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EN
Abstract Detailed investigations on the possibility for determination of the oxygen stoichiometry in YBa2Cu3Oy superconducting samples by measuring the absorbance of the colored Co(III)-EDTA and Cu(II)-EDTA complexes in one solution have been performed. The absorptivity of the complexes at pH 2.5 and 4.9 as well as Beer’s law have been studied. The content of the solution for the sample dissolving has been established. The stoichiometry of the oxidation-reduction reaction between Cu(III) from the sample and Co(II) in the solution has been proved. The possibility to dissolve the sample in air has been tested. As a result a simple and rapid spectrophotometric method for the determination of the δ non-stoichiometric oxygen coefficient in YBa2Cu3O6.5+δ samples has been developed without precise measurement of the sample mass. The standard deviation of the δ- and y-coefficient results is 0.017. The reproducibility of the y-values in relative units (sr ) is 0.2%. The accuracy of the results has been confirmed by the method, which is based on the absorbance measurement of the I 3−-starch compound. Graphical abstract [...]
EN
Complex formation and liquid-liquid extraction were studied in systems containing indium(III), 4-(2-pyridylazo)resorcinol (PAR), phenylmethoxybis(tetrazolium) salt (MBT), water and chloroform. The following MBTs, which differ only by the number of -NO2 groups in their cationic parts, were used: 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis(2,5-diphenyl-2H-tetrazolium chloride) (Blue Tetrazolium chloride, BT), 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis[2-(4-nitrophenyl)-5-phenyl-2H-tetrazolium chloride] (Nitro Blue Tetrazolium chloride, NBT) and 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis[2,5-di(4-nitrophenyl)-2H-tetrazolium chloride] (Tetranitro Blue Tetrazolium chloride, TNBT). The composition of the formed ternary complexes was determined, In:PAR:MBT=1:2:2, and the optimum conditions for their extraction found: pH, shaking time, concentration of the reagents and the sequence of their addition. Some key constants were estimated: constants of extraction (Kex), constants of association (β) and constants of distribution (KD). BT appears to be the best MBT for extraction of the In(III)-PAR species, [In3+(OH)3(PAR)2]4−, (Log Kex=10.9, Log β=9.8, Log KD=1.12, R%=92.7%). Several additional characteristics concerning its application as extraction-spectrophotometric reagent were calculated: limit of detection (LOD = 0.12 µg cm−3), limit of quantification (LOD = 0.40 µg cm−3) and Sandell’s sensitivity (SS =1.58 ng cm−2); Beer’s law is obeyed for In(III) concentrations up to 3.2 µg mL−1 with a molar absorptivity coefficient of 7.3×104 L mol−1 cm−1 at λmax=515 nm. [...]
EN
Environmental tobacco smoke (ETS) contains many toxic compounds which include substances classified as aldehydes (e.g. formaldehyde) and inorganic substances such as cyanide ions. The information on the determination of these compounds in water is available, but the monitoring data on the level of these substances in human body fluids are still lacking. In this work the procedure for determining cyanide ions and formaldehyde in samples of human nasal discharge by simple spectrophotometric technique is presented.
EN
The multivariate calibration methods, partial least squares (PLS) and principle component regression (PCR) have been used to determine phenanthridine, phenanthridinone and phenanthridine N-oxide in spiked human plasma samples. Resolution of binary and ternary mixtures of analytes with minimum sample pre-treatment and without analyte separation has been successfully achieved analyzing the UV spectral data. The net analyte signal (NAS) concept was also used to calculate multivariate analytical figures of merit such as limit of detection, selectivity and sensitivity. The simultaneous determination of three analytes was possible by PLS and PCR processing of sample absorbance in the 210–355 nm region. Good recoveries were obtained for both synthetic mixtures and spiked human plasma samples. [...]
EN
The present research work discusses the simple, specific and economical UV Spectrophotometric method has been developed using acetonitrile-water (80:20v/v) as a diluent to estimate elagolix sodium content in bulk and pharmaceutical dosage formulation. Spectrophotometric method has been developed for the estimation of elagolix sodium in Tablet dosage form. The maximum wavelength λmax was found to be 274.5 nm. A recovery percentage of elagolix sodium in tablet formulation was observed in the range of (98.85-100.72%). Beers law was obeyed in the concentration range of 12-48 μg/ml. Calibration curves shows a linear relationship between the absorbance and concentration. The line equation y = 24.851x - 0.0232 with (R2 = 0.9979). The LOD and LOQ are 0.00133 μg/ml and 0.00403 μg/ml respectively. Validation was performed Linearity, specificity, accuracy, precision, LOD and LOQ. The sample solution was stable up to 48 hours.
