The UCD Crystallization Group was established in 1996 to provide a platform for the investigation of process engineering aspects of industrial crystallization systems. In particular, it has focused on the development and use of in-process monitoring and measurement techniques, and on the development of reliable process scale-up methods.
UCD Crystallization Research Group Equipment Details
Two EasyMaxTM automated lab reactors (ALRs) with dosing, from Mettler Toledo, are used in conjunction with PAT technologies such as the Kaiser RAMANRXN2 HYBRIDTM and Mettler Toledo FBRMTM, iC-10TM, pH SevenMultiTM systems, by means of the iC software platform, to heighten understanding of crystallization processes in-situ.
The EasyMaxTM system, is a two block ALR, controlled via touch pad or by PC. This is a standalone ALR with no external heat exchanger required. It has a peltier heat exchange system allows a crystallization range from -40 to 180 ºC. Variable agitators and reactor sizes, from 50 to 100 mls, are also provided.
EasyMax System with Kaiser RAMANRXN2 HybridTM in-situ
Also shown is the Kaiser PhAT probe technology for quantifying tabletted APIs and blended powders The Kaiser RAMANRXN2 HYBRIDTM analyzer is used to understand and create polymorphic design spaces from the 50ml to 21 scales. This system has a 'wet end' immersion optic for quantifying in-situ polymorphic transformations in crystallization process. Also provided is the new Kaiser PhAT probe technology which increased the solid sampling size from 2/500 microns to 6mm. The increase in sample size allows the quantification of API to sugar dosing in tabletted APIs or in blended powders.
EasyMax System with FBRMTM (S400), iC-10TM and pH SevenMultiTM in-situ
Three FBRMTM systems (S400, M400 and D600L) are used for the assessment of crystallization characteristics such as particle nucleation, growth, dimension, agglomeration and attrition from 50 mL to 90 L scales. These systems are also used in conjunction with feedback control strategies so particle dimension can be maintained on scale. Two Mid-IR probes, ReactIR 4000TM and iC-10TM, from Mettler Toledo are used for the development of both quantitative and qualitative real time supersaturation (dissolved concentration) assessment and control. This technology when used in conjunction with direct feedback control softewares (iC Control LabMax / EasyMax) facilitates automated methods for controlling supersaturation. A pH SevenMultiTM, from Mettler Toledo, is a two probe pH system used in conjunction with the EasyMax to understand pH precipitation and reactive crystallizations.
HEL polyBLOCKTM with turbidity
The polyBLOCKTM from HEL is a four pot reactor system which is coupled with turbidity . This platform is used for the creation of solubility and metastability design spaces. This screening device allows the challenges between alternative crystallization techniques, such as cooling and anti-solvent methods, to be identified and in turn process choice can be made.
The Malvern MastersizerTM particle sizer is used for the assessment of particle size both at line and in line. This particle sizing technique is based on laser diffraction and works well at low slurry densities. Correlations between this technology and other particle measurement techniques, such as the FBRM, are made. PVMTM probe for in-situ assessment of particle morphology. PVMTM (Particle Vision Measurement) system from Mettler Toledo is used to gain an understanding on the attained in-situ particle morphology. It is also coupled with FBRMTM data to heighten understanding of oiling out, agglomeration, attrition, seeding and polymorphic transformations. The HEL (www.helgroup.com) AutoLabTM system, with turbidity is an Automated Lab Reactor (ALR) used in conjunction with PAT technologies so an increase in understanding of crystallization processes can be gained.
ALR with iC-10TM IR probe and FBRMTMFBRM probe
The LabMaxTM system shown is a 1 L automated lab reactor (ALR) used for the development and scale-up of crystallization processes. This ALR platform is coupled with PAT technologies, such as FBRMTM (D600L) and iC-10TM by means of the new Mettler Toledo iC software platform, for the development of direct feedback control strategies so as particle size, form and the dissolved concentration can be maintained on scale and during tech transfers.