Methylene Blue Poly(Vinyl Chloride) Membrane Electrode Based on the Methylene Blue-Teteraphenylborate Ion-Pair Complex and Its Application to Pharmaceutical Analysis

Abstract

A methylene blue (MB) poly (vinyl chloride) membrane electrode based on MBtetraphenylborate (TPB) ion-pair complex is described. The linear response covers the range 1x10^?2 - 1x10^?6 mol dm^?3 MB solution, with a slope of 56.5±0.5 mv/decade (pH range 3.0-1 0.0). The detection limit is 7.75x 10^?7 mol dm^?3. The electrode shows stability, good reproducibility and fast response. Interferences from common inorganic cations and some organic bases are negligible. These characteristics of the electrode enabled it to be used successfully for the determination of MB in injection.     

Determination of Lysine in Nutrition Sample by Adsorption Voltammetry

Abstract

Lysine can be determined by adsorptive voltammetry after derivatization with acetaldehyde in 1.3 x 10^?2mol/ L borax-NaOH buffer solution (containing 4 x 10^?3mol/ L of CH₃CHO at pH10). The Schiff's base product of the derivation can be adsorbed on a hanging mercury electrode and reduced with peak potential of about -1.33v (vs.SCE) after 120s pre-concentration time. The derivative peak height is linearly proportional to the concentration for lysine in the range 6.0 x 10^?7-1.0 x 10^?5mol/ L. The detection limit is 4.0 x 10^?7mol/ L. Using this method, we have directly determined lysine in nutrition samples without any pre-separation step.     

Determination of Nitrite in Aqueous Solutions using the Linear Sweep Voltammetry Technique

ABSTRACT

An electrochemical method using linear sweep voltammetry techniques was developed to determine nitrite ion in aqueous solution in the presence of nitrate. Nitrite solutions exhibited a well-defined oxidation wave at +1.0V vs SCE at vitreous carbon, while no oxidation process was observed for nitrate solutions. The pH of the nitrite solutions varied from 2.37 to 5.60 and no change was observed in the Ep values, except for the pH 5.60 solution, where little change was verified. The potential also did not vary with change in the nitrite concentration in the 5.0 x 10^?5 to 7.0 x 10^?4 mol L^?1 range. Very good straight lines for plots of current versus nitrite concentration in the 7.0 x 10^?5 to 7.0 x 10^?4 mol L^?1 range were obtained; the correlation coefficient was never worse than 0.990. The nitrite determination was also performed in the presence of 1.0 x 10^?3 mol L^?1 of NO₃ ^? ions. The addition of NO₃ ^? did not change significantly the current values even when it was added in one hundred times molar excess.     

Flow-Injection Determination of Glucose by a Photoinduced Chemiluminescent Reaction

Abstract

A flow-injection procedure for the photochemical determination of glucose has been developed. The method is based on the photo-oxidation of glucose sensitized by 9,10-anthraquinone-2.6-disulfonate (disodium salt). The hydrogen peroxide formed in the photochemical reaction was measured by means of the chemiluminescent reaction with luminol and hematin. A linear calibration graph was obtained over the range 2.0x10^?6-8.5 x 10^?5 mol L^?1. The method was applied to determining glucose in blood serum, urine and fruit juices.     

Direct Determination of Labile Monomeric Aluminum in Natural Waters By A.C. Oscillopolarography in the Presence of Rubeanic Acid

ABSTRACT

A simple and sensitive electrochemical method for the direct determination of labile (monomeric inorganic Al speciation) Al concentration in natural waters is developed in this paper. It is based on the use of a.c. oscillopolarography in the presence of rubeanic acid (RA). The optimal experimental conditions are: 1 mol/L NaAc-HAc buffer (pH 5.4) and a RA concentration of 6x10^?4 mol/L. The response is linear over the 2x10^?7 to 2x10^?6 mol/L concentration range. The detection limit is 1x10^?7 mol/L and the relative standard deviation (at the 1.2 x 10^?6 mol/L level) is 5.5%. The method has been applied to the direct determination of labile monomeric Al concentrations in various natural samples. The results were verified by the classic ion exchange method.     

