Effect of speed, loading and spray pattern on coating variability in a pan coater

A computational study using the discrete element method was performed to study the effect of pan speed, fill level and the design of the spray pattern on the coating variability of tablets coated in a rotating pan. The method simulates the movement of tablets in the pan and calculates the residence time of each tablet inside the spray zone, which is directly related to the amount of coating received by the tablet. The computational method was experimentally validated using a Laser Induced Breakdown Spectroscopy based analytical method. The simulations showed that the axial mixing was the most critical parameter affecting the coating variability. Although axial mixing was found to be better at higher pan speed, it did not affect the coating variability significantly. Lower variability was obtained when a 100% fill level was used as compared to 67% fill. Four spray patterns were used, two idealized (full surface spray and a symmetric band spray) and two realistic (5-ellipse and 5-circular spray guns). The full and band spray showed similar results while the ellipse and circular patterns were similar to each other (and much worse than the other two patterns) at all speeds and fill levels.     

Development of a fiber-coupled laser-induced breakdown spectroscopy instrument for analysis of underwater debris in a nuclear reactor core

To inspect the post-accident nuclear core reactor of the TEPCO Fukushima Daiichi nuclear power plant (F1-NPP), a transportable fiber-coupled laser-induced breakdown spectroscopy (LIBS) instrument has been developed. The developed LIBS instrument was designed to analyze underwater samples in a high-radiation field by single-pulse breakdown with gas flow or double-pulse breakdown. To check the feasibility of the assembled fiber-coupled LIBS instrument for the analysis of debris material (mixture of the fuel core, fuel cladding, construction material and so on) in the F1-NPP, we investigated the influence of the radiation dose on the optical transmittance of the laser delivery fiber, compared data quality among various LIBS techniques for an underwater sample and studied the feasibility of the fiber-coupled LIBS system in an analysis of the underwater sample of the simulated debris in F1-NPP. In a feasible study conducted by using simulated debris, which was a mixture of CeO₂ (surrogate of UO₂), ZrO₂ and Fe, we selected atomic lines suitable for the analysis of materials, and prepared calibration curves for the component elements. The feasible study has guaranteed that the developed fiber-coupled LIBS system is applicable for analyzing the debris materials in the F1-NPP.     

Diagnostics of First Wall Materials in Device by Polarization-Resolved a Magnetically Confined Fusion Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy （LIBS） is a powerful analytical tool for real- time diagnostics and detection of multiple elements deposited at the first wall of magnetically confined plasma ft~sion devices. Recently, we have tested LIBS in our laboratory for application to in situ real-time diagnostics in the fusion device EAST. In this study, we applied polarization- resolved LIBS （PR-LIBS） to reduce the background continuum and enhance the resolution and sensitivity of LIBS. We used aluminium （A1） （as a substitute for Be） and the first wall materials tungsten （W） and molybdenum （Mo） to investigate polarized continuum emission and signal-to- background ratio （SBR）. A Nd：YAG laser with first, second and third harmonics was used to produce plasma. The effects of the laser polarization plane, environmental pressure and polarizer detection angle were investigated. The spectra obtained without using a polarizer （i.e. LIBS） were compared with those obtained with a polarizer （PR-LIBS）. Distribution of emission spectral intensity was observed to follow Malus＇ law with respect to variation in the angle of detection of the polarizer. The spectra obtained by PR-LIBS had a higher SBR and greater stability than those obtained by LIBS, thereby enhancing the reliability of LIBS for quantitative analyses. A comparison of A1, Mo and W showed that W exhibited a higher continuum with stronger polarization than the low-Z elements.     

Elemental and proximate analysis of coal by x-ray fluorescence assisted laser-induced breakdown spectroscopy

Although laser-induced breakdown spectroscopy (LIBS), as a fast on-line analysis technology, has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants, the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present. In this paper, we propose a novel x-ray fluorescence (XRF) assisted LIBS method for high repeatability analysis of coal quality, which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal, but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements. With the combination of elemental lines in LIBS and XRF spectra, the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal. Quantitative analysis results show that the relative standard deviation (RSD) of C is 0.15%, the RSDs of other elements are less than 4%, and the standard deviations of calorific value, ash content, sulfur content and volatile matter are 0.11 MJ kg−1, 0.17%, 0.79% and 0.41% respectively, indicating that the method has good repeatability in determination of coal quality. This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.     

