An accurate detection of micro-collapse during the lyophilisation of a 5% w/v lactose solution using a combination of novel techniques: intelligent laser speckle imaging (ILSI) and through-vial impedance spectroscopy (TVIS)

TL;DR

This study combines innovative optical and electrical techniques, ILSI and TVIS, to accurately detect micro-collapse during lyophilisation of lactose, enabling better process control and energy efficiency.

Contribution

It introduces a novel integrated approach using ILSI and TVIS for real-time detection of micro-collapse in freeze drying processes.

Findings

Successful detection of micro-collapse using combined techniques

Real-time monitoring improves process control

Potential reduction in energy costs and product waste

Abstract

Context: In a freeze drying (FD) process, an accurate observation and control of the process parameters at critical stages are at high importance. Particularly accurate and timely identification of the critical temperature (TC) at the end of primary drying phase would lead to heating energy cost reduction and product waste elimination by ending the process before the product's micro-collapse stage. Aim: Within this work, a combination of novel techniques optical technique called Intelligent Laser Speckle Imaging (ILSI) in association with product image texture analysis, coupled to an electrical impedance technique called through vial impedance spectroscopy (TVIS) has been applied onto the real-time product states observation process to identify the specific structural product surface/subsurface characteristics and hence the micro-collapse stage. Method: 2 cycles - one providing a profile for standard approach (non-collapsed) and another with a temperature ramp through TC to micro-collapse, TVIS provides an assessment of the onset of micro-collapse through the assessment of the acceleration in drying rate whereas the ILSI with pattern recognition detects the change in microstructure