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Four simple and sensitive methods for the assay of prazosin hydrochloride (PRH) are developed. These methods are based on the formation of coloured species by treating it either with excess N-bromosuccinimide (NBS) and determining the unconsumed NBS with p-N-methyl aminophenol sulphate (metol)-sulphanilamide (SA) reagent (method A, λ max 520 nm); with 3-methyl-2-benzothiazolinone...
A study of the transport of Hg(II) ions through a tri-n-octylamine (TOA) - sorbital monooleate (Span 80) - toluene liquid membrane has been performed with varying concentrations of HCl, KCl, TOA, Span 80 and NaOH in the feed, membrane and stripping solutions. Maximum transport was observed with 0.01 M KCl, 2.5 10 -2 M HCl, 1.5 10 -2 M TOA, 3% (w/v) Span 80 and 0.05...
A flow-injection analysis (FIA) method for the ultraviolet spectrophotometric determination of copper in copper ores is described. The ore samples are dissolved in concentrated perchloric acid, the excess acid is neutralized with ammonia solution, and the resulting solution is used for the determination of copper. The UV-FIA system is based on the reaction of copper (II) ions with pyrophosphate and...
A flowthrough spectrophotometric sensor for the determination of cobalt at the nanogram per millilitre level using pyridoxal 4-phenylthiosemicarbazone as reagent and integrated preconcentration and detection in the flow cell is proposed. The method is highly selective for cobalt(II); it features detection and determination limits of 0.02 and 0.06 μg ml -1 respectively, and a linear range...
This paper reports a method for determining the stability constants of complexes in a system of coexisting mononuclear and polynuclear complexes based on analysis of dual isosbestic points. First it is necessary to determine the dissociation degrees of either of the two complexes concerned in two directions, and then their stability constants. With this method, the conditional constant can be evaluated...
A solid-state nitrate ion-selective electrode based on an Urushi matrix membrane was developed. Urushi, a natural oriental lacquer, has excellent mechanical strength and binding affinity for metal electrodes. Using the same technique for a dip-coating ion-selective electrode, an electrode was prepared by coating and hardening a sensing membrane on the metal base. The effects of the metal electrode...
The synthesis and spectral characterization of several tetra-substituted aluminum 2, 3-naphthalocyanine dyes for the determination of metal ions is reported. The synthesis is done by means of a homogeneous phase reaction, replacing the previously used heterogeneous method. The new scheme allows for improved product yields, higher purity, better product reproducibility and can be monitored at different...
The permselectivity of neurotransmitters such as dopamine, epinephrine, and norepinephrine at overoxidized polypyrrole (OPPY)-film-coated glassy carbon electrodes has been investigated. The chemically-modified electrodes exhibit attractive permselectivity and antifouling properties of rejecting anionic species, e.g. ascorbate, etc. Compared with the response of neurotransmitters at modified electrodes...
Four simple and sensitive visible spectrophotometric methods (A-D) have been described for the assay of doxorubicin hydrochloride either in pure form or in pharmaceutical formulations. Method A was developed based on oxidation of the drug with Fe(III) to produce Fe(II), which subsequently reacts with 1,10-ortho-phenanthroline to form a red colored complex (λ max : 510 nm) at pH...
A rapid and reliable procedure for the determination of gold in geological samples is reported that involves MnO 2 and HCl treatment of the samples followed by ethyl acetate extraction of gold and determination at the ppm and sub-ppm levels by flame atomic absorption spectrometry after evaporating off the organic solvent. The method was tested for the quantitative recovery of gold from the...
A novel method for the rapid dissolution of fused silicates in mineral acid is described. Fusion with 2.5 g of a KBO 2 -K 2 CO 3 (3:2, w/w) mixture in a platinum crucible at 1000°C will decompose 0.1 g of silicate samples such as basalt rock, glass sand and powdered glass in 10 min, and the cooled fusion cakes can be completely dissolved by 20 ml of 3 N mineral acids such...
A solvent extraction technique involving no critical clean-up steps was developed for the determination of methylmercury (MeHg) in environmental and biological samples by aqueous phase ethylation, room temperature precollection, gas chromatographic separation and cold vapor atomic fluorescence spectrometric detection. Samples were first digested with KOH-methanol, then acidified prior to extraction...
Trace metals in water were preconcentrated with silica gel modified with salicylaldoxime and determined by AAS. Optimum conditions for the maximum recovery of metal ions, viz. Cu(II), Ni(II), Co(II), Zn(II) and Fe(III), for both batch and column methods were developed. The efficiency of the adsorbent with respect to different experimental conditions was established.
Phosphate and carbonate buffers serve as excellent pH buffers at circumneutral values of pH, except for systems requiring significant concentrations of heavy metals, which are severely restricted by the low solubilities of heavy metal phosphates and carbonates. 3-(N-morpholino)propanesulfonic acid (MOPS; pK a 7.2) is a suitable replacement buffer at circumneutral values of pH. However, only...
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 1 ...
A method is described for the voltammetric determination of titanium(IV) using a carbon paste electrode modified in situ with cetyltrimethylammonium bromide. The cationic micellar surfactant adsorbs onto the electrode particularly at negative potentials, simultaneously preconcentrating titanium(IV) as the oxalate complex with reduction to titanium(III). Anodic stripping voltammetry exploiting reoxidation...
Some new chelating ion-exchange resins containing a hydroxamic acid moiety attached to a divinylbenzene styrene (DVBS) copolymer, i.e. glycine hydroximate in DVBS (GH-DVBS), anthranilic acid hydroximate in DVBS (AAH-DVBS), malonic acid dihydroximate in DVBS (MAH-DVBS) and iminodiacetic acid dihydroximate in DVBS (IDAAH-DVBS), have been synthesized and their various physicochemical characteristics...
The Briggs-Rauscher reaction is known as a nonlinear and non-equilibrium chemical oscillation reaction. The reaction solution is composed of malonic acid as organic substrate, hydrogen peroxide and iodate in sulphuric acid as oxidizing agent, and manganese (II) as metal catalyst. The calorimetric behaviour, in terms of the total heat Q and the heat evolving rate q for each chemical oscillation, was...
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