Abstract
| Language | English |
|---|---|
| Pages | 4403–4415 |
| Number of pages | 13 |
| Journal | Crystal Growth and Design |
| Volume | 18 |
| Issue number | 8 |
| DOIs | |
| Publication status | Published - 15 Jun 2018 |
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Keywords
- crystal engineering
- shape control
- temperature cycling
- particle tracking
- online shape analysis
- choice of solvent
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Crystal shape modification via cycles of growth and dissolution in a tubular crystallizer. / Neugebauer, Peter; Cardona, Javier; Besenhard, Maximilian O.; Peter, Anna; Gruber-Woelfler, Heidrun; Tachtatzis, Christos; Cleary, Alison; Andonovic, Ivan; Sefcik, Jan; Khinast, Johannes G.
In: Crystal Growth and Design, Vol. 18, No. 8, 15.06.2018, p. 4403–4415.Research output: Contribution to journal › Article
TY - JOUR
T1 - Crystal shape modification via cycles of growth and dissolution in a tubular crystallizer
AU - Neugebauer, Peter
AU - Cardona, Javier
AU - Besenhard, Maximilian O.
AU - Peter, Anna
AU - Gruber-Woelfler, Heidrun
AU - Tachtatzis, Christos
AU - Cleary, Alison
AU - Andonovic, Ivan
AU - Sefcik, Jan
AU - Khinast, Johannes G.
PY - 2018/6/15
Y1 - 2018/6/15
N2 - Besides size and polymorphic form, crystal shape takes a central role in engineering advanced solid materials for pharmaceutical and chemical industry. This work demonstrates how multiple cycles of growth and dissolution can manipulate the habit of an acetylsalicylic acid crystal population. Considerable changes of the crystal habit could be achieved within minutes due to rapid cycling, i.e., up to 25 cycles within <10 min. The required fast heating and cooling rates were facilitated using a tubular reactor design allowing for superior temperature control. The face specific interactions between solvent and the crystals’ surface result in face specific growth and dissolution rates and hence alterations of the final shape of the crystals in solution. Accurate quantification of the crystal shapes was essential for this work, but is everything but easy. A commercial size and shape analyser had to be adapted to achieve required accuracy. Online size, and most important shape, analysis was achieved using an automated microscope equipped with a flow-through cell, in combination with a dedicated image analysis routine for particle tracking and shape analysis. Due to the implementation of this analyser, capable of obtaining statistics on the crystals’ shape while still in solution (no sampling and manipulation required), the dynamic behaviour of the size shape distribution could be studied. This enabled a detailed analysis of the solvent’s effect on the change in crystal habit.
AB - Besides size and polymorphic form, crystal shape takes a central role in engineering advanced solid materials for pharmaceutical and chemical industry. This work demonstrates how multiple cycles of growth and dissolution can manipulate the habit of an acetylsalicylic acid crystal population. Considerable changes of the crystal habit could be achieved within minutes due to rapid cycling, i.e., up to 25 cycles within <10 min. The required fast heating and cooling rates were facilitated using a tubular reactor design allowing for superior temperature control. The face specific interactions between solvent and the crystals’ surface result in face specific growth and dissolution rates and hence alterations of the final shape of the crystals in solution. Accurate quantification of the crystal shapes was essential for this work, but is everything but easy. A commercial size and shape analyser had to be adapted to achieve required accuracy. Online size, and most important shape, analysis was achieved using an automated microscope equipped with a flow-through cell, in combination with a dedicated image analysis routine for particle tracking and shape analysis. Due to the implementation of this analyser, capable of obtaining statistics on the crystals’ shape while still in solution (no sampling and manipulation required), the dynamic behaviour of the size shape distribution could be studied. This enabled a detailed analysis of the solvent’s effect on the change in crystal habit.
KW - crystal engineering
KW - shape control
KW - temperature cycling
KW - particle tracking
KW - online shape analysis
KW - choice of solvent
UR - https://pubs.acs.org/journal/cgdefu
U2 - 10.1021/acs.cgd.8b00371
DO - 10.1021/acs.cgd.8b00371
M3 - Article
VL - 18
SP - 4403
EP - 4415
JO - Crystal Growth and Design
T2 - Crystal Growth and Design
JF - Crystal Growth and Design
SN - 1528-7483
IS - 8
ER -