Search results for "LIMIT"
showing 10 items of 2826 documents
Chlorinated acetic and propionic acids in pine needles from industrial areas
1998
Abstract Concentrations of chlorinated acetic and propionic acids in pine needles from the surroundings of a pulp and paper mill and a metal reclamation plant were measured. Different ways of extraction and chromatographic separation were tried. Ultrasonic extraction with water of the powdered needles was found to be efficient. The acids were analysed as their pentafluorobenzyl esters with GC-ECD. The ECD sensitivity of the pentafluorobenzyl derivatives was good. The detection limit was below 1 ng/g for the chlorinated acetic and propionic acids. The concentrations of dichloroacetic acid and 2,2-dichloropropionic acid in fresh needles were on the 0–4 ng/g level. Monochloroacetic acid, 2-chl…
Analysis of Polycyclic Aromatic Hydrocarbons and Their Oxygen-Containing Derivatives and Metabolites in Soils
2010
Although polycyclic aromatic hydrocarbons (PAHs) have been extensively studied, the knowledge of their oxygen-containing derivatives and metabolites (OPAHs) in soils is limited. We modified and tested an existing analytical protocol involving pressurized liquid extraction of soil followed by fractionation of target compounds into PAHs and OPAHs on a silica gel column and gas chromatography/ mass spectrometry-based separation and quantification. Polycyclic aromatic hydrocarbons and carbonyl-OPAHs were quantified directly after separation on silica gel columns, and hydroxyl/carboxyl-OPAHs were quantified after silylation with N,O-bis(trimethylsilyl)trifluoroacetamide. Recoveries between 78 an…
Determination of n-alkanes, PAHs and hopanes in atmospheric aerosol: evaluation and comparison of thermal desorption GC-MS and solvent extraction GC-…
2019
Organic aerosol (OA) constitutes a large fraction of fine particulate matter (PM) in the urban air. However, the chemical nature and sources of OA are not well constrained. Quantitative analysis of OA is essential for understanding the sources and atmospheric evolution of fine PM, which requires accurate quantification of some organic compounds (e.g., markers). In this study, two analytical approaches, i.e., thermal desorption (TD) gas chromatography-mass spectrometry (GC-MS) and solvent extract (SE) GC-MS were evaluated for the determination of n-alkanes, polycyclic aromatic hydrocarbons (PAHs), and hopanes in ambient aerosol. For the SE approach, the recovery obtained is 89.3–101.5&…
Derivatization of tertiary amphetamines with 9-fluorenylmethyl chloroformate for liquid chromatography: determination of N-methylephedrine.
2000
The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) was evaluated for the derivatization of tertiary amphetamines prior to liquid chromatographic analysis. Conditions for the derivatization were investigated, including the reaction time, the derivatization reagent concentration and the pH, using N-methylephedrine as a model compound. On the basis of these studies, a method for the quantification of N-methylephedrine is presented. The method involves derivatization with FMOC at ambient temperature and separation of the derivatives formed on a LiChrospher C18, 5 μm, 125 × 4 mm id column using acetonitrile–water gradient elution. The proposed procedure shows good linearity, accuracy…
Hard Cap Espresso Machine Extraction of Polyphenolic Compounds from Pulses
2018
A hard cap espresso machine was employed for the extraction of polyphenolic compounds from food samples as dry legumes and pulses. 100 mg of ground dry sample was mixed with a dispersing agent and placed in a refillable stainless steel capsule with a borosilicate filter. A complete polyphenol extraction was achieved by using 150 mL ethanol 50 % (v/v) in water and determined by Folin-Ciocalteu spectrophotometric method. The method provided a limit of detection of 0.4 mg g<sup>-1</sup>. The whole extraction procedure was achieved in less than one minute using the mild extraction conditions of 72°C and 19 bars given by the domestic machine. Fifteen varieties of food samples (3 lent…
Chemiluminometric determination of the pesticide 3-indolyl acetic acid by a flow injection analysis assembly
2005
Abstract A new method is proposed for the chemiluminescent determination of the pesticide 3-indolyl acetic acid by means of an flow injection analysis system. The chemiluminescence emission is obtained by oxidation of the analyte with Ce (IV) in nitric acid and presence of β-cyclodextrine. The continuous-flow method allows the determination of 159 samples h−1 of 3-indolyl acetic acid in an interval of concentrations over the range 0.5–15.0 mg l−1. The limit of detection was 0.1 μg l−1 and the R.S.D. (n, 17) at 2.0 mg l−1 of the pesticide level was 2.7%. The method was applied to water samples.
Determination of mercury in dry-fish samples by microwave digestion and flow injection analysis system cold vapor atomic absorption spectrometry
1997
Abstract Flow injection analysis system cold vapor atomic absorption spectrometry (FIAS-CV-AAS) preceded by a wet digestion in a microwave oven, as a method for measuring mercury in fish was studied. The digestion process and conditions of the FIAS (carrier concentration: HCl 3% v v ; reducing agent: SnCl2 2% w v : filling and injection times: 8 and 25 min, respectively; and sample volumes) were optimized. The analytical parameters of the proposed method (detection limit = 7.7 ng/g; precision intraassay = 6.7%; interassay = 14.0%) demonstrates its adequacy and are similar to the ones (detection limit = 19.4 ng/g; precision intraassay = 11.2%; interassay = 15.9%) obtained using a conventiona…
Flow injection Fourier transform infrared determination of caffeine in coffee
1999
Abstract A fully automatized procedure has been developed for the Fourier transform infrared (FT-IR) spectroscopic determination of caffeine in coffee samples. The method involves the on-line extraction of caffeine with CHCl3. Samples, weighed inside empty PTFE cartridges of 0.5 cm internal diameter (i.d.) and 1.5 ml volume, were humidified with four drops of 0.25 M NH3. The cartridge was installed in a flow manifold, in which samples were extracted in a closed-flow system with 1 ml CHCl3 during 6 min. Four hundred microliters of the extract were introduced in a microflow cell and absorbance measured as a function of time at 1659 cm−1, with a baseline established between 1900 and 830 cm−1, …
Flow injection determination of free and total cholesterol in animal greases using enzymes in non-aqueous media
1998
A non-covalently coimmobilized bienzymic reactor of horseradish peroxidase (HRP) and cholesterol oxidase (COD), operating in a continuous organic flowing stream of 1 × 10–3 M p-anisidine in buffer-saturated (pH 7.0) toluene, has been employed for cholesterol determination in animal greases, such as pig, beef, and chicken fat, and codfish liver oil. The method provides a good linear relationship up to 1.8 × 10–3 M cholesterol and average recoveries of 99.5%, a high sensitivity, with a detection limit of 1 × 10–6 M of cholesterol and a good precision (an interday RSD of 1.8% for the determination of total cholesterol in a codfish oil sample). The method permits the direct spectrophotometric d…
Flow injection-spectrophotometric determination of cresol compounds in water by reaction withp-aminophenol
1993
A spectrophotometric method has been developed for the simultaneous determination ofo-cresol andm-cresol in water by reaction withp-aminophenol (PAP). Three different methodologies have been assayed; (i) batch analysis, after reaction in an alkaline medium in the presence of dissolved molecular oxygen as oxidizing agent, (ii) a stopped-flow procedure, carried out in the presence of KIO4 and (iii) a flow injection method based on the same approach. The batch procedure requires 22 min for the full development of colour witho-cresol and 12 min form-cresol. In the stopped-flow mode, using KIO4 and a reaction time of 12 min, better sensitivity can be obtained for both compounds and limits of det…