Biomedical subjects

I López-García

Publications and source records attributed to I López-García.

8 recordsLinked to original sources

PubMed2004

Thickness dependence of structural relaxation in spin-cast, glassy polymer thin films.

The isothermal structural relaxation of glassy, spin-cast polymer thin films has been investigated. Specifically, the thickness h of freshly cast poly(methyl methacrylate) thin films was measured over time using spectroscopic ellipsometry. The spin-cast films exhibit a gradual decrease in thickness, which is attributed to structural relaxation of the glass combined with simultaneous solvent loss. In all cases, h was found to be greater than the equilibrium thickness h(infinity) , which is obtained by cooling slowly from the melt. It is observed that both the rate of the volume relaxation and the fractional departure from h(infinity) (referred to as delta(0) ) increase with increasing film thickness. In the limit of very thin films, the initial h is close to h(infinity) , and delta(0) is small, whereas in thick films (>500 nm) , a plateau value of delta(0) of 0.16 is observed, which is close to the volume fraction of the solvent at the vitrification point. This dependence of delta(0) on thickness is observed regardless of the substrate, polymer molecular weight, or angular velocity during spin casting. Enhanced mobility near film surfaces could be leading to greater relaxation in thinner films prior to, and immediately after, the vitrification of the polymer during the deposition process.

Journal Article↗

PubMed2004

Purge-and-trap capillary gas chromatography with atomic emission detection for volatile halogenated organic compounds determination in waters and beverages.

A method for the simultaneous determination of 10 volatile halogenated organic compounds (VHOCs), including four trihalomethanes (THMs), in waters and beverages was developed. The analytes were stripped from the aqueous sample by a flow of helium, preconcentrated in a capillary trap and thermally desorbed using a purge-and-trap (PT) system. This was followed by capillary gas chromatography with microwave-induced plasma atomic emission spectrometry (GC-AED). For element-specific detection, three wavelengths were monitored, corresponding to chlorine (479 nm), bromine (478 nm) and iodine (193 nm). Each chromatographic run took 21 min, including the purge time. After careful choice of the experimental conditions, the performance of the system was evaluated. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients for linear calibration were at least 0.9987. Detection limits, calculated for 5 ml sample volume, ranged from 0.05 microg l(-1) for chloroform to 0.5 microg l(-1) for tetrachloromethane. The method was successfully applied to the quantitative analysis of water samples of different origin and also of several beer and juice samples. The tap water samples analyzed contain variable concentrations of the four trihalomethanes, ranging from 1.0 to 66.5 microg l(-1), depending of the compound. Whereas chloroform, bromodichloromethane and bromoform were found in some of the juice samples, only chloroform was detected in the beer samples. The method is reliable and can be used for routine monitoring in water and beverages.

Beverages↗

PubMed2003

Stability of arsenobetaine levels in manufactured baby foods.

The stability of arsenobetaine in baby foods under different experimental conditions is evaluated. Total arsenic was analyzed by electrothermal atomic absorption spectrometry, and the speciation of arsenicals was carried out by coupling liquid chromatography to hydride generation-atomic absorption spectrometry. The highest arsenic levels in the analyzed baby foods corresponded to those containing plaice (2 to 3 microg/g). The speciation data indicated that arsenobetaine, a nontoxic species, was the only arsenical present in the baby foods analyzed at levels between 0.2 and 3 microg/g. Two different procedures for extracting arsenicals from baby foods, involving a water-methanol-chloroform mixture and enzymatic hydrolysis, were tested, and similar results were obtained. Furthermore, the arsenobetaine levels remained unchanged when the baby foods were stored for different times or when the samples were freeze-dried, thus confirming the stability of arsenobetaine and the nonappearance of other arsenic species by interconversion. The reliability of the procedure was checked by analyzing a certified reference material.

Arsenicals↗

PubMed2002

Determination of pesticides in waters by capillary gas chromatography with atomic emission detection.

Capillary gas chromatography with atomic emission detection (GC-AED) was successfully used to separate and quantify 14 pesticides (organochlorines, organophosphorus compounds and pyrethrins) in water samples after liquid-liquid extraction with ethyl acetate. Monitoring the emission lines for elements such as chlorine, bromine and sulfur ensures nearly specific chromatograms for these elements, and markedly increases selectivity. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients relating to linearity were at least 0.999. Each chromatographic separation takes 21 min and, since two injections are necessary, it requires approximately 1 h to analyze one sample. The method shows a precision of 4.3-8.2% (RSD), depending on the compound. The application of liquid-liquid extraction with ethyl acetate led to recoveries from spiked samples ranging from 76 to 113%. The sensitivity and linearity for the elements chlorine, sulfur, nitrogen and phosphorus were checked under the optimized conditions at their customary emission wavelength. The sensitivity and linearity for these compounds decreased in the order (atom and emission wavelength) Cl (479 nm)>S (181 nm)>P (178 nm)>N (174 nm). A study of the GC-AED system's response to chlorine concentration in eight pesticide molecules was performed and a linear relationship was found with a correlation coefficient of 0.987.

