The spectrophotometric determination of trace molybdenum (VI) after collection and elution as molybdate ion on protonated chitin

Collection and elution method for inorganic anion on protonated chitin has been applied to the spectrophotometric determination of molybdenum (VI). The molybdenum (VI) is collected as molybdate ion on a column of chitin in weak acidic medium which is easily eluted with a small volume of 0.1 M ammonia buffer solution (pH 10). The molybdenum (VI) in the eluent is determined by bromopyrogallol red-Zephiramine method spectrophotometrically. Beer's law is obeyed over the concentration range of 0.1-0.8 mug of molybdenum (VI) in 1 ml of eluent at 634 nm. The apparent molar absorptivity is 6x10(4) dm(3) mol(-1) cm(-1). The tolerance limits for WO(4)(2-), VO(3)(-), CrO(4)(2-) and Fe (III) is low, that is, 1-100 times that of molybdenum (VI), but some metal ions and common inorganic anions do not interfere in concentration range of 1000-5000 times that of molybdenum (VI). The present method can be applied to the determination of molybdenum (VI) in natural water samples.     

Simple and rapid spectrophotometric determination of iron after preconcentration as its 1,10-phenanthroline complex on the natural polymer "chitin"

Preconcentration by collection of metal complexes on chitin has been applied to the spectrophotometric determination of iron in water. The iron is collected as its 1,10-phenanthroline (phen) complex on a column of chitin in the presence of tetraphenylborate as counter-ion. The iron(II)-phen complex retained on the chitin is eluted with an acetone-1M acetic acid mixture (8:2 v/v), and the absorbance of the eluate is measured at 512 nm. Beer's law is obeyed over the concentration range 1.1-11.2 mug of iron in 10 ml of eluate. In the presence of EDTA as masking agent, Ca, Mg, Al, Mn, Zn, Cd and Pb do not interfere in concentrations up to 100 times that of iron(II) and Co, Ni and Cu do not interfere in concentrations up to 20 times that of iron(II). Common inorganic anions do not interfere in concentrations up to 10,000 times that of iron(II). The proposed method has been applied to determination of iron in tap water.     

Indirect spectrophotometric determination of chromium(VI)

A new simple and sensitive spectrophotometric method for the determination of chromium(VI) is established. It relies upon the oxidation of iron(II) with the titled ion, in acidic medium, to form iron(III) which is complexed with tiron to form a stable blue color with maximum absorption at 650 nm. Adherence to Beer's law is observed in the range 10–100 μg of chromium(VI) per 25 ml, with a molar absorptivity of 5.6 × 10³ liters mol^?1 cm^?1, sensitivity index of 0.0093 μg cm^?1, relative error of ?5.0 to +0.3%, and relative standard deviation of 0.3–4.0%, depending on the concentration level. Furthermore, the reaction needs neither temperature control nor an extraction step.     

On the spectrophotometric flow injection determination of chromium(VI) in natural waters after on-line preconcentration on activated alumina

The feasibility of chromium(VI) preconcentration on to activated alumina in a continuous flow system with spectrophotometric detection was investigated. Chemical and flow variables, and the influence of concomitant species were studied both with and without preconcentration systems. The best results were obtained by using a 2.5 cm long, 1.6 mm i.d. alumina minicolumn, and selecting 1 x 10(-4) M nitric acid as the preconcentrating medium and 0.1 M ammonium hydroxide as the eluent. The eluted chromium(VI) was mixed with diphenylcarbazide in acidic medium and the absorbance of the colored complex was measured at 540 nm. Linear calibrations for 5, 25 and 50 ml sample volumes were established over the concentration ranges 10-50 mug 1(-1), 2-10 mug 1(-1) and 1-5 mug 1(-1) with sensitivity enhancements of 44, 196 and 392 and detection limits (3sigma) of 3.0 mug 1(-1), 0.3 mug 1(-1) and 0.2 mug 1(-1), respectively. The methods is relatively fast and cheap. Natural waters were analyzed with use of the developed procedure.     

