Extraction-spectrophotometric determination of germanium(IV) with mandelic acid and malachite green

A method has been developed for determination of germanium, based on complexation with mandelic acid and extraction of the ion-associate formed with Malachite Green (MG) into chlorobenzene. A weakly acidic aqueous solution (pH 2.5-3.5) at room temperature is used and indirect determination is achieved by measuring the absorbance of MG in the extract, at 628 mn. The calibration graph is linear over the range (0.17-8.63) x 10(-6) (0.05-2.50 mug of germanium); the apparent molar absorptivity is 1.33 x 10(5) 1.mole(-1).cm(-1). The interferences from Fe, Ti, Sn(IV), Mo, and SB(III) can be eliminated by addition of trans-1,2-diaminocyclohexanetetra-acetic acid and sodium diethyldithiocarbamate.     

Spectrophotometric methods for the determination of tamoxifen citrate

Three simple and sensitive spectrophotometric methods for the determination of tamoxifen citrate have been developed. They are based on the formation of an ion-association complex between the drug and a dye, Erioglaucine A, which is extractable into chloroform and has an absorption maximum at 625 nm (method A), oxidation with excess potassium permanganate and the determination of unconsumed permanganate using Fast Green FCF (method B), or by the formation of a coloured cobalt thiocyante coordination complex which is extracted into benzene and measured at 635 nm (method C). Beer's law limits for methods A, B, and C are 0.5-3.0 mug ml(-1), 1.0-6.0 mug ml(-1) and 100-500 mug ml(-1), respectively. No interference was observed from tableting additives and the applicability of the methods was examined by analysing tablets containing tamoxifen. The quantities determined were 99.0-100.03% of the exptected values.     

Flotation-spectrophotometric determination of trace of germanium with isochromatic dye ion-pairs formed by rhodamine 6G and tetrabromofluorescein

A flotation spectrophotometric method for the determination of germanium with isochromatic dye ion-pairs is described. The molar ratio of germanium to rhodamine 6G to tetrabromofluorescein is 1:5:5. The apparent molar absorptivity is 5.8 x 10(5) l mol(-1) cm(-1) at 531 nm. Beer's law is obeyed over the concentration range of 5.0 x 10(-8)-1.25 x 10(-6) mol l(-1). The proposed method is sensitive and accuracy and can be applied satisfactorily to the determination of germanium in vegetables.     

A spectrophotometric method for the determination of copper ions and its application to the co-precipitation of copper in the crystallization of sodium

The molar absorptivity of the cyanide complexes [Cu(CN)(3)](2-) and [Cu(CN)(4)](3-), at their isosbestic wavelength (235 nm) is 1.13 x 10(3) l.mole(-1)mm.(-1) and can be used for the quantitative determination of micro-amounts of copper in the ppm range. The determination of 1-10 mug of Cu(2+) per g of NaCl, or 0.25-2.5 mug ml , is described in detail. The co-precipitation of copper with NaCl crystallizing from aqueous solutions has been studied by this method.     

Rapid, selective, direct and derivative spectrophotometric determination of titanium with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone

A simple and sensitive spectrophotometric method is developed for the determination of titanium in aqueous medium. The metal ion forms a reddish brown coloured complex with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone (2,4-DHBINH) in the pH range 1-7. The complex shows two absorption maxima, one at 430 nm and the other at 500 nm. The reagent shows appreciable absorbance of 430 nm and negligible absorbance at 500 nm at pH 1.5. Beer's law is obeyed in the range 0.09 to 2.15 mug ml(-1) of titanium(IV). The molar absorptivity and the Sandell's sensitivity of the method are 1.35 x 10(4) 1 mol(-1) cm(-1) and 0.0049 mug cm(-2), respectively. A method for the determination of titanium by first-order derivative spectrophotometry is also proposed. The methods have been employed successfully for the determination of titanium in several alloy and steel samples.     

Specific thin-layer chromatographic method for the determination of theophylline in plasma in the presence of some other drugs.

