Ash characteristics in controlled diode laser pyrolysis of chlorinated rubber

This paper describes the effects of 60 W High Power Diode Laser (HPDL) beams on the removal of chlorinated rubber (CR) paint from concrete surfaces and the ash particles generated from this process. The physical characteristics, including shape and size distribution of the removed and collected airborne CR particles, down to a size of around 1 μm in diameter, were determined using optical microscopy and image analysis. The shape of the particles observed was highly irregular, displaying no symmetry. The size distribution of the collected particles was found to range between 1–2000 μm, with the maximum concentration being found between 29 and 60 μm. The chemical characteristics of the CR ash particles were investigated by means of ESEM and EDX techniques. From a comparative analysis, it was found that the concentration of chlorine within the CR material was significantly reduced after HPDL treatment. This, together with DTA/TGA results indicated a combustive degradation of the CR polymer through the interaction with the process gas, oxygen, and the laser irradiation. Also, a strong correlation between laser power and average particle sizes has been found, with higher powers generally producing larger particle sizes. Opposite effects have been found by changing the oxygen flow rate, with higher oxygen flow producing, on average, smaller particles. An interpretation of the combustion process, as well as a brief discussion on operational safety and environmental impact of the products is attempted.     

Cavity Ring-Down Spectroscopy coupled with helium microwave-induced plasma for fluorine detection

Cavity Ring-Down Spectroscopy with a tunable diode laser has been used for the detection of fluorine at trace levels. A homemade experimental setup was constructed to accommodate the microwave-induced plasma glow discharge inside the optical cavity. The energy delivered by helium plasma discharge was successfully used not only for the dissociation of fluorine molecules but, more importantly, also for the excitation of fluorine atoms into their metastable level 3s⁴P_5/2. The absorption observed at the 3s⁴P_5/2–3p⁴D^o_7/2 transition (corresponding to a 685.603-nm atomic line) was used for fluorine atom detection. Good agreement between theoretical and measured absorption line shapes confirmed the selectivity of fluorine atomic absorption. We observed an absorption coefficient of 4 ? 10⁻⁶ cm⁻¹, corresponding to a detection of F(3s⁴P_5/2) atoms at about 1.5 ? 10⁶ atoms cm⁻³. These data demonstrate that we achieved a detection limit of 100 ng g⁻¹ under the conditions of our initial homemade experimental setup. However, the optimization of the system may lead to the improvement of the detection limit by approximately two orders of magnitude.     

Determination of clofentezine in medical herb extracts by chromatographic methods combined with diode array scanning densitometry

The aim of this study is to report a new procedure for extraction, cleanup and determination of clofentezine in herb extracts by ultrasound‐assisted solvent extraction, SPE and multidimensional planar chromatography with diode array detector (MDPC‐DAD) and/or HPLC‐DAD. The application of various extraction solvents in SPE experiments conducted on octadecyl silane coupled with styrene‐divinylbenzene cartridges for fractionation and purification samples has been described. Normal‐phase systems were used in MDPC experiments on silica layer. The procedure described for the determination of compounds is inexpensive and can be applied to the routine analysis of analytes in plant extracts, after preliminary cleanup and concentration, e.g. by SPE. Application of MDPC‐DAD and HPLC‐DAD is especially useful for correct identification of components of difficult, complicated mixtures, e.g. analytes in medical herbs.     

High-resolution spectroscopy and preliminary global analysis of C-H stretching vibrations of C2H4 in the 3000 and 6000 cm regions

Ethylene (ethene, H₂C=CH₂) is a naturally occurring compound in ambient air that affects atmospheric chemistry and global climate. The C₂H₄ spectrum is available in databases only for the 1000 and 3000 cm⁻¹ ranges.In this work, the ethylene absorption spectrum was measured in the 6030-6250 cm⁻¹ range with the use of a high resolution Bruker IFS 125HR Fourier-spectrometer and a two-channel opto-acoustic spectrometer with a diode laser. As a secondary standard of wavelengths, the methane absorption spectrum was used in both cases.A preliminary analysis was realized thanks to the tensorial formalism developed by the Dijon group that is implemented in the XTDS software package [39]. We considered the two combination bands ν₅+ν₉ and ν₅+ν₁₁ as an interacting dyad. Parameters for the ν₉/ν₁₁ dyad were fitted simultaneously from a re-analysis of previously recorded supersonic expansion jet FTIR data, while parameters for the v₅=1 Raman level were taken from literature. More than 600 lines could be assigned in the 6030-6250 cm⁻¹ region (and also 682 in the 2950-3150 cm⁻¹ region) and effective Hamiltonian parameters were fitted, including Coriolis interaction parameters. The dyad features are globally quite well reproduced, even if there are still problems at high J values.     

Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater

This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a β-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100 μg/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.     

Infrared diode laser spectroscopy of the ν = 2 band of AlF

A vibrational–rotational spectrum of the ν = 2 transitions of a high-temperature molecule AlF was observed between 1490 and 1586 cm⁻¹ with a diode laser spectrometer. Measurements were made on the ν = 3–1, 4–2, 5–3 and 8–6 bands at a temperature of 900 °C. Measured spectral lines were fitted to effective band constants ν₀, B_ν and D_ν for each band. Present measurements were made with only one Pb-salt laser diode. Physical significance of the effective band constants is discussed.     

Frequency modulated spectroscopy as a probe of molecular collision dynamics

We describe the application of frequency modulated spectroscopy (FMS) with an external cavity tuneable diode laser to the study of the scalar and vector properties of inelastic collisions. CN X(2)Sigma(+) radicals are produced by polarized photodissociation of ICN at 266 nm, with a sharp velocity and rotational angular momentum distribution. The collisional evolution of the distribution is observed via sub-Doppler FMS on the A(2)Pi-X(2)Sigma(+) (2,0) band. He, Ar, N(2), O(2) and CO(2) were studied as collider gases. Doppler profiles were acquired in different experimental geometries of photolysis and probe laser propagation and polarization, and on different spectroscopic branches. These were combined to give composite Doppler profiles from which the speed distributions and specific speed-dependent vector correlations could be determined. The angular scattering dynamics with species other than He are found to be very similar, dominated by backward scattering which accompanies transfer of energy between rotation and translation. The kinematics of collisions with He are not conducive to the determination of differential scattering and angular momentum polarization correlations. Angular momentum correlations show interesting differences between reactive and non-reactive colliders. We propose that this reflects differences in the potential energy surfaces, in particular, the nature and depth of attractive potential wells.     

Characteristics of high power diode laser removal of multilayer chlorinated rubber coatings from concrete surfaces

This paper reports the technical feasibility and process characteristics of removing chlorinated rubber (CR) coatings from concrete surfaces utilising a 60 W continuous wave (cw) diode laser operating at 810 nm wavelength. Coating layers of various thickness have been removed under an oxygen shroud-gas, as well as Ar and N₂. Optical microscopy and energy dispersive analysis of X-rays (EDX) have been utilised to verify this. The reflectivity properties of the CR material from the visible to the near infrared wavelengths, as well as their behaviour under high temperatures have been examined with a normal incidence spectrometer and a differential thermal analysis/thermal gravimetric analysis (DTA/TGA) system. The resulting drop in reflectivity explains the possibility of sustaining the combustion, even though the reflection coefficient of white CR at 810 nm is almost 100%.     

二极管泵浦无机液体激光器出光实验研究

 为探索新的高能激光体系，搭建了二极管泵浦的液体激光器。采用激光二极管作为泵浦光源，单侧泵浦掺钕离子的无机激光液体，进行了出光实验。通过测量输出光束的近场分布、脉冲波形和光谱，证实实现了激光输出，输出激光的波长为1 053 nm。输出的单脉冲激光能量达到47 mJ，光-光转换效率达到14%。其光-光转换效率高出闪光灯泵浦液体条件下2个数量级，说明该激光体系具有向高能激光体系发展的前景。     

Chemical speciation by sequential injection analysis: an overview

The simplicity of the sequential injection (SIA) manifold and its low need for maintenance makes it an ideal tool in speciation. As miniaturization and reduction of reagent consumption are also ultimate goals in chemical sensing, it is useful to review the use of combined injection and programmed flow as a central issue in designing SIA systems with chemical sensors and structurally simplified chemical analysers. This overview gives an insight into the current state, analytical scope and performance characteristics of sequential injection systems as analytical tools for speciation. The suitability of SIA for speciation analysis is illustrated by the methods used in the conduits of sequential injection systems for the chemical conversion of different chemical forms into detectable chemical species. Configurations of the basic sequential injection speciation analysis systems were designed around a multi-syringe-time-based-injection system with one detector, direct and indirect speciation of different forms using a single detector including diode array detection and direct speciation of different forms using multiple detection.

Examples showing the use of SIA for the simultaneous determination or speciation of metal ions, inorganic anions and organic compounds are given with some recent results from our research groups.