subject:(Crystallization)

Georgia Tech

1. Encarnacion-Gomez, Luis G. Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis.

Degree: PhD, Chemical and Biomolecular Engineering, 2015, Georgia Tech

URL: http://hdl.handle.net/1853/54322

► The work presented in this thesis is aimed to design efficient reactive crystallization operations that could potentially be implemented in the manufacture of enantiomerically pure… (more)

▼ The work presented in this thesis is aimed to design efficient reactive crystallization operations that could potentially be implemented in the manufacture of enantiomerically pure compounds and β-lactam antibiotics. Multiple aspects of solution thermodynamics, reaction engineering and crystallization from complex solutions are involved and will be discussed in detail through the following chapters. The first piece of this work utilizes reactive crystallization for the manufacture of enantiomerically pure amino acids. Chemo-enzymatic stereoiversion reactions are used to enrich saturated or supersaturated solutions to favor the selection of a desired enantiomer. L-Methionine and L-Phenylalanine were resolve successfully from racemic mixtures by cyclic stereoinversion. r D-amino acids were oxidized by D-amino acid oxidase (D-AAO) and the resulting ketoacid was subsequently reduced by ammonia borane producing a racemic-mixture After the necessary enantiomeric enrichment was reached, system conditions were changed to induce supersaturation and promote crystal formation. In each case crystals with chemical and enantiomeric purities greater than 99% wt. were recovered. experimental information about reaction and crystallization kinetics was used to developed models. Such models were used to design model-based optimizations in which the productivity of the operation was enhanced by selecting an optimal temperature profile. The second example is a reactive crystallization towards the manufacture of β-lactam antibiotics. One of the major drawbacks of the utilization of enzymes towards the manufacture of β-lactam antibiotics is the fact that the same enzyme that catalyzes the synthesis of the antibiotic also catalyzes its hydrolysis and thus, its degradation. The reaction scheme is a kinetically controlled synthesis in which the desired product is an intermediate within the network. Hence, the focus of this work is to design an efficient reactive crystallization in which the product is crystallized before it is consumed by hydrolysis. In order to accomplish this goal we have study solution equilibria, reaction kinetics, and crystallization kinetics. Even though crystallization kinetics of ampicillin has been previously reported; the reported models are not applicable to a reactive crystallization scheme for a variety of reasons. In this work, we have developed a robust model that can be applied to multiple crystallization protocols that are consistent with the conditions at which the enzymatic reaction can be performed. Finally, a reactive-crystallization scheme in which ampicillin was successfully recovered from solution was developed. In this work, crystal seeds were used to promote crystallization of the desired product from the complex media. The results indicated that is possible to perform the reaction and crystallization in parallel, and still recover crystals with high purity. This work is the first example in which ampicillin was produced and recovered with high purity in a single stage. Previous work on… Advisors/Committee Members: Rousseau, Ronald W. (advisor), Bommarius, Andreas S. (committee member), Kawajiri, Yoshiaki (committee member), Realff, Matthew J. (committee member), Liotta, Charles (committee member).

Subjects/Keywords: Crystallization; Reactive-crystallization; Enantiomers; Antibiotics

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APA (6^th Edition):

Encarnacion-Gomez, L. G. (2015). Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis. (Doctoral Dissertation). Georgia Tech. Retrieved from http://hdl.handle.net/1853/54322

Chicago Manual of Style (16^th Edition):

Encarnacion-Gomez, Luis G. “Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis.” 2015. Doctoral Dissertation, Georgia Tech. Accessed March 01, 2021. http://hdl.handle.net/1853/54322.

MLA Handbook (7^th Edition):

Encarnacion-Gomez, Luis G. “Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis.” 2015. Web. 01 Mar 2021.

Vancouver:

Encarnacion-Gomez LG. Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis. [Internet] [Doctoral dissertation]. Georgia Tech; 2015. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1853/54322.

Council of Science Editors:

Encarnacion-Gomez LG. Design and operation of enzymatic reactive crystallization: Applications in chiral purity and kinetically controlled synthesis. [Doctoral Dissertation]. Georgia Tech; 2015. Available from: http://hdl.handle.net/1853/54322

2. 東條, 陽介. 自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ.

Degree: Nara Institute of Science and Technology / 奈良先端科学技術大学院大学

URL: http://hdl.handle.net/10061/6670

Subjects/Keywords: Crystallization

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APA (6^th Edition):

東條, �. (n.d.). 自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ. (Thesis). Nara Institute of Science and Technology / 奈良先端科学技術大学院大学. Retrieved from http://hdl.handle.net/10061/6670

Note: this citation may be lacking information needed for this citation format:
No year of publication.
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

東條, 陽介. “自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ.” Thesis, Nara Institute of Science and Technology / 奈良先端科学技術大学院大学. Accessed March 01, 2021. http://hdl.handle.net/10061/6670.

Note: this citation may be lacking information needed for this citation format:
No year of publication.
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

東條, 陽介. “自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ.” Web. 01 Mar 2021.

Note: this citation may be lacking information needed for this citation format:
No year of publication.

Vancouver:

東條 �. 自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ. [Internet] [Thesis]. Nara Institute of Science and Technology / 奈良先端科学技術大学院大学; [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10061/6670.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation
No year of publication.

Council of Science Editors:

東條 �. 自己組織化金属触媒による半導体薄膜の新規結晶化手法に関する研究 : Novel Crystallization Method of Amorphous Semiconductor Thin Films by using Self-Assembled Metalic Catalyst; ジコソシキカキンゾクショクバイニヨルハンドウタイハクマクノシンキケッショウカシュホウニカンスルケンキュウ. [Thesis]. Nara Institute of Science and Technology / 奈良先端科学技術大学院大学; Available from: http://hdl.handle.net/10061/6670

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation
No year of publication.

