Molecular absorption spectrometry by electrothermal evaporation in the graphite furnace-X Determination of chloride traces by AlCl ma in graphite cuvettes after liquid-liquid extraction of chloride with triphenyltin hydroxide

The determination of traces of chloride by means of the molecular absorption of AlCl in graphite cuvettes is described. An extraction method for separation and preconcentration of the chloride has been developed, to avoid matrix effects. Extraction was done with 0.03M triphenyltin hydroxide in o-xylene, and stripping with 0.025M barium hydroxide. The method is sensitive and specific for chloride. The detection limit is about 1.5 ng of chloride, and the chloride content of 20 ml of 10(-7)M solution can be determined. The determination is possible in presence of excess of bromide and iodide.     

Extraction-spectrophotometric determination of iron(II) by ternary complex formation with pyrocatechol violet and cetyltrimethylammonium bromide

A method for iron(II) determination based on reaction with Pyrocatechol Violet to form a 1:2 binary complex at pH 5-7 is described and has been extended to an extraction-spectrophotometric procedure for the determination of iron(II) by formation of the 1:2:2 iron(II)-Pyrocatechol Violet-cetyltrimethylammonium bromide ternary complex. The molar absorptivities of the binary and ternary complexes at 595 and 605 nm are 6.55 x 10(4) and 1.35 x 10(5)1.mole(-1).cm(-1), respectively. The method has been successfully applied to the determination of iron in felspar, Portland cement and sodium hydroxide.     

Determination of iodide and bromide by ion chromatography with post-column reaction detection

During an investigation into the mechanism of the biosynthesis of thyroid hormones, it became necessary to determine traces of iodide and bromide in biological matrices as well as in food. A vydac 302-IC anion-exchange column with methanesulphonic acid as the mobile phase was used for the ion chromatographic separation of iodide and bromide. A post-column reaction detector was developed based on the reaction between iodide or bromide, chloramine-T and 4,4'-bis(dimethylamino)diphenylmethane. Methods with minimal sample preparation are described for determination of iodide or bromide in serum, milk, salt and water. The detection limit is ca. 20 pg iodide and 15 ng bromide injected.     

Spectrofluorimetric determination of traces of bromide

A Spectrofluorimetric method for the determination of traces of bromide has been developed. The method is based on the bromination of fluorescein after bromide and hypochlorite form bromine, giving the less fluorescent eosin. The fluorescence decrease is used as the analytical signal. The calibration graph is linear over the range 10 to 80 g/1. The detection limit is 3 g/1 and the relative standard deviation 1.0%. The method has been satisfactorily applied to the determination of bromide in natural waters.     

Coulometric titration of acids in isopropanol-II Electrode reactions with lithium chloride and tetraethylammonium bromide as supporting electrolytes

Cathodic reactions in methanol and isopropanol have been investigated in the presence of both lithium chloride and tetraethylammonium bromide as supporting electrolytes. A side-reaction in lithium chloride medium leads to the formation of insoluble lithium hydroxide but base is generated stoichiometrically in tetraethylammonium bromide by reduction of solvent, oxygen and traces of water. Tetraethylammonium bromide is recommended as supporting electrolyte for the coulometric titration of acids in isopropanol.     

Determination of trace amounts of bromide by flow injection/stopped-flow detection technique using kinetic-spectrophotometric method

A simple, sensitive and selective method for the determination of bromide in seawater by using a flow injection/stopped-flow detection technique was examined. The detection system was developed for a new kinetic-spectrophotometric determination of bromide in the presence of chloride matrix without any extraction and/or separation. The detection was based on the kinetic effect of bromide on the oxidation of methylene blue (MB) with hydrogen peroxide in a strongly acidic solution. Large amounts of chloride could enhance the sensitivity of the method as an activator. The decolorisation of the blue color of MB was used for the spectrophotometric determination of bromide at 746 nm. A stopped-flow approach was used to improve the sensitivity of the measurement and provide good linearity of the calibration over the range of 0-3.2 μg ml⁻¹ of bromide. The relative standard deviation was 0.74% for the determination of 2.4 μg ml⁻¹ bromide (n = 5). The detection limit (3σ) was 0.1 μg ml⁻¹ with a sampling frequency of 12 h⁻¹. The influence of potential interfering ions was studied. The proposed method was applied to the determination of bromide in seawater samples and provided satisfactory results.     

