Search results for "Spectroscopy"
showing 10 items of 10293 documents
Microwave-assisted vapour-generation Fourier transform infrared spectrometric determination of carbonate in waters
1998
Abstract A microwave-assisted vapour-generation Fourier transform infrared spectrometric procedure is proposed for the determination of total carbonate in waters. The method is based on the simultaneous injection of 100 μl of sample and 300 μl of 0.1 M nitric acid in a two-channel manifold with a merging zone; a coil located inside a microwave oven encourages the removal of CO 2 . The carbon dioxide is separated from the distilled water employed as carrier by means of gas–liquid separator and is introduced by a nitrogen carrier flow inside a long-path infrared absorption gas cell, from which the corresponding flow analysis recording is registered as a function of time in the wavenumber rang…
Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion.
2010
Abstract A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g−1 concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO3 and H2O2 followed by dilution with water containing KBr/KBrO3 and hydroxylamine and reduction with SnCl2 in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g−1 with a recovery percentage of 95 ± 4% at an added concentration of 5 ng g−1. The concentration level …
GFAAS determination of selenium in infant formulas using a microwave digestion method.
1994
A method for determining the selenium content of infant formulas is proposed. It includes wet digestion with nitric acid and hydrogen peroxide in medium pressure teflon bombs in a microwave oven and determination by graphite furnace atomic absorption spectrometry (GFAAS). The absence of interferences is checked. Values obtained for the limit of detection (19.4 ng/g), precision (RSD = 2.2%) and accuracy by analysis of a reference material show that the method is reliable.
Determination of total mercury in nuts at ultratrace level
2014
Abstract Total mercury, at μg kg−1 level, was determined in different types of nuts (cashew nut, Brazil nuts, almond, pistachio, peanut, walnut) using a direct mercury analyser after previous sample defatting and by cold vapour atomic fluorescence spectrometry. There is not enough sensitivity in the second approach to determine Hg in previously digested samples due to the strong matrix effect. Mercury levels in 25 edible nut samples from Brazil and Spain were found in the range from 0.6 to 2.7 μg kg−1 by using the pyrolysis of sample after the extraction of the nut fat. The accuracy of the proposed method was confirmed by analysing certified reference materials of Coal Fly Ash-NIST SRM 1633…
Determination of phytic acid and its degradation products by ion-pair chromatography (IPC) coupled to inductively coupled plasma-sector field-mass sp…
2004
We developed a method for the determination of phytic acid (IP6) and its degradation products (IP1-IP5) by ion-pair chromatography coupled to a double focussing inductively coupled plasma-sector field-mass spectrometer (ICP-SF-MS). For the detection of the phosphorus species a mass resolution (m/Δm) of 4000 was needed in order to separate the 31P+ signal from the interfering clusterions. The separation of the six phosphorus species was enabled by a gradient elution using tetrabutylammonium hydroxide (TBA) as ion-pair reagent. Calibration data were reported and a detection limit of 230 ng g−1 for IP6 could be obtained. The method was firstly proved for a hydrolyzate of commercially available…
Green, rapid and simultaneous determination of ‘alternative preservatives’ in cosmetic formulations by gas chromatography-mass spectrometry
2022
Abstract Some hydroxylated compounds commonly used in cosmetic formulations including short chain glycols, benzylic alcohols, and organic acids show antimicrobial activity, although they are not considered as preservatives according to the existing European legislation. These ‘alternative preservatives’ are not exempt of potential side-effects for cosmetics users. The aim of this work is to develop a simple and affordable analytical method useful for the simultaneous and green determination of fourteen compounds used as ‘alternative preservatives’ in cosmetic samples with different matrices. The proposed method allows a rapid sample preparation by simple dissolution or dispersion of the sam…
FTIR determination of Aspartame and Acesulfame-K in tabletop sweeteners.
2004
Two different strategies for sweeteners determination in tabletop samples by Fourier transform middle-infrared (FTIR) spectrometry, an off-line and a fully mechanized extraction of Aspartame and Acesulfame-K with different mixtures of chloroform and methanol, have been developed. The off-line method involves the extraction of both active principles by sonication of samples with 25:75 v/v CHCl3/CH3OH and direct measurement of the peak height values at 1751 cm(-1), corrected using a baseline defined at 1850 cm(-1) for Aspartame, and measurement of the peak height at 1170 cm(-1) in the first-order derivative spectra, corrected by using a horizontal baseline established at 1850 cm(-1), for Aces…
Quality control of pharmaceuticals containing clenbuterol by thermal lens spectrometry.
1996
An ultrasensitive absorptiometric procedure for the determination of clenbuterol in pharmaceutical preparations was developed. Clenbuterol was diazotized with nitrite and coupled with 1-(naphthyl)ethylenediamine, and the absorbance of the azo dye formed was measured by both spectrophotometry and ultrasensitive thermal lens spectrometry (TLS). The TLS limit of detection was 1.5 ppb, 14-fold lower than with a Hewlett-Packard diode array spectrophotometer. Thus, the TLS procedure can be advantageously applied to quality control of clenbuterol at the individual dose level and in small samples. Repeatability as relative standard deviation was 1.5% (50 ppb, n = 6).
Oxidation of adrenaline and noradrenaline by solved molecular oxygen in a FIA assembly.
2002
A simple and effective procedure is proposed for the study and simultaneous determination of adrenaline and noradrenaline. The fluorimetric determination of both substances is performed in a flow injection assembly and by oxidation of both drugs with the solved molecular oxygen. The influence of different parameters is empirically studied and the interpretation of the reaction mechanism is also added. The determination of adrenaline is monitored at 450 nm and the outputs at 520 nm correspond to the adrenaline and noradrenaline global amount; for both lectures lambda(exc) 329 nm. The influence of temperature is relevant and analytical determination occurred at 55 degrees C by immersing the s…
Sensitive determination of methylenedioxylated amphetamines by liquid chromatography.
2001
Different strategies for the liquid chromatographic determination of methylenedioxylated amphetamines were evaluated: separation and detection of underivatized analytes by (i) UV or (ii) fluorescence, (iii) derivatization with 3,5-dinitrobenzoyl chloride followed by separation and UV detection of the derivatives formed and (iv) derivatization with 9-fluorenylmethyl chloroformate (FMOC) and subsequent separation and fluorimetric detection of the derivatives. The compounds tested were 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDE). On the basis of these studies, a new procedure for the chromatographic determination of…