Oregon State University

3. Leu, Lii-ping. Dynamics and control of continuous crystallizers.

Degree: PhD, Chemical Engineering, 1981, Oregon State University

URL: http://hdl.handle.net/1957/41758

► The theoretical analysis of an unseeded, isothermal mixed-suspension mixed-product-removal (MSMPR) crystallizer with a fines trap is developed. The lumped parameter system equations are presented for… (more)

Subjects/Keywords: Crystallization

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APA (6^th Edition):

Leu, L. (1981). Dynamics and control of continuous crystallizers. (Doctoral Dissertation). Oregon State University. Retrieved from http://hdl.handle.net/1957/41758

Chicago Manual of Style (16^th Edition):

Leu, Lii-ping. “Dynamics and control of continuous crystallizers.” 1981. Doctoral Dissertation, Oregon State University. Accessed March 01, 2021. http://hdl.handle.net/1957/41758.

MLA Handbook (7^th Edition):

Leu, Lii-ping. “Dynamics and control of continuous crystallizers.” 1981. Web. 01 Mar 2021.

Vancouver:

Leu L. Dynamics and control of continuous crystallizers. [Internet] [Doctoral dissertation]. Oregon State University; 1981. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1957/41758.

Council of Science Editors:

Leu L. Dynamics and control of continuous crystallizers. [Doctoral Dissertation]. Oregon State University; 1981. Available from: http://hdl.handle.net/1957/41758

4. Hoetmer, G. (author). Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization.

Degree: 2012, Delft University of Technology

URL: http://resolver.tudelft.nl/uuid:9f803313-1eb2-4073-91ea-b41ef823dc60

►

Different industries make use of encapsulated particles, from the pharmaceutical industry for target drug delivery to the agricultural industry for masking of odor and flavor… (more)

Subjects/Keywords: crystallization

…2-2-2 Chemical processes . . . . . . . . . . . . 2-3 Cooling crystallization… …2-3-1 Encapsulation using cooling crystallization 2-4 Electrospray crystallization… …2-4-1 Crystallization using electrospray . . . . . 2-4-2 Encapsulation using electrospray… …3-1-1 Cooling crystallisation . . . . . . . . 3-1-2 Electrospray crystallization… …3-2 Experiments with cooling crystallization . . 3-3 Experiments with electrospray…

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APA (6^th Edition):

Hoetmer, G. (. (2012). Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization. (Masters Thesis). Delft University of Technology. Retrieved from http://resolver.tudelft.nl/uuid:9f803313-1eb2-4073-91ea-b41ef823dc60

Chicago Manual of Style (16^th Edition):

Hoetmer, G (author). “Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization.” 2012. Masters Thesis, Delft University of Technology. Accessed March 01, 2021. http://resolver.tudelft.nl/uuid:9f803313-1eb2-4073-91ea-b41ef823dc60.

MLA Handbook (7^th Edition):

Hoetmer, G (author). “Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization.” 2012. Web. 01 Mar 2021.

Vancouver:

Hoetmer G(. Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization. [Internet] [Masters thesis]. Delft University of Technology; 2012. [cited 2021 Mar 01]. Available from: http://resolver.tudelft.nl/uuid:9f803313-1eb2-4073-91ea-b41ef823dc60.

Council of Science Editors:

Hoetmer G(. Encapsulating pharmaceutical crystals: A comparison between cooling and electrospray crystallization. [Masters Thesis]. Delft University of Technology; 2012. Available from: http://resolver.tudelft.nl/uuid:9f803313-1eb2-4073-91ea-b41ef823dc60

Michigan State University

5. Goetsch, Alayna Michelle. Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions.

Degree: MS, Department of Chemistry, 2004, Michigan State University

URL: http://etd.lib.msu.edu/islandora/object/etd:33304

Subjects/Keywords: Crystallization

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APA (6^th Edition):

Goetsch, A. M. (2004). Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions. (Masters Thesis). Michigan State University. Retrieved from http://etd.lib.msu.edu/islandora/object/etd:33304

Chicago Manual of Style (16^th Edition):

Goetsch, Alayna Michelle. “Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions.” 2004. Masters Thesis, Michigan State University. Accessed March 01, 2021. http://etd.lib.msu.edu/islandora/object/etd:33304.

MLA Handbook (7^th Edition):

Goetsch, Alayna Michelle. “Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions.” 2004. Web. 01 Mar 2021.

Vancouver:

Goetsch AM. Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions. [Internet] [Masters thesis]. Michigan State University; 2004. [cited 2021 Mar 01]. Available from: http://etd.lib.msu.edu/islandora/object/etd:33304.

Council of Science Editors:

Goetsch AM. Spectroscopic characterization of 6-cyano-2-naphthol for use as a crystallization initiatior [sic] in aqueous solutions. [Masters Thesis]. Michigan State University; 2004. Available from: http://etd.lib.msu.edu/islandora/object/etd:33304

University of Arizona

6. Abbott, Robert Leonard, 1941-. A continuous crystallization apparatus .

Degree: 1966, University of Arizona

URL: http://hdl.handle.net/10150/318531

Subjects/Keywords: Crystallization.

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APA (6^th Edition):

Abbott, Robert Leonard, 1. (1966). A continuous crystallization apparatus . (Masters Thesis). University of Arizona. Retrieved from http://hdl.handle.net/10150/318531

Chicago Manual of Style (16^th Edition):

Abbott, Robert Leonard, 1941-. “A continuous crystallization apparatus .” 1966. Masters Thesis, University of Arizona. Accessed March 01, 2021. http://hdl.handle.net/10150/318531.

MLA Handbook (7^th Edition):

Abbott, Robert Leonard, 1941-. “A continuous crystallization apparatus .” 1966. Web. 01 Mar 2021.

Vancouver:

Abbott, Robert Leonard 1. A continuous crystallization apparatus . [Internet] [Masters thesis]. University of Arizona; 1966. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10150/318531.

Council of Science Editors:

Abbott, Robert Leonard 1. A continuous crystallization apparatus . [Masters Thesis]. University of Arizona; 1966. Available from: http://hdl.handle.net/10150/318531

University of Arizona

7. Kraljevich, Zlatica Idalia, 1949-. Experimental and theoretical study of fines destruction in a mixed suspension crystallizer .

Degree: 1977, University of Arizona

URL: http://hdl.handle.net/10150/348141

Subjects/Keywords: Crystallization.

