It is found in this work that variation of laser power density in low-pressure plasma spectrochemical analysis of hydrogen affects sensitively the hydrogen emission intensity from the unwanted and yet ubiquitous presence of ambient water. A special experimental setup has been devised to allow the simple condition of focusing/defocusing the laser beam on the sample surface. When applied to zircaloy-4 samples prepared with various hydrogen impurity concentrations using low-pressure helium surrounding gas, good-quality hydrogen emission lines of very high signal to background ratios were obtained with high reproducibility under weakly focused or largely defocused laser irradiation. These measurements resulted in a linear calibration line with nonzero intercept representing the residual contribution from the recalcitrant water molecules. It was further shown that this can be evaluated and taken into account by means of the measured intensity ratio between the oxygen and zirconium emission lines. We have demonstrated the applicability of this experimental approach for quantitative determination of hydrogen impurity concentrations in the samples considered.
Global pollution from toxic metal waste has resulted in increased research on toxic metal adsorption. A cellulose acetate–polyurethane (CA–PU) film adsorbent was successfully prepared in this research. The cellulose acetate–polyurethane film adsorbent was prepared with a polycondensation reaction between cellulose acetate and methylene diphenyl diisocyanate. The CA–PU bond formation was confirmed by functional group analysis obtained from Fourier transform infrared (FTIR) spectroscopy. The obtained film was characterized for improved tensile and thermal properties with the addition of methylene diphenyl diisocyanate (MDI). The adsorption ability of the obtained film was evaluated with laser-induced breakdown spectroscopy (LIBS). The best film adsorbent from the LIBS was selected and studied for adsorption isotherm. The FTIR analysis confirmed the formation of the CA–PU bond from the polycondensation between cellulose acetate and the methylene diphenyl diisocyanate. The result showed that the addition of methylene diphenyl diisocyanate (MDI) resulted in the urethane network’s growth. The characterization result showed an improvement in the morphology, thermal stability, and tensile strength of the film. The LIBS studies showed improvement in the adsorption of Pb2+ with CA–PU compared with the neat CA. The isotherm studies revealed that Pb2+ adsorption by cellulose acetate–polyurethane film adsorbent was heterogeneously dependent on the Freundlich isotherm model (R2 = 0.97044). Overall, the polycondensation method proposed by this study enhanced the Pb2+ removal, and was comparable to those reported in previous studies.
A crucial safety measure to be strictly observed in the operation of heavy-water nuclear power plants is the mandatory regular inspection of the concentration of deuterium penetrated into the zircaloy fuel vessels. The existing standard method requires a tedious, destructive, and costly sample preparation process involving the removal of the remaining fuel in the vessel and melting away part of the zircaloy pipe. An alternative method of orthogonal dual-pulse laser-induced breakdown spectrometry (LIBS) is proposed by employing flowing atmospheric helium gas without the use of a sample chamber. The special setup of ps and ns laser systems, operated for the separate ablation of the sample target and the generation of helium gas plasma, respectively, with properly controlled relative timing, has succeeded in producing the desired sharp D I 656.10 nm emission line with effective suppression of the interfering H I 656.28 nm emission by operating the ps ablation laser at very low output energy of 26 mJ and 1 μs ahead of the helium plasma generation. Under this optimal experimental condition, a linear calibration line is attained with practically zero intercept and a 20 μg/g detection limit for D analysis of zircaloy sample while creating a crater only 10 μm in diameter. Therefore, this method promises its potential application for the practical, in situ, and virtually nondestructive quantitative microarea analysis of D, thereby supporting the more-efficient operation and maintenance of heavy-water nuclear power plants. Furthermore, it will also meet the anticipated needs of future nuclear fusion power plants, as well as other important fields of application in the foreseeable future.
The use of polymeric material in heavy metal removal from wastewater is trending. Heavy metal removal from wastewater of the industrial process is of utmost importance in green/sustainable manufacturing. Production of absorbent materials from a natural source for industrial wastewater has been on the increase. In this research, polyurethane foam (PUF), an adsorbent used by industries to adsorb heavy metal from wastewater, was prepared from a renewable source. Castor oil-based polyurethane foam (COPUF) was produced and modified for improved adsorption performance using fillers, analyzed with laser-induced breakdown spectroscopy (LIBS). The fillers (zeolite, bentonite, and activated carbon) were added to the COPUF matrix allowing the modification on its surface morphology and charge. The materials were characterized using Fourier-transform infrared (FTIR), scanning electron microscopy (SEM), and thermal gravimetry analysis (TGA), while their adsorption performance was studied by comparing the LIBS spectra. The bentonite-modified COPUF (B/COPUF) gave the highest value of the normalized Pb I (405.7 nm) line intensity (2.3), followed by zeolite-modified COPUF (Z/COPUF) (1.9), and activated carbon-modified COPUF (AC/COPUF) (0.2), which indicates the adsorption performance of Pb2+ on the respective materials. The heavy metal ions’ adsorption on the B/COPUF dominantly resulted from the electrostatic attraction. This study demonstrated the potential use of B/COPUF in adsorption and LIBS quantitative analysis of aqueous heavy metal ions.
A series of measurements have been performed on the time dependences of the intensities of helium, hydrogen, and deuterium emission lines from the corresponding laser-induced helium plasma at atmospheric pressure for two different He flow rates. The prolonged H ␣ and H  emissions along with their constant intensity ratio over a relatively extended period indicate the need to provide an alternative excitation mechanism other than the well-known thermal excitation process in a hot plasma. This additional excitation mechanism is also related to the metastable excited state of a He atom as indicated by the similar characteristics of the observed time dependence of the emission intensities. The enhanced intensity and lifetime of He emission at a high He flow rate was explained in terms of the collision-induced increase in the number of He atoms excited to above the 2 1 S 0 metastable state, which was also responsible for the delayed excitation of H and D atoms via an energy transfer mechanism involving a Penning-like chemi-ionization process. Finally, the benefits of He-assisted delayed excitation of H and D atoms and the aforementioned enhanced intensity and lifetime at a high He flow rate were demonstrated by the achievement of clearly resolved H ␣ and D ␣ emission lines.
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