Quantitative analysis of C,Si, Mn,Ni, Cr and Cu in low-alloy steel under ambient conditions via laser-induced breakdown spectroscopy

A diode-pumped solid-state laser(DPSSL) with a high energetic stability and long service life is applied to ablate the steel samples instead of traditional Nd:YAG laser pumped by a xenon lamp,and several factors, such as laser pulse energy, repetition rate and argon flow rate, that influence laser-induced breakdown spectroscopy(LIBS) analytical performance are investigated in detail.Under the optimal experiment conditions, the relative standard deviations for C, Si, Mn, Ni, Cr and Cu are 3.3%–8.9%, 0.9%–2.8%, 1.2%–4.1%, 1.7%–3.0%, 1.1%–3.4% and 2.5%–8.5%,respectively, with the corresponding relative errors of 1.1%–7.9%, 1.0%–6.3%, 0.4%–3.9%,1.5%–6.3%, 1.2%–4.0% and 1.2%–6.4%. Compared with the results of the traditional spark discharge optical emission spectrometry technique, the analytical performance of LIBS is just a little inferior due to the less stable laser-induced plasma and smaller amount of ablated sample by the laser. However, the precision, detection limits and accuracy of LIBS obtained in our present work were sufficient to meet the requirements for process analysis. These technical performances of higher stability of output energy and longer service life for DPSSL, in comparison to the Q-switch laser pumped by xeon lamp, qualify it well for the real time online analysis for different industrial applications.     

Experimental investigation of atomic and ionic titanium lines,diatomic TiOγ transition and continuum background radiation via magnetically confined LIBS

This paper is focused on the clarification of the behaviour of various atomic, ionic, and TiO_γ (A³Φ – X³Δ, Δν =0) diatomic transition lines as well as the continuum radiations in laser-induced titanium plasma plume by a pair of NdFeB. Depending on their different amount of impressionability from applied fields and electron-impact excitation rate, the responses of each component in optical emission spectrum and background continuum radiation to different applied magnetic field strengths (~ 0.42–1.12 T) are significantly different. At magnetic fields of 0.98 and 1.12 T, the amount of impressionability for Ti i: 388.2 nm is higher than others, while for TiO_γ molecular transitions, the amount of impressionability factor in a 0.98 T field strength is considerable, because in the first moments after the laser pulse the continuum radiation is dominant, by applying an external magnetic field, this amount of radiation be reduced. The temporal evolution of the optical emission lines shows that choosing a suitable time delay and gate width has a considerable role in further impressionability of externally applied field in case of different elements. The electron density N_e varied from 0.99×10¹⁷ to 11.53×10¹⁷ cm⁻³, and the plasma temperature T_e, was obtained in a range of 4835–16818 K by employing maximum applied field of 1.12 T. The supplementary investigations will be conducted towards further improvements of the purposeful analysis of each component in confined plasma by magneto-LIBS technique in order to find new approaches in the field of magnetic confinement.     

Effect of Melting Iron-Based Alloy Temperature on Carbon Content Observed in Laser-Induced Breakdown Spectroscopy

Our recent work has determined the carbon content in a melting ferroalloy by laser-induced breakdown spectroscopy (LIBS). The emission spectrum of carbon that we obtained in the laboratory is suitable for carbon content determination in a melting ferroalloy but we cannot get the expected results when this method is applied in industrial conditions: there is always an unacceptable error of around 4% between the actual value and the measured value. By comparing the measurement condition in the industrial condition with that in the laboratory, the results show that the temperature of the molten ferroalloy samples to be measured is constant under laboratory conditions while it decreases gradually under industrial conditions. However, temperature has a considerable impact on the measurement of carbon content, and this is the reason why there is always an error between the actual value and the measured value. In this paper we compare the errors of carbon content determination at different temperatures to find the optimum reference temperature range which can fit the requirements better in industrial conditions and, hence, make the measurement more accurate. The results of the comparative analyses show that the measured value of the carbon content in molten state (1620 K) is consistent with the nominal value of the solid standard sample (error within 0.7%). In fact, it is the most accurate measurement in the solid state. Based on this, we can effectively improve the accuracy of measurements in laboratory and can provide a reference standard of temperature for the measurement in industrial conditions.     

