An Easy Spectrophotometric Method for the Determination of Hypochlorite Using Thionin

A simple, rapid, and sensitive spectrophotometric method has been developed for the determination of hypochlorite using thionin. The method is based on the reaction of hypochlorite with potassium iodide in acidic medium to liberate iodine. The liberated iodine bleaches the violet color of thionin, which is measured at 600 nm. The decrease in absorbance is directly proportional to the concentration of hypochlorite. Beer’s law is obeyed in the range 0.2– 1.2 µg/mL of hypochlorite. The molar absorptivity, Sandell’s sensitivity, detection limit, and quantitation limit are found to be 1.489 × 10⁴ L/(mol cm), 3.25 × 10⁻³ µg cm⁻², 0.1026 µg/mL, and 0.3112 µg/mL, respectively. The method has been successfully applied to the determination of hypochlorite in various samples of natural water, tap water, milk, etc.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 8, 2005, pp. 798–801.Original English Text Copyright © 2005 by Narayana, Mathew, Vipin, Sreekumar, Cherian.The text was submitted by the authors in English.     

Optimized and Validated Spectrophotometric Methods for the Determination of Roxatidine Acetate Hydrochloride in Drug Formulations Using 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone and <Emphasis Type="Italic">p</Emphasis>-Chloranilic Acid

Two simple and sensitive spectrophotometric procedures are proposed for the determination of roxatidine in pure form and in tablets. Both methods are based on the charge transfer complexation reaction of the drug with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) or p-chloranilic acid resulting in colored products. In both cases, the absorbance measurement was made at 530 nm. Beer’s law was obeyed in the concentration ranges 5–65 and 10–260 µg mL⁻¹ with DDQ and p-chloranilic acid, respectively. A series of variables were studied to optimize the reaction conditions. No interference was observed from the common excipients present in the formulations. The described methods were applied successfully for the analysis of roxatidine in pharmaceutical preparations. Statistical comparison of the results with those from our UV reference method shows excellent agreement. Both methods are validated statistically and do differ significantly in accuracy.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 7, 2005, pp. 715–722.Original English Text Copyright © 2005 by Nafisur Rahman, Mohammad Kashif.The text was submitted by the authors in English.     

Contribution of Diffuse Reflectance Spectroscopy to Monitoring the Synthesis Improvement of Encapsulated Complexes

Diffuse reflectance spectroscopy (DRS) can be regarded as a solid state technique contribution to monitoring the process of encapsulation of transition metal complexes into cavities of zeolites. By employing DRS, it was revealed that the effectiveness of a method suggested for higher encapsulation of a tris(bipyridine) cobalt(II) complex into zeolite Y can easily be manifested. In addition to that, simple diffuse reflectance spectra give information about a relative amount of two spin states of the cobalt bipyridine complexes and their alteration upon the method used.__________From Koordinatsionnaya Khimiya, Vol. 31, No. 8, 2005, pp. 618–620.Original English Text Copyright © 2005 by Zanjanchi, Tabatabaeian, Hosseinzadeh.This text was submitted by the authors in English.     

The Color Reaction of Mercury(II) with the New Reagent 2-Methylthiophenyldiazoaminoazobenzene and Its Application

A new and very sensitive and selective chromogenic reagent, 2-methylthiophenyldiazoaminoa-zobenzene (MTDAA), was synthesized and studied in detail for the determination of trace mercury(II) in water samples. The method is based on the color reaction between MTDAA and mercury(II). It was found that mercury(II) reacts with MTDAA in Na₂B₄O₇-NaOH buffer solution (pH = 10.0) to form 1 : 2 red complexes; these show maximum absorption at 520 nm. Beer’s law is obeyed in 0–15 µg of mercury(II) in 25 mL of solution. The apparent molar absorptivity of the complex is 1.33 × 10⁵ L/(mol cm); its limit of quantification, limit of detection, and relative standard deviation are 0.75 ng/mL, 0.27 ng/mL, and 1.0%, respectively, giving better sensitivity. The influence of the reaction variables and the effect of interfering ions are reported; most of the metal ions in water samples can be tolerated in considerable amounts. Only a few ions can interfere with the determination of trace mercury(II), but these can be eliminated by prior extraction. The proposed method is sensitive, simple, and rapid. It has been applied to the determination of trace mercury(II) in water samples with satisfactory results.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 7, 2005, pp. 703–706.Original English Text Copyright © 2005 by Guo, Din, Tian, Liu, Chang, Meng.The text was submitted by the authors in English.     