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APA (6^th Edition):

Kraljevich, Zlatica Idalia, 1. (1977). Experimental and theoretical study of fines destruction in a mixed suspension crystallizer . (Masters Thesis). University of Arizona. Retrieved from http://hdl.handle.net/10150/348141

Chicago Manual of Style (16^th Edition):

Kraljevich, Zlatica Idalia, 1949-. “Experimental and theoretical study of fines destruction in a mixed suspension crystallizer .” 1977. Masters Thesis, University of Arizona. Accessed March 01, 2021. http://hdl.handle.net/10150/348141.

MLA Handbook (7^th Edition):

Kraljevich, Zlatica Idalia, 1949-. “Experimental and theoretical study of fines destruction in a mixed suspension crystallizer .” 1977. Web. 01 Mar 2021.

Vancouver:

Kraljevich, Zlatica Idalia 1. Experimental and theoretical study of fines destruction in a mixed suspension crystallizer . [Internet] [Masters thesis]. University of Arizona; 1977. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10150/348141.

Council of Science Editors:

Kraljevich, Zlatica Idalia 1. Experimental and theoretical study of fines destruction in a mixed suspension crystallizer . [Masters Thesis]. University of Arizona; 1977. Available from: http://hdl.handle.net/10150/348141

University of Arizona

8. Sikdar, Subhas Kumar, 1944-. SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER .

Degree: 1975, University of Arizona

URL: http://hdl.handle.net/10150/285063

Subjects/Keywords: Crystallization.

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APA (6^th Edition):

Sikdar, Subhas Kumar, 1. (1975). SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER . (Doctoral Dissertation). University of Arizona. Retrieved from http://hdl.handle.net/10150/285063

Chicago Manual of Style (16^th Edition):

Sikdar, Subhas Kumar, 1944-. “SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER .” 1975. Doctoral Dissertation, University of Arizona. Accessed March 01, 2021. http://hdl.handle.net/10150/285063.

MLA Handbook (7^th Edition):

Sikdar, Subhas Kumar, 1944-. “SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER .” 1975. Web. 01 Mar 2021.

Vancouver:

Sikdar, Subhas Kumar 1. SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER . [Internet] [Doctoral dissertation]. University of Arizona; 1975. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10150/285063.

Council of Science Editors:

Sikdar, Subhas Kumar 1. SECONDARY NUCLEATION MECHANISMS AND KINETICS IN A CONTINUOUS-FLOW SEEDED CRYSTALLIZER . [Doctoral Dissertation]. University of Arizona; 1975. Available from: http://hdl.handle.net/10150/285063

University of Arizona

9. Cise, Michael David, 1943-. CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER .

Degree: 1971, University of Arizona

URL: http://hdl.handle.net/10150/287711

Subjects/Keywords: Crystallization.

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APA (6^th Edition):

Cise, Michael David, 1. (1971). CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER . (Doctoral Dissertation). University of Arizona. Retrieved from http://hdl.handle.net/10150/287711

Chicago Manual of Style (16^th Edition):

Cise, Michael David, 1943-. “CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER .” 1971. Doctoral Dissertation, University of Arizona. Accessed March 01, 2021. http://hdl.handle.net/10150/287711.

MLA Handbook (7^th Edition):

Cise, Michael David, 1943-. “CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER .” 1971. Web. 01 Mar 2021.

Vancouver:

Cise, Michael David 1. CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER . [Internet] [Doctoral dissertation]. University of Arizona; 1971. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10150/287711.

Council of Science Editors:

Cise, Michael David 1. CRYSTAL GROWTH AND NUCLEATION KINETICS OF THE POTASSIUM SULFATE SYSTEM INA CONTINUOUS-FLOW, SEEDED CRYSTALLIZER . [Doctoral Dissertation]. University of Arizona; 1971. Available from: http://hdl.handle.net/10150/287711

University of Arizona

10. Sutradhar, Bhagya Chandra. Processes that make larger crystal particles.

Degree: 1992, University of Arizona

URL: http://hdl.handle.net/10150/185878

► The particle size or crystal size distribution (PSD or CSD) of a solid product from a crystallizer is important in handling the solid. CSD related… (more)

▼ The particle size or crystal size distribution (PSD or CSD) of a solid product from a crystallizer is important in handling the solid. CSD related properties might be improved with larger particle size. The principle of particle size increase in continuous crystallization processes is to remove fine particles at a faster rate than large ones. Two technologies based on this principle are the Double Draw-Off (DDO) and the Fines Dissolving (FD) crystallizer configurations. Design charts were developed for the Fines Dissolving crystallizer. It was found that the particle size increase passes through a maximum value as the fines classification cut size is increased. Based on this information a design protocol was suggested for the FD crystallizer. A limited amount of data are required for this method of design. The modified DDO crystallizer configuration was developed in order to obtain particle size increase in processes with high natural slurry density for which a build-up of solid is impractical. This involved a recycle of a part of the overflow (in DDO operation) after further classification of particles to remove fines in a size range L(F1) to L(F2), thus controling the slurry density in the crystallizer. Design equations and design charts for this configuration were developed. Analysis showed that a stream with some fines in it might be more effective in decreasing the slurry density than a clear filtered liquor. Particle size increase was demonstrated for sodium chloride crystallization in caustic liquor using the FD, DDO and modified DDO crystallizers. A fines/feed flow modification as well as actual fines dissolution was used in the FD experiments. Significant size increase was observed in both cases. These experiments indicated that appreciable dissolution cost would be involved in FD operation. The DDO experiments produced large crystal particles with associated increase in slurry density. Slurry density information from large scale operations indicated that DDO operation would be possible for DDO ratios upto about 2.5. The modified DDO configuration also produced larger particles. However, size increases were less than expected. Loss of supersaturation outside the crystallizer might be the reason. Appreciable reduction of crystallizer vessel fouling was observed in the DDO and modified DDO experiments. Randolph et al. (1990) demonstrated significant particle size increase for calcium sulfite precipitation in flue gas desulfurization (FGD) liquor using a DDO crystallizer. Experimental particle sizes were appreciably larger than predicted values. A partial fines dissolving model was proposed to explain this behavior. It was shown that dissolution of particles smaller than 8 μm in only about 2.8% of the recycle stream was enough for the additional size increase. Advisors/Committee Members: Randolph, Alan D (advisor), Shadman, Farhang (committeemember), Guzman, Roberto (committeemember), Raghavan, Srini (committeemember), Hiskey, J. Brent (committeemember).

