Indication Ion Square Wave Voltammetric Determination of Thiamine and Ascorbic Acid

Abstract

Cd²⁺ ion was used as an electrochemical indicator to detect V_B1 or Vc using square ware voltammetry (SWV) at a mercury film‐coated glassy carbon (GC) electrode. At pH=10 NH₃‐NH₄Cl buffer, a new cathodic peak was found at ?0.360 V (vs.SCE) by addition of thiamine, and the peak current of SWV was linear with the concentration of thiamine in the range of 1×10^?6 to 4×10^?3 M. On the other hand, the SWV peak current of Cd²⁺ at ?0.856 V linearly decreased with addition of ascorbic acid in the range of 6×10^?6～10^?3 M. The effects of interference, such as citric acid, DL‐malic acid, and calcium panlothenate, on thiamine or ascorbic acid determination were investigated. This method was successfully applied to the determination of thiamine or in pharmaceutical preparation.     

New Rapid Assay for Nafcillin by Spectrofluorimetry in Pharmaceutical Dosage

Abstract

A method for the spectrofluorimetric determination of nafcillin is proposed (λ_ex = 226 nm, λ_em = 366 nm), for concentrations between 0.10 and 1.0 μg mL^?1. The method was performed in ethanol/water medium (30% V/V), at apparent pH 6.0 provided by adding of phosphate buffer solution with pH = 6.20.

The obtained values of detection and determination limits are 0.016 and 0.054 μg mL^?1, respectively.

The method was successfully applied to assay a commercial injection containing nafcillin sodium monohydrate.     

A Fluorimetric Method for the Determination of Cyanide with Fluorescein and Iodine∗

Abstract

A rapid, simple and sensitive fluorimetric method has been developed for the determination of cyanide with fluorescein as fluorogenic reagent (λ_ex = 494 nm, λ_em = 514 nm) at pH 6.0–7.0. A linear calibration curve was obtained in the range 0.004–2.0 μg CN^?/25 ml. The detection limit is 0.004 μg CN^-/25 ml. The method was successfully applied to the determination of cyanide in waste water.

     

Pyrocatechol-1-Aldehyde 2-Benzothiazolylhydrazone As Reagent for the Spectrofluorimetric Determination of Nanogram Amounts of Gallium in Urine and Blood Serum

Abstract

A method is developed for the spectrofluorimetric determination of 1–80 ng.ml^?1 of gallium with pyrocatechol-1-aldehyde 2-benzothiazolylhydrazone, in a 50% (v/v) DMSO-Water medium at apparent pH 4.0 (monochloracetic/monochloracetate buffer). Λ_ex = 400nm, Λ_em = 504 nm (corrected). Interferences have been evaluated and the method applied to the determination of gallium in human urine and blood serum samples.     

Kinetic Spectrophotometric Determination of Traces of Manganese(II) by Its Catalytic Effect on Oxidation of 4‐Hydroxycoumarin with Potassium Permanganate in River Water Samples

Abstract

A new kinetic method for determination of traces of manganese(II) based on its catalytic effect on the oxidation of 4‐hydroxycoumarine with KMnO₄ at pH=1.35 and at a temperature of 25°C was proposed. The reaction was followed spectrophotometrically by measuring the decrease in the absorbance of the dye at 525 nm. The calibration graph is linear in the range 20–200 ng/cm³. The effects of certain foreign ions upon the reaction rate were determined for assessment by the selectivity of the method. The proposed method has been applied for determination of manganese(II) in river water samples with satisfactory results.     

Extract-Photometric Determination of Vanadium with Isophthaldihydroxamic Acid

Abstract

The spectrophotometric study of violet complex isophthaldihydroxamic acid-vanadium extracted into solution of trioctylmethylammonium chloride in ethylacetate was made (λ_max = 380 nm, ? = 7500 l.mol^?1.cm^?1; λ_max = 510 nm, ? = 5510 l.mol^?1 .cm^?1; stoichiometries, 1:1 and 1:2, V:reagent). A new method for the extract-spectrophotometric determination of V(V) in the range 14–80 μg of vanadium is proposed.     

Spectrophotometric Determination of Formaldehyde

ABSTRACT

A simple and very sensitive method for the determination of formaldehyde is described. Formaldehyde reacts with phloroglucinol in acid medium producing a yellow dye with λ_max at 435nm. The method is useful for the determination of formaldehyde in the range 0-2.5μg in an overall volume of 10mL with molar absorptivity of 8.3 × 10⁴1 mol^?1 cm^?1 and a relative standard deviation of 2% at 1.5μg level (n=10).     