A new procedure for the spectrophotometric determination of nitrogen(II) oxide in solutions

A new simple and reliable procedure was developed for the spectrophotometric determination of nitrogen(II) oxide. The procedure is based on the determination of excess oxygen after its reaction with NO. Alkaline solutions of thiourea dioxide were used for the determination of oxygen. It was found that the decomposition of an alkaline solution of thiourea dioxide under aerobic conditions is accompanied by the formation of dithionite, and its concentration is proportional to the concentration of oxygen in the solution. The absorbance of the resulting dithionite was measured at 315 nm. The solutions obeyed Beers law at oxygen concentrations of 1 × 10^–5–1.5 × 10^–3 M. The analytical range for NO was 1 × 10^–5–1.5 × 10^–3 M. The proposed procedure was also used for the determination of nitrogen(II) oxide in aqueous-ethanolic solutions.Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 27–29.Original Russian Text Copyright © 2005 by Pukhovskaya, Guseva, Makarov, Naidenko.     

Solid Phase Extraction and Spectrophotometric Determination of Silver with 2-(2-Quinolylazo)-5-Dimethylaminophenol

A new chromogenic reagent, 2-(2-quinolylazo)-5-Dimethylaminophenol (QADMAP) was synthesized, and a sensitive, selective, and rapid method was developed for the determination of the μg/L level of silver ions. The method is based on the rapid reaction of silver(I) with QADMAP and the solid phase extraction of the colored chelate using a C₁₈ cartridge. The QADMAP reacts with Ag(I) in the presence of a citric acid-sodium hydroxide buffer solution (pH 5.0) and a sodium dodecyl sulfonate (SDS) medium to form a violet chelate of molar ratio 1 : 2 (silver to QADMAP). This chelate was enriched by solid phase extraction with C₁₈ cartridge, and the retained chelate was eluted from the cartridge using ethanol (with 1% acetic acid). In the ethanol medium (with 1% acetic acid), the molar absorptivity of the chelate was 1.25 × 10⁵ L mol⁻¹ cm⁻¹ at 584 nm. Beer’s law was obeyed in the range 0.01–0.6 μg/mL. The relative standard deviation for eleven replicate samples of 0.01 μg/mL was 1.86%. The detection limit is 0.02 μg/L in the original samples. The method was applied to the determination of μg/L levels of silver ions in water with good results.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 6, 2005, pp. 566–570.Original English Text Copyright © 2005 by Huang, Yang, Hu, Yin.This article was submitted by the authors in English.     

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.     

Kinetic Determination of Mercury(II) at Trace Level from Its Catalytic Effect on a Ligand Substitution Process

