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J J Laserna

Publications and source records attributed to J J Laserna.

12 recordsLinked to original sources
PubMed2003

Chemical imaging using microline laser ablation: performance comparison of Gaussian and flat top lasers.

In previous studies, the potential of a microline imaging arrangement for surface characterization of solid samples in air at atmospheric pressure using laser-induced plasma spectrometry (LIPS) has been demonstrated. An improvement of this approach to obtain a uniform ablation along the microline focus that leads to a representative spatial distribution of elements on the sample surface is presented. For this purpose, the influence of beam energy distribution of two types of Nd:YAG pulsed lasers (a Gaussian laser and a flat top laser) on lateral resolution, intensity profiles of elements, chemical distribution maps, and plasma electron temperature has been investigated. As models of homogeneous and compositionally patterned samples, a stainless steel sample and a photovoltaic cell were chosen for this study. The results demonstrated that the Gaussian laser provides the best lateral resolution, but more redeposition at both sides of the microline crater, while the chemical maps obtained with the flat top laser matched with the distribution of the constituents of the sample surface.

Energy-Generating Resources↗
PubMed2003

Automated line-focused laser ablation for mapping of inclusions in stainless steel.

An automated line imaging arrangement for two-dimensional (2D) and three-dimensional (3D) generation of chemical maps of inclusions in stainless steel by laser-induced plasma spectrometry (LIPS) is presented. The plasma was generated in air at atmospheric pressure by focusing a flat-top Nd:YAG laser beam operating at 532 nm to a microline on the sample surface. The emitted light from the microline plasma was projected through an imaging spectrograph onto a charge-coupled device (CCD) detector to generate a spatially and spectrally resolved data set. Compositional distribution maps of inclusion constituents (Mn, Mg, Ca, Al, and Ti) in stainless steel of different grades have been generated. Comparative studies with the point-to-point LIPS mapping method have been performed, resulting in a 51-fold reduction in the number of pulses and analysis time when the microline imaging approach is employed. The results illustrate the capability of microline imaging LIPS for fast-automated acquisition of tomographic maps with spatial resolution of 50 microm between adjacent craters and 4.8 microm along the microline.

Journal Article↗
PubMed2001

Time-resolved laser-induced plasma spectrometry for determination of minor elements in steelmaking process samples.

A pulsed Nd:YAG laser operating on the fourth (266 nm) and second (532 nm) harmonics has been used to generate plasmas on the target surface in air at atmospheric pressure. The influence of wavelength on quantitative analysis of 4 minor elements in stainless steel samples (Si, Ti, Nb and Mo) was investigated. Stainless steel samples with different elemental concentrations were prepared and analyzed by laser-induced plasma spectrometry (LIPS). The effect of laser wavelength on analytical figures of merit (calibration curves, correlation coefficients, linear dynamic ranges, analytical precision, and accuracy values) was found to be negligible when internal standardization (an Fe line) and time-resolved laser-induced plasma are employed. For both wavelengths, the calibration curves presented a good linearity and an acceptable linear dynamic range in the concentration interval investigated. For the four elements studied, limits of detection lower than 150 microg g(-1) were achieved. To evaluate the influence of wavelength on precision and accuracy, a set of fifteen high-alloyed steel samples from different stages of steelmaking process have been analyzed. Finally, the long-term stability of the analytical measurements for Mo with 532 nm wavelength has been discussed. RSD values were lower than 5.3% for the elements studied.

Journal Article↗
PubMed1996

Direct determination of diuretic drugs in urine by capillary zone electrophoresis using fluorescence detection.

Four diuretic drugs banned in sport (amiloride, triamterene, bendroflumethiazide and bumetanide) have been separated by capillary zone electrophoresis (CZE) and detected using conventional fluorescence spectrometry. The effect of pH on electrophoretic parameters such as migration time, peak efficiency and peak height is discussed. Complete separation of the four drugs is achieved in less than 8 min at pH 8. No interference due to endogenous urine components is observed and thus direct urine analysis is feasible. Analytical figures of merit including precision and limits of detection are presented. Limits of detection range between 0.5 fmol for triamterene and 21.6 fmol for bumetanide.

Amiloride↗
PubMed1996

Space and time-resolved laser-induced breakdown spectroscopy using charge-coupled device detection.

Space and time-resolved studies of laser induced plasmas in air at atmospheric pressure are presented. Photovoltaic solar cells have been used as samples. The second harmonic (532 nm) of a Nd : YAG laser at an irradiance of 18 x 10(12) W/cm(2) has been used. The precise focus of the beam allows a microanalysis at a 0.02 mm(2) surface area working in single-shot mode. The use of an intensified charge-coupled device (CCD) detector has allowed time-resolved studies in both imaging or spectroscopy modes. The two-dimensional capability of the CCD has enabled the study of atomic and ionic species distribution along the plume. Most data have been recorded using single-laser shot experiments. Spectral lines have been assigned to transitions in atomic components of the material under investigation in the neutral or ionic states of the corresponding atoms. Effects of delay in improving spectral resolution and some examples of spectral characterization of species as a function of its decay are shown.

