Assessment of the critical factors affecting the porosity of roller compacted ribbons and the feasibility of using NIR chemical imaging to evaluate the porosity distribution
“…The spectral baseline increased as the roll pressure was increased. These results confirm that NIR spectroscopy detects the physical changes in the ribbons when the roll pressure changes, as described by previous studies (11)(12)(13)(14)(15). The fact that the ribbons were composed of only one material (MCC 200) means that spectral changes are the result of physical changes and not chemical changes.…”
Section: Spectra Variation Dependencesupporting
confidence: 90%
“…The density variations in roller compacts have been recently investigated with ultrasonic testing and X-ray tomography (10). A recent study demonstrates the density distribution along the ribbon by analyzing off-line images of MCC ribbons obtained via near-infrared (NIR) chemical imaging (11). This technique relates the intensity of the pixels with the porosity of the ribbon via a calibration method.…”
Abstract. Three different approaches have been evaluated for monitoring ribbon density through realtime near-infrared spectroscopy measurements. The roll compactor was operated to produce microcrystalline cellulose (MCC) ribbons of varying densities. The first approach used the slope of the spectra which showed a variation through the ribbon that could be attributed to density. A second qualitative approach was also developed with a principal component analysis (PCA) model with spectra taken in-line during the production of ribbons in an ideal roll pressure range. The PCA (i.e., real-time) density scans show that the model was able to qualitatively capture the density responses resulting from variation in process parameters. The third approach involved multivariate partial least squares (PLS) calibration models developed at wavelength regions of 1,120-1,310 and 1,305-2,205 nm. Also, various PLS models were developed using three reference methods: caliper, pycnometer, and in-line laser. The third approach shows a quantitative difference between the model-predicted and the measured densities. Models developed at high-wavelength region showed highest accuracy compared with models at low-wavelength region. All the PLS models showed a high accuracy along the spectra collected throughout the production of the ribbons. The three methods showed applicability to process control monitoring by describing the changes in density during in-line sampling.
“…The spectral baseline increased as the roll pressure was increased. These results confirm that NIR spectroscopy detects the physical changes in the ribbons when the roll pressure changes, as described by previous studies (11)(12)(13)(14)(15). The fact that the ribbons were composed of only one material (MCC 200) means that spectral changes are the result of physical changes and not chemical changes.…”
Section: Spectra Variation Dependencesupporting
confidence: 90%
“…The density variations in roller compacts have been recently investigated with ultrasonic testing and X-ray tomography (10). A recent study demonstrates the density distribution along the ribbon by analyzing off-line images of MCC ribbons obtained via near-infrared (NIR) chemical imaging (11). This technique relates the intensity of the pixels with the porosity of the ribbon via a calibration method.…”
Abstract. Three different approaches have been evaluated for monitoring ribbon density through realtime near-infrared spectroscopy measurements. The roll compactor was operated to produce microcrystalline cellulose (MCC) ribbons of varying densities. The first approach used the slope of the spectra which showed a variation through the ribbon that could be attributed to density. A second qualitative approach was also developed with a principal component analysis (PCA) model with spectra taken in-line during the production of ribbons in an ideal roll pressure range. The PCA (i.e., real-time) density scans show that the model was able to qualitatively capture the density responses resulting from variation in process parameters. The third approach involved multivariate partial least squares (PLS) calibration models developed at wavelength regions of 1,120-1,310 and 1,305-2,205 nm. Also, various PLS models were developed using three reference methods: caliper, pycnometer, and in-line laser. The third approach shows a quantitative difference between the model-predicted and the measured densities. Models developed at high-wavelength region showed highest accuracy compared with models at low-wavelength region. All the PLS models showed a high accuracy along the spectra collected throughout the production of the ribbons. The three methods showed applicability to process control monitoring by describing the changes in density during in-line sampling.
“…It is well known that increasing in roll pressure produces ribbons with higher tensile strength due to higher degree of material consolidation in the nip region; when these ribbons were milled, the granule size was larger compare to ribbons produced at a lower roll pressure (40). Also, the granule size increased when MgSt-M was replaced with MgSt-D.…”
Abstract. Qualitative risk assessment methods are often used as the first step to determining design space boundaries; however, quantitative assessments of risk with respect to the design space, i.e., calculating the probability of failure for a given severity, are needed to fully characterize design space boundaries. Quantitative risk assessment methods in design and operational spaces are a significant aid to evaluating proposed design space boundaries. The goal of this paper is to demonstrate a relatively simple strategy for design space definition using a simplified Bayesian Monte Carlo simulation. This paper builds on a previous paper that used failure mode and effects analysis (FMEA) qualitative risk assessment and Plackett-Burman design of experiments to identity the critical quality attributes. The results show that the sequential use of qualitative and quantitative risk assessments can focus the design of experiments on a reduced set of critical material and process parameters that determine a robust design space under conditions of limited laboratory experimentation. This approach provides a strategy by which the degree of risk associated with each known parameter can be calculated and allocates resources in a manner that manages risk to an acceptable level.
“…The difference between the distance advanced by the plunger with and without the particle will be transmitted into a signal to calculate the envelope volume of the particle. The GeoPyc® 1360 pycnometer has been used by several researchers for the determination of envelope density of ribbed roller compacted flakes (21,24).…”
Abstract. This study assessed the utility of near-infrared (NIR) spectroscopy for the real-time monitoring of content uniformity and critical quality attributes (tensile strength, Young's modulus, and relative density) of ribbed roller compacted flakes made by axially corrugated or ribbed rolls. A custom-built setup was used to capture off-line NIR spectra from the flakes containing micronized chlorpheniramine maleate, microcrystalline cellulose, lactose, and magnesium stearate. The partial least square regression method was employed to build calibration models from these off-line NIR spectra using experimental design and validated using test set validation. During calibration model development, various factors, such as spectral acquisition mode, probe positioning, spectral preprocessing method, and beam size, were investigated to improve the prediction ability of the models. The statistical results obtained for calibration models and their validation revealed that dynamic spectral acquisition and proper probe positioning were very crucial to minimize the incorporation of variability in NIR spectra resulting from the flake's undulation. Calibration and validation statistics also suggested the importance of selecting appropriate spectral preprocessing method and beam size. In this study, best calibration models resulted from standard normal variate followed by first derivative preprocessed dynamic spectra captured using beam sizẽ 1.2 mm. Best calibration models constructed from off-line NIR spectra were used in real-time analysis of flake attributes. Finally, adequacy of best calibration models was established from real-time prediction results. Overall, with the proposed setup, it was possible to monitor the roller compaction process in real time for various properties associated with the ribbed flakes in a rapid, efficient, and nondestructive manner.
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