A simple spectrodensitometric method for the direct determination of theophylline was developed from measurement of the absorbance of the compound on silica gel layers irradiated at 275 nm. Auantities as low as 0.010 mug can be detected and a linear relationship was obtained between peak area and the amount of the drug in the spots from 0.025-0.200 mug. The recovery over the usual range of plasma concentration (2.5-20 mug/ml) was 95-107%. The method is sufficiently sensitive and specific for clinical purposes and the time for the assay is about 2 h. Caffeine, frequently present in human plasma, was well separated from theophylline at all concentration levels as were several other drugs commonly used in respiratory problems.     

Spectrophotometric multicomponent determination of sunset yellow, tartrazine and allura red in soft drink powder by double divisor-ratio spectra derivative, inverse least-squares and principal component regression methods

Double divisor-ratio spectra derivative (graphical method), classical least-squares and principal component regression (two numerical methods) methods were developed for the spectrophotometric multicomponent analysis of soft drink powders and synthetic mixtures containing three colorants without any chemical separation. The graphical method is based on the use of derivative signals of the ratio spectra using double divisor. In this method, the linear determination ranges were 2-8 mug ml(-1) sunset yellow, 4-18 mug ml(-1) tartrazine and 2-8 mug ml(-1) allura red in 0.1 M HCl. In the numerical methods, a training set was randomly prepared by using 18 samples containing between 0 and 8 mug ml(-1) of sunset yellow, 0-18 mug ml(-1) of tartrazine and 0-8 mug ml(-1) of allura red. The chemometric calibrations were calculated by using the prepared training set and its absorbances at seven points (from 375.0 to 550.0 nm) in the spectral region 325-584 nm. The proposed methods were validated by using synthetic ternary mixtures and applied to the simultaneous determination of three colorants in soft drink powders. The obtained results were statistically compared with each other.     

Simultaneous determination of naproxen, salicylic acid and acetylsalicylic acid by spectrofluorimetry using partial least-squares (PLS) multivariate calibration

Determination of naproxen, salicylic acid and acetylsalicylic acid has been carried out in mixtures of up to three components by recording emission fluorescence spectra between 300 and 520 nm with an excitation wavelength of 290 nm. The excitation-emission spectra of these compounds are strongly overlapped, which does not permit their direct determination without previous separation by conventional methodologies. Here, a method is proposed for the determination of these chemicals by the use of a full-spectrum multivariate calibration method, partial least-squares (PLS). The experimental calibration matrix was designed with 18 samples. The concentrations were varied between 0.1 and 1.0 mug ml(-1) for naproxen, 0.5 and 5.0 mug ml(-1) for salicylic acid and from 2.0 to 12.0 mug ml(-1) for acetylsalicylic acid. The cross-validation method was used to select the number of factors. To check the accuracy of the proposed method, the optimized model, obtained using PLS-1, was applied to the determination of these compounds in pharmaceuticals and human serum samples previously spiked with different amounts of each chemical.     

Kinetic-spectrophotometric determination of trace amounts of As(III) based on its inhibitory effect on the redox reaction between bromate and hydrochloric acid

A simple, sensitive, rapid and reliable method has been developed for spectrophotometric determinations of As(III) in the presence of As(V) based on its inhibition effect on the redox reaction between bromate and hydrochloric acid. The decolorization of methyl orange by the reaction products was used to monitor the reaction spectrophotometrically at 525 nm. The method allows the determination of arsenic in the range of 6-1000 mug l(-1). The relative standard deviation for 10 determinations of 40 mug l(-1) of As(III) was 1.43% and the limit of detection, corresponding to a signal to noise ratio of three, was 3.4 mug l(-1). The proposed method was applied to the determination of As(III) in water samples with satisfactory results.     

A sensitive spectrophotometric method for the determination of methyl alcohol in air and water

A sensitive spectrophotometric method for the indirect determination of methyl alcohol in air and water is described. The methyl alcohol is oxidized to formaldehyde which is then determined in acidic medium with p-aminoazobenzene and sulphur dioxide. Beer's law is obeyed in the range 100-600 mug of methyl alcohol in 25 ml of final solution and the wavelength of maximum absorption is 505 nm. The lower limit of determination is 5 mug ml in the sample. Several common organic co-pollutants do not interfere. The method can be used for determination of methyl alcohol in blood.     