A catalytic kinetic method (CKM) is presented for the determination of mercury(II) based on its catalytic effect on the rate of substitution of N-methylpyrazinium ion (Mpz⁺) onto hexacyanoferrate(II). The progress of the reaction was monitored spectrophotometrically at 655 nm by registering the increase in absorbance of the product [Fe(CN)₅(Mpz]²⁻ under the reaction conditions: 5 × 10⁻³ mol L⁻¹ [Fe(CN)₆]⁴⁻), 5 × 10⁻⁵ mol L⁻¹ [Mpz⁺], T = 25.0 ± 0.1°C, pH 5.00 ± 0.02 and ionic strength, I = 0.1 mol L⁻¹ (KNO₃). Quantitative rate data at specified experimental conditions showed a linear dependence of the absorbance after fixed time A _t on the concentration of mercury(II) catalyst in the range 20.06–702.1 ng mL⁻¹. The maximum relative standard deviations and percentage errors for the determination of mercury(II) in the range of 20.06–200.6 ng mL⁻¹ were calculated to be 1.7 and 2.7% respectively. The detection limit was found to be 7.2 ng mL⁻¹ of mercury(II). Accuracy (expressed in terms of recoveries) was in the range of 98–103%. Figures of merit and interference due to many cations and anions was investigated and discussed. The applicability of the method was demonstrated by determining the mercury(II) in different synthetic samples and confirming the results using atomic absorption spectrophotometry. The proposed method allowed determination of mercury(II) in the range 20.06–702.1 ng mL⁻¹ with very good selectivity and an output of 30 samples h⁻¹.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 6, 2005, pp. 654–661.Original English Text Copyright © 2005 by Surendra Prasad.This article was submitted by the author in English.     

Determination of trace europium(III) based on a new fluorescence enhancement system of europium(III) with N,N′-<Emphasis Type="Italic">bis</Emphasis>-(4-N-aminothiourea-2-amylidene)-4,4′-diaminodiphenyl sulfone by EDTA or alumin in N,N-dimethylformamide

A new bis-Schiff base ligand, N,N-bis-(4-N-aminothiourea-2-amylidene)-4,4-diaminodiphenyl sulfone (ARADS), was synthesized. The solutions of its complex with Eu³⁺ in DMF can emit the intrinsic fluorescence of Eu³⁺. The fluorescence intensity of the complex was enhanced 20–30-fold in the presence of EDTA (or alum). The influence of seven kinds of solvents (DMF, CH₃CN, THF, acetone, CH₃OH, C₂H₅OH, and DMSO) on the intensity of fluorescence was studied. The results showed that the Eu³⁺-ARADS-EDTA (or alum) system emits its strongest fluorescence in DMF. Thus, the system can be used to develop a new method for the determination of europium(III). The excitation and emission wavelengths are 395 and 615 nm, respectively. Under optimal conditions, the fluorescence intensities vary linearly with the concentration of Eu³⁺ in the range 6.0 × 10^–10–5.2 × 10^–5 mol/L, with a detection limit of 5.0 × 10^–10 mol/L. The interference from some rare earth metals and other inorganic ions are described. The method is a selective, sensitive, rapid, and simple analytical procedure for the determination of europium(III) in high-purity yttrium oxide and synthetic samples. The mechanism of fluorescence enhancement was also studied.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 4, 2005, pp. 372–377.Original English Text Copyright © 2005 by Tianlin Yang, Wenwu Qin, and Weisheng Liu.The article was submitted by the authors in English.     

Activity enhancement of CuZn-impregnated FSM-16 by modification with 1,3-butanediol for steam reforming of methanol

Catalytic activities of CuZn-impregnated FSM-16 catalysts, prepared by the conventional impregnation method and a modified impregnation method with 1,3-butanediol, in steam reforming of methanol were examined. The catalytic activity of the modified CuZn-impregnated FSM-16 was remarkably higher than that of the one prepared by the conventional impregnation method. Characterization of the catalysts by XRD and TPR showed that the enhancement in catalytic activity is due to an improvement in copper dispersion. The amount of 1,3-butanediol, the calcination temperature, and the amount of metal loading were varied to seek the optimal catalyst with the highest methanol conversion. Besides 1,3-butanediol, other organic compounds such as 1,3-propanediol, ethylene glycol, and citric acid also resulted in an enhancement in catalytic activity, while propanol did not.From Kinetika i Kataliz, Vol. 46, No. 1, 2005, pp. 64–72.Original English Text Copyright © 2005 by Jakdetchai, Takayama, Nakajima.This article was submitted by the authors in English.     

