Search results for "Spectroscopy"
showing 10 items of 10293 documents
Methylmercury and inorganic mercury determination in fish by cold vapour generation atomic absorption spectrometry
2000
Abstract Given that organic mercury is more dangerous than the inorganic form and that it is converted into methylmercury by biological methylation, we have studied and optimized a simple method for measuring both organic and inorganic mercury contents in fish, using a spectroscopic vapour generation technique, with a sequential reduction of the digested sample with stannous chloride and sodium tetrahydroborate. Prior to applying the method the sample was subjected to alkaline wet digestion. Due to the matrix interferences calibration curves with matrix addition were needed for mercury determinations. The analytical parameters of the method were: linearity from 10 to 200 ng of Hg in the red…
Chromatographic Separation of Cresol Isomers by a β‐Cyclodextrin: Application for the Determination of Volatile Phenols in Alcoholic Beverages
2006
Abstract The chromatographic separation of o‐cresol, m‐cresol, and p‐cresol by using β‐cyclodextrin as a chiral reagent has been studied. Conditions for the chromatographic separation of these isomers by using the cyclodextrin in the mobile phase or bonded in the stationary phase were optimized, and both procedures provided good results for the resolution of the chromatographic peaks. The use of fluorimetric detection (λexc 275 nm λem 300 nm) allows detection and quantification limits of the µg/L for eight studied phenols by using both procedures. The determination of volatile phenols in alcoholic beverages must be carried out using the cyclodextrin in the mobile phase because of the co‐elu…
Flow-injection spectrophotometric determination of arylamines and sulphonamides by diazotization and coupling in a micellar medium
1991
Abstract In a sodium dodecyl sulphate (SDS) micellar solution, the rate of coupling of a diazonium ion with N-(1- naphthyl)ethylenediamine (NED) increases greatly, the protonation of the resulting azo dyes takes place at higher pH values and the dyes are more soluble. These favourable features were applied to the development of a simple flow-injection spectrophotometric procedure for the determination of diazotizable substances of pharmaceutical interest. Limits of detection in the range 0.2–0.5 μg ml−1 (signal-to-noise ratio=3), with relative standard deviation of 0.7–3% (n=3) for 5 μg ml−1 standards, were obtained.
Determination of sulfide in waters by flow-injection solid phase spectrophotometry
2000
A highly sensitive flow injection solid-phase spectrophotometric method was developed for the determination of sulfide in waters. The method is based on the formation of Methylene Blue (MB) by reaction between sulfide and N,N-dimethyl-p-phenylenediamine chloride in presence of Fe(III) in acidic medium. The MB formed was adsorbed on C18 bonded silica, located inside a laboratory-made flow cell, which was placed in the optical path of the spectrophotometer. Analyte retention and detection at 666 nm were performed simultaneously, followed by elution with a mixture of methanol and hydrochloric acid. Several variables of the system, such as amine concentration, acidity of the reaction medium, re…
Arsenic content of Spanish cows' milk determined by dry ashing hydride generation atomic absorption spectrometry.
1994
SummaryThe arsenic content of cows' milk consumed in Spain was determined. A procedure using dry ashing hydride generation atomic absorption spectrometry was developed for the purpose. Experimental conditions for the destruction of organic matter were established and an interference study was carried out. The method developed has a detection limit of 0·1 ng/g, a relative SD of 5%, and a recovery (mean ± CSI) of 100 ± 4%. The accuracy of the method was checked by analysis of a certified sample of IAEA milk powder (mean ± CSI: certified, 4·85 ± 0·32 ng/g; found, 5·04 ± 0·81 ng/g). The proposed procedure was used to analyse cows' milk samples. The extremely low arsenic levels found do not pres…
Selective flow-injection biamperometric determination of sulfur-containing amino acids and structurally related compounds
2001
Abstract A simple and selective flow-injection method for the determination of cysteine and methionine is proposed. The method is based on the reaction of the amino acid with chloramine-T and the subsequent reaction of the excess of chloramine-T with an acidic solution of iodide producing a stoichiometric amount of tri-iodide (diminution of the flow-injection analysis (FIA) peak) which is determined biamperometrically using two platinum electrodes polarized at 100 mV. The calibration graph is linear up to 10 μg ml−1 of cysteine and 30 μg ml−1 of methionine; the limit of detection is 0.06 and 0.1 μg ml−1; the repeatability (also as percent of a series of 70 continuous FIA peaks of 5 μg ml−1 …
Flow injection biamperometric determination of chloramine-T in environmental, pharmaceutical and veterinary samples
2000
Abstract A flow injection assembly for the determination of chloramine-T is proposed. The sample (213 μl) is inserted into the carrier, de-ionized water flowing at 4.1 ml min−1. This carrier merges with a mixture of potassium iodide and sulphuric acid, and the resulting solution flows to the flow cell through a reactor 66 cm long. The chloramine-T oxidises the iodide to tri-iodide. The resulting iodide/iodine ratio is biamperometrically tested. The calibration graph is linear up to 65 μg ml−1 chloramine-T; the limit of detection is 0.5 μg ml−1; the relative standard deviation (r.s.d) of the calibration slope is 2.8% for a series of eight independent calibrations. The r.s.d. of a series of 7…
Determination of sertraline in rat plasma by HPLC and fluorescence detection and its application toin vivopharmacokinetic studies
2012
A simple, rapid, and sensitive HPLC method based on 9H-fluoren-9-ylmethyl chloroformate derivatization for the quantification of sertraline in rat plasma has been developed, requiring a plasma sample of only 0.1 mL, which was deproteinized and derivatized for 5 min in two single steps. The obtained derivative was stable at room temperature and was determined by HPLC using a fluorescence detector. The analytical column was a C(18) column and the mobile phase was acetonitrile and water (80:20, v/v). Calibration curves were linear in the range of 10-500 ng/mL. The limit of detection was approximately 3 ng/mL, and the lower limit of quantification was established at 10 ng/mL. The bias of the me…
A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos.
2005
Abstract A FTIR methodology has been developed for the simultaneous determination of Cypermethrin and Chlorpyrifos in pesticide commercially available formulations. The method involves the extraction of both active principles with CHCl3 and direct measurement of the peak area values between 1747 and 1737 cm−1 corrected with a baseline defined at 2000 cm−1 for Cypermethrin and peak height values established at 1549 cm−1 corrected using a baseline situated at 1650 cm−1 for Chlorpyrifos. The limits of detection achieved were of the order of 0.7 and 0.4% (w/w), and the relative standard deviation 0.4 and 0.2% for Cypermethrin and Chlorpyrifos, respectively. The developed procedure provided stat…
Direct determination of ethanol and methanol in liquid samples by means of vapor phase-Fourier transform infrared spectroscopy
1997
Abstract A FTIR procedure is proposed for the direct determination of methanol and ethanol in liquid samples, such as alcoholic beverages and eau-de-cologne, based on vapor generation from small injected volumes of untreated samples into a heated Pyrex glass reactor in which, at a temperature of 80°C, ethanol and methanol are volatilized and introduced into a long-path IR gas cell by means of a N2 carrier flow. The IR spectra obtained present two characteristic ethanol bands (1050 and 880 cm−1) and a single characteristic methanol band (1030 cm−1). The measurement of the area of the transient recording obtained for the wavenumber range between 1025–950 and 950–820 cm−1 allows us the determi…