Spectrophotometric determination of mercury in environmental sample and fungicides based on its complex with o-carboxy phenyl diazoamino p-azobenzene

In the present method a new reagent o-carboxyphenyl diazoamino p-azobenzene has been synthesised for the determination of mercury spectrophotometrically. The method is based on the reaction of mercury with the reagent in alkaline medium where the reagent is in the aci-form. The purple violet coloured dye-mercury complex showed an absorption maxima at 540 nm. Beer's law is valid over the concentration range of mercury from 0.08 to 0.8 mug ml(-1) (0.08-0.8 ppm). The molar absorptivity and Sandell's sensitivity were found to be 2.22x10(5) mol(-1) cm(-1) and 0.0009 mug cm(-2), respectively. The method has been successfully applied to the determination of mercury in air, water, soil and fungicide samples.     

Separation of antimony(III) with iodide and dithizone by sorption on polyurethane foam from sulphuric acid medium for its spectrophotometric determination in glasses

A method for quantitative separation of antimony(III) by sorption on polyether based polyurethane foam and its spectrophotometric determination has been described. The method involves formation of a pink-red complex of antimony(III) with iodide (0.045M) and dithizone (2.3 x 10(-5)M) in 0.25-0.75M H(2)SO(4) medium, sorption of the complex on polyurethane foam (within 45 min) at room temperature followed by its elution with acidified acetone (acetone containing 0.008% H(2)SO(4)) and spectrophotometric measurement at 507.2 nm ( = 2.56 x 10(4) l mol cm). The method obeys Beer's law from 0.1 to 6.0 mug antimony(III). Tolerance limits of other ions are Co (100 mug), Ni (100 mug), Fe (10 mug), Cu (0.5 mug), Sn (20 mug), Zn (100 mug), As (100 mug), Mn (200 mug), Pb (50 mug), Ti (100 mug), V (50 mug), etc. Interference by iron and copper have been eliminated by treating with KOH prior to the extraction of antimony. The method has been standardized with glass samples spiked with known amounts of antimony and applied to the determination of antimony in various glasses.     

Fluorimetric trace determination of cerium(III) with sodium triphosphate

Sodium triphosphate acts as a specific reagent for enhancing the fluorescence intensity of cerium(III). The purpose of this study was to investigate the spectrofluorimetric determination of trace amounts of Ce(III) in sodium triphosphate solution. The excitation and emission wavelengths are 303.5 nm and 353 nm respectively. Optimum sodium triphosphate concentration is found to be 0.074 g l(-1) at room temperature. The fluorescence varies linearly with the concentration of cerium(III) in the range 0.001-45 mug ml(-1). The detection limit is 9.4 x 10(-4)mug ml(-1). The relative standard deviations for 30 mug ml(-1) and 0.05 mug ml(-1) Ce(III) in 0.074 g l(-1) sodium triphosphate solution are 1.1% and 0.72% respectively. Quenching effects of other lanthanides and some inorganic anions are described. This method is a direct and rapid analytical method for the determination of Ce(III) in rare earth mixtures and cerium concentrates.     

Flow injection spectrophotometric determination of trace amounts of selenium

A simple, rapid and sensitive flow injection spectrophotometric method for determination of selenium (0.005-1.5 mug ml(-1)) is described. The method is based on the catalytic effect of Se(IV) on the reduction reaction of thionine (TN) with sulphide ion, monitored spectrophotometrically at 598 nm. The detection limit is 5 ng ml(-1) the relative standard deviation for eight replicate measurements is 1.1% for 1 mug ml(-1) of selenium. The sampling rate is 25-30 samples h(-1). The procedure was applied successfully to the determination of selenium in real samples.     

