Search results for "LIMIT"
showing 10 items of 2826 documents
Direct determination of lead in human milk by electrothermal atomic absorption spectrometry
1999
Abstract Infants are particularly sensitive to the toxic effects of lead. Since milk is their only or main food it is important to know the contribution of milk to lead intake. The purpose of this study was to develop a direct method for determining the lead content of human milk by electrothermal atomic absorption spectrometry when a deuterium lamp is the only background correction available. The optimum conditions for lead determination in breast milk: sample dilution in Triton ×-100, modifier (75 μg of palladium) and nitric acid contents (2%) and the graphite furnace program (mineralization: 1100°C; atomization: 2300°C) were selected. The analytical parameters are: linearity (20–300 ng m…
Quality control of Metamitron in agrochemicals using Fourier transform infrared spectroscopy in the middle and near range
2006
Abstract Two vibrational spectrometry-based methodologies were developed for Metamitron determination in pesticide formulations. Fourier transform-middle infrared (FT-MIR) procedure was based on the extraction of Metamitron by CHCl 3 and latter determination by peak area measurement between 1556 and 1533 cm −1 , corrected with a two points baseline established from 1572 to 1514 cm −1 . Fourier transform-near infrared (FT-NIR) determination was made after the extraction of Metamitron in acetonitrile and measuring the peak area between 6434 and 6394 cm −1 corrected using a two points baseline defined between 6555 and 6228 cm −1 . Repeatability, as relative standard deviation, of 5 independent…
Determination of Paint Solvents by Vapour Phase Fourier Transform Infrared Spectrometry.
1997
Abstract A fast procedure has been developed for the direct determination of paint solvents. The method is based on the injection of small volumes of untreated solvent mixtures into a heated Pyrex glass reactor in which the sample is volatilized and introduced by means of a flow of nitrogen into an IR multiple pass gas cell and the spectrum in the mid-IR region is registered as a function of time. Data found for samples are interpolated in calibration graphs obtained by injecting different volumes of pure compounds which constitute the solvent mixture. A methylisobutylketone (MIBK) toluene mixture was used as test system to develop the proposed procedure. The method provides a limit of dete…
Solid-phase FT-Raman determination of caffeine in energy drinks
2005
Abstract A solid-phase vibrational spectrometry-based methodology (solid-phase Fourier transform-Raman spectrometry, SP-FT-Raman) has been developed for caffeine determination in commercial energy drink samples. The Raman spectra of caffeine, fixed on a C18 solid phase packed into a glass tube of 5 mm i.d., was obtained directly between 3500 and 70 cm −1 . In order to quantify caffeine, Raman intensity between 573 and 542 cm −1 corrected using a baseline defined between 580 and 540 cm −1 was used. A repeatability of 3%, as relative standard deviation of five analysis of a 200 mg l −1 concentration, and a limit of detection of 18 mg l −1 were obtained. The SP-FT-Raman procedure provides a sa…
Determination of uranium in tap water by ICP-MS
2000
A fast and accurate procedure has been developed for the determination of uranium at microg L(-1) level in tap and mineral water. The method is based on the direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma mass spectrometer (ICP-MS). Uranium was determined at the mass number 238 using Rh as internal standard. The method provides a limit of detection of 2 ng L(-1) and a good repeatability with relative standard deviation values (RSD) about 3% for five independent analyses of samples containing 73 microg L(-1) of uranium. Recovery percentage values found for the determination of uranium in spiked natural samples varied between 91% and 106%…
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…
Analysis of Chlorpyrifos in Water, Fruit Juice, and Honeybee Extract by Chemiluminescent Elisa
2008
Abstract The suitability of competitive enzyme-linked immunosorbent assays (ELISAs) with chemiluminescent detection-based immobilized antigen (indirect assay) for rapid and accurate determination of chlorpyrifos in various food matrices was tested. The limit of detection (LOD) values were 1–1.75 ng mL−1, the standard curve midpoint (IC50) was 3.5 ng mL−1, and the assay duration was 1.5 h. Assay application to the analysis of honeybee extract resulted in chlorpyrifos recoveries varying between 62 and 83% in 5–15 ng mL−1 herbicide concentration range.
Spectrofluorimetric Determination of Iproniazid and Isoniazid in a FIA System Provided with a Solid-Phase Reactor
1998
Abstract A FIA assembly is proposed for the fluorimetric determination of iproniazid and isoniazid. The oxidation of both drugs is carried out by H2O2. The excess of reagent is destroyed and removed from the flow-injection manifold by means of a metallic copper reactor which acts as catalyst in the decomposition of H2O2 and a home made debubbler. The calibration graphs were linear up to 14 μg ml−1 and 10 μg ml−1 (n=6) for iproniazid and isoniazid, respectively, with limits of detection of 0.008 μg ml−1 and 0.005 μg ml−1. The sample throughput was 24 h−1 for both drugs. The influence of foreign compounds was studied and the procedure was applied to determination of iproniazid and isoniazid i…
A microanalytical method for ammonium and short-chain primary aliphatic amines using precolumn derivatization and capillary liquid chromatography.
2007
Abstract A new microscale method is presented for the determination of ammonium and primary short-chain aliphatic amines (methylamine, ethylamine, propylamine, n -butylamine and n -pentylamine) in water. The assay uses precolumn derivatization with the reagent o -phthaldialdehyde (OPA) in combination with the thiol N -acetyl- l -cysteine (NAC), and capillary liquid chromatography with UV detection at 330 nm. The described method is very simple and rapid as no preconcentration of the analytes is necessary, and the volume of sample required is only 0.1 mL. Under the proposed conditions good linearity has been obtained up to a concentration of the analytes of 10.0 mg L −1 , the limits of detec…