Determination of tellurium in copper, lead and selenium by atomic-absorption spectrometry after extraction of the trioctylmethylammonium-tellurium bromide complex

A simple, rapid and sensitive combined solvent extraction and atomic-absorption spectrometric method has been developed for the determination of tellurium in copper, lead, selenium and blister copper. Tellurium is extracted as the trioctylmethylammonium-tellurium(IV) bromide complex into butyl acetate and determined by flame atomic-absorption spectrometry of the extract. As little as 1 mug of tellurium in a sample can be determined. The extraction of tellurium from hydrobromic acid solution with trioctylamine has also been investigated.     

Molecular absorption spectrometry (MAS) by electrothermal evaporation in a graphite furnace-XIII Determination of traces of fluoride by mas of AlF after liquid-liquid extraction of fluoride with triphenylantimony(V) dihydroxide

The determination of traces of fluoride by means of the molecular absorption of AlF volatilized in graphite cuvettes is described. An extraction method for separation and preconcentration of the fluoride has been developed, to avoid matrix effects. The fluoride is extracted with 10(-3)M triphenylantimony(V) dihydroxide in M1BK, and stripped with 0.025M barium hydroxide. The method is sensitive and specific for fluoride. The detection limit is about 0.3 ng of fluoride, and the fluoride content of 6 ml of 10(-7)M solution can be determined. The determination is possible in presence of various ions, but it is estimated that usage of trace matrix separation leads to a considerable improvement in the relative detection limits (by 2-3 orders of magnitude), levels as low as 0.01 ppm being detectable in some matrices.     

Extraction by reversed micelles of triton N-42 for the spectrophotometric determination of cetyltrimethylammonium bromide

Micellar preconcentration of 1 : 2 associates of Bromophenol Blue with cetyltrimethylammonium bromide is proposed to improve the procedure for the spectrophotometric determination of cationic surfactants. The preconcentration procedure involves quantitative extraction by reversed micelles of Triton N-42 in decane followed by the decomposition of the micellar solution with chloroform. The loss of 10^–7–10^–5 M cetyltrimethylammonium bromide in 5–100-fold preconcentration was not supported by the added-found method (RSD = 3–5%). The determination limit for cetyltrimethylammonium bromide is 2 × 10^–7 M.Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 17–21.Original Russian Text Copyright © 2005 by Demidova, Bulavchenko.     

Substoichiometric determination of mercury with cetyltrimethylammonium bromide

A radiometric method based on substoichiometric isotope dilution analysis has been developed for the determination of mercury using cetyltrimethylammonium bromide (CTAB) as the substoichiometric reagent. The method is based on the extraction of mercury as an ionassociation complex of tetraiodomercurate(II) ion with a substoichiometric amount of CTAB in benzene. The calibration graph was found to be linear in the range 0–10 μg Hg (II) in the aqueous phase of 10 ml volume. A detection limit of 0.06 μg·ml⁻¹ could be achieved by the proposed method. The relative standard deviation of the method was found to be 3.0% and the method has been successfully applied to study the determination of mercury in various synthetic mixtures.     