Liquid-Liquid Extraction,Photometric and Atomic Absorption Spectrophotometric Determination of Mercury

Abstract

A selective and sensitive spectrophotometric and atomic absorption spectrophotometric method is developed for the determination of traces of mercury with N-phenylcinnamohydroxamic acid (PCHA) in the environment. Mercury is extracted into a chloroform solution of PCHA at pH 8.5-10.0 and determined by AAS. The mercury hydroxamate binary complex is yellow in colour having a maximum absorbance at 390 nm and molar absorptivity 4.3 × 10³ 1 mol^?1 cm^?1, sandell sensitivity 0.0466 μg/cm². The ternary system using 1-(2-pyridylazo)-2-naphthol has molar absorptivity 8.82 × 10³ 1 mol^?1 cm^?1 at 550nm, sandell sensitivity 0.0228 μ/cm². Beer's law is obeyed in the concentration range of 2.37-38.0 ppm and 0.80-19.5 ppm of mercury for binary and ternary system, respectively. The extraction of Hg-PCHA binary system is studied with a liquid cation exchanger, bis-(2-ethyl hexyl) phosphoric acid (HDEHP) and found to have better selectivity than Hg-PCHA-PAN system. The molar absorptivity of the Hg-PCHA-HDEHP system is 8.82 × 10³ 1 mol^?1 cm^?1 at 390 nm and Beer's law is obeyed in the concentration range of 0.47-20 ppm of mercury.

The present method is applied to the determination of mercury in eye drops, aurvedic drugs and environmental samples.     

Kinetic-Fluorimetric Determination of Choline and Acetylcholine by Oxidation with Ce(IV)

Abstract

A kinetic fluorimetric method for the determination of choline and acetylcholine based on the oxidation of these analytes by Ce(IV) in a sulfuric acid medium yielding fluorescent Ce(III) is proposed. The calibration graph of each analyte is linear over the range 1.7x10^?5 ? 1×10^?3 M and the relative standard deviation is about 2% in both cases. The rate of appearance of Ce(III) fluorescence was found to be influenced by various processes in addition to the oxidation reaction and experiments were carried out in order to elucidate them.     

Cationic Surfactant Ion-Selective PVC Membrane Electrode Containing Macrocyclic Diimine Crown Ether

ABSTRACT

DP⁺ ion-selective PVC membrane electrode based on 2,3,11,12-dibenzo-5,9-diaza-4,9(10)-cis-diimino-1,13-dioxacyclopentadecane as a novel macrocyclic diimine crown ether is proposed. o-Nitrophenyl octyl ether as plasticizer and potassium tetrakis(4-chlorophenyl)borate as lipophilic salt were used. The electrode exhibits a Nernstian response for 1.0 x 10^?2-1.0 x 10^?6 mol 1^?1 DPCl with a slope of 58 mVdecade^?1. The detection limit is 2.5 x 10^?7 mol 1^?1. The electrode response was stable over a wide pH range (3-11). The lifetime of the electrode was about 2 months. The electrode shows a high selectivity towards inorganic cations. Among the organic cations tested, only hexadecyltrimethylammonium ion interferes. The electrode was suitable for determining the critical micelle concentration and as an end-point detector in the potentiometric titration of the cationic surfactants.     

Study of the Fluorescence Enhancement of Eu-Y-DEM-Dibenzoylmethane-Ammonia System

Abstract

The fluorescence enhancement and solvent effect of Eu-dibenzoylmethane-ammonia system was studied. The fluorescence intensity of the system can be greatly increased by y³⁺. The maximum fluorescence intensity was obtained at pH 8.9 – 9.5. The fluorescence intensity is a linear function of Eu²⁺ in the range of 1.0x10^?9 M -4.0x10^?8 M. The detection limit is 1.1x10^?10 M. The optimized procedure is applied to the determination of europium in lanthanide oxide samples.     

Flow Injection Chemiluminescence Determination of Etamsylate with Electrogenerated Hypochlorite

Abstract

A fast and simple electrogenerated unstable reagent chemiluminescence system for flow injection analysis of etamsylate is described, based on a decrease in the chemiluminescence intensity from the luminol-hypochlorite system. The response is linear to the concentration of etamsylate in the range from 1x10⁹ to 8x 10^?9. The detection limit is 6 x 10^?10 g ml^?1. The relative standard deviation is 3.1% at 2 x 10^?9 g ml^?1 (n=7). The proposed method is suitable for automatic and continuous analysis and has been successfully tested for determination of etamsylate in pharmaceutical formulations.

     

Application of Membrane-Selective Electrodes for the Determination of Pioglitazone Hydrochloride in the Presence of Its Acid Degradant or Metformin Hydrochloride in Tablets and Plasma

Abstract

Polyvinyl chloride (PVC) membrane sensors for the determination of pioglitazone hydrochloride (PIO) and metformin hydrochloride (MET) were described by using the ion association complexes between these drugs with either sodium tetraphenyl-borate (TPB) or ammonium reineckate (RNC) counter ions. The performance characteristics of the sensors were evaluated according to IUPAC recommendations, reveal a fast, stable and linear response over the concentration range 3.162 × 10^?5 ? 1 × 10^?2 M for PIO and 1 × 10^?3 ? 1 × 10^?1 M for MET. The sensors are used for determination of PIO and MET in tablets and plasma. The developed method was found to be simple, accurate and precise when compared with the reported method.     