Fluorometric Determination of Traces Of Mg(II) Using 1, 5-Dihydroxyanthracuinone as Reagent

Abstract

The florescent characteristics of the complex formed by 1, 5-dihydroxyanthraquinone with Mg(II) in aqueous ethanol (λ_ex 490 nm,λ_em=600 nm; pH_ap=9.1-9.6; 10% H₂O; reagent concentration=4×10^?5M) are described. The stoichiometry and the stability constant (1:1 and log K=4.90) are determined. A new fluorometric method for the determination of 10-100 ppb Mg(II) is proposed.     

Spectrophotometric Study of 1, 3-Cyclohexanedione Bisthiosemicarbazone Monohydrochloride -Bi (III) Complex. Determination of Bi (III)

Abstract

The spectrophotometric study was made of red-violet 1, 3-cyclohexanedione bis-thiosemicarbazone-Bi (III) in an acidic dimethylformamide-water solution (λ_max = 540 nm, ? = 3.3 × 10^?4 1. mol^?1. cm^?1, stoichiometry 3:1, apparent stability constant (6.0 × 10¹⁰). A new method for the spectrophotometric determination of Bi (III) is proposed for concentrations between 0.7 and 7.4 ppm. The relative error (95 % confidence level) is 0.5 % for 3.7 ppm of Bi (III).

The extraction with methyl isobutyl ketone of the red-violet complex was also studied spectrophotometrically (λ_max = 550 nm, ? = 3.34 × 10⁴ 1. mol^?1.cm^?1, stoichiometry 2:1). A new method for the extraction-spectrophotometric determination of Bi (III) is proposed for concentrations, in aqueous phase, between 0.2 and 1.2 ppm. The relative error (95 % confidence level) is 0.8 % for 0.9 ppm of Bi (III).     

Dispersive liquid-liquid microextraction followed by spectrofluorimetry as a simple and accurate technique for determination of thiamine (vitamin B1)

Dispersive liquid-liquid microextraction (DLLME) combined with spectrofluorimetry was applied to the extraction, pre-concentration and analysis of thiamine (vitamin B₁). The procedure is based on (a) the oxidation of thiamine with ferricyanide to form fluorescent thiochrome (TC), (b) the trapping of TC into a microextraction solvent, and (c) spectrofluorometric determination. Microextraction solvent and disperser solvent are directly injected into an aqueous solution containing TC. After centrifuging, phase separation is performed by sedimenting the fine droplets of the microextraction solvent on the bottom of a test tube. The settled phase is transferred into a fluorometer for the determination of thiamine at excitation/emission wavelengths of 375/438 nm. Under the optimized experimental conditions, the method provides a linear dynamic range of 0.2–100 ng mL^?1, a detection limit of 0.06 ng mL^?1, and a relative standard deviation of 3.0%. The method was successfully applied to pharmaceutical formulations and human urine. The results were validated by recovery test and by comparison with other methods, and were found to be highly satisfactory.     

Low-Temperature Phosphorescence Analysis of Mebendazole and Related Imidazoles

Abstract

Native low-temperature phosphorescence of mebendazole and flubendazole in ethanol is used for the determination of these imidazoles in anthelmintic preparations with wavelength maxima and detection limits of λ_EXC = 322 nm, λ_EM = 454 nm; 10 ng ml^?1 and λ_EXC = 325 nm, = λ_EM = 455 nm; 5 ng ml^?1, respectively, with linear response up to 8 μg ml^?1 and 9 μg ml^?1, respectively. The structural basis of these phenomena is discussed for both compounds and for related imidazoles and benzimidazoles. Apart from good sensitivity and excellent specificity offered by the technique, the use of cryogenic equipment (liquid nitrogen, special cuvettes, expensive dewar cells) implies some disadvantages for routine analyses.     