Subjects/Keywords: Crystallization.

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APA (6^th Edition):

Sutradhar, B. C. (1992). Processes that make larger crystal particles. (Doctoral Dissertation). University of Arizona. Retrieved from http://hdl.handle.net/10150/185878

Chicago Manual of Style (16^th Edition):

Sutradhar, Bhagya Chandra. “Processes that make larger crystal particles. ” 1992. Doctoral Dissertation, University of Arizona. Accessed March 01, 2021. http://hdl.handle.net/10150/185878.

MLA Handbook (7^th Edition):

Sutradhar, Bhagya Chandra. “Processes that make larger crystal particles. ” 1992. Web. 01 Mar 2021.

Vancouver:

Sutradhar BC. Processes that make larger crystal particles. [Internet] [Doctoral dissertation]. University of Arizona; 1992. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10150/185878.

Council of Science Editors:

Sutradhar BC. Processes that make larger crystal particles. [Doctoral Dissertation]. University of Arizona; 1992. Available from: http://hdl.handle.net/10150/185878

University of Limerick

11. Keshavarz, Leila. The importance of impurity on pharmaceutical processes.

Degree: 2019, University of Limerick

URL: http://hdl.handle.net/10344/8485

►

peer-reviewed

Solution crystallization processes are widely treated as binary systems consisting of a solute and a solvent. For real systems, additional components such as additives… (more)

▼

peer-reviewed

Solution crystallization processes are widely treated as binary systems consisting of a solute and a solvent. For real systems, additional components such as additives and impurities may significantly impact crystallization processes even when present in very small amounts. An understanding of the mechanistic role of additives and impurities is therefore essential to design and control crystallization processes. This thesis first describes the solubility and crystallization of pure active pharmaceutical ingredients (API’s) from solution. Subsequently, it discusses the thermodynamic, kinetic and crystallization effects, caused by impurities. Eventually, these knowledge were applied to optimize impurity removal processes by using a combined experimental-modelling approach to investigate a mother-liquor recycle operation and improve properties on the processability of API. The gravimetric solubility method and how solubility models cope with industrially-relevant complex products belonging to the α-Thio-β-chloroacrylamide family which is a class of highly versatile synthetic intermediates was examined. One of the drawbacks of the gravimetric method is the evaporation of solvents which is due to elevated operating temperature or the volatile nature of the solvent itself. Solubility data at higher temperatures, beyond the atmospheric boiling point of solvents, allows for an increase in crystallization yield. A pressurized-synthetic methodology was presented as a new technique for determining high-temperature solubility data even beyond the atmospheric boiling point. With the gravimetric method in combination with HPLC analysis, the effect of impurities (4-nitrophenol and 4’-chloroacetanilide) on the solubility of paracetamol has been determined and modelled. To study the effect of volume on the nucleation kinetics of paracetamol, an automated FBRM-method was applied to record induction times. The shear rate was rationalized to be the part of the kinetic parameter that changes most significantly when changing the crystallizer type, up to a specific volume beyond which the effect becomes negligible. Induction time experiments were used in combination with the classical nucleation theory and demonstrated that the impurities employed reduced the nucleation rate. The impurities did not affect the solid−liquid interfacial energy but significantly reduced the kinetic factor. The poor compression ability of paracetamol is well known. The crystal habit of paracetamol was altered in the present of structurally similar impurity (4’-chloroacetanilide) to improve the compaction behaviour of the paracetamol crystals. An experimental design space was developed and utilized to select the most important process parameters for impurity incorporation. As a result, it was feasible to accurately control the compressibility and the amount of 4’-chloroacetanilide in the solid phase of paracetamol by simply choosing the required alcohol as the solvent for crystallization. In crystallization process, recycle of mother liquor…

Advisors/Committee Members: Frawley, Patrick J., SFI.

Subjects/Keywords: solution crystallization; API; pharmaceutical processes; crystallization

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APA (6^th Edition):

Keshavarz, L. (2019). The importance of impurity on pharmaceutical processes. (Thesis). University of Limerick. Retrieved from http://hdl.handle.net/10344/8485

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Keshavarz, Leila. “The importance of impurity on pharmaceutical processes.” 2019. Thesis, University of Limerick. Accessed March 01, 2021. http://hdl.handle.net/10344/8485.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Keshavarz, Leila. “The importance of impurity on pharmaceutical processes.” 2019. Web. 01 Mar 2021.

Vancouver:

Keshavarz L. The importance of impurity on pharmaceutical processes. [Internet] [Thesis]. University of Limerick; 2019. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10344/8485.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Keshavarz L. The importance of impurity on pharmaceutical processes. [Thesis]. University of Limerick; 2019. Available from: http://hdl.handle.net/10344/8485

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Cornell University

12. Moore, David. Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties.

Degree: PhD, Materials Science and Engineering, 2015, Cornell University

URL: http://hdl.handle.net/1813/39325

► In this work I present both a phenomenological and fundamental study of the crystallization of the organic-inorganic halide perovskites; this includes determining the overall structural… (more)