Novel Mixed-Valence μ-Oxo-Bridged Trinuclear Manganese Complexes [Mn3O(O2CR)6L3] (R=4-Cl-C6H4OCH2, 3-Cl-C6H5, BrCH2, L=3-Methylpyridine or Water): Structures and Magnetic Properties

Preparation of three new mixed-valence oxo-centered trinuclear manganese complexes [Mn₃O(O₂CR)₆L₃] (R=4-Cl-C₆H₄OCH₂, 1, 3-Cl-C₆H₅, 2, BrCH₂, 3; L=3-methylpyridine or water), by reaction of N-n-Bu₄MnO₄ with appropriate reagents in ethanol and 3-methelpyridine is reported. The crystal structure of 1 has shown to have an oxo-centered Mn₃O unit with peripheral ligands provided by bridging carboxylate and terminal 3-methylpyridine groups, and with an approximate 3-fold symmetry axis for the whole cluster. Variable temperature magnetic susceptibilities of the complexes in the range 1.5-300 K have been measured and are interpreted in terms of the Kambe vector-coupling method and Van Vleck equation; J (cm^?1), J' (cm^?1), g, and R parameters obtained are -8.2, -10.9, 2.04, 2.15 x 10^?3 (1); -7.3, -11.1, 2.20, 3.32 x 10^?3 (2); -2.1, -4.1, 1.97, 2.34 x 10^?3 (3). There is weak antiferromagnetic exchange between manganese ions. Effects of bridging and terminal ligands on the J, J' values and spin ground state are discussed.     

Isonitroso-4-Methyl-2-Pentanone for Solvent Extraction and Spectrophotometric Determination of Palladium (II) at Trace Level

Abstract

Isonitroso-4-methyl-2-pentanone (HIMP) is proposed as a new reagent for extraction and photometric determination of Pd(II). The reagent forms a yellow complex with palladium in the pH range 4.0-5.0. The complex extracted into chloroform was measured at 330 nm. The molar absorptivity was found to be 5.37 × 10³ 1 mol^?1 cm^?1 and Sandell's sensitivity 20 ng cm^?2 Beer's law was obeyed over the concentration range 0.1-10.0 μg/ml of palladium. The method is applicable for palladium estimation in Ores and catalysts.     

Rapid and Sensitive Spectrophotometric Determination of Hafuium(IV) With 2-(5-Bromo-2-Pyridylazo)-5-Diethylaminophenol

Abstract

Hafnium(IV) reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in the pH range 3.3–11.0 to yield a sparingly soluble red-coloured chelate that can be dissolved with Triton X-100. Effect of initial pH of metal ion and order of addition of reagents was studied in detail. The 1:3 complex adheres to Beer's law over the concentration range 0.02–1.12 μg/ml of Hf(IV), has a molar absorptivity 1.33x10⁵ 1 mol^?1cm^?1, Sandell sensitivity 1.3 ng cm^?2, formation constant (log K) 11.94 and the method had a relative standard deviation of ± 1.5%. Effect of 60 diverse ions on the determination of hafnium(IV) was studied. This fairly selective method is the most sensitive so far reported for the spectrophotometric determination of hafnium(IV).     

Spectrophotometic Determination Of Tin In Steels With2-(5-Nltro-2-Pyridylazo)-5-[N-n-Propyl-N-(3-Sulfopropyl)Amino]phenol

ABSTRACT

A highly sensitive azo dye, 2-(5-nitro-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]phenol (Nitro-PAPS), is used as a colorimetric reagent for the determination of tin(IV) content. Nitro-PAPS reacts with tin(IV) to form a water-soluble complex in 1.0 M acetic acid. Full color development is attained within 5 minutes, and maintains constant absorbance for at least 24 hours. The apparent molar absorptivity is 7.7 x 10⁴ dm³ mol^?1 cm^?1 at a maximum wavelength of 580 ran. Beer's law is obeyed for tin(IV) in the range of 0-1.2 μg ml^?1. The proposed method is successfully applied to the determination of trace amounts of tin in steels.     

