrometry (ETAAS). The gallium preconcentration conditions and the ETAAS measurement conditions were optimized. Gallium was quantitatively concentrated with the zeolites coprecipitate from pH 6.0 to 8.0. The coprecipitate was easily dissolved in nitric acid, and an aliquot of the resulting solution was introduced directly into a tungsten metal furnace. The atomic absorbance of gallium in the resulting solution was measured by ETAAS. An ashing temperature of 400 degrees C and an atomizing temperature of 2600 degrees C were selected. The calibration curve was linear up to 3.0 microg of gallium and passed through the origin. The detection limit (S/N > or = 3) for gallium was 0.08 microg/100 cm3. The relative standard deviation at 1.0 microg/100 cm3 was 3.0% (n = 5). The proposed method has been successfully applied to trace gallium analysis in environmental water samples.     

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.     

The differential pulse polarographic determination of chromium in gallium arsenide

The method described for the determination of chromium in gallium arsenide is based on the catalytic current produced by nitrate in the electrolytic reduction of the chromium(VI)-diethylenetriaminepentaacetate complex. Matrix effects, primarily caused by gallium, are discussed in detail. The method is suitable for determinations of chromium at levels as low as about 1 μg g^?1 with about 50 mg of sample; the r.s.d. is better than 10%.     

3,5,7,4'-Tetrahydroxyflavone (kaempferol) as a chromogenic reagent for gallium and indium

3,5,7,4'-Tetrahydroxyflavone (kaempferol) forms yellow chelates with indium and gallium. Based on this reaction, a sensitive spectrophotometric method for the determination of gallium and indium alone and in presence of other metals and alloys has been developed. Beer's law is obeyed up to 2.8 and 1.44 ppm for indium and gallium respectively.     

Determination of gallium in geological materials by graphite-furnace atomic-absorption spectrometry

A graphite-furnace atomic-absorption spectrometric method has been worked out for the determination of traces of gallium in silicate rocks and minerals. The samples are opened up by fusion with a lithium carbonate-boric acid mixture and the cake is taken up with 2M nitric acid. Addition of nickel nitrate to this solution elminates the severe matrix effects allowing gallium solutions in nitric acid to be used as calibration standards. No separations are necessary. Results are quoted for 14 standard silicate rocks and two minerals. The RSD is 2.9%, and the sensitivity is 27 pg of gallium for 1% absorption.     

Determination of submicrogram amounts of gallium by ion-exchanger fluorimetry Determination of gallium in natural waters

A method for microdetermination of gallium at ng/ml level has been developed, based on ion-exchanger fluorimetry. The gallium reacts with salicylidene-o-aminophenol to give a highly fluorescent complex, which is fixed on a dextran-type cationic resin. The fluorescence of the resin, packed in a 1-mm silica cell, is measured directly with a solid-surface attachment. The range of concentration of the method is 2.0-10.0 ng/ml, the RSD 1.3% and the detection limit 0.3 ng/ml. The method has been applied to the determination of gallium in natural waters. The gallium content found in tap water was higher than that in raw water. This is related to the use of commercial aluminium salts in the water-treatment plant.     

Flame atomic absorption spectrometric determination of lead in waste water and effluent after preconcentration using a rapid coprecipitation technique with gallium phosphate

A determination method for lead in waste water and effluent was studied using flame atomic absorption spectrometry after preconcentration of lead by the rapid coprecipitation technique with gallium phosphate. Lead ranging from 0.5 to 50 μg was quantitatively coprecipitated with gallium phosphate from 100–150 mL sample solution (pH ∼5). The presence of gallium phosphate did not affect the atomic absorbance of lead. Since the concentration of gallium in the final sample solution is also measurable by flame atomic absorption spectrometry at 250.0 nm without further dilution, the rapid coprecipitation technique, which does not require complete collection of the precipitate, becomes possible using a known amount of gallium and measuring the concentrations of both lead and gallium in the final sample solution by flame atomic absorption spectrometry. The 32 diverse ions tested gave no significant interferences in the lead determination. The method proposed here is rapid and has good reproducibility. Received: 16 August 1999 / Revised: 6 October 1999 / Accepted: 14 October 1999     

The Spectrophotometric Determination of gallium (III) Using O-Hydroxyhydroquinonephathalein in the Presence of Surfactant Micellar

Abstract

The color reaction systems between various metal ions and o-hydroxyhydroquinonephthalein(Qnph) as a xanthene dye, in the presence of various water soluble surfactants(cationic. anionic, non-ionic surfactants) alone or in combination, were systematically investigated at various pH areas. The coexistence of cationic and non-ionic surfactants, such as Zephiramine (Zp) and Brij 35, was most effective for the color reaction systems between Qnph and gallium(III), as a metal ion, at weakly acidic media. By using the color reaction between Qnph and gallium(III) in the coexistence of Zp and Brij 35, an improved and sensitive spectrophotometric determination of gallium(III) was proposed as method 1, and the calibration curve was rectilinear in the range of 0～7.0 μg of gallium(III) in a final solution of 10ml at pH 6.4. The apparent molar absorptivity was 1.5 × 10⁵ 1 mol^?1 cm^?1 at 560 nm, and the interference of foreign ions was decreased by ½～ ¼-fold in comparison with other methods; method 3—in the presence of Zp alone at pH 6.4, method 2—in the presence of Tween or Brij 35 alone, without Zp, at pH 8. Thus, the use of Qnph as a xanthene dye and the combination of cationic and non-ionic surfactants, such as Zp and Brij 35(perhaps, on the mixed micellar media), was most effective and its color reaction was used for the separative assay of gallium(III).     

Solvent extraction and separation of gallium, indium and thallium with N-benzylaniline

A simple and rapid method is proposed for the separation of tervalent gallium, indium and thallium by solvent extraction with N-benzylaniline in chloroform from different concentrations of hydrochloric acid. Thallium and gallium are extracted from 1M and 7.0-7.5M hydrochloric acid respectively. Indium is finally extracted from hydriodic acid. These metals in the final extracts are determined complexometrically. Interference from some cations can easily be eliminated by reduction with sulphite, followed by selective oxidation of thallium(I) to thallium(III) with saturated bromine water, and from others by the use of thioglycollic acid as a masking agent in the extraction of gallium and indium. Most common anions cause no interference. Log-log plots of distribution coefficients vs. concentration of amine for gallium, indium and thallium indicate a 2:1 limiting mole ratio of amine to these metals.     

Substoichiometric neutron-activation determination of gallium: extraction from HCl with tri-n-octylphosphine oxide in cyclohexane

A highly precise method for the determination of traces of gallium by neutron activation is described. Conditions for the extraction of gallium are reported and general requirements for substoichiometric isolation of cations from HCl with neutral donors are discussed. The mean of determinations of gallium at concentrations of 40 ng ml in a solution prepared by dissolving a standard reference aluminium alloy was 213.9 +/- 1.3 ng. The relative standard deviation and the total error of the method (based on the SRM value) were 0.7 and 10.5% respectively.     

Spectrophotometric determination of the pH scale in ethane-1,2-diol

A highly selective method is described for the determination of gallium at the ppm-level in manganese nodules and geological reference samples. After dissolution of the sample, gallium is adsorbed on Dowex 1 (chloride form) from hydrochloric acid solution containing titanium trichloride, which reduces iron(III) so that it is not adsorbed. After elution with dilute nitric acid and evaporation, gallium is determined by atomic-absorption spectrometry with an air-acetylene flame.