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P López Mahía

Publications and source records attributed to P López Mahía.

7 recordsLinked to original sources

Application of programmed-temperature split/splitless injection to the trace analysis of aliphatic hydrocarbons by gas chromatography.

The dependence of the programmed-temperature solvent split sampling technique using a PSS (programmed-split/splitless) injection mode on different variables affecting the introduction of large sample volumes for a mixture of alkanes in capillary GC was evaluated. Apart from the studies found in the literature on different factors such as speed of injection. presence of adsorbent in the liner, internal diameter of the liner, initial and final injector temperature, split flow-rate and initial split time, affecting the chromatographic signal of different compounds, others were studied whose influence has not been considered until now. They include length of the microsyringe needle, adsorbent distribution in the liner, injection volume on analyte discrimination, speed of injector heating, time which the column stays at the initial temperature and time that the injector stays at the final temperature. Once finalised, the study of the PSS injection mode was compared with the conventional mode of gas chromatography splitless injection, and found that the proposed method increases sensitivity in GC trace analysis. Finally, the application of both injection modes in the determination of aliphatic hydrocarbons was tested in an atmospheric particulate sample.

Chromatography, Gas↗

Capillary zone electrophoresis for the determination of light-absorbing anions in environmental samples.

A rapid and simple method for separation and determination of inorganic anions by capillary zone electrophoresis was described. The detection was carried out directly with a diode array detector. The experimental conditions, such as concentration of carrier electrolyte, capillary length, voltage, and temperature were optimized. In order to improve selectivity, different organic modifiers were also investigated. The baseline separation of 10 light-absorbing anions was accomplished within 3.5 min with a background electrolyte consisting of 50 mM sodium tetraborate containing 5% MeOH. Linear plots were obtained in the concentration range of 0.1-10 microg/ml. With sample stacking injection, the quantitation limits of the anions were found to be in the range of 0.02-0.1 microg/ml. The proposed method was successfully applied to the determination of inorganic anions in environmental samples and in effluents of a power plant.

Anions↗

Direct analysis of inorganic anions in samples with high salt content by capillary zone electrophoresis.

Trace-level inorganic anions in seawater are separated efficiently by capillary zone electrophoresis using direct UV detection. The carrier electrolyte is 50 mM borate at pH 9.3 and contained 1.5M NaCl. This buffer solution is adopted to prevent interference from high concentrations of the chloride ion in seawater. No electro-osmotic flow reverser is used to shorten the analysis time. The experimental conditions such as the concentration of NaCl in the carrier electrolyte, capillary inner diameter, applied current, and temperature are optimized. Linear plots are obtained in the concentration range of 0.1 to 20 microg/mL. The quantitation limits of the anions are in the order of 0.02 to 0.1 microg/mL. The proposed method may be applicable to the determination of inorganic anions in other environmental samples and effluents of a power plant.

Anions↗

Optimization of microwave-assisted extraction of hydrocarbons in marine sediments: comparison with the Soxhlet extraction method.

Microwave energy was applied to extract polycyclic aromatic hydrocarbons (PAHs) and linear aliphatic hydrocarbons (LAHs) from marine sediments. The influence of experimental conditions, such as different extracting solvents and mixtures, microwave power, irradiation time and number of samples extracted per run has been tested using real marine sediment samples; volume of the solvent, sample quantity and matrix effects were also evaluated. The yield of extracted compounds obtained by microwave irradiation was compared with that obtained using the traditional Soxhlet extraction. The best results were achieved with a mixture of acetone and hexane (1:1), and recoveries ranged from 92 to 106%. The extraction time is dependent on the irradiation power and the number of samples extracted per run, so when the irradiation power was set to 500 W, the extraction times varied from 6 min for 1 sample to 18 min for 8 samples. Analytical determinations were carried out by high-performance liquid chromatography (HPLC) with an ultraviolet-visible photodiode-array detector for PAHs and gas chromatography (GC) using a FID detector for LAHs. To test the accuracy of the microwave-assisted extraction (MAE) technique, optimized methodology was applied to the analysis of standard reference material (SRM 1941), obtaining acceptable results.

Chromatography, Gas↗

Resolution of benzo[a]pyrene in complex mixtures of other polycyclic aromatic hydrocarbons. Comparison of two spectrofluorimetric methods applied to water samples.

Two spectrofluorimetric methods, second-derivative constant-energy synchronous luminescence (SDCESL) and constant-wavelength synchronous luminescence (CWSL) in combination with multiple linear regression (MLR), for the quantification of benzo[a]pyrene (BaP) at sub-ng mL-1 levels, in the presence of benzo[b]fluoranthene (BbFt), benzo[k]fluoranthene (BkFt), benzo[ghi]perylene (BghiP) and indeno[1,2,3-cd]pyrene (IP), were developed and compared in detail. SDCESL presents lower limits of detection and quantification than CWSL/MLR and also gives more exact and precise results for levels close to the quantification limit. For BaP, SDCESL achieved quantification limits of 0.019 ng mL-1 in river waters and 0.007 ng mL-1 in drinking waters. This work offers a sensitive, precise, accurate, rapid, simple and economic methodology for monitoring BaP in waters for public consumption, meeting all the requirements of the EC Directive 98/83/CE that fixes the maximum admissible limit for this polycyclic aromatic hydrocarbon in drinking waters at of 0.010 ng mL-1.

Benzo(a)pyrene↗

Overall migration and specific migration of bisphenol A diglycidyl ether monomer and m-xylylenediamine hardener from an optimized epoxy-amine formulation into water-based food simulants.

The overall and specific migrations of BADGE n = 0 monomer and m-XDA hardener from a BEPOX LAB 889 (Gairesa internal code), epoxy system cured at room temperature, into three water-based food simulants are studied. Hydrolysis of BADGE n = 0 was observed in all of these simulants, giving more polar products. We thus propose changing the EEC Directives, which at present only legislate for levels of BADGE n = 0 monomer in the simulants, to include the hydrolysis products of BADGE monomers. Another alternative would be to express all the migration levels due to BADGE and its derived products in terms of BADGE itself.

Benzhydryl Compounds↗

Sensitive and rapid reversed-phase liquid chromatography-fluorescence method for determining bisphenol A diglycidyl ether in aqueous-based food simulants.

A method has been developed for determination of bisphenol A diglycidyl ether (BADGE) in 3 aqueous-based food simulants: water, 15% (v/v) ethanol, and 3% (w/v) acetic acid. BADGE is extracted with C18 cartridges and the extract is concentrated under a stream of nitrogen. BADGE is quantitated by reversed-phase liquid chromatography with fluorescence detection. Relative precision at 200 micrograms/L was 3.4%, the detection limit of the method was 0.1 micrograms/L, and recoveries of spiking concentrations from 1 to 8 micrograms/L were nearly 100%. Relative standard deviations for the method ranged from 3.5 to 5.9%, depending on the identity of the spiked aqueous-based food simulant.

Acetates↗