Search results for "LIMIT"
showing 10 items of 2826 documents
New optical paper sensor for in situ measurement of hydrogen sulphide in waters and atmospheres
2016
A novel and low-cost colorimetric sensor for the determination of hydrogen sulphide in environmental samples has been developed. This sensor is based on the immobilization of the reagent N,N-Dimethyl-p-phenylenediamine and FeCl3 in paper support, in which the H2S is adsorbed in order to give rise to the formation of methylene blue as reaction product. The sensor has been applied to determine H2S in water and air samples. Two different sampling systems for H2S caption from the air have been assayed: active and passive sampling. The analytical properties of the different systems have been obtained and compared. The analytical signals, corresponding to the methylene blue, have been obtained me…
A new flow cell design for chemiluminiscence analysis.
2001
The present study proposes a new flow cell called a bundle cell for chemiluminescence analysis. The results obtained were compared with those achieved by manual and automated batch procedures and flow manifolds with different cells: an common quartz flow cell, a helix cell and the most used spiral cell. Figures of merit such as limit of detection, sensitivity, accuracy and precision for the Cr(III) determination were established with light emission produced by catalysed Cr(III) luminol oxidation by hydrogen peroxide in a basic aqueous solution. An improvement in sensitivity about 50% as compared with the spiral cell and even larger with respect to the other flow cells tested was observed. T…
Addition of thiourea and hydrochloric acid: Accurate nanogram level analysis of mercury in humic-rich natural waters by inductively coupled plasma ma…
2020
Abstract An analytical method was developed for the direct determination of total mercury in natural waters at low ng L−1 level by inductively coupled plasma mass spectrometry (ICP-MS). The presented method overcomes previously observed problems relating to poor spike recoveries by adding 0.12% thiourea in addition to 3% HCl to all samples and standards. The sample preparation is fast and easy to perform by the developed method since it requires only the addition of HCl and thiourea to the water samples. A very low instrument detection limit (0.4 ng L−1) was obtained without time-consuming preconcentration procedures. The accuracy and precision of the developed method were found excellent b…
Copper, iron and zinc determinations in human milk using FAAS with microwave digestion
2000
Abstract A method for determining copper, iron and zinc in human milk was optimized and validated. It includes microwave mineralization of the sample and measuring the elements by flame atomic absorption spectroscopy (FAAS). Only 2 ml of milk is needed, and the method is free of matrix interferences. The values obtained for the detection limits (0.07; 0.07; 0.11 μg/ml milk, for copper, iron and zinc) precision of the method, intra-assay (2.9; 5.2; 6.1%RSD for copper, iron and zinc) and accuracy, evaluated using recovery assays (98.8; 100.4; 95.9% for copper, iron and zinc) show that the method is useful for the purpose mentioned. Moreover, the method is rapid and simple, and the determinati…
Determination of methamphetamine in urine samples with sodium 1,2-naphthoquinone-4-sulphonate
1994
Optimal conditions have been studied for the determination of methamphetamine in urine samples by an extractive-spectrophotometric method with sodium 1,2-naphthoquinone-4-sulphonate (NQS) as reagent. These conditions are: NaHCO3 pH 10, NQS 6.3 × 10−3 mol/l and heating for 5 min at 45°C. The accuracy and precision of the method were tested. The detection limits were 0.2 mg/l in the standard and 0.9 mg/l when 5 ml of urine sample were taken. The standard deviation of blank urine was evaluated from 12 different samples. The relative errors found in the determination of methamphetamine in urine were lower than 10% if the methamphetamine-amphetamine ratio was higher than 4.
Influence of the differentiation system on the analytical parameters for the spectrophotometric determination of clonazepam in urine
1991
Abstract Electronic and mathematical differentiation of the ultraviolet visible spectra were compared from the study of the analytical parameters of the direct determination of clonazepam in urine samples. Third-order derivative spectra were used. The mathematical differentiation provides higher sensitivity, a lower limit of detection, and better accuracy and precision than the electronic one. The use of a diode array instrument provides lower sensitivity than that found using a conventional spectrometer; however, the limit of detection obtained in both cases is of the same order.
Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry.
2007
A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters aff…
First‐Derivative Fourier‐Transform Infrared Determination of Oxadiazon in Commercial Herbicide Formulations
2008
Abstract A Fourier‐transform infrared (FTIR) method has been developed for the quantification of oxadiazon in herbicide formulations. The method involves the extraction of the active ingredient by sonication of the samples with CHCl3 and direct measurement of the peak area values in first‐order derivate spectra from 1770 cm−1 to 1774 cm−1 corrected with a baseline point located at 1950 cm−1 and after a 5‐point smoothing. A limit of detection (3 s) of 0.03 mg g−1 and a typical relative standard deviation (RSD) of 1.3% were found. Results obtained were comparable with those found by liquid chromatography with UV detection. The proposed method involves a 7‐times reduction in solvent consumptio…
Analysis of LSD in human body fluids and hair samples applying ImmunElute columns.
2000
Immunoaffinity extraction units (LSD ImmunElute) are commercially available for the analysis of lysergic acid diethylamide (LSD) in urine. The ImmunElute resin contains immobilized monoclonal antibodies to LSD. We applied the ImmunElute procedure to serum and also to human hair samples. For hair analysis the samples were first extracted with methanol under sonication. The extracts were then purified using the ImmunElute resin. LSD analysis was carried out with HPLC and fluorescence detection. The immunoaffinity extraction provides highly purified extracts for chromatographic analysis. The limit of detection (signal-to-noise ratio = 3) has been determined to be < 50 pg regardless of which sa…
Comparison and improvement of the existing methods for the determination of aflatoxins in human serum by LC-MS/MS
2010
Aflatoxins are toxic metabolites of some Aspergillus flavus, A. parasiticus and A. nomius strains that occur in many foods and feeds. Aflatoxin B1 is the most abundant and toxic member of the family, and it is also the most potent hepatocarcinogen known. In order to estimate the potential human health risk of aflatoxin B1, it is useful to measure its blood concentration. In this work a rapid liquid chromatography coupled to mass spectrometry (LC-MS/MS) method for the simultaneous determination of aflatoxins B1, B2, G1 and G2 and its metabolites, aflatoxins M1 and M2 in human serum, is proposed. Small serum volumes have been used and the extracts have been obtained without any clean-up proce…