Ion-Chromatographic Determination of Borates and Sulfides with the Use of a Developing Column

Aspects of the sensitive and selective determination of borates and sulfides were considered. A method was proposed for substantially increasing the sensitivity of the ion-chromatographic determination of weak acids by their conversion into corresponding salts on an auxiliary column with a cation exchanger in the K form. It was demonstrated that the detection limit of the cations under consideration can be decreased to 5–10 µg/L and the selectivity of the method is sufficient for the determination of trace borates in strongly mineralized waters like sea water.__________Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 8, 2005, pp. 832–836.Original Russian Text Copyright © 2005 by Kolotilina, Dolgonosov.     

Electrochemical Oxidation of Iodide in the Presence of Benzenesulfinic Acids and Its Application to the Quasi-Catalytic Determination of Benzenesulfinic Acids

The mechanism of the electrochemical oxidation of iodide in the presence of 4-toluenesulfinic acid was studied in an aqueous solution using cyclic voltammetry and controlled-potential coulometry. The results indicate that the anodically generated iodine reacts with 4-toluenesulfinic acid through a quasi-catalytic process. In addition, the results indicate the suitability of iodide as a mediator for the determination of 4-toluene-sulfinic acid in aqueous solutions. The quasi-catalytic peak currents are linearly dependent on the 4-toluene-sulfinic acid concentrations in the range 6.0 ×10⁻³ − 8.0 × 10⁻⁶ M.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 6, 2005, pp. 598–602.Original English Text Copyright © 2005 by Davood Nematollahi, Zinat Forooghi, Esmail Tammari.This article was submitted by the authors in English.     

Electrothermal vaporization in inductively coupled plasma atomic emission spectrometry for direct multielement analysis of food samples with slurry sampling

Slurry sampling followed by electrothermal vaporization (ETV) was used as sample introduction technique in inductively coupled plasma atomic emission spectrometry (ICP-AES) for the direct determination of trace elements in food samples. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating reagent to promote vaporization and the transportation of analytes. The main factors affecting the analytical signals were investigated in detail. Under optimum operating conditions, the detection limits (DL) for this method varied from 1.8 (Cu) to 215 ng/mL (Zn), while the relative standard deviations (RSD) were in the range 2.6% (Cu)-7.2% (Zn). The proposed method was successfully applied to the direct determination of trace amounts of V, Cu, Cr, Fe, Zn, and La in rice without any chemical pretreatment. The precision was evaluated by analyzing a standard reference material (tea leaves, GBW 07605) and comparing the results from this method with results obtained by pneumatic nebulization (PN) ICP-AES after the wet-chemical decomposition of the same sample.From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 3, 2005, pp. 286–290.Original English Text Copyright © 2005 by Chen.This article was submitted by the author in English.     

Determination of nanomole quantities of lower aldehydes by cold-vapour atomic absorption spectrometry

A method is described for the determination of 10–100 nmole of methanal and 20–150 nmole of ethanal and propanal. The method is based on the oxidation of aldehydes to the corresponding acids by mercuric ion which in turn is reduced to elemental mercury, followed by cold-vapour atomic absorption spectrometry. Calibration plots were constructed between the concentration of each aldehyde and absorbance, while the calibration from the conventional cold vapour procedure was used for total aldehydes determination. The method is selective and can be used for aldehyde determination in the presence of ketones, acetals, alcohols, acids, esters, ethers, organic chlorides and epoxides. This simple method is characterised by 98–102% recoveries and standard deviations of 3%.     

Analytical characteristics of electrodes selective for cationic phospholipid–Ba <Superscript>2+</Superscript> complexes

The interaction between organic cations of phospholipids products of their hydrolysis with the PMo₁₂O ₄₀ ^3– heteropoly anion was studied. A procedure was proposed for the direct potentiometric determination of phospholipids using ion-selective electrodes bearing poorly soluble ion pairs formed by the complexes of lecithin or ethanolamine glycerophosphate and Ba²⁺ and PMo₁₂O ₄₀ ^3– heteropoly counter anion as ionophores. The procedure is simple, rapid, sufficiently sensitive, and selective.Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 60–63.Original Russian Text Copyright © 2005 by Golovei, Tkach.     