▼ In this work I present both a phenomenological and fundamental study of the crystallization of the organic-inorganic halide perovskites; this includes determining the overall structural evolution, extraction of kinetic parameters for the primary crystallization step, and establishing several processing-structure relationships. In addition, I will show examples of the application of the primary results to control crystal growth and enhance the material's performance in working devices. The organic-inorganic halide perovskites have shown great promise as a potential next generation photovoltaic (PV) material with device efficiencies exceeding 17%. For the last 2-3 years most research efforts have been dedicated to understanding the general operating principles of perovskite PV devices and engineering better device architectures. Although these efforts have resulted in an unprecedented increase in efficiencies over a very short period of time, many reports point to film or crystal morphology as a limiting factor. In order to control film and crystal growth a better understanding of this systems fundamental crystallization behavior is needed. Employing in-situ wide angle X-ray scattering allowed for the determination of the general evolution of thin films cast from solution. This initial work revealed an Ostwald Step Rule path in which the final perovskite is preceded by a solid-state precursor structure. Understanding the general evolution allowed for monitoring of the precursor-perovskite transition to establish processing-structure relationships. One such relationship is the temperature profile used in the annealing step, optimization of this profile results in better film coverage and better crystal texture, both of which increase device performance. The second major study was to elucidate the disposition of the constituent salts during crystallization and confirmed that all reagent salts are completely dissociated during film formation. This result led to the realization that the crystallization was insensitive to the lead source allowing for manipulation of the system kinetics by using alternate lead compounds. Finally, a study of the kinetics of the precursor-perovskite transition provided for the extraction of the activation energy. Combined with the previous work, the kinetics study gave the insights needed to determine a general formula for the precursor structure as well as a general pathway for the solid-state transformation. The implication of the work presented here is better control of perovskite thin film growth through manipulation of the processing and chemistry employed. Several recent reports, as well as my own experimental results, are beginning to show the value of this understanding through better films, made at lower temperatures and faster times, and providing improved performance in working PV devices. Advisors/Committee Members: Schlom, Darrell (chair), Marohn, John A. (committee member), Estroff, Lara A. (committee member), Wiesner, Ulrich B. (committee member).

Subjects/Keywords: perovskite; crystallization; kinetics

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APA (6^th Edition):

Moore, D. (2015). Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties. (Doctoral Dissertation). Cornell University. Retrieved from http://hdl.handle.net/1813/39325

Chicago Manual of Style (16^th Edition):

Moore, David. “Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties.” 2015. Doctoral Dissertation, Cornell University. Accessed March 01, 2021. http://hdl.handle.net/1813/39325.

MLA Handbook (7^th Edition):

Moore, David. “Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties.” 2015. Web. 01 Mar 2021.

Vancouver:

Moore D. Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties. [Internet] [Doctoral dissertation]. Cornell University; 2015. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1813/39325.

Council of Science Editors:

Moore D. Crystal Growth Of Organic-Inorganic Lead Halide Perovskites: Impact Of Kinetic Parameters On Morphology, Structure And Properties. [Doctoral Dissertation]. Cornell University; 2015. Available from: http://hdl.handle.net/1813/39325

University of Debrecen

13. Ime, Brendan Usoro. Development Of Plc-Controlled Crystallization Model .

Degree: DE – Természettudományi és Technológiai Kar – Fizikai Intézet, 2014, University of Debrecen

URL: http://hdl.handle.net/2437/193139

During thesis development I introduced with general concepts of crystallization and became more familiar with Czochralski crystal growth method. I designed my apparatus model for GaAs crystal growth, presented its structure, main parts and operation. Advisors/Committee Members: Misák, Sándor (advisor).

Subjects/Keywords: PLC-CONTROLLED; CRYSTALLIZATION

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APA (6^th Edition):

Ime, B. U. (2014). Development Of Plc-Controlled Crystallization Model . (Thesis). University of Debrecen. Retrieved from http://hdl.handle.net/2437/193139

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Ime, Brendan Usoro. “Development Of Plc-Controlled Crystallization Model .” 2014. Thesis, University of Debrecen. Accessed March 01, 2021. http://hdl.handle.net/2437/193139.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Ime, Brendan Usoro. “Development Of Plc-Controlled Crystallization Model .” 2014. Web. 01 Mar 2021.

Vancouver:

Ime BU. Development Of Plc-Controlled Crystallization Model . [Internet] [Thesis]. University of Debrecen; 2014. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/2437/193139.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Ime BU. Development Of Plc-Controlled Crystallization Model . [Thesis]. University of Debrecen; 2014. Available from: http://hdl.handle.net/2437/193139

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Hong Kong University of Science and Technology

14. Yip, Rebecca. Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals.

Degree: 2017, Hong Kong University of Science and Technology

URL: http://repository.ust.hk/ir/Record/1783.1-88751 ; https://doi.org/10.14711/thesis-991012571959403412 ; http://repository.ust.hk/ir/bitstream/1783.1-88751/1/th_redirect.html

► The triterpene Oleanolic Acid (C₃₀H₄₈O₃) OA-H which has poor aqueous solubility crystallizes from various organic solvents, particularly alcohols, to give solvate co-crystals. Chapter 2 describes… (more)

▼ The triterpene Oleanolic Acid (C₃₀H₄₈O₃) OA-H which has poor aqueous solubility crystallizes from various organic solvents, particularly alcohols, to give solvate co-crystals. Chapter 2 describes the preparation of a number of these solvates and their characterization by pXRD and SXRD. The control of the formation of solvated versus anhydrous phases are also discussed and appears to be controlled by the initial temperature of crystallization, with lower temperatures favoring solvates. A predicted unit cell from powder diffraction data is discussed for the oleanolic acid anhydrous phase, for which a single-crystal is difficult to obtain. In Chapter 3, the ability of oleanolic acid to form salts with various amines and its potential as a chiral resolving agent via the formation of diastereomeric salts is explored. Oleanolic acid is a chiral acid and thus it may be able to resolve racemic organic bases, hence it can be a potential resolving agent for cations. Various racemic amines were used to study the effectiveness of oleanolic acid as a resolving agent for cations. In our investigation, we discovered that oleanolic acid forms a hydrated salt when recrystallized with S-2-methylpiperidine. However, there occurs some H/Me disorder of the amine and both R- and S-isomers are incorporated in the same crystal. Thus, the S-isomer is resolved with only 50% enantiomeric excess. Whilst the 2-methylpiperidine is not well resolved, its stereoisomer – 3-methylpiperidine was also recrystallized with oleanolic acid to resolve the S-isomer, with almost 100% enantiomeric excess. Furthermore, the amine s-butylamine was also successfully resolved using oleanolic acid as a chiral resolving agent. Therefore, our studies demonstrate the great potential for oleanolic acid as a low-cost, efficient chiral resolving agent via the formation of diastereomeric salts. The use of oleanolic acid as a resolving agent is not limited to diastereomeric salt formation. Chapter 4 investigates the potential for oleanolic acid as a chiral resolving agent via the formation of co-crystals with neutral molecules. In particular, we investigate the ability of oleanolic acid to resolve chiral alcohols via cocrystallization of solvated phases, owing to oleanolic acid’s ability to form solvated phases as demonstrated in Chapter 2. Oleanolic acid was found to partially resolve (2R, 3R) 2,3-butanediol by forming a co-crystal phase whilst oleanolic acid sodium salts were able to partially resolve s-butanol. Given the potential of oleanolic acid for various applications and the importance of molecular perturbation on structural chemistry, the studies conducted in chapters 2, 3 and 4 are then expanded to oleanolic acid synthetic derivatives and similar triterpenes, ursolic acid and glycyrrhetinic acid, in Chapter 5 to study the differences in structure and crystallization that may occur when slight changes are made to the oleanolic acid structure. It was discovered that oleanolic acid derivatives appear to crystallize in different…