Journal Article↗
PubMed1996

Applications of laser-induced breakdown spectrometry (LIBS) in surface analysis.

The applicability of laser-induced breakdown spectrometry (LIBS) for surface analysis is presented in terms of its lateral and depth resolution. A pulsed N(2) laser at 337.1 nm (3.65 J/cm(2)) was used to irradiate solar cells employed for photovoltaic energy production. Laser produced plasmas were collected and detected using a charge-coupled device. An experimental device developed in the laboratory permits an exact synchronization of sample positioning using an XY motorized system with laser pulses. Multielement analysis with lateral resolution of up to 30 microm is feasible with the present system. Three-dimensional capabilities of the system are used for studies on the distribution of carbon impurities at the surface of the solar cells.

Journal Article↗
PubMed1995

Determination of antipyrine metabolites in human plasma by solid-phase extraction and micellar liquid chromatography.

A rapid solid-phase extraction (SPE) procedure was developed for the quantitative isolation of three important antipyrine (dipyrone) metabolites from human plasma: 4-formylaminoantipyrine (FAA), 4-aminoantipyrine (AA) and 4-methylaminoantipyrine (MAA). Separation and quantitation were performed using micellar liquid chromatography (MLC) with a 0.1 mol l-1 sodium dodecyl sulfate (SDS)-2.5% pentanol mobile phase and UV detection at 262 nm. The metabolites were well resolved in less than 5 min using an octadecyl silica-bonded stationary phase. The extraction procedure involved passing 0.3 ml of plasma sample through a disposable SPE cartridge packed with C18 bonded porous silica. The adsorbed metabolites were removed from the cartridge with methanol. The eluent was evaporated to dryness and the residue was reconstituted with mobile phase and injected into the chromatographic system. The cartridge blank interferent peaks, the effects on reproducibility of sample loading in the cartridge and volume needed for desorption of metabolites were evaluated. The concentration of metabolites ranged between 2.4 and 4 micrograms ml-1. The present procedure yields recoveries for the three metabolites ranging from 93 to 100%. The relative standard deviation (Sr) ranged between 1.2 and 13.6%. Limits of detection (LODs) were 10.5, 11.5 and 17.0 ng ml-1 for FAA, AA and MAA, respectively.

Aminopyrine↗
PubMed1994

Capillary zone electrophoresis for the rapid screening of banned drugs in sport.

Capillary zone electrophoresis was used to analyze some drugs illegally used in sports. The spectroscopic characteristics and electrophoresis migration parameters of diuretics, narcotics-analgesics and beta-blockers were established. Analytical figures of merit including parameters on the precision of migration and limits of detection are discussed. Results for the separation of drugs of different doping families are discussed. An analysis of urine from a patient receiving daily doses of atenolol is presented.

Adrenergic beta-Antagonists↗
PubMed1990

Surface-enhanced Raman analysis of sulfa drugs on colloidal silver dispersion.

Surface-enhanced Raman spectrometry (SERS) of three sulfa drugs (sulfadiazine, sulfamerazine, and sulfamethazine) is reported. Silver colloidal dispersions prepared by simple borohydride reduction of silver nitrate are used as substrates. The capability of SERS for spectral fingerprinting of analytes with close structural properties using easily prepared substrates and relatively simple instrumentation is illustrated. By careful attention to the timing in the measurement, quantitative information can be obtained from silver colloids. Linearity was achieved up to 100 ng mL-1. Limits of detection range in the low nanograms per milliliter level.

Colloids↗
PubMed1989

Mixture analysis and quantitative determination of nitrogen-containing organic molecules by surface-enhanced Raman spectrometry.

Surface-enhanced Raman spectrometry (SERS) on a silver-coated filter paper substrate of nitrogen-containing organic molecules is reported. A correction procedure for standardization of measurements is proposed and evaluated to solve the difficult problem of quantitation of adsorbate in SERS. The relative standard deviation obtained through this procedure is around 15%. Linearity (r = 0.999) was achieved up to 50 micrograms/mL aminoacridine. A limited dynamic range is observed, however, due to the limited number of SERS active sites in the substrate. Spectral fingerprinting of three-component mixtures by concentration-dependent selective molecular adsorption on the substrate is also reported.

Aminoacridines↗
PubMed1988

Analysis by surface enhanced Raman spectroscopy on silver hydrosols and silver coated filter papers.

Surface enhanced Raman spectrometry (SERS) is an analytical technique with a sensitivity comparable to that of conventional molecular absorption or fluorescence spectroscopy, with the additional major advantage of selectivity inherent in vibrational spectroscopies. The analytical application of flowing silver hydrosols is described. Under the controlled experimental conditions of flow injection analysis, it was possible to detect as low as 30 ng of p-aminobenzoic acid. The linear range was two orders of magnitude (1-100 microg ml(-1)) with a signal reproducibility of 3.2%. Silver coated filter paper is another SERS active substrate that is simple to prepare and handle. The SERS spectra of several nitrogen-containing molecules were obtained on these substrates. The effects of laser power and paper hydration are described. The relative advantages of both substrates are compared.

Journal Article↗