Flow injection determination of bromide ion in a developer using bromide ion-selective electrode detector

A potentiometric flow injection determination method for bromide ion in a developer was proposed, by utilizing a flow-through type bromide ion-selective electrode detector. The sensing membrane of the electrode was Ag(2)S-AgBr membrane. The response of the electrode detector as a peak-shape signal was obtained for injected bromide ion in a developer. A linear relationship was found to exist between peak height and the concentration of the bromide ion in a developer in a concentration range from 1.0x10(-3) to 1.0x10(-2) mol l(-1). The relative standard deviation for 10 injections of a 6x10(-3) mol l(-1) bromide ion in a developer was 1.3% and the sampling rate was ca 17-20 samples h(-1). The present method was free from the interference of an organic reducing reagent, an organic substance in a developer sample solution for the determination of bromide ion in a developer.     

Determination of silver in copper and lead metals and alloys and in zinc and selenium by atomic-absorption spectrometry after separation by extraction of the tri-n-octylmethylammonium-silver bromide complex

A simple and sensitive combined solvent extraction and atomic-absorption spectrometric method has been developed for the determination of silver in copper and lead metals and alloys and in zinc and selenium. Optimal conditions have been established for the extraction and determination of silver. Silver is extracted as the tri-n-octylmethylammonium-silver bromide complex and determined by atomic-absorption spectrometry by spraying the extract directly into the flame. As little as 0.2 mug of silver in a sample can be determined.     

HPLC法分析复方异丙托溴铵溶液雾化气溶胶成分

建立HPLC法同时测定吸入用复方异丙托溴铵溶液雾化气溶胶中硫酸沙丁胺醇和异丙托溴铵两组分的含量.采用C18(4.6mm x250 mm,5 μm)色谱柱,流动相为1.2 g/L的1-庚烷磺酸钠溶液(磷酸调节pH 3.2左右)(A)-乙腈(B),等度洗脱,流速为1.0mL/min,进样量为50 μL,分析时间15 min...     

Highly selective spectrophotometric flow-injection determination of trace amounts of bromide by catalytic effect on the oxidation of m-cresolsulfonephthalein by periodate

A new flow-injection method is reported for the determination of bromide. The method is based on catalytic effect of bromide on the oxidation of m-cresolsulfonephthalein by periodate in acidic media. The reaction was followed spectrophotometrically by measuring the decrease in absorbance at 528 nm. The influence of pH, reagent concentration and manifold variables on the sensitivity was studied. Under optimum conditions, a calibration graph was obtained in the range of 0.160-20.00 microg ml(-1) bromides with a limit of detection of 0.150 microg ml(-1) bromide. The relative standard deviation for ten replicate measurement of 1.0 microg ml(-1) bromide was 2.1%. The influence of potential interfering ions on the selectivity was studied. The method successes to measure bromide in the presence of other halide ions. The method was used to measure bromide in river water and tap water.     

Determination of demecarium bromide and related compounds by high-performance liquid chromatography

A high-performance liquid chromatographic method for the determination of demecarium bromide and related process intermediate and companion products is described. The compounds of interest are separated by isocratic reversed-phase chromatography on a mu Bondapak CN column using UV detection. The reproducibility of the method and stability of demecarium bromide is demonstrated. Applications presented for the method include quantitation of demecarium bromide in aqueous solutions and control of the raw material.     

Spectrophotometric determination of microamounts of scandium with o-chlorophenylfluorone and cetyltrimethylammonium bromide

The reaction of scandium(III) with o-chlorophenylfluorone (o-CIPF) in the presence of cetyltrimethylammonium bromide (CTMAB) has been studied. In an acetate buffer at pH 4.4, a red-purple complex is obtained, with maximum absorption at 569 nm and a molar absorptivity of 1.31 x 10(5)1.mole(-1).cm(-1). The composition of the complex is found to be 1:2:2 Sc-o-CIPF-CTMAB. Beer's law is obeyed over the range 0-12 mug/25 ml scandium. The proposed method has been used for determination of trace scandium in tungsten ores after its prior separation by solvent extraction.     

