Search results for "Sample"
showing 10 items of 2270 documents
Simultaneous determination of As, Cd, Cr and Pb in aqua regia digests of soils and sediments using electrothermal atomic absorption spectrometry and …
2002
A method was developed for the simultaneous multi-element determination of As, Cd, Cr and Pb in aqua regia digests of soils and sediments using an electrothermal atomic absorption spectrometer with a transversely heated graphite atomizer and longitudinal Zeeman-effect background correction. A fast furnace program with no pyrolysis stage or chemical modifier was used, and the total duration of the time-temperature program of the graphite furnace was 45 s. The method detection limits calculated from blank samples were 9.5 μg l−1, 0.18 μg l−1, 6.2 μg l−1 and 2.5 μg l−1 for As, Cd, Cr and Pb, respectively. Sample preparation procedures are briefly described. The accuracy of the method was confi…
Determination of ruthenium in photographic emulsions - Development and comparison of different sample treatments and mass spectrometric methods
1999
Different sample treatment procedures were combined with inductively coupled plasma mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (NTI-MS) for the determination of ruthenium traces in photographic emulsions. Dissolution of the samples in concentrated ammonia solution was used in connection with ICP-MS by external calibration, which has the advantage of a simple sample preparation technique but introduces high amounts of the silver matrix into the mass spectrometer. On the other hand, isotope dilution mass spectrometry (IDMS) with an enriched 99Ru spike solution was applied for ICP-MS and NTI-MS measurements, respectively, in connection with a significant reduc…
On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.
2007
Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of…
On-line in-tube solid phase microextraction-capillary liquid chromatography method for monitoring degradation products of di-(2-ethylhexyl) phthalate…
2014
Abstract The main di-(2-ethylhexyl) phthalate (DEHP) degradation products, (2-ethylhexyl) phthalate (MEHP), diethyl phthalate (DEP) and dibutyl phthalate (DBP), have been tested. The proposed cost-effective method combines on-line, in-tube solid-phase micro extraction (IT-SPME) in in-valve configuration and capillary liquid chromatography with UV diode array detection (Cap-LC-DAD). Acidification of the samples at pH 3 improved markedly the estimation of MEHP. Aliquots of 4 mL of acidified water samples were directly processed. After sample loading, the analytes were desorbed with the mobile-phase and transferred to the monolithic capillary column. Satisfactory linearity and precision, absen…
Simple and commercial readily-available approach for the direct use of ionic liquid-based single-drop microextraction prior to gas chromatography
2009
A simple and commercial readily-available approach that enables the direct use of ionic liquid (IL)-based single-drop microextraction (SDME) prior to gas chromatography (GC) is presented. The approach is based on thermal desorption (TD) of the analytes from the IL droplet to the GC system, by using a robust and commercially-available thermodesorption system. For this purpose, a two-glass-tube concentrically disposed system was designed. The inner tube is a laboratory-cut Pyrex tube (20mm length) that houses the ionic liquid droplet from the SDME process, and the outer tube is a commercially-available TD glass tube (187 mm length) commonly employed for stir-bar sorptive extractions (SBSE). I…
Near infrared determination of Diuron in pesticide formulations
2005
Abstract A simple, fast and environmentally friendly near infrared (NIR)-based methodology was developed for Diuron determination in pesticide formulations. This methodology was based on the pesticide extraction with acetonitrile and subsequent transmittance measurement determination by peak area measurement between 2021 and 2047 nm, corrected with a single point baseline established at 2071 nm. The repeatability, as relative standard deviation of five independent analysis of a 15.3 mg g −1 Diuron standard was 0.03% and the limit of detection 0.013 mg g −1 . The reagent consumption was clearly reduced in front of a chromatographic reference procedure from 39.1 ml acetonitrile per sample, re…
Supercritical fluid extraction and high performance liquid chromatography determination of homosalate in lipsticks
2001
Supercritical fluid extraction of homosalate is reported for the first time. Extraction parameters such as pressure, time of extraction, use of modifier, temperature and sample mass were studied. The proposed method was assayed for the extraction of homosalate in sunscreen lipsticks. Efficient recoveries were obtained after 5 min of dynamic extraction with supercritical CO2 and 15% ethanol as modifier at 300 bar and 60°C, flow rate 4 mL min−1. Extracts were dissolved in ethanol, and homosalate determined by HPLC using water—acetic acid—ethanol mobile phase and flow rate of 1 mL min−1. UV detection was at 309 nm using homosalate in ethanol solutions as standards, limit of detection 4 μg mL−1…
Analysis of organic pollutants in water at trace levels using fully automated solid-phase extraction coupled to high-performance liquid chromatography
1997
A method has been developed for the determination of trace levels of 32 pesticides, 19 explosives and 16 polycyclic aromatic hydrocarbons (PAH) in water in three individual steps. Solid-phase enrichment (SPE) is coupled to high-performance liquid chromatography (HPLC) with a fully automated system. The organic pollutants are enriched on reusable cartridges packed with adsorbent materials: pesticides and explosives on a mixed bed of divinylbenzene-ethylvinylbenzene copolymers (LiChrolut EN®) and perfluorinated polyethylene (PolyF®), and polycyclic aromatic hydrocarbons on C18-modified silica (Zorbax® ODS1). Thermally assisted desorption (TAD) has been shown to increase the recovery of analyt…
Solid-Phase Microextraction Liquid Chromatography/Tandem Mass Spectrometry To Determine Postharvest Fungicides in Fruits
2003
A method to determine five postharvest fungicides (dichloran, flutriafol, o-phenylphenol, prochloraz, tolclofos methyl) in fruits (cherries, lemons, oranges, peaches) has been developed using solid-phase microextraction (SPME) coupled to liquid chromatography (LC) with photodiode array (DAD), mass spectrometry (MS), or tandem mass spectrometry (MS/MS) with ion trap detection. Extraction involved sample homogenization with an acetone/water solution (5:1), filtration, and acetone evaporation prior to fiber extraction. The pesticides were isolated with a fused-silica fiber coated with 50-microm Carbowax/template resin. The effects of pH, ion strength, sample volume, and extraction time were in…
Off-line solid-phase microextraction and capillary electrophoresis mass spectrometry to determine acidic pesticides in fruits.
2003
A method based on solid-phase microextraction (SPME) and capillary electrophoresis/mass spectrometry (CE/ MS) is described for determining simultaneously five acidic pesticides (o-phenylphenol, ioxynil, haloxyfop, acifluorfen, picloram) in fruits. The CE device is coupled to an electrospray interface by a commercial sheath-flow adapter. Emphasis is placed on fulfillment of the speed and sensitivity requirements. The best separation is achieved using 32 mM ammonium formate/acid formic buffer at pH 3.1, with a working voltage of 25 kV. The MS detection of the five pesticides was performed in negative ionization mode. Full-scan spectra with base peaks corresponding to [M-H]- were obtained exce…