Search results for "Analytical"

Validation of Methylmercury Determinations in Aquatic Systems by Alkyl Derivatization Methods for GC Analysis Using ICP-IDMS

2001

Isotope dilution mass spectrometry (IDMS), using an inductively coupled plasma quadrupole mass spectrometer (ICPMS) and a species-specific methylmercury spike was applied to validate the commonly used GC method for methylmercury (MeHg+) determination, which is based on the formation of volatile methylethylmercury by derivatization with NaBEt4. The spike compound, Me201Hg+, was synthesized by reaction of 201Hg-enriched mercury chloride with methylcobalamin. By analyzing different environmental aquatic samples, it was found that in most cases, transformation of MeHg+ into elemental mercury (Hg0) took place. From investigations of synthetic solutions, it could be followed that halide ions are …

Answer to the Letter to the Editor by Dr. Sanjay Pralhad Shirsat concerning the article “Separation of isobutyl alcohol and isobutyl acetate by extra…

2015

Quartz-capillary gas chromatography of chlorinated phenols and catechols

1983

The gas chromatography of all chlorinated phenols and catechols on a non-polar SE-30 quartz-capillary column has been studied. The relative retention times of the individual components are given and the elution order is discussed. All of the chlorophenols and chlorocatechols can be separated under appropriate operating conditions but simultaneous determination of all the compounds studied resulted in overlapping peaks. Theortho-effect in catechols is stronger than that in phenols. A different order of elution for the compounds studied to that of the corresponding acetate esters is found. Generally, longer retention times for the latter are observed.

FIA-Fluorimetric assembly for the determination of noradrenaline hydrochloride by a solid-phase reactor with immobilized hexacyanoferrate(III)

1997

An FIA assembly provided with immobilized hexacyanoferrate(III) is proposed for the fluorimetric determination of noradrenaline hydrochloride. The oxidative reagent is immobilized by means of a strong anion-exchange resin. The FIA manifold is very simple and the calibration graph is linear over the range 0.5–75mgl−1 noradrenaline hydrochloride with an r.s.d of 0.88% (17 replicates) and a sample throughput of 84h−1. Foreign compounds such as NaCl, sucrose, lactose and sodium sulfate caused no significant errors. The procedure is applied to the determination of noradrenaline in a medicinal formulation.

Determination of aminoglycoside and macrolide antibiotics in meat by pressurized liquid extraction and LC-ESI-MS

2010

A simple method for the simultaneous determination of dihydrostreptomycin, spectinomycin, spiramycin, streptomycin, tilmicosin, and tylosin in meat has been developed using pressurized liquid extraction and LC-triple quadrupole MS (LC-ESI-MS/MS). The pressurized liquid extraction operational parameters were optimized and no protein precipitating and fat removing steps were required. A gradient HPLC separation was developed with ion-pair mobile phases consisting of aqueous 1 mM heptafluorobutyric acid water and methanol. Protonated molecules were used as precursor ions for CID. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of three fragment ion transition…

Comparative assessment of solid-phase extraction clean-up procedures, GC columns and perfluoroacylation reagents for determination of type B trichoth…

2005

Abstract Various solid-phase extraction (SPE) procedures for clean-up, two perfluoroacylation reagents (pentafluoropropionic anhydride (PFPA) and heptafluorobutyric anhydride (HFBA)) and two chromatographic columns (HP-1701 and HP-5) have been assessed comparatively to achieve the determination of type B trichothecenes (deoxynivalenol (DON), nivalenol (NIV), 3- and 15-acetyldeoxynivalenol (3- and 15-ADON)) in wheat grain by gas chromatography (GC)–electron-capture detection (ECD). Spiked wheat samples were extracted with acetonitrile–water (84:16, v/v). Tested SPE procedures were MycoSep 225 column, Florisil and different cartridges prepared in the laboratory with mixtures of various sorben…

Contributions to the application of the transferability principle and the multipolar modeling of H atoms: electron-density study of L-histidinium dih…

2006

The electron density of L-histidinium dihydrogen orthophosphate orthophosphoric acid has been determined from X-ray and neutron diffraction data at low temperature (120 K). Topological analysis of the electron density has been used to analyse the effect of the multipolar refinement strategy on the electron-density model in the hydrogen-bonding regions. The electron density at low temperature has also been used to acquire high-quality experimental thermal parameters at room temperature using the transferability principle. Molecular vibrations, TLS and normal mode analysis are discussed and studied at both temperatures.

The use of topological models in analytical chemistry

2005

In the present paper, the possible analytical applications of two toplogical models, the DARC model and the group contribution model, are discussed. Both models are applied to obtain calibration laws, which relate UV and IR characteristics with the chemical structure of ethylene oxide condensates. The group contribution model is also applied to determine the contribution of each part of the different compounds involved in a chemical interaction process, having established the sensitization parameters of benzodiazepines and anionic surfactants from the micellar enhancement fluorescence.

Fluorimetric determination of binding constants between micelles and chemical systems

1991

Abstract A fluorimetric method is adapted to determine the binding constants (K) between different systems and micelles. The method is based on the variation of the fluorescence of the system in the presence of increasing amounts of a surfactant agent. This method permits the determination of binding constants in strong acid or alkaline media. The binding constants of 1-naphthol and 2-(4-alkylamino-2 hydroxyphenyl)benzo-X azoles (X being an O or an S atom, PAS-O and PAS-S) with cationic, anionic, and nonionic surfactants have been determined by the proposed method. Values from 49,100 M−1 for the interaction between PAS-S and CTAB in basic medium to 10 M−1 for the interaction of 1-naphthol w…

Spectroscopic and chromatographic study of the interaction of nonionic micelles with the aluminum-morin complex

1989

Abstract The interaction of the aluminum-morin system with different nonionic surfactants has been studied spectrophotometrically and by high-performance liquid chromatography. It has been found that ethylene oxide-propylene oxide condensate surfactants sensitize the spectrophotometric determination of aluminum with morin more than ethylene oxide condensate surfactants. Binding ratio parameters for the different surfactants with free morin have been also estimated from the analysis of chromatographic vacant peaks.