Determination of bromide ions in seawater using flow system with chemiluminescence detection

A simple flow-based procedure with chemiluminescence (CL) detection is proposed for bromide ion determination in seawater. The procedure was based on the oxidation of bromide to bromine by chloramine-T followed by the reaction of bromine with luminol resulting in CL emission. Since no significant reaction within chloramine-T and luminol was observed, the detection was carried out without bromine extraction from the oxidant medium. The proposed flow system had a sampling rate of 40 determinations per hour, reagents consumption of 100 μg luminol and 60 μg chloramine-T per determination, a limit of detection of 0.5 mg l⁻¹ bromide ions, a linear concentration range (r = 0.999 and n = 7) between 0 and 100 mg l⁻¹, and a coefficient of variance better than 2.5% (for 10 measurements of a 10 mg l⁻¹ Br⁻ solution) were achieved. The analytical system was applied for the determination of bromide in seawater and estuarine-water samples, obtaining an analyte recovery ranging from 94 to 102% and comparing the results with a reference spectrophotometric method no significant difference was observed in 95% confidence level.     

Improved tribenzylamine-silver bromide extraction/atomic-absorption spectrophotometric method for the determination of silver in ores, related materials and zinc process solutions

An improved tribenzylamine extraction/atomic-absorption method for the determination of silver in ores, related materials and zinc process solutions is described. The method, which involves the separation of silver by a single methyl isobutyl ketone extraction of the tribenzylamine-silver bromide ion-association complex from ~ 0.5-2M sulphuric acid-0.14M potassium bromide, is simpler and more rapid than a previous method based on a triple chloroform extraction of the complex. Silver is stripped with 12M hydrochloric acid containing 1% thiourea as a complexing agent. Thiourea is destroyed with nitric and perchloric acids and silver is ultimately determined by atomic-absorption spectrophotometry in an air-acetylene flame, at 328.1 nm, in a 10% v v hydrochloric acid-1% v v diethylenetriamine medium. Cadmium and bismuth are partly co-extracted but do not interfere. Results obtained by this method are compared with those obtained previously by the tribenzylamine/chloroform extraction method and with those obtained by a direct acid-decomposition/atomic-absorption method.     

The determination of bromide in a local anaesthetic hydrochloride by capillary electrophoresis using direct UV detection

The determination of residual amounts of bromide in a local anaesthetic hydrochloride by capillary electrophoresis was developed. Direct UV detection at 200 nm was used for the determination of the bromide content. The separation capacity of the system must be sufficient when bromide is determined in the presence of a large excess of chloride since electromigration dispersion of the highly concentrated chloride peak may impair the resolution. The background electrolyte (BGE) contained both acetonitrile and methanesulphonic acid in order to improve the selectivity and minimise the electromigration dispersion. The system was optimised with respect to resolution of the chloride and the bromide peaks by statistical experimental design using a multivariate optimisation program. The developed method was validated in accordance with the ICH guidelines and proved to be suitable for its intended use.     

Kinetic-spectrophotometric method for the determination of trace amounts of bromide in seawater

A novel simple, sensitive and rapid kinetic-spectrophotometric method is proposed for the determination of trace amounts of bromide. The method is based on its catalytic effect on the oxidation of methylene blue (MB) by hydrogen peroxide in strongly acidic solution. The oxidation reaction is activated by large amounts of chloride and can be monitored spectrophotometrically by measuring the decrease in the absorbance of MB at 746 nm. The determination of bromide is performed by a fixed-time method at the first 100 s from the initiation of the reaction. Unlike other kinetic-spectrophotometric methods for the determination of bromide, the proposed method does not require heating the solution. Bromide can be determined in the range from 80 to 960 μg l⁻¹ with the detection limit of 35 μg l⁻¹. The relative standard deviation of ten replicate determination of 480 μg l⁻¹ bromide was 1.4%. The influence of potential interfering ions was studied. The proposed method was satisfactorily applied to the determination of bromide in seawater without interfering effect from chloride ion.