Search results for "Reproducibility"
showing 10 items of 1976 documents
Thermal Lens Spectrometric Detection of Catecholamines after Oxidation to Aminochromes
1992
Abstract Experimental conditions for the spectrophotometric and thermal lens spectrometry (TLS) detection of catecholamines after oxidation to aminochromes with hexacyanoferrate (III) are optimized. At the low concentrations used in TLS, and in a 0.07 M citrate buffer, catecholamine oxidation can be performed at pH 7 and is immediate, whereas a lower pH value is required in spectrophotometry to avoid aminochrome polymerisation, the oxidation reactions being much slower. Similar TLS sensitivities are obtained for all catecholamines which facilitates HPLC evaluation. Sensitivity can be enhanced using a 50% ethanol-water medium. The linear dynamic range extends over two orders of magnitude, th…
Electrochemical detection of chloride ions using Ag-based electrodes obtained from compact disc
2022
Abstract In this work electrochemical sensors fabricated from compact disc material (waste or new) are used to quantify chloride ions in different types of samples. All three electrodes, working, counter, and pseudo-reference electrodes, were fabricated from the compact disc and directly used. Different parameters were studied in order to demonstrate the possibility of using this waste material for efficient and low-cost electrochemical sensors. Chloride sensing performance was evaluated using linear scan voltammetry as the detection technique. A sensitivity of 0.174 mA mM−1 cm−2 with a limit of detection of 20 μM and excellent selectivity against many interferents was observed. Selectivity…
Vanadium and molybdenum concentrations in particulate from Palermo (Italy): analytical methods using voltammetry
2014
The main purpose of this work was to develop a reliable method for the determination of vanadium (V) and molybdenum (Mo) in atmosphere particles or aerosols because they can not be readily measured using conventional techniques. For this research, 30 particulate samples were collected from five different stations located at Palermo, Italy. We used the catalytic adsorptive stripping voltammetry and differential pulsed voltammetry to measure Vand Mo in atmospheric particulate, respectively. The represented method includes advantages of high sensitivity, high selectivity, simplicity, reproducibility, speed and low costs. The quantification limits for V and Mo are, respectively, 0.57 and 0.80 n…
Selective chlorine determination by gas diffusion in a tandem flow assembly and spectrophotometric detection with o-dianisidine
2001
Abstract A fast, selective, sensitive and automated method for determination of free chlorine in industrial formulations and water samples is proposed. The automation of the flow assembly is based on the “tandem flow” approach, which uses a set of solenoid valves acting as independent switches. The operating cycle for obtaining a typical analytical transient signal can easily be programmed by means of friendly software running in the Windows environment. The manifold is provided with a gas diffusion unit which permits the removal of interfering species as well as concentrating the chlorine. The determination of chlorine is performed on the basis of the oxidation of o-dianisidine as the colo…
Multi-class determination of antimicrobials in meat by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry
2008
A multi-residue method using pressurized liquid extraction (PLE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for determining trace levels of 31 antimicrobials, including beta-lactams, lincosamides, macrolides, quinolones, sulfonamides, tetracyclines, nitroimidazoles and trimethoprim. The extraction method required pre-homogeneization of the meat with EDTA-washed sand and subsequent one-static-cycle extraction for 10 min with 40 ml of water at 1500 psi and 70 degrees C. The effect of operation temperature, pressure, flush volume, and static cycles on PLE performance was studied. Average recoveries ranged from 75 to 99% with relative standard deviations <1…
Development of stir bar sorptive-dispersive microextraction mediated by magnetic nanoparticles and its analytical application to the determination of…
2014
A novel microextraction technique combining the principles of stir bar sorptive extraction (SBSE) and dispersive micro-solid phase extraction (DμSPE) is presented. The main feature of the method is the use of a neodymium-core stirring bar physically coated with a hydrophobic magnetic nanosorbent. Depending on stirring speed, the magnetic sorbent either acts as a coating material to the stir bar, thus affording extraction alike SBSE, or as a dispersed nanosorbent medium for the collection and extraction of the target analytes, in close analogy to DμSPE. Once the stirring process is finished, the strong magnetic field of the stir bar prevails again and rapidly retrieves the dispersed MNPs. Al…
Evaluation of solid-phase extraction and stir-bar sorptive extraction for the determination of fungicide residues at low-microg kg(-1) levels in grap…
2004
Abstract A liquid chromatography–mass spectrometry method has been developed for determining bitertanol, carboxin, flutriafol, pyrimethanil, tebuconazole and triadimefon. The evaluation of both atmospheric pressure interfaces (API), atmospheric pressure chemical ionization (APCI) and electrospray (ESI) using positive and negative ionization modes, clearly shows that the studied pesticides are more sensitive using APCI in positive mode. Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) have been assessed for extracting these compounds in grape. The recoveries obtained by SPE in samples spiked at the limit of quantification (LOQ) level ranged from 60…
Analysis of currently used pesticides in fine airborne particulate matter (PM 2.5) by pressurized liquid extraction and liquid chromatography-tandem …
2008
During and after the application of currently used pesticides (CUPs) a significant fraction of applied pesticides can be lost to the air. A confirmatory and rapid procedure has been developed for the determination of four fungicides (carbendazim, thiabendazol, imazalil and bitertanol), three insecticides (imidacloprid, methidathion and pyriproxyfen), one helicide (methiocarb) and one acaricide (hexythiazox) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by pressurized liquid extraction (PLE) followed by a direct injection into LC-MS/MS. The main parameters affecting the performance of the electrospray ionizatio…
Quantification of low levels of amorphous content in sucrose by hyperDSC.
2005
A method was developed for the quantification of low levels of amorphous content in sucrose with hyperDSC. The method was based on the fact that the change of specific heat at the glass transition is linearly proportional to the amorphous content. It was found out that as annealing time increased, the glass transition temperature moved to a higher temperature and the change of specific heat increased. DeltaC(p) for annealed totally amorphous sucrose was 0.761+/-0.012 Jg(-1) degrees C(-1). Synthetic mixtures with various proportions of crystalline and amorphous sucrose were prepared. The following linear regression between DeltaC(p) and amorphous content was obtained: DeltaC(p)=0.0075x - 0.0…
Combining Haar Wavelet and Karhunen Loeve Transforms for Medical Images Watermarking
2014
This paper presents a novel watermarking method, applied to the medical imaging domain, used to embed the patient’s data into the corresponding image or set of images used for the diagnosis. The main objective behind the proposed technique is to perform the watermarking of the medical images in such a way that the three main attributes of the hidden information (i.e., imperceptibility, robustness, and integration rate) can be jointly ameliorated as much as possible. These attributes determine the effectiveness of the watermark, resistance to external attacks, and increase the integration rate. In order to improve the robustness, a combination of the characteristics of Discrete Wavelet and K…