Abstract
The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5% w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.
| Language | English |
|---|---|
| Pages | 878-885 |
| Number of pages | 8 |
| Journal | Chemical Engineering Science |
| Volume | 101 |
| Early online date | 27 May 2013 |
| DOIs | |
| Publication status | Published - 1 Sep 2013 |
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Keywords
- Raman spectrometry
- cellobiose octaacetate
- image analysis
- agitation time
- particle properties
- particle filtration–drying
Cite this
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Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman spectrometry. / Hamilton, Peter; Littlejohn, David; Nordon, Alison; Sefcik, Jan; Slavin, Paul; Andrews, John; Dallin, Paul.
In: Chemical Engineering Science , Vol. 101, 01.09.2013, p. 878-885.Research output: Contribution to journal › Article
TY - JOUR
T1 - Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman spectrometry
AU - Hamilton, Peter
AU - Littlejohn, David
AU - Nordon, Alison
AU - Sefcik, Jan
AU - Slavin, Paul
AU - Andrews, John
AU - Dallin, Paul
N1 - Notice: This is the author's version of a work that was accepted for publication in Chemical Engineering Science. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Chemical Engineering Science, [101, 20 Sept., (2013)] DOI: 10.1016/j.ces.2013.05.035
PY - 2013/9/1
Y1 - 2013/9/1
N2 - The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5% w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.
AB - The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5% w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.
KW - Raman spectrometry
KW - cellobiose octaacetate
KW - image analysis
KW - agitation time
KW - particle properties
KW - particle filtration–drying
UR - http://www.scopus.com/inward/record.url?scp=84883458626&partnerID=8YFLogxK
UR - http://www.journals.elsevier.com/chemical-engineering-science
U2 - 10.1016/j.ces.2013.05.035
DO - 10.1016/j.ces.2013.05.035
M3 - Article
VL - 101
SP - 878
EP - 885
JO - Chemical Engineering Science
T2 - Chemical Engineering Science
JF - Chemical Engineering Science
SN - 0009-2509
ER -