Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals
An experimental study has been conducted to evaluate the capability of a seeded batch cooling crystallization with a temperature cycling method to produce a narrow crystal size distribution and grow a desired polymorphic form of sulfathiazole crystals. The study used focused beam reflectance measur...
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American Chemical Society
2009
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iium-3742011-07-11T04:35:11Z http://irep.iium.edu.my/374/ Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals Abu Bakar, Mohd Rushdi Nagy, Zoltan K. Rielly, Chris D. QD Chemistry TP Chemical technology An experimental study has been conducted to evaluate the capability of a seeded batch cooling crystallization with a temperature cycling method to produce a narrow crystal size distribution and grow a desired polymorphic form of sulfathiazole crystals. The study used focused beam reflectance measurement (FBRM), and attenuated total reflectance ultraviolet/visible (ATR-UV/vis)spectroscopy for the in situ monitoring and control of the process. Based on the FBRM readings, the process was driven using a feedback control approach that employs alternating cycles of heating and cooling phases so that the number of counts, corresponding to the number of seed particles, is maintained, whilst the square-weighted chord length distribution, indicating the dynamic progress of the growth of the seeds in the system, is increased. Results of the experiments show that the temperature cycling method promoted Ostwald ripening, which helped in accelerating the growth and enhancing the size uniformity of the product. The method also has a good prospect to be implemented for the control of polymorphic purity. Seeds of Form I and Form II could be grown from n-propanol and water, respectively. Form I seeds in water were first transformed into Form II and/or swamped by nuclei of Form II, before the growth of the newly formed crystals took place. Seeds of Form II and Form III in n-propanol, however, were not able to grow at all. This study confirmed that the nucleation and growth of sulfathiazole crystals are solvent-mediated, and the insight into these phenomena was captured very well by the in situ monitoring tools. American Chemical Society 2009 Article PeerReviewed application/pdf en http://irep.iium.edu.my/374/1/oprd_2009_rushdi.pdf Abu Bakar, Mohd Rushdi and Nagy, Zoltan K. and Rielly, Chris D. (2009) Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals. Organic Process Research & Development, 13 (6). pp. 1343-1356. ISSN 1083-6160 http://pubs.acs.org/doi/abs/10.1021/op900174b doi:10.1021/op900174b |
| repository_type |
Digital Repository |
| institution_category |
Local University |
| institution |
International Islamic University Malaysia |
| building |
IIUM Repository |
| collection |
Online Access |
| language |
English |
| topic |
QD Chemistry TP Chemical technology |
| spellingShingle |
QD Chemistry TP Chemical technology Abu Bakar, Mohd Rushdi Nagy, Zoltan K. Rielly, Chris D. Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| description |
An experimental study has been conducted to evaluate the
capability of a seeded batch cooling crystallization with a temperature cycling method to produce a narrow crystal size distribution and grow a desired polymorphic form of sulfathiazole crystals. The study used focused beam reflectance measurement (FBRM), and attenuated total reflectance ultraviolet/visible (ATR-UV/vis)spectroscopy for the in situ monitoring and control of the process. Based on the FBRM readings, the process was driven using a
feedback control approach that employs alternating cycles of
heating and cooling phases so that the number of counts, corresponding to the number of seed particles, is maintained, whilst the square-weighted chord length distribution, indicating the dynamic progress of the growth of the seeds in the system, is increased. Results of the experiments show that the temperature cycling method promoted Ostwald ripening, which helped in accelerating the growth and enhancing the size uniformity of the product. The method also has a good prospect to be implemented
for the control of polymorphic purity. Seeds of Form I and Form II could be grown from n-propanol and water, respectively. Form I seeds in water were first transformed into Form II and/or swamped by nuclei of Form II, before the growth of the newly formed crystals took place. Seeds of Form II and Form III in n-propanol, however, were not able to grow at all. This study confirmed that the nucleation and growth of sulfathiazole crystals are solvent-mediated, and the insight into these phenomena was captured very well by the in situ monitoring tools. |
| format |
Article |
| author |
Abu Bakar, Mohd Rushdi Nagy, Zoltan K. Rielly, Chris D. |
| author_facet |
Abu Bakar, Mohd Rushdi Nagy, Zoltan K. Rielly, Chris D. |
| author_sort |
Abu Bakar, Mohd Rushdi |
| title |
Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| title_short |
Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| title_full |
Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| title_fullStr |
Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| title_full_unstemmed |
Seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| title_sort |
seeded batch cooling crystallization with temperature cycling for the control of size uniformity and polymorphic purity of sulfathiazole crystals |
| publisher |
American Chemical Society |
| publishDate |
2009 |
| url |
http://irep.iium.edu.my/374/ http://irep.iium.edu.my/374/ http://irep.iium.edu.my/374/ http://irep.iium.edu.my/374/1/oprd_2009_rushdi.pdf |
| first_indexed |
2023-09-18T20:07:29Z |
| last_indexed |
2023-09-18T20:07:29Z |
| _version_ |
1777407255546691584 |