Spectrophotometric determination of ascorbic acid with potassium hexacyanoferrate(III)

A new, simple and rapid method of determination of ascorbic acid in amounts of 45-360 mug is described. The ascorbic acid is determined spectrophotometrically at 420 nm from the decrease in absorbance it causes in 1 x 10(-3)M hexacyanoferrate(III) in McIlvaine buffer at pH 5.2. The proposed method is suitable for the determination of ascorbic acid in pharmaceutical preparations and probably natural products.     

Spectrophotometric determination of vanadium(v) and its application to vanadium steels containing chromium, molybdenum, tungsten and manganese

A newly synthesized reagent, N-o-toluoyl-N-o-tolylhydroxylamine is used in a sensitive and selective spectrophotometric method for determination of vanadium(V). The method has been successfully applied to vanadium determination in Mn-Mo-Cr-V steels. The system in 2-6M hydrochloric acid medium obeys Beer's law at 510 nm in the range of vanadium concentration from 0.5 to 10.0 mug ml .     

Extractive spectrophotometric methods for the assay of sildenafil citrate (Viagra) in pure form and in pharmaceutical formulations

Two simple and sensitive extractive spectrophotometric methods for the determination of sildenafil citrate (SC) are proposed. The methods are based on the formation of ion-association complexes of sildenafil citrate with bromocresol green (BCG, method A) and with chromoxane cyanine R (CCR, method B) in aqueous acidic buffer. The complex species, extractable to chloroform phase, were quantitatively measured at 415 and 460 nm for methods A and B, respectively. Beer's law was obeyed in the SC concentration range 1.25-25 mug ml(-1) with a limit of detection 0.16 mug ml(-1) and 1.5-60 mug ml(-1) with a limit of detection 0.18 mug ml(-1), respectively, for methods A and B. The methods have been successfully applied to the analysis of bulk drug and its tablets. No interference was observed from common pharmaceutical adjuvants.     

A sensitive determination of paraquat by spectrophotometry

A sensitive spectrophotometric method for the determination of a widely used herbicide, paraquat using a versatile reducing agent sodium borohydride is described. Paraquat is reduced with sodium borohydride in an alkaline medium to give a blue radical ion with an absorbance maxima at 600 nm. Beer's law is obeyed in the range of 0.05-0.5 mug ml(-1) of paraquat. The molar absorptivity and Sandell's sensitivity are found to be 2.9 x 10(5) l mol(-1) cm(-1) and 0.0006 mug cm(-2) respectively. The important analytical parameters and the optimum reaction conditions were evaluated. The method is free from the interference of other commonly used pesticides and metal ions. The method was applied successfully to the determination of paraquat in human samples, such as blood, urine and mother's milk compared to food and environmental samples.     

A rapid spectrophotometric method for determination of piperazine

A spectrophotometric method has been developed for the determination of piperazine and its salts (citrate, phosphate, and tartrate) without prior separation, based on the interaction of piperazine or any of its salts with phenothiazine and N-bromosuccinimide in aqueous methanol. The products exhibit absorption maxima at 448, 595 and 645 nm. Measurements are made at 595 nm. Beer's law is obeyed in the concentration range 0.5-5 mug/ml for piperazine salts and 0.5-3 mug/ml for piperazine hexahydrate. The method is rapid, simple and successful for analysis of some pharmaceutical preparations.     

Spectrophotometric determination of zinc with hydrazidazol in the presence of Triton X-100 and its application in metal analysis

A new spectrophotometric method for the determination of zinc is proposed. The chromogenic agent Hydrazidazol forms a 1:1 chelate with zinc in the presence of Triton X-100 in a medium containing 20-40% ethanol. The molar absorptivity and conditional formation constant have been found to be 2.7 x 1O(4) l.mole(-1).cm(-1) (at 640 nm) and 10(5.32) respectively. Beer's law is obeyed for zinc over the range of 0.2-0.8 mug/ml with a standard deviation of 0.024 mug/ml. The method can be applied to the determination of zinc in cadmium metal and its oxide after preconcentration by selective extraction of zinc thiocyanate into ethyl acetate in the presence of EDTA and thiosulphate as masking agents.