On-line quality control in polymer processing using hyperspectral imaging

L’industrie du plastique se tourne de plus en plus vers les matériaux composites afin d’économiser de la matière et/ou d’utiliser des matières premières à moindres coûts, tout en conservant de bonnes propriétés. L’impressionnante adaptabilité des matériaux composites provient du fait que le manufacturier peut modifier le choix des matériaux utilisés, la proportion selon laquelle ils sont mélangés, ainsi que la méthode de mise en œuvre utilisée. La principale difficulté associée au développement de ces matériaux est l’hétérogénéité de composition ou de structure, qui entraîne généralement des défaillances mécaniques. La qualité des prototypes est normalement mesurée en laboratoire, à partir de tests destructifs et de méthodes nécessitant la préparation des échantillons. La mesure en-ligne de la qualité permettrait une rétroaction quasi-immédiate sur les conditions d’opération des équipements, en plus d’être directement utilisable pour le contrôle de la qualité dans une situation de production industrielle. L’objectif de la recherche proposée consiste à développer un outil de contrôle de qualité pour la qualité des matériaux plastiques de tout genre. Quelques sondes de type proche infrarouge ou ultrasons existent présentement pour la mesure de la composition en-ligne, mais celles-ci ne fournissent qu’une valeur ponctuelle à chaque acquisition. Ce type de méthode est donc mal adapté pour identifier la distribution des caractéristiques de surface de la pièce (i.e. homogénéité, orientation, dispersion). Afin d’atteindre cet objectif, un système d’imagerie hyperspectrale est proposé. À l’aide de cet appareil, il est possible de balayer la surface de la pièce et d’obtenir une image hyperspectrale, c’est-à-dire une image formée de l’intensité lumineuse à des centaines de longueurs d’onde et ce, pour chaque pixel de l’image. L’application de méthodes chimiométriques permettent ensuite d’extraire les caractéristiques spatiales et spectrales de l’échantillon présentes dans ces images. Finalement, les méthodes de régression multivariée permettent d’établir un modèle liant les caractéristiques identifiées aux propriétés de la pièce. La construction d’un modèle mathématique forme donc l’outil d’analyse en-ligne de la qualité des pièces qui peut également prédire et optimiser les conditions de fabrication.The use of plastic composite materials has been increasing in recent years in order to reduce the amount of material used and/or use more economic materials, all of which without compromising the properties. The impressive adaptability of these composite materials comes from the fact that the manufacturer can choose the raw materials, the proportion in which they are blended as well as the processing conditions. However, these materials tend to suffer from heterogeneous compositions and structures, which lead to mechanical weaknesses. Product quality is generally measured in the laboratory, using destructive tests often requiring extensive sample preparation. On-line quality control would allow near-immediate feedback on the operating conditions and may be transferrable to an industrial production context. The proposed research consists of developing an on-line quality control tool adaptable to plastic materials of all types. A number of infrared and ultrasound probes presently exist for on-line composition estimation, but only provide single-point values at each acquisition. These methods are therefore less adapted for identifying the spatial distribution of a sample’s surface characteristics (e.g. homogeneity, orientation, dispersion). In order to achieve this objective, a hyperspectral imaging system is proposed. Using this tool, it is possible to scan the surface of a sample and obtain a hyperspectral image, that is to say an image in which each pixel captures the light intensity at hundreds of wavelengths. Chemometrics methods can then be applied to this image in order to extract the relevant spatial and spectral features. Finally, multivariate regression methods are used to build a model between these features and the properties of the sample. This mathematical model forms the backbone of an on-line quality assessment tool used to predict and optimize the operating conditions under which the samples are processed

A multivariate data analysis approach to tablet sticking on an industrial scale: a qualitative case study of an ibuprofen-based formulation

