Vacuum Compression Molding as sample preparation for thermal analysis of thermoplastic materials.

Transcription

1 Vacuum Compression Molding as sample preparation for thermal analysis of thermoplastic materials. Dr. Daniel Treffer, CEO and Founder STK Annual Meeting, May 15th 2018 Innovation in Thermal Analysis and Calorimetry STK Annual Meeting

2 What is Vacuum Compression Molding? VCM Tool Perfect samples STK Annual Meeting

3 How did it start? - Start with my phd in the field of pharmaceutical engineering at the Institute of Prof. Khinast in September First contact with hot-melt extrusion. Measurement of material properties. Problems 1. Bubbles Kollidon VA64 HPMCAS 2. Degradation 3. Shrinkage e.g. Rheo Data 4. Sticking Soluplus Kollidon VA64 Reproducible measurements are impossible! STK Annual Meeting

4 The light-bulb moment 13. February 2014 The hands on experience of a new material Teflon foil reinforced with glass-fibres STK Annual Meeting

5 Introduction Video STK Annual Meeting

6 What are the innovations? Compaction pressure (vacuum) Movable piston VCM Insert Solidifying #1 Adaptable sample chamber Powder or flakes etc. Geometrically defined sample, no voids or bubbles Front foils #2 Peelable sample chamber STK Annual Meeting

7 VCM Essentials Vacuum Unit 0,1 mbar 1 atm Heating Unit 300 C 25 C Cooling Unit SLOW & FAST STK Annual Meeting

8 Flawless Samples Rotate them STK Annual Meeting

9 Applications Solubility Surface Tension Rheology Diffusion Hardness Notch Impact Strength Density Dynamic Mechanical Analysis Stability Thermal Conductivity Dissolution Heat Capacity Spectroscopy STK Annual Meeting

10 Complex Viscosity (Pas) Rheology (Discs 8-25 mm) Shear Flow Soluplus homogenous with bubbles Conventional Increased accuarcy with VCM Treffer et al Shear Rate (s -1 ) 140 C 150 C 160 C STK Annual Meeting

11 Extensional Viscosity (Pas) Rheology (Bars 10x40 mm) Extensional Flow Homogeneous Soluplus Conventional 25s -1 10s -15s-1 3s -1 1s -1 New insights via VCM Strain Hardening 0.3s s -1 with bubbles early rupture Trouton Ratio Time [s] STK Annual Meeting

12 mdsc Signal DSC Measurements (Discs 5 mm) powder powder too noisy 1st heating VCM sample HPMCAS VCM Troiss et al T G = 145 C DSC crucible 0 Temperature ( C) STK Annual Meeting

13 Heat capacity (J/kgK) Conductivity (W/mK) DSC Measurements (Discs 5 mm) Thermal Conductivity via DSC Soluplus 2 Samples Thicknesses mdsc and Math 0.4 mm 3 mm Troiss (2017) Temperature ( C) STK Annual Meeting

14 Diffusion Rate (µg/day) Formulation Screening (Multilayer Systems) (Discs 5-25mm) IVR e.g. Ø 50 mm $761 m Merck & Co Cross Section Drug loaded core Diffusion Barrier VCM multilayer prototype Co-extruded version Diffusion Barrier Drug Loaded Core 100 µm 4 mm 100 µm Lateral surface sealed with barrier glue. 0 Eder et al Time (days) Diffusion Barrier STK Annual Meeting

15 Intensity (counts) Formulation Screening (ASD Stability) Testing of ASD stability after 1, respectively 4 weeks of storage at accelerated conditions (40 C and 75% RH) via DSC and WAXS VCM prepared from cryo milled blend shows small melting endotherm in first heating 10% API + 90% Eudragit E (4 weeks) 10% API + 90% Eudragit E (1 week) 10% API + 90% Eudragit E Eudragit E 2θ API STK Annual Meeting

16 Released Fenofibrate [%] Released Fenofibrate [%] Formulation Screening (Dissolution Testing) Tablets with defined geometries Order Order Time [min] Time [min] STK Annual Meeting

17 Released Fenofibrate [%] Released Fenofibrate [%] Formulation Screening (Dissolution Testing) Tablets with defined geometries Order Order Time [min] Time [min] STK Annual Meeting

18 Applications STK Annual Meeting

19 NOWHERE NOW HERE A little change can make a big difference STK Annual Meeting

20 Contact STK Annual Meeting