Malachite green as a reagent for detection and spectrophotometric determination of chromium(VI)

A sensitive and inexpensive method of spectrophotometric determination of chromium(VI), based on the absorbance of its complex with malachite green and acetic acid at pH 2.5 is reported. The complex shows a molar absorptivity of 8 x 10(4) l.mole(-1) cm(-1) at 560 nm, using malachite green and acetic acid as reference solution. The effect of time, temperature, pH and reagent concentration is studied and optimum operating conditions are established. Beer's law is applicable in the concentration range 2.0-22.8 mug/ml chromium(VI). The resin beads act as a catalyst and as little as 1.6 mug of chromium(VI) is detected in the resin phase as compared to 4.1 mug in the solution phase. The standard deviation in the determinations is +/-0.40 mug/ml for a 10.35 mug/ml solution.     

Flow procedure for ion-exchange preconcentration and on-line spectrophotometric determination of iron(III) as its thiocyanate complex

On-line ion-exchange preconcentration of iron(III) on a conventional cation exchange resin with spectrophotometric detection based on thiocyanate complexation is described. The calibration graph is linear over the range 0.01–0.2 g ml^–1 and the detection limit (3 ) is 6 ng ml^–1 for a 6-ml sample. No interference effects were detected. The recovery of iron from the resin is 95%. 12 samples h^–1 can be analysed.     

Studies and application of catalytic kinetic spectrophotometric determination of trace chromium(VI) sensitized by microemulsion medium

A new catalytic kinetic spectrophotometric method for the determination of trace amount of chromium (VI) in microemulsion medium has been developed. The method is based on the catalytic effect of chromium (VI) on the oxidation of nuclear fast red in the presence of Tween-80 microemulsion and HAc-NaAc buffer solution (pH = 5.2). The linear ranges are in the range of 0 approximately 0.0480 microg mL(-1) of Cr (VI) at 528 nm and the detection limit is 1.56x10(-9)g mL(-1). The method has been applied in determination of Cr (VI) in water and food samples with satisfactory results. The relative standard deviation is less than 4.6 % and the recovery is 93.5 approximately 104 %.     

Indirect spectrophotometric determination of traces of antimony(III) based on its oxidation by chromium(VI) and reaction of chromium(VI) with diphenylcarbazide

An indirect method for the determination of antimony(III) is described. Antimony(III) is oxidized to antimony(V) by chromium(VI) and the excess of chromium(VI) is then determined spectrophotometrically with diphenylcarbazide. Optimal conditions were established for both the determination of antimony(III) and the elimination or reduction of interferences. Antimony(III) can be determined quickly and easily in the range 0.05–5 mg l^?1; the relative standard deviation is 2% for 1.0 mg l^?1 antimony(III). The method is applicable to marine sediments and geothermal waters.     

Method for the determination of chromium (VI) as chromium (VI)-dibenzyidithiocarbamate

Dibenzyldithiocarbamic acid (DBDC) exhibits the ability to speciate between chromium(VI) and chromium(III), since only the chromium(VI) will form complexes with DBDC. The complex is then extracted into an organic solvent and assayed using an ultraviolet-visible (UV-VIS) spectrophotometer at 498.8 nm. Using 250 ml of aqueous sample detection limits less than 1 ng/ml are possible, while the linear range extends to 500 gmg/ml when working at 498.8 nm. Oxidation of the chromium(III) to chromium (VI) using cerium (IV) enables the determination of total chromium and subsequently the chromium (III) in solution. Evaluation of the method with a standard reference material produced only 4.81 part per thousand error in the determination of chromium(VI).     

Ion flotation—spectrophotometric determination of traces of chromium(VI)

Ion flotation is used to concentrate chromium(VI) in the range 3–70μg l^-1 from 14 samples. The chromium(III)—diphenylcarbazone complex formed by reaction with diphenylcarbazide is floated efficiently with sodium lauryl sulfate, and the subsided foam is measured spectrophotometrically after simple dilution. Continuous flotation methods at solution flow rates of 2, 3 and 4 l h^-1 are discussed.     