Parameters Optimization of Laser-Induced Breakdown Spectroscopy Experimental Setup for the Case with Beam Expander

Improvement of measurement precision and repeatability is one of the issues cur?rently faced by the laser-induced breakdown spectroscopy (LIBS) technique, which is expected to be capable of precise and accurate quantitative analysis. It was found that there was great poten?tial to improve the signal quality and repeatability by reducing the laser beam divergence angle using a suitable beam expander (BE). In the present work, the influences of several experimental parameters for the case with BE are studied in order to optimize the analytical performances: the signal to noise ratio (SNR) and the relative standard deviation (RSD). We demonstrate that by selecting the optimal experimental parameters, the BE-included LIBS setup can give higher SNR and lower RSD values of the line intensity normalized by the whole spectrum area. For validation purposes, support vector machine (SVM) regression combined with principal component analysis (PCA) was used to establish a calibration model to realize the quantitative analysis of the ash content. Good agreement has been found between the laboratory measurement results from the LIBS method and those from the traditional method. The measurement accuracy presented here for ash content analysis is estimated to be 0.31%, while the average relative error is 2.36%.     

Nondestructive Determination of Cu Residue in Orange Peel by Laser Induced Breakdown Spectroscopy

Laser induced breakdown spectroscopy(LIBS) is an emerging tool with rapid,nondestructive,green characteristics in qualitative or quantitative analyses of composition in materials.But LIBS has its shortcomings in detect limit and sensitivity.In this work,heavy metal Cu in Gannan Navel Orange,which is one of famous fruits from Jiangxi of China,was analyzed.In view of LIBS's limit,it is difficult to determinate heavy metals in natural fruits.In this work,nine orange samples were pretreated in 50-500 μg/mL Cu solution,respectively.Another one orange sample was chosen as a control group without any pollution treatment.Previous researchers observed that the content of heavy metals is much higher in peel than in pulp.So,the content in pulp can be reflected by detecting peel.The real concentrations of Cu in peels were acquired by atomic absorption spectrophotometer(AAS).A calibration model of Cu I 324.7 and Cu Ⅰ 327.4was constructed between LIBS intensity and AAS concentration by six samples.The correlation coefficient of the two models is also 0.95.All of the samples were used to verify the accuracy of the model.The results show that the relative error(RE) between predicted and real concentration is less than 6.5%,and Cu Ⅰ 324.7 line has smaller RE than Cu Ⅰ 327.4.The analysis demonstrated that different characteristic lines decided different accuracy.The results prove the feasibility of detecting heavy metals in fruits by LIBS.But the results are limited in treated samples.The next work will focus on direct analysis of heavy metals in natural fruits without any pretreatment.This work is helpful to explore the distribution of heavy metals between pulp and peel.     

The Spectral Emission Characteristics of Laser Induced Plasma on Tea Samples

Laser induced breakdown spectroscopy(LIBS) provides a useful technique for food security as well as determining nutrition contents.In this paper,optical emission studies of laser induced plasma on commercial tea samples were carried out.The spectral intensities of Mg,Mn,Ca,Al,C and CN vibration bands varying with laser energy and the detection delay time of an intensified charge coupled device were studied.In addition,the relative concentrations of six microelements,i.e.,Mg,Mn,Ca,Al,Na and K,were analyzed semi-quantitatively as well as H,for four kinds of tea samples.Moreover,the plasma parameters were explored,including electron temperature and electron number density.The electron temperature and electron number density were around 11000 K and 10~(17) cm~(-3),respectively.The results show that it is reasonable to consider the LIBS technique as a new method for analyzing the compositions of tea leaf samples.