Internal Standard Quantitative Method Of Tetrodotoxin By Capillary Electrophoresis

ABSTRACT

An internal standard quantitative method of tetrodotoxin by capillary electrophoresis was developed, ephedrine hydrochloride being chosen as the internal standard of tetrodotoxin. The calibration curve was built with the correlation coefficient of 0.9997, and the linear range was from 0.01 mg.ml^?1 to 10.0 mg-ml^?1 with the detection limit of 1.0 x 10^?3 mg.m1^?1. RSD of the migration time of ephedrine hydrochloride and tetrodotoxin were all less than 1.0 %. The method was applied to determine tetrodotoxin in the poisonous frilled fish samples.     

Room Temperature Phosphorescence Optosensor for Terbium

Abstract

A solid surface room temperature phosphorescence optosensing method has been developed for the determination of terbium(III) based on the adsorption of its binary complex with 1,4-bis (l'-phenyl-3′-methyl-5′-pyrazolone-4′-) butanedione-(1,4) (BPMPBD) onto the hydrogen form of a strong cation exchange resin packed in a flow cell in an aqueous flow system. The phosphorescence intensity is a linear function of the concentration of terbium in the range of 8x10^?9 M-6x10^?7 M, and the detection limit is 3x10^?9 M terbium. The response mechanism was also studied. The present optosensor has been used for the determination of trace amounts of terbium in synthetic samples with satisfactory results.     

Analytical Study of New Creatininium and Tetramethyl-ammonium Cation Selective Membrane Electrodes

Abstract

Two new liquid membrane electrodes which respond to creatininium and tetramethylammonium cations are described. The creatininium cation electrode exhibits rapid and near Nernstian response to creatininium cation activity, at pH 3, in the 10^?3?10^?1 mol/L range. The useful concentration range extends to 10^?4 mol/L. The tetramethyl-ammonium cation electrode exhibits rapid and near Nernstian response to tetramethylammonium cation activity, at pH 2–11.5, in the 2x10^?5? 10^?1 mol/L range. Major interferences for the creatininium electrode are Na⁺, K⁺, NH⁺ ₄ and creatine. The pK_a of the creatininium cation was calculated. A method is described for the potentiometric precipitation titration of tetramethylammonium cation with sodium tetraphenylboron. Amounts of tetramethylammonium in the range 20–200 μol have been determined using Gran's plots, with an average error of about 0.6%.     

Study of Fluorescence System of Gmanylic Acid-Tb3+ and the Determination of Gmanylic Acid

Abstract

It was found that gmanylic acid (GMP) can be selectively completed with Tb³⁺ at pH 6.0-6.6, which then emits strong fluorescence characteristic of Tb³⁺. This reaction can be used for the determination of GMP in presence of adenylic acid (AMP), uridylic acid (UMP) and cylidylic acid (CMP). A linear relationship is obtained between the fluorescence intensity and GMP concentration in the range of 2.0×10^?7 - 1.0×10^?4M. The detection limit is 2.0×10^?8 M. The results showed that the composition ratio and apparent stability constant of GMP-Tb complex were 1:1 for GMP Tb³⁺- and 2.3×10^?5, respectively.     

Trace Analysis of Vanadium in Environment as its Ternary Complex with N-p Methoxyphenyl-2-Furylacrylohydroxamic Acid and 3-(o-Carboxyphenyl)-1-Phenyltriazine-N-Oxide

Abstract

A method is presented for the highly sensitive, selective, and rapid determination of vanadium (V) at sub-microgram levels in rocks, animal tissues, plant tissues and natural waters. The method is based on the selective extraction of vanadium (V) from strongly acidic (3-8 M hydrochloric acid) medium with solution of N-p-methoxyphenyl-2-furylacrylohydroxamic acid (MFHA) in chloroform. The reddish-violet extract (molar absorbance 8.6x10³ 1 mole^?1 cm^?1 at λ max 545 nm) is then equilibrated with 3-(o-carboxyphenyl)-1-phenyltriazine-N-oxide (CPPTNO) at pH = 1.5. The resulting ternary complex has enhanced colour (molar absorbance 1.4 × 10⁴ 1 mole^?1 cm^?1 at Λ max 450 nm). The ternary system obeys Beer's Law at 450 nm over the range 0-18 μ g/ml of vanadium. The extraction system achieves 20-fold enrichment of vanadium and enables the determination of the metal down to parts per billion (ng 1^?1) levels. The method tolerates the presence of a large number of anions and cations which are normally present with vanadium in rocks, plant tissues, animal tissues and natural waters. The applicability of the method was tested by the analysis of vanadium in these matrices. MFHA was selected from nine hydroxamic acids as it provided maximum sensitivity and selectivity.