Subjects/Keywords: Organic solvents ; Crystallization

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APA (6^th Edition):

Yip, R. (2017). Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals. (Thesis). Hong Kong University of Science and Technology. Retrieved from http://repository.ust.hk/ir/Record/1783.1-88751 ; https://doi.org/10.14711/thesis-991012571959403412 ; http://repository.ust.hk/ir/bitstream/1783.1-88751/1/th_redirect.html

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Yip, Rebecca. “Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals.” 2017. Thesis, Hong Kong University of Science and Technology. Accessed March 01, 2021. http://repository.ust.hk/ir/Record/1783.1-88751 ; https://doi.org/10.14711/thesis-991012571959403412 ; http://repository.ust.hk/ir/bitstream/1783.1-88751/1/th_redirect.html.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Yip, Rebecca. “Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals.” 2017. Web. 01 Mar 2021.

Vancouver:

Yip R. Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals. [Internet] [Thesis]. Hong Kong University of Science and Technology; 2017. [cited 2021 Mar 01]. Available from: http://repository.ust.hk/ir/Record/1783.1-88751 ; https://doi.org/10.14711/thesis-991012571959403412 ; http://repository.ust.hk/ir/bitstream/1783.1-88751/1/th_redirect.html.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Yip R. Structural chemistry of salts, solvates and cocrystals of oleanolic acid and other pharmaceuticals. [Thesis]. Hong Kong University of Science and Technology; 2017. Available from: http://repository.ust.hk/ir/Record/1783.1-88751 ; https://doi.org/10.14711/thesis-991012571959403412 ; http://repository.ust.hk/ir/bitstream/1783.1-88751/1/th_redirect.html

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Delft University of Technology

15. Essed, A.C. (author). Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation.

Degree: 2015, Delft University of Technology

URL: http://resolver.tudelft.nl/uuid:08bfaaaa-f8a6-4fc4-8af1-3955897dc19a

► The design and operation of current industrial crystallizers is largely based on experience and practiced skills rather than sound understanding of the process. Crystallization equipment… (more)

▼ The design and operation of current industrial crystallizers is largely based on experience and practiced skills rather than sound understanding of the process. Crystallization equipment is selected from a number of state-of-art industrial crystallizers followed by optimization for that particular type of equipment. Various physical phenomena which are strongly entangled occur in these crystallizers. The current equipment-based design and optimization of crystallizers causes a lack of control over these physical phenomena. Within the TU Delft Process and Energy department, the development of a task-based design strategy has been initiated in order to obtain better control over the physical events governing the crystallizer product quality. This task-based design is a phenomena-based approach in which fundamental building blocks representing a physical process are used for design. A task based design library model was developed in gPROMS which can be applied to a wide range of crystallization processes concerning the nature of the chemical system, operation mode, flowsheet configuration and crystallizer type. However, the crystallization method is solely based on cooling crystallization. In this thesis research, the task-based design tool is extended with the crystallization method of 'membrane distillation-assisted crystallization'. The main objective was the development of a predictive model for membrane distillation-assisted crystallization with a focus on the process performance. The employed membrane distillation configuration is a 'sweeping gas membrane distillation' arrangement. A mathematical model is developed in gPROMS for the sweeping gas membrane distillation module, followed by validation with experimental obtained data. Validation of the sweeping gas membrane distillation model shows that the model results are adequate. A sensitivity analysis has been performed and compared to literature to obtain more knowledge about the performance of the employed sweeping gas membrane distillation module for this thesis. Subsequently, the sweeping gas membrane distillation model is integrated in the task-based design model library in order to develop the superstructure of membrane distillation-assisted crystallization. The developed superstructure has been validated as well with experimental obtained data in which comes forward that the membrane distillation-crystallization model performs as intended. As the membrane distillation-crystallization model performs adequately, it can be used as a predictive model tool. Since membrane distillation-assisted crystallization is a relatively new concept, case studies were performed in order to gain more insight in the process. In the case studies the membrane distillation-assisted crystallization model was performed under different circumstances. The results from the case studies can be used to aid in design and optimization of new experiments. Based on the findings of the validation procedures, sensitivity analysis and case studies, it can be concluded that the membrane… Advisors/Committee Members: Kramer, H.J.M. (mentor), Anisi, F. (mentor).

Subjects/Keywords: crystallization; membrane distillation

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APA (6^th Edition):

Essed, A. C. (. (2015). Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation. (Masters Thesis). Delft University of Technology. Retrieved from http://resolver.tudelft.nl/uuid:08bfaaaa-f8a6-4fc4-8af1-3955897dc19a

Chicago Manual of Style (16^th Edition):

Essed, A C (author). “Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation.” 2015. Masters Thesis, Delft University of Technology. Accessed March 01, 2021. http://resolver.tudelft.nl/uuid:08bfaaaa-f8a6-4fc4-8af1-3955897dc19a.

MLA Handbook (7^th Edition):

Essed, A C (author). “Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation.” 2015. Web. 01 Mar 2021.