Abstract: Objectives: Sticking is one of the most common and damaging issues that occur during tablet manufactur- ing. Sticking is the adhesion of powder onto tooling surfaces during compression. Because of the numerous factors involved in its occurrence, understanding tablet sticking requires the simultaneous investigation of these factors to clarify their possible interactions. However, conducting such a study experimentally can pre- sent a significant financial and technical burden. In this study, we aimed to leverage the large amount of data that is usually generated during industrial manufacturing to gain insights into sticking. Methods: This was achieved by collecting and analyzing a total of 71 historical batches that used an ibu- profen-based formulation. We associate each batch with a hundred parameters, including a qualitative descriptor of sticking, and employ a predefined methodology based primarily on multivariate data analysis. Results and Conclusions: Our results highlight the role of lubrication, water content, and the low melt- ing point of ibuprofen in its sticking tendency. Based on these findings, we propose and discuss an indus- trial manufacturing data analysis approach to sticking and its associated systematic methodology, consisting of collection, exploration, and data modeling

Insights into tablet sticking: a quantitative case study with an ibuprofen and methocarbamol-based formulation

Abstract: Objectives and Methods: Tablet sticking is a continuous accumulation of pharmaceutical powder onto tooling surfaces during compression. Its occurrence greatly impacts tablet productivity, quality attributes, and tooling age. In a previous study, the authors proposed a multivariate data analysis approach to gain insights into tablet sticking directly on the industrial stage. The objective was to determine the combin- ation of factors that could help distinguish between batches affected and unaffected by sticking. The pre- sent study aims to generalize this approach by extending it to quantitative predictions of punch sticking intensity. A total of 345 variables was gathered on 28 industrial batches of an ibuprofen and methocarba- mol-based formulation. Result and Conclusion: Using PLS regression models, it was shown that the association of granulation duration and compression force allows to significantly explain 60% of sticking variations of studied for- mulation. In addition, unlike the classification models developed in the earlier work, the validation resi- dues in the present study were found to be normally distributed (Shapiro–Wilks p value = 0.96) and independent from the target variable (R2 = 9.5%)

Injection de mousses composites bois/plastiques d'origine post-consommation

Dans cette étude, des matériaux composites bois/plastiques moussés ont été produits par une méthode de moulage par injection. En particulier, les composites sont constitués de fibres de bois et d'une matrice de polyoléfines recyclées (mélange de HDPE et PP). La décomposition thermique de l'azodicarbonamide (ACA), un agent gonflant chimique, fournit le gaz nécessaire à la formation de la mousse microcellulaire. Afin d'étudier ces composites, nous avons varié la concentration de bois, la température du moule ainsi que la teneur en agent gonflant. La caractérisation microscopique des échantillons comprend l'analyse de la structure cellulaire, de l'épaisseur de peau ainsi que de la morphologie des fibres. Les résultats montrent que la température du moule et la teneur en agent gonflant ont très peu d'influence sur la morphologie cellulaire à l'intérieur de la plage de valeurs étudiées. Par ailleurs, l'augmentation de la teneur en fibres augmente le diamètre cellulaire à cause de la nature de l'interface bois/plastiques. Enfin, les tests mécaniques en flexion, torsion, impact et traction ont pour but de caractériser l'effet du bois et du moussage sur ces matériaux tout en liant les propriétés mécaniques aux analyses microscopiques. On observe que les propriétés des échantillons sont supérieures en présence de fibres de bois mais légèrement inférieures lorsque moussés

Optimization of a landfill gas collection shutdown based on an adapted first-order decay model

Abstract: LandGEM’s equation was reformulated to include two types of refuse, fast decaying refuse (FDR) and slow decaying refuse (SDR), whose fractions and key modeling parameters k and L0 were optimized independently for three periods in the life of the Montreal-CESM landfill. Three scenarios were analyzed and compared to actual biogas collection data: (1) Two-Variable Scenario, where k and L0 were optimized for a single type of refuse; (2) Six-Variable Scenario, where three sets of k and L0 were optimized for the three periods and for a single type of refuse; and (3) Seven-Variable Scenario, whereby optimization was performed for two sets of k and L0, one associated with FDR and the second with SDR, and for the fraction of FDR during each of the three periods. Results showed that the lowest error from the error minimization technique was obtained with the Six-Variable Scenario. However, this scenario’s estimation of gas generation was found to be rather unlikely. The Seven-Variable Scenario, which allowed for considerations about changes in landfilling trends, offered a more reliable prediction tool for landfill gas generation and optimal shutdown time of the biogas collection system, when the minimum technological threshold would be attained. The methodology could potentially be applied mutatis mutandis to other landfills, by considering their specific waste disposal and gas collection histories

