Vibrational Spectroscopic and Ultrasound Analysis for In-Process Characterization of High-Density Polyethylene/Polypropylene Blends during Melt Extrusion

Barnes, Susan E.; Brown, Edward A.; Sibley, M. G.; Edwards, Howell G. M.; Scowen, Ian J.; Coates, Phil

doi:10.1366/0003702053946001

Cited by 40 publications

(15 citation statements)

References 23 publications

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“…Spectroscopic, ultrasonic and X-ray scattering techniques have proven invaluable to monitor structure development, composition and material properties during processing [17][18][19][20][21][22].…”

Section: Introductionmentioning

confidence: 99%

Effect of processing parameters on the morphology development during extrusion of polyethylene tape: An in-line small-angle X-ray scattering (SAXS) study

Heeley

Gough

Hughes

et al. 2013

Polymer

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Ray scattering (SAXS). AbstractThe in-line development of crystalline morphology and orientation during melt extrusion of low density polyethylene (LDPE) tape at nil and low haul-off speeds has been investigated using Small-Angle X-Ray Scattering (SAXS). The processing parameters, namely haul-off speed and distance down the tape-line have been varied and the resulting crystalline morphology is described from detailed analysis of the SAXS data. Increasing haul-off speed increased orientation in the polymer tape and the resulting morphology could be described in terms of regular lamellar stacking perpendicular to the elongation direction. In contrast, under nil haul-off conditions the tape still showed some orientation down the tape-line, but a shish-kebab structure prevails. The final lamellae thickness (~50 Å) and bulk crystallinity (~20%), were low for all processing conditions investigated, which is attributed to the significant shortchain branching in the polymer acting as point defects limiting lamellae crystal growth.2

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Section: Introductionmentioning

confidence: 99%

Effect of processing parameters on the morphology development during extrusion of polyethylene tape: An in-line small-angle X-ray scattering (SAXS) study

Heeley

Gough

Hughes

et al. 2013

Polymer

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“…NIR spectroscopy has been applied in-line and in the transmission mode during single screw hot-melt extrusion to monitor the HDPE/PP [16,17] and LDPE/PP [18] polymer melt composition in the extrusion die. Further, NIR spectroscopy has been used to monitor the ethylene vinylacetate copolymer composition in the extrusion die during single screw extrusion [19][20][21] , and for the quantification of the copolymer composition in a polypropylene and ethylene vinyl acetate blend [22] during twin screw extrusion.…”

Section: Introductionmentioning

confidence: 99%

In-line NIR spectroscopy for the understanding of polymer–drug interaction during pharmaceutical hot-melt extrusion

Saerens

Dierickx

Quinten

et al. 2012

European Journal of Pharmaceutics and Biopharmaceutics

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The aim was to evaluate near-infrared spectroscopy for the in-line determination of the drug concentration, the polymer-drug solid-state behaviour and molecular interactions during hot-melt extrusion.Kollidon ® SR was extruded with varying metoprolol tartrate (MPT) concentrations (20, 30, and 40%) and monitored using NIR spectroscopy. A PLS model allowed drug concentration determination. The correlation between predicted and real MPT concentrations was good (R²=0.97). The predictive performance of the model was evaluated by the root mean square error of prediction, which was 1.54%. Kollidon®SR with 40% MPT was extruded at 105°C and 135°C to evaluate NIR spectroscopy for in-line polymer-drug solid state characterization.NIR spectra indicated the presence of amorphous MPT and hydrogen bonds between drug and polymer in the extrudates. More amorphous MPT and interactions could be found in the extrudates produced at 135°C than at 105°C. Raman spectroscopy, DSC and ATR FT-IR were used to confirm the NIR observations. Due to the instability of the formulation, only in-line Raman spectroscopy was an adequate confirmation tool. NIR spectroscopy is a potential PAT-tool for the in-line determination of API-concentration and for the polymer-drug solid state behaviour monitoring during pharmaceutical hot-melt extrusion.

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“…Raman spectroscopy enables rapid, non-destructive and in-line measurements, and has previously been used during hot-melt extrusion (single screw extrusion) to monitor EVA copolymer melt composition [7,8] , to analyze film formulations [9] , and to monitor the composition of a series of highdensity polyethylene (HDPE)/polypropylene (PP) blends [10,11] . It has also been implemented in a twin screw extrusion process to determine the concentration of Irganox additive in polypropylene [12] .…”

Section: Introductionmentioning

confidence: 99%

Raman spectroscopy for the in-line polymer–drug quantification and solid state characterization during a pharmaceutical hot-melt extrusion process

Saerens

Dierickx

Lenain³

et al. 2011

European Journal of Pharmaceutics and Biopharmaceutics

136

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The aim of this study was to evaluate the suitability of Raman spectroscopy as a Process Analytical Technology (PAT) tool for the in-line determination of the active pharmaceutical ingredient (API) concentration and the polymer-drug solid state during a pharmaceutical hot-melt extrusion process. For in-line API quantification, different metoprolol tartrate (MPT) -Eudragit ® RL PO mixtures, containing 10, 20, 30, and 40% MPT respectively, were extruded and monitored in-line in the die using Raman spectroscopy. A PLS model, regressing the MPT concentrations versus the in-line collected Raman spectra, was developed and validated, allowing real-time API concentration determination. The correlation between the predicted and real MPT concentrations of the validation samples is acceptable (R²=0.997) The predictive performance of the calibration model is rated by the root mean square error of prediction (RMSEP), which is 0.59%. Two different polymer-drug mixtures were prepared to evaluate the suitability of Raman spectroscopy for in-line polymer-drug solid state characterization. Mixture 1 contained 90% Eudragit ® RS PO and 10% MPT, and was extruded at 140°C, hence producing a solid solution. Mixture 2 contained 60% Eudragit ® RS PO and 40% MPT, and was extruded at 105°C, prod ucing a solid dispersion. The Raman spectra collected during these extrusion processes provided two main observations. First, the MPT Raman peaks in the solid solution broadened compared to the corresponding solid dispersion peaks, indicating the presence of amorphous MPT. Secondly, peak shifts appeared in the spectra of the solid dispersion and solid solution compared to the physical mixtures, suggesting interactions between Eudragit ® RS PO and MPT, most likely hydrogen bonds. These shifts were larger in the spectra of the solid solution. DSC analysis confirmed these Raman solid state observations and the interactions seen in the spectra. Raman spectroscopy is a potential PAT-tool for in-line determination of the API-concentration and the polymer-drug solid state during pharmaceutical hot-melt extrusion.

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Vibrational Spectroscopic and Ultrasound Analysis for In-Process Characterization of High-Density Polyethylene/Polypropylene Blends during Melt Extrusion

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Cited by 40 publications

References 23 publications

Effect of processing parameters on the morphology development during extrusion of polyethylene tape: An in-line small-angle X-ray scattering (SAXS) study

Effect of processing parameters on the morphology development during extrusion of polyethylene tape: An in-line small-angle X-ray scattering (SAXS) study

In-line NIR spectroscopy for the understanding of polymer–drug interaction during pharmaceutical hot-melt extrusion

Raman spectroscopy for the in-line polymer–drug quantification and solid state characterization during a pharmaceutical hot-melt extrusion process

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