Vancouver:

Essed AC(. Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation. [Internet] [Masters thesis]. Delft University of Technology; 2015. [cited 2021 Mar 01]. Available from: http://resolver.tudelft.nl/uuid:08bfaaaa-f8a6-4fc4-8af1-3955897dc19a.

Council of Science Editors:

Essed AC(. Modeling of Membrane Distillation-assisted Crystallization: Employing ’Sweeping Gas Membrane Distillation’ for Supersaturation Generation. [Masters Thesis]. Delft University of Technology; 2015. Available from: http://resolver.tudelft.nl/uuid:08bfaaaa-f8a6-4fc4-8af1-3955897dc19a

Massey University

16. Ibell-Pasley, Nicholas. Directional amorphous lactose crystallization.

Degree: M. Eng., Bioprocess Engineering, 2018, Massey University

URL: http://hdl.handle.net/10179/15205

► It was proposed that during industrial drying of lactose crystals a surface layer of amorphous lactose may be formed in a flash drier and then… (more)

▼ It was proposed that during industrial drying of lactose crystals a surface layer of amorphous lactose may be formed in a flash drier and then crystallized during fluid bed drying. This crystallization is hypothesized to occur in one of two directions depending on the conditions, inside-out resulting in a dry product, and outside-in trapping moisture. In the inside-out case the moisture is driven outside the product, in the outside in case this moisture would be contained by a surface layer of crystalline lactose The trapped moisture from the outside-in case is proposed to slowly diffuse through the crystal layer during storage and cause handling problems, explaining observed differences between industrial products. To investigate this scenario the crystallization of amorphous lactose was modelled, and crystallization trials were conducted to try and achieve inside-out and outside-in crystallization. William-Landel-Ferry (WLF) and Arrhenius type kinetics were found to fit literature data for amorphous crystallization. Predictions made using these models showed that amorphous lactose crystallization under the high temperature conditions in a fluid bed dryer was possible. A method for isolating the enthalpy change associated with crystallization of amorphous lactose from simultaneous thermal analysis data was developed. This method shows promise for observing the crystallization process, but it may not be suitable for amorphous lactose quantification. Two methods were designed to achieve inside-out and outside-in crystallization of amorphous lactose. This required the temperature and water activity conditions to be precisely and independently controlled in lab trials. Simultaneous thermal analysis was used to monitor the crystallization of amorphous lactose samples under these conditions. Following the simultaneous thermal analysis, the samples were monitored for moisture release. Both the inside-out and outside-in crystallized samples were observed to slowly release moisture, increasing the measured relative humidity above the expected equilibrium value. Afterwards the samples were analysed and found to still contain low levels of amorphous lactose. The source of the rise in relative humidity could not be definitively attributed to either trapped moisture or ongoing crystallization but would not be expected had crystallization not been induced. Based on these findings it is recommended that a lactose crystal fluid bed drier is operated at conditions which would not allow for amorphous lactose crystallization. These conditions could be determined using the kinetic models fitted here.

Subjects/Keywords: Lactose; Drying; Crystallization

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APA (6^th Edition):

Ibell-Pasley, N. (2018). Directional amorphous lactose crystallization. (Masters Thesis). Massey University. Retrieved from http://hdl.handle.net/10179/15205

Chicago Manual of Style (16^th Edition):

Ibell-Pasley, Nicholas. “Directional amorphous lactose crystallization.” 2018. Masters Thesis, Massey University. Accessed March 01, 2021. http://hdl.handle.net/10179/15205.

MLA Handbook (7^th Edition):

Ibell-Pasley, Nicholas. “Directional amorphous lactose crystallization.” 2018. Web. 01 Mar 2021.

Vancouver:

Ibell-Pasley N. Directional amorphous lactose crystallization. [Internet] [Masters thesis]. Massey University; 2018. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10179/15205.

Council of Science Editors:

Ibell-Pasley N. Directional amorphous lactose crystallization. [Masters Thesis]. Massey University; 2018. Available from: http://hdl.handle.net/10179/15205

University of Texas – Austin

17. Hyun, Jeongmin. Design and engineering of epitope specific antibodies.

Degree: PhD, Cell and Molecular Biology, 2016, University of Texas – Austin

URL: http://hdl.handle.net/2152/68580

► The knowledge of three-dimensional structures of membrane proteins aids in structure-based drug design, since about 60% of approved drug targets are known as membrane proteins.… (more)

▼ The knowledge of three-dimensional structures of membrane proteins aids in structure-based drug design, since about 60% of approved drug targets are known as membrane proteins. To date, chaperone-assisted protein co-crystallization that bypass the need for animal immunization is becoming an attractive method to elucidate structures of recalcitrant targets such as proteins with intrinsically disordered domains as found in membrane proteins. Here we describe antibody-engineering strategies for developing crystallization chaperones. Toward this goal, we (1) engineered EE peptide-specific single-chain variable fragment (scFv) to improve biophysical characteristics, (2) constructed synthetic single domain antibody library to be specific for targets by phage display, and (3) de novo designed FLAG peptide-specific antibodies using a novel computational method. In the first study, we converted peptide-specific scFv to antigen-binding fragment (Fab), which is the most successful format of antibody-based crystallization chaperones for integral membrane proteins so far. The larger size of Fab/EE increased the overall stability without disruption of binding affinity and extended crystal contact areas those are favorable characteristics for use as a crystal chaperone. In the second study, a 10⁶ synthetic phage display single domain antibody (sdAb) library was constructed and used to identify sdAbs binding the repeat in toxin domain of B.pertussis adenylate cyclase toxin (ACT). This protein is an intrinsically disordered calcium binding protein with no homology to any known protein structure and is a candidate vaccine antigen. From phage-based screening, we isolated three sdAbs to be used for further characterization. In the last study, we utilized an in silico approach to the design the antibodies using OptCDR that is a general computational method that employs de novo design of complementarity determining regions (CDRs) to engineer antibody-antigen interactions. Using this method, we designed CDRs binding the minimal FLAG peptide (sequence: DYKD) and isolated four antibodies with high specificity and nanomolar affinity for the DYKD. The result demonstrates that antibody specificity based on in silico design method can guide future engineering of antibody-based crystallization chaperone. Taken together, we have identified antibodies with improved binding properties and biophysical characteristics for using as crystallization chaperones without animal immunization to help guide future antibody chaperone engineering for the structural investigation of diverse target proteins. Advisors/Committee Members: Maynard, Jennifer A., 1974- (advisor), Hoffman, David W. (committee member), Keatinge-Clay, Adrian T. (committee member), Webb, Lauren J. (committee member), Barrick, Jeffrey E. (committee member).