Monitoring the concentration of flowing pharmaceutical powders in a tableting feed frame

Abstract: The use of process analytical technology (PAT) tools is increasing steadily in the pharmaceutical industry. Such tools are now located throughout the process. When producing tablets, the tableting step itself may be the ideal moment to assess final product composition. Being the last unit operation in tablet production where the elements are still free flowing, it is relatively straightforward to ascertain the composition of the blend in real time. However, a single probe cannot be expected to monitor the composition of every component of a multicomponent blend. In this study, three PAT tools (light-induced fluorescence spectroscopy, near-infrared spectroscopy and color (RGB) imaging) simultaneously checked the composition of powder blends flowing through the feeding unit (feed frame) of a tablet press. The results demonstrate the potential of these tools in monitoring changes in the concentration of a multicomponent mixture in real time, providing users with means to both scrutinize the process and better understand phenomena occurring inside the feed frame

Specificity of process analytical tools in the monitoring of multicomponent pharmaceutical powders

Abstract: The application of Process Analytical Technologies in pharmaceutical manufacturing has been the subject of many studies. Active pharmaceutical ingredient monitoring in real time through- out the manufacturing process is commonly the target of many such implementations. The tools in place must be sensitive to, and selective of, the parameter(s) to be monitored, i.e. in the case of component quantification, they must respond to the component in question and be robust against all others. In this study, four different ingredients (riboflavin, ferrous fumarate, ginseng, and ascorbic acid) in a multi-component blend were monitored by three different tools (near infrared spectroscopy, laser-induced fluorescence and red-green-blue camera) using a full factor- ial design. The goal was to develop efficient and robust concentration-reading/prediction models able to assess and monitor component interference. Despite relatively high complexity of the blend studied, the three tools demonstrated reasonable specificity for the tracked ingredients (and showed advantages when combined), taking into account larger acceptance criteria typical of dietary products. In certain cases, some interference might lead to biased predictions, high- lighting the importance of good calibration. The tools tested and the methodology proposed has divulged their potential in monitoring these components, despite the complexity of the 31- component blend

Developing a quality by design approach to model tablet dissolution testing: an industrial case study

Abstract: This study applied the concept of Quality by Design (QbD) to tablet dissolution. Its goal was to propose a quality control strategy to model dissolution testing of solid oral dose products according to International Conference on Harmonization guidelines. The methodology involved the following three steps: (1) a risk analysis to identify the material- and process-related parameters impacting the critical quality attributes of dissolution testing, (2) an experimental design to evaluate the influence of design factors (attributes and parameters selected by risk analysis) on dissolution testing, and (3) an investigation of the relationship between design factors and dissolution profiles. Results show that (a) in the case studied, the two parameters impacting dissolution kinetics are active pharmaceutical ingredient particle size distributions and tablet hardness and (b) these two parameters could be monitored with PAT tools to predict dissolution profiles. Moreover, based on the results obtained, modeling dissolution is possible. The practicality and effectiveness of the QbD approach were demonstrated through this industrial case study. Implementing such an approach systematically in industrial pharmaceutical production would reduce the need for tablet dissolution testing

Pharmaceutical tablet compression: measuring temporal and radial concentration profiles to better assess segregation