Flow injection direct spectrophotometric assay for the speciation of trace chromium(III) and chromium(VI) using chromotropic acid as chromogenic reagent

A new rapid and sensitive FI assay is reported for the simultaneous direct spectrophotometric determination of trace Cr(VI) and Cr(III) in real samples. The method is based upon the reaction of Cr(VI) with chromotropic acid (CA) in highly acidic medium to form a water-soluble complex (λ_max = 370 nm). Cr(III) reacts with CA only after its on-line oxidation to Cr(VI) by alkaline KIO₄. The determination of each chromium species in the sample was achieved by absorbance differences. The calibration curves were linear over the range 3-4000 μg l⁻¹ and 30-1200 μg l⁻¹ for Cr(VI) and Cr(III), respectively, while the precision close to the quantitation limit was satisfactory in both cases (s_r = 3.0% for Cr(VI) and 4.0% for Cr(III) (n = 10) at 10 and 50 μg l⁻¹ level, respectively). The method developed proved to be adequately selective and sensitive (c_L = 1 and 10 μg l⁻¹ for Cr(VI) and Cr(III), respectively). The application of the method to the analysis of water samples (tap and mineral water) gave accurate results based on recovery studies (93-106%). Analytical results of real sample analysis were in good agreement with certified values.     

Derivative spectrophotometric determination of iridium after preconcentration of its 1-(2-pyridylazo)-2-naphthol complex on microcrystalline naphthalene

Iridium is preconcentrated from the large volume of its aqueous solution using 1-(2-pyridylazo-2-naphthol) (PAN) on microcrystalline naphthalene in the pH range of 4.5-6.0. The solid mass after filtration is dissolved with 5 ml of dimethylformamide (DMF) and the metal determined by first derivative spectrophotometry. The detection limit is 20 ppb (signal to noise ratio = 2) and the calibration curve is linear over the concentration range 0.25-75.0 mug in 5 ml of the final DMF solution with a correlation coefficient of 0.9996 and relative standard deviation of +/- 1.1%. Various parameters such as the effect of pH, volume of aqueous phase, choice of solvent, reagent and naphthalene concentration, shaking time and interference of a number of metal ions on the determination of trace amount of iridium have been studied in detail to optimize the conditions for its determination in synthetic samples corresponding to various standard alloys and environmental samples.     

Simultaneous determination of chromium(VI) and chromium(III) at trace levels by adsorptive stripping voltammetry

A new methodology was proposed for the speciation of chromium by differential pulse adsorptive stripping voltammetry (DPAdSV) using pyrocatechol violet (PCV) and N-(2-hydroxyethyl)ethylenediamine-N,N′,N′-triacetic acid (HEDTA) as complexing agents. In this procedure, a partial least squares (PLS) regression was used for the resolution of the strongly overlapping voltammetric signals from mixtures of Cr(III) and Cr(VI) in the presence of PCV and HEDTA. The relative error in absolute value was <6% when concentrations of several mixtures were calculated. The analysis of the possible effect of the presence of foreign ions in the solution was performed. The procedure was successfully applied to the speciation of chromium in different samples of natural water.     

A simple and rapid spectrophotometric method for the determination of nitrite by its decolorizing effect on peroxovanadate complex

A rapid, simple, and most economical spectrophotometric method was proposed for the determination of nitrite in various water samples, soil samples, and roots of leguminous plants. The method is based on decolorizing effect of nitrite on complex formed between hydrogen peroxide and vanadate in acidic medium. The decolorization of that complex by nitrite was exploited to monitor the reaction spectrophotometrically at 470 nm.The method was optimized for effect of concentrations of ammonium metavanadate, hydrogen peroxide, various acids, concentrations of sulphuric acid, order of reagents addition and color stability. The color of the complex was found to be stable for about 2 days, and the stability constant of the complex was also calculated by modified Job's method. The linearity range of the calibration graph was over 6.67-66.7 microg ml(-1) of nitrite with molar absorptivity, 0.276 x 10(3) mol(-1) l cm(-1) and Sandell's sensitivity, 0.1667 microg cm(-2). The method was applied successfully for the determination of nitrite in soil samples, various wastewater samples and roots of leguminous plants.     

