Kinetics of the Aqueous-Ethanol Solution Mediated
Transformation between the Beta and Alpha Polymorphs of p‑Aminobenzoic Acid
Version 2 2018-04-20, 23:44
Version 1 2018-01-22, 16:42
Posted on 2018-04-20 - 23:44
A quantitative kinetics analysis
of the solution-mediated phase
transformations in aqueous-ethanol between the enantiotropically related
alpha and beta polymorphs of p-aminobenzoic acid
(PABA) is presented. A new temperature-controlled transmission flow-cell
design for use with a laboratory X-ray source which can be utilized
for diffraction or scattering experiments is described. This transmission
cell in combination with in situ slurry X-ray diffraction
is utilized to provide a quantitative analysis of the percentage by
mass of respective solid phases in flowing suspensions, coupled with
solution concentration as measured with UV–vis spectroscopy.
The separate phases are identified through individual fingerprint
peaks, the (1 0 3) reflection at 2θ = 15.6°
relating to the alpha phase and the (0 2 2) reflection at 2θ = 25.3° for the beta phase. Examination of
the conversion of a slurry of beta PABA in a 70:30 water/ethanol solvent
mixture to the alpha polymorph, at a temperature range of 24–30
°C reveals the rate of dissolution of the beta phase is consistent
with zero order kinetics (rate constant kdβ 6.80 × 10–4 to 8.17 × 10–5 wt % s–1), while the growth of the alpha phase
follows first order kinetics (kgα 1.00 × 10–3 to 2.50 × 10–4 wt % s–1). Extrapolation of the growth and dissolution
rate constants yields a transformation temperature for the phase interconversion
of 22–24 °C. Overall the data are consistent with a fast
de-supersaturation of the solution concentration indicating a dissolution-controlled
polymorphic transformation process.
CITE THIS COLLECTION
DataCite
3 Biotech
3D Printing in Medicine
3D Research
3D-Printed Materials and Systems
4OR
AAPG Bulletin
AAPS Open
AAPS PharmSciTech
Abhandlungen aus dem Mathematischen Seminar der Universität Hamburg
ABI Technik (German)
Academic Medicine
Academic Pediatrics
Academic Psychiatry
Academic Questions
Academy of Management Discoveries
Academy of Management Journal
Academy of Management Learning and Education
Academy of Management Perspectives
Academy of Management Proceedings
Academy of Management Review
Turner, Thomas D.; Caddick, Steve; Hammond, Robert B.; Roberts, Kevin J.; Lai, Xiaojun (2018). Kinetics of the Aqueous-Ethanol Solution Mediated
Transformation between the Beta and Alpha Polymorphs of p‑Aminobenzoic Acid. ACS Publications. Collection. https://doi.org/10.1021/acs.cgd.7b01551
or
Select your citation style and then place your mouse over the citation text to select it.
SHARE
Usage metrics
Read the peer-reviewed publication
AUTHORS (5)
TT
Thomas D. Turner
SC
Steve Caddick
RH
Robert B. Hammond
KR
Kevin J. Roberts
XL
Xiaojun Lai
KEYWORDS
PABAdissolution rate constants yieldsorder kineticssolution concentrationUVdissolution-controlled polymorphic transformation processbeta phasetemperature-controlled transmission flow-cell designslurry X-ray diffractionsolution-mediated phase transformations2 θAqueous-Ethanol Solution Mediated Transformationlaboratory X-ray source