Application of 1,2-Dihydroxybenzene-3,5-disulfonic Acid for the Separation and Preconcentration of Trace Molybdenum and Its Determination by Third Derivative Spectrophotometry

Molybdenum was quantitatively extracted form large volumes of aqueous solutions of various samples by 1,2-dihydroxybenzene-3,5-disulfonic acid (Tiron) and tetradecyldimethylbenzylammonium chloride (TDBA) on microcrystalline naphthalene in the pH range 6.5–8.5. After filtration, the solid residue consisting of molybdenum complex and naphthalene was dissolved in 5 mL of chloroform and molybdenum was determined by third derivative spectrophotometry. Alternatively, molybdenum can be quantitatively adsorbed on Tiron-TDBA-naphthalene adsorbent packed in a column and determined in a similar manner. About 0.02 µg of molybdenum can be concentrated in a column from 500 mL of aqueous sample, where its concentration is as low as 0.04 ng/mL. Various parameters such as the effect of pH, the volume of the aqueous phase, and the interference of a number of metal ions with the determination of molybdenum have been studied in detail to optimize the analysis of standard alloys and biological samples.__________From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 7, 2005, pp. 698–702.Original English Text Copyright © 2005 by Mohammad Ali Taher, Sayed Ziae Mohammadi Mobarakeh.The text was submitted by the authors in English.     

X-ray Fluorescence Determination of Carbon,Nitrogen, and Oxygen in Fish and Plant Samples

The potentials of X-ray fluorescence analysis in the determination of carbon, nitrogen, and oxygen in materials of plant and animal origin were studied. The contribution of photoelectron excitation to the analytical signal and the effect of uncertainties in the attenuation coefficient on the calculation of element concentrations by the absorption correction method were estimated. Methods for calculating analyte concentrations using simple linear regression with absorption correction and multiple regression were compared. The results were also compared with those of pyrolysis-gas-chromatography. The error of the method was 1–2% for element concentrations between 10 and 50% and 25% in the range of nitrogen concentration 1–2%.__________Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 5, 2005, pp. 485–489.Original Russian Text Copyright © 2005 by Farkov, Ilicheva, Finkelshtein.     

Application of the Hertz-Langmuir Equation to Studying the Kinetics of Dehydration of Solid Compounds in Air

A simple and reliable method was suggested for studying thermal dehydration of solid substances. The method is based on the application of the Hertz-Langmuir equation to determining the rate of decomposition in air and on the use of the third-law method for calculating the enthalpy of the process.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 3, 2005, pp. 384–389.Original Russian Text Copyright © 2005 by L’vov, Ugolkov.     

Indirect Kinetic–Spectrophotometric Determination of Resorcinol, Catechol, and Hydroquinone

A rapid, simple, and sensitive method for the determination of trace amounts of resorcinol, catechol, and hydroquinone in aqueous media has been proposed. The method is based on their reaction with nitrite. The excess nitrite is then determined by a kinetic method based on its reaction with Neutral Red. The reaction is monitored spectrophotometrically by measuring the decrease in the absorbance at 530 nm by a fixed time method. Resorcinol, catechol, and hydroquinone could be determined by the proposed method in the ranges of 0.1–2.0 mg/mL, 0.25–2.0 mg/mL and 0.1–3.0 mg/mL, respectively. The method was applied to the determination of resorcinol and catechol in pharmaceutical formulations with satisfactory results.     

Phosphorimetric Determination of Active Components in Medicinal Preparations

The use of room-temperature phosphorescence was proposed for the determination of active components containing naphthalene rings in their structures in medicinal preparations. It was demonstrated that this method can be used for the determination of active components in combined preparations.__________Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 5, 2005, pp. 479–484.Original Russian Text Copyright © 2005 by Rekharskaya, Polenova, Borzenko.