Abstract: Concentration monitoring inside a tablet press feed frame is important not only to assess the composition of the powder blend compressed into tablets but also to detect quality affecting phenomena such as powder segregation. Near infrared spectroscopy has been successfully used to monitor powder concentration inside the feed frame; however, so far, this methodology does not provide information on local spatial variability, since it probes a very small area of powder sample. Near infrared chemical imaging (NIR CI) has the potential to improve process monitoring because it can simultaneously acquire a plurality of spectra covering nearly the entire width of the feed frame, thereby making it possible to detect local variations in powder concentration. The present work uses both NIRS and NIR CI to monitor the concentration of Ibuprofen and Ascorbic acid in multi-component mock pharmaceutical blends flowing through the feed frame of an industrial tablet press. The concentrations of Ibuprofen and Ascorbic acid were successfully monitored in multi-component powder blends. NIR spectral wavelength ranges and pre-treatments were simultaneously optimized via a genetic algorithm. N-way PLS approach for concentration monitoring was found to be more suitable than regular PLS when analyzing spectral images and provided the ability to visualize spatial segregation

Acute changes in peritoneal morphology and transport properties with infectious peritonitis and mechanical injury

Acute changes in peritoneal morphology and transport properties with infectious peritonitis and mechanical injury. Peritoneal clearance studies were performed in rats undergoing acute peritoneal dialysis. Some of these animals were then exposed to laparotomy and mechanical drying of the peritoneum. Peritoneal clearance studies were repeated at intervals up to 11 days. Another group of rats was placed on daily peritoneal dialysis and allowed to spontaneously develop peritonitis which was not treated. These rats underwent peritoneal transport studies at differing durations of infection. In all groups, animals were sacrificed at the time of the last transport studies for morphological assessment of the peritoneum by light microscopy, scanning electron microscopy, and transmission electron microscopy. The results showed similar decreases in drainage volume and increases in glucose absorption and protein losses with both infection and drying. Both types of injury resulted in extensive mesothelial structural changes. While drying caused mainly denudation of the mesothelial surface, infectious peritonitis was associated with separation of mesothelial cells, and the appearance of numerous white blood cells between and on mesothelial cells. Exposure to peritoneal dialysis alone had no obvious effects on anatomy. Although changes in the peritoneal microcirculation and deeper structures cannot be excluded as contributing to peritoneal transport alterations, the findings suggest that alterations of mesothelium might explain some of the changes in peritoneal transport properties under the conditions of these studies.Modifications aiguës de la morphologie et des propriétés de transport du péritoine par péritonite infectieuse et lésion mécanique. Des études de clearance péritonéale ont été entreprises chez des rats en dialyse péritonéale aiguë. Certains de ces animaux étaient soumis à une laparotomie et à un séchage mécanique du péritoine. Les études de clearance péritonéale étaient répétées à des intervalles allant jusqu'à 11 jours. Un autre groupe de rat était placé en dialyse péritonéale journalière, et il pouvait développer spontanément une péritonite qui n'était pas traitée. Chez ces rats ont été effectuées des études de transport péritonéal à différents stades d'infection. Dans tous les groupes, les animaux étaient sacrifiés lors de la dernière étude de transport afin d'étudier morphologiquement le péritoine par microscopie optique, microscopie électronique à balayage, et microscopie électronique par transmission. Les résultats ont montré des diminutions du volume de drainage et des augmentations de l'absorption du glucose et des pertes protéiques identiques avec l'infection ou le séchage. Les deux types de lésions ont entrainé des modifications structurelles mésothéliales importantes. Tandis que le séchage entrainait principalement une dénudation de la surface mésothéliale, la péritonite infectieuse était associée à une séparation des cellules mésothéliales, et à l'apparition de nombreux globules blancs entre et sur les cellules mésothéliales. L'exposition à la dialyse péritonéale seule n'avait pas d'effets anatomiques évidents. Bien que la contribution aux altérations du transport péritonéal de modifications de la micro-circulation péritonéale et des structures plus profondes ne puisse être exclue, ces résultats suggèrent que les altérations du mésothélium pourraient expliquer certaines des modifications des propriétés de transport péritonéal dans les conditions de ces études