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Title: Investigating nucleation control in batch and flow using non-photochemical laser-induced nucleation
Author: Mackenzie, Alasdair Morgan
ISNI:       0000 0004 7429 8823
Awarding Body: University of Edinburgh
Current Institution: University of Edinburgh
Date of Award: 2017
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The practical application of non-photochemical laser-induced nucleation (NPLIN) to continuous flow was investigated. Supersaturated aqueous solutions were screened with a 5 ns pulsed laser (532 nm 44 MW cm-2) for NPLIN activity. Upon irradiation succinic acid nucleated at S20 = 4.3 and adipic acid at S20 = 2.0 - 3.0. NPLIN activity is reported for the first time in nicotinic acid (S20 = 2.6 - 3.0). No overall pattern was observed of chemical structure on NPLIN activity. From inorganic compounds similarly screened, ammonium chloride (S20 = 1.04 - 1.20) was identified as most suitable for further tests. It was shown to have an increase of NPLIN crystals with higher supersaturation from 13 at S = 1.038 to 252 at S = 1.135. A quadratic increase in number of crystals with increased laser power. The effects of NPLIN upon ammonium chloride are diminished upon filtration through a 0.2 μm poly (ether sulfone) filter, reducing the number of crystals from 350 to 10 per 70 mJ pulse (25 MW cm-2). The use of NPLIN in continuous flow was demonstrated from the first time. A S23 = 1.1 solution of aqueous ammonium chloride in flow produced crystals when irradiated by 10 pulses s-1 of a 1064 nm 6 ns laser. When the laser was stopped, crystals were no longer produced and the system returned to flowing supersaturated solution. Lab scale apparatus for continuous NPLIN experiments was developed. A design involving a re-dissolution step and loop flow was constructed for both laminar and slug-flow regimes. Nucleation of ammonium chloride (S = 1.1) was demonstrated in both systems. Repeatable NPLIN experiments were hindered by spontaneous nucleation. Spontaneous nucleation in flow was observed around areas where supersaturated solution passed from one component to another. Spontaneous nucleation was also observed upon cooling (25 to 10 °C). Filtration was observed to both suppress NPLIN and spontaneous nucleation in flow.
Supervisor: Pulham, Colin ; Alexander, Andrew ; Mount, Andrew Sponsor: Not available
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: Crystallisation ; homogeneous nucleation ; NPLIN ; non-photochemical laser-induced nucleation