Colorimetric Sensing of the Insensitive Energetic Material 3-Nitro-1,2,4-triazol-5-one (NTO) Using l-Cysteine Stabilized Gold Nanoparticles and Copper(II)

Abstract

Since conventional sensitive explosives have given rise to unforeseen accidents during storage and transport, the demand of modern armies for insensitive energetic materials is on the rise. There are very few determination methods for the most widely used insensitive energetic materials such as 3-nitro-1,2,4-triazole-5-one (NTO). Thus, the aim of this work is the development of a rapid and practical nanoparticle-based colorimetric sensor for determination of NTO. The detection principle of the sensor involved electrostatic attraction of NTO anion to the ammonium group of l-cysteine functionalized gold nanoparticles (AuNP-Cys), followed by the formation of a Cu²⁺-coordination complex between particles to result in AuNPs agglomeration. The concomitant color change was from red to violet. The surface plasmon resonance band of AuNPs at 520?nm shifted to 650?nm upon chemical reaction and agglomeration. Spectroscopic evaluation was made by taking the ratio of 650?nm absorbance to that of 520?nm, and correlating this ratio to NTO concentration. The analytical performance characteristics of this ratiometric sensor for NTO as the molar absorptivity (ε); limits of detection (LOD) and quantification (LOQ) were: ε = (8.62?±?0.29) × 10³ L mol^?1 cm^?1, LOD = 0.25?mg L^?1, and LOQ = 0.85?mg L^?1. The sensor was applied to various energetic material mixtures containing 2,4,6-trinitrotoluene, hexahydro-1,3,5-trinitro-1,3,5-triazine, octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine, and tetryl. Additionally, the possible interference effects of commonly found soil ions such as Cl^–, NO₃^–, SO₄^2–, PO₄^3–, Mg²⁺, Ca²⁺, Na⁺, and K⁺ were studied. The proposed method was statistically validated against a literature liquid chromatography–tandem mass spectrometry (LC/MS-MS) method.     

Triphenyltetrazolium chloride as a new analytical reagent for molybdenum(VI): Application to plant analysis

Solvent extraction of molybdenum(VI) ion associate with triphenyltetrazolium chloride (TTC) has been studied. TTC was proposed as reagent for the spectrophotometric determination of micro amounts of molybdenum(VI) at λ_max 250 nm. The optimum conditions for extraction of molybdenum(VI) as an ionassociation complex with TTC has been determined. Beer’s law is obeyed in the range of 0.5–10 μg/mL molybdenum(VI). The molar absorptivity of the ion-pair is 1 × 10⁶ L/mol cm. The sensitivity of the method is 9.6 × 10⁻⁵ μg/cm². The characteristic values for the extraction equilibrium and the equilibrium in the aqueous phase are: distribution constant K _D = 32.64, extraction constant K _ex = 2.19 × 10¹⁰ association constant β = 6.71 × 10⁸. The interferences of different cations, anions on molybdenum(VI) determination were also investigated. A sensitive and selective method for the determination of microquantities of molybdenum(VI) has been developed. The determination was carried out without preliminary separation of molybdenum. A novel procedure of molybdenum(VI) extraction and spectrophotometric determination in different plant samples was examined.     

Complex Formation Equilibria of Iron(III) With 2-Hydroxy-3- Pyridinol and 2-Mercapto-3-Pyridinol. Spectrophotometry Determination of Iron(III) In Multivitamins

ABSTRACT

The complex equilibria of iron(III) with 2-hydroxy-3-pyridinol (HHP), and 2-mercapto-3-pyridinol (MHP) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaCIO₄). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance pH-graphs. After considering all the different parameters a simple, rapid, sensitive and selective method for spectrophotometric determination of trace levels of iron(III) was proposed based on the formation of (Fe -MHP) complex at pH 2.5 (λ_max = 640 nm, ? = l×10⁴ L mol^?1 cm^?). The interference of a large number of foreign ions was investigated. The method has been applied successfully for the determination of iron content in some multivitamins with mineral preparations and infant milk products.     

Spectrophotometric Study of 1,2,7-Trihydroxyanthraquinone-Mg(II) Complex. Determination of Mg(II)

Abstract

The spectrophotometric study of violet complex Anthrapurpurin-Mg(II) in a basic medium and a hydroalcoholic solution was made (δ_max - 530 nm., ? = 3.5 × 10³ 1 mol^?1 cm^?1, stoichiometry 1:1, apparent constant of stability log K = 9. 26). A new method for the spectrophotometric determination of Mg(II) is proposed for concentrations between one and six ppm. Relative errors between replicate samples were 0.90 %.     

