A novel method for the direct and sensitive analysis of powder samples has been developed by utilizing the characteristics of a transversely excited atmospheric (TEA) CO(2) laser. In this study, a powder sample was placed in a container and covered by a metal mesh; the metal mesh functions to control the blowing-off of the powder. The container was then perpendicularly attached on a metal surface. When a TEA CO(2) laser (1.5 J, 200 ns) was focused on the metal surface, a large hemispherical gas plasma (radius of around 8 mm) with long emission lifetime (several tens of microseconds) was produced without ablating the metal surface. The high-speed expansion force of the gas plasma samples the powder covered by the metal mesh and fine powder particles are sent into the gas plasma region to be dissociated and excited. Sensitive semi-quantitative analysis was made on organic powder samples such as powdered rice, starch, seaweed (agar), and supplements. The detection limit of heavy metals of Cr in powdered mineral supplement was approximately 0.55 mg/kg.
A laser-induced-breakdown-spectroscopy (LIBS) experiment with a unique double-pulse setup and operated in low-pressure (3 kPa) He ambient gas is performed to study the detection of light elements, such as hydrogen (H) and deuterium (D), as well as elements of high excitation energies, such as fluorine (F) and chlorine (Cl), which are usually difficult to detect using ordinary LIBS techniques. A nanosecond Nd:YAG laser operated in its fundamental wavelength with energy of 54 mJ is focused onto the Al target to generate the He plasma. Another picosecond Nd:YAG laser operated in its fundamental wavelength with energy of 2 mJ is focused onto the sample surface and activated 2 μs before the operation of the nanosecond laser. The application to polyvinyl chloride (PVC) and polytetrafluoroethylene (PTFE) samples produces sharp and high-intensity Cl-and F-emission lines. Meanwhile, the sharp and well-resolved H−D-emission lines with merely 0.18 nm wavelength separation are also clearly detected from a zircaloy sample. Further measurement of a set of zircaloy samples containing different concentrations of D yields a linear calibration curve with a zero intercept. The detection limit of D is found to be about 10 ppm.S ince the discovery of laser-induced-breakdown spectroscopy (LIBS) around 1980, it has found applications in many fields, such as material analysis, fossil characterization, analysis of art and paintings, biological study, food and drug analysis, industrial applications, surface mapping, environmental monitoring, isotopic analysis, and a most remarkable application in the mega project of Mars exploration. Although the popularity of LIBS is evidenced by its huge number of publications, it can still benefit from overcoming its inability to detect very-low-mass atoms, such as hydrogen (H) and deuterium (D), which are important in nuclear engineering and the surveillance of nuclear terrorism. The detection of H and D in zircaloy is particularly important in both light and
To clarify the excitation mechanism of hydrogen in transversely excited atmospheric-pressure (TEA) CO2 laser-induced helium gas plasma, atomic emission characteristics of H, C, F, and He were studied using a Teflon sheet (thickness of 2 mm) attached to a metal subtarget. The TEA CO2 laser (750 mJ, 200 ns) was focused on the Teflon sheet in the surrounding He gas at 1 atm. Atomic emissions of H, C, F, and He occurred with a long lifetime, a narrow spectrum width, and a low-background spectrum. The correlation emission intensity curves of H–He and F–He indicated a parabolic functions. To explain the emission characteristics, we offered a model in which helium metastable atoms (He*) play an important role in the excitation processes; namely, atoms collide with helium metastable atoms (He*) to be ionized by the Penning effect, and then recombine with electrons to produce excited states, from which atomic emissions occur.
We present in this report the results of experimental study on the spectrochemical analysis of powder samples using subtarget supported micro mesh (SSMM) sample holder in low pressure ambient gases. The study is substantiated by establishing the analyte excitation mechanism with the evidence of shock wave plasma generation and the high temperature induced subsequently required for the thermal excitation and emission of the ablated atoms. The application of SSMM sample holder using Cu subtarget and stainless steel micro mesh to a number of powder samples in low pressure ambient gases are shown to produce generally sharp emission lines with low background, without suffering from intensity reduction and matrix effect commonly found in the use of pelletized powder samples. The same excellent spectral quality is demonstrated by its application to the analysis of rice samples which is the major staple diets in a large number of countries. In particular the analysis of Zn in rice is shown to exhibit a linear calibration line with extrapolated zero intercept and a detection limit of < 0.87 μg/g which is promising for quantitative analysis.
Rapid quantitative analyses of powder samples available in tiny amounts have successfully been conducted by utilizing a transversely excited atmospheric (TEA) CO2 laser-induced He gas plasma. In this study, 4 mg of powder sample was homogeneously mixed with 4 mg of high-vacuum silicon grease and the silicon grease–mixed powder sample (SMP) was painted on a metal surface, which serves as a subtarget. The grease functions to strongly bind the powder and to suppress blow-off of the powder particles. When a TEA CO2 laser (750 mJ, 10.6 μm, 200 ns) was directly focused on the metal subtarget in He gas at 1 atmosphere, a hightemperature He gas plasma was induced, producing a profusion metastable He atoms. It is assumed that the powder particles together with the silicon grease were vaporized to be effectively atomized and excited through metastable He atoms. The result revealed that this technique can be widely employed in the rapid semi-quantitative analyses of powder samples present in minute amounts. A quantitative analysis of loam soil containing different concentrations of Cu was successfully demonstrated, resulting in a good linear calibration curve. The detection limits of Cr and Pb in loam soil were approximately 4 and 13 mg/kg, respectively. Also, we confirmed that this technique can be applied to check the quality of commercial products such as gold film (Au foil), mineral supplement tablets, and prestigious cosmetic powders.
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