Rapid spectrophotometric determination of chromium(III)

A spectrophotometric procedure is suggested for the determination of Cr(III). The reaction between Cr(III) and 2-(5-bromo-2-pyridylazo)-5-dimethylaminophenol is accelerated by sodium dodecyl sulphate(SDS), sodium benzoate causes a further increase in the absorbance of the chelate. The optimum pH range for the reaction is 5-5.8(benzoate buffer). The chelate exhibits maximum absorbance at 590 nm, obeys Beer's law over the concentration range 0.02-0.56 microg/ml of Cr(III), has molar absorptivity of 7.8 x 10(4) 1. mol(-1) cm(-1) and a Sandell sensitivity of 0.66 ng/cm. The metal to ligand ratio is 1:2 in the absence of SDS and 1:1 in its presence. A procedure for the determination of Cr(III) and Cr(VI), when present together, is described. The method has been applied to the analysis of Cr(III) in tap water.     

Ion-chromatographic determination of chromium (VI)

Summary A simple ion-chromatographic method has been developed for the selective determination of chromium (VI) using UV-photometric detection. The anion exchanger was based on a matrix of a 2-hydroxyethyl-methacrylate copolymer; the mobile phase consisted of phosphate buffer and sodium perchlorate. The relative standard deviation was 2.26%. Application was made to waste waters of the metallurgical industry.     

Sequential injection wetting film extraction applied to the spectrophotometric determination of chromium(VI) and chromium(III) in water

The spectrophotometric determination of Cr(VI) and Cr(III) via sequential injection was used to demonstrate the sensitivity enhancement provided by a newly developed wetting film extraction system. The reaction product of Cr(VI) with 1,5-diphenylcarbazide was ion-paired with perchlorate and extracted into an organic wetting film consisting of octanol and 4-methyl-2-pentanone on the inner wall of a Teflon tube. The wetting film, with the extracted analyte, was then eluted with 100 mul acetonitrile and the analyte determined spectrophotometrically at 546 nm. Important optimized parameters were the selection of wetting film and elution solvents, the flow rate, the length and diameter of the extraction coil and the conditions for the formation of the ion paired chelate. Cr(III) was previously oxidized to Cr(VI) and calculated as the difference between total Cr and Cr(VI). An enrichment factor of 25 and a detection limit of 2.0 mug l(-1) Cr(VI) were achieved with a sampling frequency of 17 h(-1). The calibration curve was linear up to 100 mug l(-1) Cr(VI) (r = 0.999). The relative standard deviations were 2.8 and 2.0% at the 25 and 100 mug l(-1) levels.     

Enhanced spectrophotometric determination of chromium (VI) with diphenylcarbazide using internal standard and derivative spectrophotometry

In the present work, erioglaucine A was applied as internal standard to enhanced spectrophotometric determination of chromium (VI) with diphenylcarbazide. The following procedure was used: (1) addition of internal standard and formation of ion pairs of Cr (VI) with benzyltributylammonium bromide (BTAB) (sample volume 100 ml), (2) extraction to 10 ml of methylene chloride, (3) evaporation in nitrogen stream, and (4) redissolution in a micro-volume with addition of diphenylcarbazide for color development (final volume 200 mul). The preconcentration factor achieved was about 400 and it was shown that, using internal standard, the analytical errors due to sample treatment were reduced. The analytical signals for chromium and internal standard were obtained at 591.30 and 653.50 nm from first derivative spectra, normalized against (1)D(653.50nm). The analytical characteristics evaluated were: detection limit = 0.06 mug l(-1), quantification limit = 0.19 mug l(-1), precision for 1 mug l(-1) 14.2%, and for 10 mug l(-1) 3.2%, correlation coefficient of linear regression was 0.9985. The proposed procedure was applied to determination of chromium (VI) in tap water. Total chromium was determined by electrothermal atomic absorption spectrometry, the recovery of hexavalent chromium added was then evaluated and compared with the results of the proposed procedure. In this experiment, good agreement was obtained between results obtained by the two methods.     

Application of 2,2′-Diquinoxalyl to the spectrophotometric determination of gold(III) and chromium(VI)

The reaction of 2,2′-diquinoxalyl with tin(II) and titanium(III) was used for spectrophotometric determination of chromium(VI) and gold(III). The conditions of the reactions were determined. The curves for determination of chromium(VI) and gold(III) were found. The influence of foreign ions was examined.