EN
Complex formation and liquid-liquid extraction have been studied for ternary complexes of vanadium(IV) with 4-(2-pyridylazo)-resorcinol (PAR) and ditetrazolium chlorides (DTC) in a water-chloroform medium. The specific ditetrazolium compounds investigated were i) 3,3′-(4,4′-biphenylene)-bis(2,5-diphenyl-2H-tetrazolium) chloride (Neotetrazolium chloride, NTC); ii) 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)-bis(2,5-diphenyl-2H-tetrazolium) chloride (Blue Tetrazolium chloride, BTC); and iii) 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)-bis[2-(4-nitrophenyl)-5-phenyl-2H-tetrazolium] chloride (Nitro Blue Tetrazolium chloride, NBT). Molar absorptivity coefficients and the composition of the complexes have been calculated. Association constants (β) have also been obtained for the interactions between the vanadium(IV) - PAR anionic chelates [VO(PAR)2]2− (I) and [VO(OH)2(PAR)2]4− (II), and ditetrazolium cations (DT2+). Some special features of NBT as an extraction-spectrophotometric reagent for vanadium(IV) have been discussed. Unlike NTC and BTC which form complexes with both I and II, NBT associates only with II. The pH interval for complete extraction of (NBT2+)2[VO(OH)2(PAR)2] is broader and allows work at lower pH values the other ion-associates of V(IV,V)-PAR that were studied. NBT is -therefore the appropriate reagent both for direct V(IV) determination and for V(IV)/V(V) separation. Some additional characteristics for the V(IV)-PAR-NBT-water-chloroform system have been determined: extraction constant, distribution constant, recovery factor, limit of detection and limit of quantification. Beer’s law is valid up to 1.4 μg mL−1 vanadium(IV) with molar absorptivity coefficient of 3.55×104 L mol−1 cm−1 at λmax=559 nm. [...]
EN
Complex formation and liquid-liquid extraction were studied in systems containing indium(III), 4-(2-pyridylazo)resorcinol (PAR), tetrazolium salt (TZS), water and chloroform. Two different TZS were used: 2,3,5-triphenyl-2H-tetrazolium chloride (TTC) and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide (MTT). The optimum conditions for extraction of In(III) as a ternary complex, (TT+)[In(PAR)2] or (MTT+)[In(PAR)2], were found: pH, extraction time, concentration of PAR and concentration of TZS. The constants of extraction (Kex), constants of association (β), constants of distribution (KD) and recovery factors (R%) were determined. The apparent molar absorptivities in chloroform were calculated to be ɛ′520=6.6×104 L mol−1 cm−1 and ɛ′515=7.1×104 L mol−1 cm−1 for the systems with TTC (I) and MTT (II), respectively. Beer’s law was obeyed for In(III) concentrations up to 3.4 µg mL−1 in both the cases. The limits of detection (LOD=0.07 µg mL−1I and LOD=0.12 µg mL−1II), limits of quantification (LOQ=0.24 µg mL−1I and LOQ=0.41 µg mL−1II) and Sandell’s sensitivities (SS) were estimated as well. [...]
EN
New simple, rapid, and accurate spectrophotometric techniques for sulphanilamides assay in combination drugs have been elaborated. The method is based on the formation of coloured products of sulphanilamides diazonium salt azoсoupling with heterocyclic azo reagent 4-(2-thiazolylazo)-resorcinol (TAR) in alkaline medium (pH 9.5) with the following measurement of their absorbance at λmax = 615 nm. Formed products are stable for 1 hour at room temperature. Effective molar absorptivities at absorbance maximum 615 nm for disazo dyes were ~ 104 M-1 cm-1. Linear ranges for sulphanilamides determination were 0.5−30.0 μg mL-1. The developed method was used for the suphanilamides determination in tablets, powder, solutions, suspensions and ointments.
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