Calibration↗

PubMed2002

On-line filtration system for determining total chromium and chromium in the soluble fraction of industrial effluents by flow injection flame atomic absorption spectrometry.

Two manifolds were assessed for the purpose of determining both the total chromium content and that present as a soluble form in industrial effluents by flow injection flame atomic absorption spectrometry (FI-FAAS). To determine the chromium content in the soluble fraction the samples were used without additional treatment, a 0.45 microm filter being included in the FI system. To determine the total chromium content, the samples were acidified with nitric acid 20% (v/v) and heated for 30 s in a microwave oven (temperatures of about 70 degrees C were reached). The problem posed by the very different concentration range in which total and soluble chromium are present was overcome by using programmed flow rate methodology and by only partially emptying the sample loop. A personal computer controlled both the rotation speed of a peristaltic pump and the volume of sample injected into the system, thus obtaining the dispersion degree required. Using the manifold proposed, the chromium content in the soluble fraction can be determined in the 0.5-20 microg mL(-1) range using a 10 microg mL(-1) single standard for calibration. To determine the total chromium content, a calibration line in the 20-200 microg mL(-1) range was obtained using a single 50 microg mL(-1) chromium standard solution. The reliability of the semi-automatic devices was verified by comparing the results obtained with those found by treating the samples and using both FAAS in a conventional way and a spectrophotometric method using diphenylcarbazide at the 95% confidence level (ANOVA test). The proposed procedures showed a RSD lower than +/-3%.

Chromium↗

PubMed2000

Selenium determination in biological fluids using Zeeman background correction electrothermal atomic absorption spectrometry.

Procedures for the direct determination of total selenium in urine, serum, and blood using electrothermal atomic absorption spectrometry are presented. In the selected experimental conditions, Zeeman correction is mandatory to compensate for the high background signals. The sample diluted and containing 0.1% (w/v) Triton X-100 is introduced directly into the electrothermal atomizer. A solution containing 15% (w/v) hydrogen peroxide, 0.65% (w/v) nitric acid, and 0.5% (w/v) nickel is injected separately into the atomizer. Calibration is carried out using the standard additions method. The detection limit is 30 pg selenium. If palladium, instead of nickel, is used as the chemical modifier, calibration can be carried out against aqueous standards, and the detection limit is 45 pg. In this case, three separate injections are required to prevent precipitation problems in the automatic injector. The reliability of the procedures is checked by analyzing three certified reference materials and by recovery studies. Mean recoveries are 99.7% for serum, 99.4% for urine, and 100.8% for blood samples. Relative standard deviation values are +/-4.0% for serum, +/-3.9% for urine, and +/-4.5% for blood.

Body Fluids↗

PubMed2000

Rapid determination of lead and cadmium in sewage sludge samples using electrothermal atomic absorption spectrometry with slurry sample introduction.

Lead and cadmium concentrations in sewage sludge samples are determined by suspending the ground samples in a solution containing 10% (v/v) concentrated hydrofluoric acid, 1% (v/v) concentrated nitric acid, 0.5% (m/v) dihydrogen ammonium phosphate and 0.1% (m/v) sodium hexametaphosphate. Aliquots of 20 microL of these suspensions (4 mg/mL) are diluted to 1000 microL with the same solution and then injected into the electrothermal atomizer. The drying stage is performed by programming a 400 degrees C temperature, a ramp time of 20 s and a hold time of 15 s on the power supply of the atomizer. No ashing step is used. Platform atomization is carried out at 1600 and 1800 degrees C for Pb and Cd, respectively. Calibration is performed using aqueous standards in the 5-75 and 0.2-5 microg/L Pb and Cd ranges, respectively. Results obtained for three certified reference materials and four samples demonstrate the reliability of the procedures described.

Cadmium↗

PubMed2000

Determination of arsenic in biological fluids by electrothermal atomic absorption spectrometry.

A procedure for the determination of the total content of arsenic in urine, serum and blood by electrothermal atomic absorption spectrometry (ETAAS) is described. Zeeman correction is used to compensate the high background signals. The samples are diluted (1 + 1 for urine and 1 + 3 for both serum and blood samples) in a medium containing 0.1% w/v Triton X-100 before being introduced directly into the furnace. A solution containing 15% w/v hydrogen peroxide, 0.65% w/v nitric acid and 0.5% w/v nickel is also introduced into the atomizer by means of a separate injection. Calibration is carried out against aqueous standards for blood and serum samples and using the standard additions method for urine samples. The detection limit is 20 pg (2 ng ml-1). The reliability of the procedure is checked by analyzing three certified reference materials and by recovery studies.

Arsenic↗