Spectrofluorimetric Flow Injection Determination of Glycerol & Ethylene Glycol with Alizarin Navy Blue

ABSTRACT

A simple and accurate procedure for indirect spectrofluorimetric determination of glycerol and ethylene glycol in aqueous media was developed. Alizarin Navy Blue can be oxidized by potassium periodate to produce a fluorescent compound, that can be detected fluorimetrically (λ_ex = 370 nm, λ_em = 516 nm) by a flow through method. Glycerol and ethylene glycol react with periodate decreasing its concentration and thus the forming the basis for an indirect determination of these compounds. The influence of acid concentration, reagent concentration and manifold variables were studied. For glycerol and ethylene glycol linear calibration curves were obtained in the ranges of 4.8 × 10^-7 – 8.7 × 10^-5 M and 6.4 × 10^-7 – 8.7 × 10^-5 M, respectively. The limit of detection (defined as the concentration that gives a signal three times the standard deviation of the background signal) for glycerol and ethylene glycol was 3.2 × 10^-7 M and 4.3 × 10^-7 M, respectively. The proposed method was applied for determination of glycerol and ethylene glycol in synthetic and real samples. The results obtained were satisfactory.     

A Fluorimetric Method for the Determination of Atmospheric Sulphur Dioxide With 2′, 7′—Dichlorofluorescein∗

Abstract

A rapid, simple and sensitive fluorimetric method has been developed for the determination of atmospheric sulphur dioxide with dichlorofluorescein as fluorogenic reagent (λ_ex = 505 nm, λ_em = 520 nm) at pH 4.0–6.0. A linear calibration curve was obtained in the range 0.01–0.40 μg SO₂/25 ml. The detection limit is 0.01 μg SO₂/25 ml. Nitrogen dioxide does not interfere with the method. The method was successfully applied to the determination of atmospheric sulphur dioxide.

     

Cyclohexane-1, 3-Dione bis (4-Methylthiosemicarbazone) as a Spectrophotometric Reagent for the Determination of Zn (II)

Abstract

The spectrophotometric study of reddish cyclohexane-1, 3-dione bis (4-methylthiosemicarbazone)-Zn(II) was made in dimethylformamide-water solution (λ_max= 475 nm, ∑ = 3.3×10⁴ 1.mole^?1. cm^?1. Sandell sensitivity = 2×10^?2 μg Zn(II).cm^?2, stoichiometry 1:1, and apparent stability constant 6.1×10⁴). A new method for the spectrophotometric determination of Zn(II) is proposed for concentrations between 0.1 and 2.5 ppm. The relative error (95% confidence level) is 0.7% for 1.0 pprn of Zn(II).

The extraction with ethylacetate of the reddish complex was also studied spectrophotometrically (λ_max = 493 nm, ∑ in organic phase = 4.8×10⁴ 1.mole^?1.cm. Sandell sensitivity = 3.4×10^?4 μg Zn(II).cm^?2, stoichiometry 1:1, apparent extraction constant 1.4×10⁴). A new method for the extraction-spectrophotometric determination of Zn(II) is proposed for concentrations, in aqueous phase, between 0.02 and 0.30 ppm. The relative error (95% confidence level) is 1.0% for 0.15 pprn of Zn(II).     

A Fluorescence Synergistic Method for the Determination of Stilboestrol

Abstract

A simple, highly sensitive and selective fluorescence synergistic method has been developed for rapid determination of stilboestrol with Triton × — 100 (λ_ex = 318nm, λ_em = 415nm) at pH 8.80 ～ 10.20. The calibration graph is linear over the range of 0.0 ～ 30.0μg/10ml. The detection limit is 0.03μg/ml stilboestrol. The method has been successfully applied for the determination of stilboestrol in tabellae stilboestrol and injectio stilboestrol with satisfactory results. It can also be applied for the determination of stilboestrol in body fluid of special patients.     

A Fluorescence Quenching Method for the Determination of Iodide Ion with Salicylfluorone and Hydrogen Peroxide

Abstract

A highly sensitive and selective fluorescence quenching method has been developed for rapid determination of iodide ion with salicylfluorone (SAF) as fluorogenic reagent (λ_ex = 495 nm, λ_em = 520 nm) at pH 2.5-3.0. The calibration graph is linear over the range 0.05-300 μg/25 ml. The detection limit is 0.05 μ/25 ml iodide. Other halide ions do not interfere with the determination even when present in large excess. The method is rapid and was successfully applied for the determination of iodide ion in sodium chloride, table salt and low sodium salt.