Subjects/Keywords: Antibody; Crystallization chaperone

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APA (6^th Edition):

Hyun, J. (2016). Design and engineering of epitope specific antibodies. (Doctoral Dissertation). University of Texas – Austin. Retrieved from http://hdl.handle.net/2152/68580

Chicago Manual of Style (16^th Edition):

Hyun, Jeongmin. “Design and engineering of epitope specific antibodies.” 2016. Doctoral Dissertation, University of Texas – Austin. Accessed March 01, 2021. http://hdl.handle.net/2152/68580.

MLA Handbook (7^th Edition):

Hyun, Jeongmin. “Design and engineering of epitope specific antibodies.” 2016. Web. 01 Mar 2021.

Vancouver:

Hyun J. Design and engineering of epitope specific antibodies. [Internet] [Doctoral dissertation]. University of Texas – Austin; 2016. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/2152/68580.

Council of Science Editors:

Hyun J. Design and engineering of epitope specific antibodies. [Doctoral Dissertation]. University of Texas – Austin; 2016. Available from: http://hdl.handle.net/2152/68580

Cape Peninsula University of Technology

18. Tshilumbu, Nsenda Ngenda. Design and development of a novel high performance emulsion explosive using nanoparticles .

Degree: 2014, Cape Peninsula University of Technology

URL: http://etd.cput.ac.za/handle/20.500.11838/930

► This study investigated water-in-oil (W/O) super-concentrated emulsions used as pumpable explosives. The aqueous phase of the emulsions is a supersaturated nitrate salt solution (at room… (more)

▼ This study investigated water-in-oil (W/O) super-concentrated emulsions used as pumpable explosives. The aqueous phase of the emulsions is a supersaturated nitrate salt solution (at room temperature), with a volume fraction of approximately 0.9. Instability of such emulsions arises either from crystallization of the dispersed phase in the system during ageing or under high shear conditions. Here, we report an alternative approach to stabilize this highly concentrated W/O emulsion by adding colloidal particles in combination with short amphiphilic molecules. Thus, the primary goal of this research concerned a phenomenological study of the dependence of surfactant-to-particle ratio as well as the particle hydrophobicity index on stability under high shear in the emulsification process, rheological properties and stability against initiation of crystallization of an internal phase both with ageing and under high shear with a view to optimize the time to the start of crystallization of the emulsion both with ageing and under high shear; to elucidate the mechanism of initiation of crystallization of an internal phase (homogeneous or heterogeneous) and shed light in the stabilization mechanism of the emulsion; to determine how the emulsion formulation content affect pumping characteristics as measured by characteristic rheological parameters. A series of five fumed silica nanoparticles, each with a different hydrophobicity index (HI) in the range of 0.60 – 3, were used in the form of single types of particles as well as binary mixtures. These particles were combined with a low molecular weight conventional surfactant, Sorbitan MonoOleate (SMO), into the oil phase prior to emulsification. It has been found that regardless of the particle hydrophobicity, fumed nanosilica alone cannot form highly concentrated W/O emulsion up to 90 vol%. Moreover, Pickering emulsions are unstable under shear conditions and thus it is difficult to make highly concentrated W/O pumpable emulsion explosives using only fumed nanosilica. The correlation between the refinement time and SMO-to-particle ratio showed a deflection point/transitional point in the stabilization mechanism. Below the transitional point the silica content dominates over SMO. Conversely, above the transitional point the particles have little effect and the SMO dominates. A thermodynamic consideration revealed that in this region only SMO is likely to adsorb at the W/O interface and controls the emulsifying process. As with refinement time, the correlation between the shear modulus and SMO/particle ratio shows a deflection /transitional point which, as before, mark the transition point between regions of particle or SMO domination. Interestingly, it was found that for each HI, the initiation of crystallization is the most delayed, both on shelf life and under high shear, when the emulsion is prepared with an SMO-to-particle ratio equaling exactly the value at this transitional point. Moreover, the research demonstrated that a drastic change in mechanism of initiation of…

Subjects/Keywords: Emulsions; Rheology; Crystallization; Nanoparticles

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APA (6^th Edition):

Tshilumbu, N. N. (2014). Design and development of a novel high performance emulsion explosive using nanoparticles . (Thesis). Cape Peninsula University of Technology. Retrieved from http://etd.cput.ac.za/handle/20.500.11838/930

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Tshilumbu, Nsenda Ngenda. “Design and development of a novel high performance emulsion explosive using nanoparticles .” 2014. Thesis, Cape Peninsula University of Technology. Accessed March 01, 2021. http://etd.cput.ac.za/handle/20.500.11838/930.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Tshilumbu, Nsenda Ngenda. “Design and development of a novel high performance emulsion explosive using nanoparticles .” 2014. Web. 01 Mar 2021.

Vancouver:

Tshilumbu NN. Design and development of a novel high performance emulsion explosive using nanoparticles . [Internet] [Thesis]. Cape Peninsula University of Technology; 2014. [cited 2021 Mar 01]. Available from: http://etd.cput.ac.za/handle/20.500.11838/930.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Tshilumbu NN. Design and development of a novel high performance emulsion explosive using nanoparticles . [Thesis]. Cape Peninsula University of Technology; 2014. Available from: http://etd.cput.ac.za/handle/20.500.11838/930

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

University of Tasmania

19. Tuck, Kenneth Edward. The kinetics of sucrose crystallization.

Degree: 1968, University of Tasmania

URL: https://eprints.utas.edu.au/21790/1/whole_TuckKennethEdward1968_thesis.pdf

► This study has been undertaken for two main purposes:- (1)To obtain factual information concerning the rate of growth of sucrose crystals; and (2)To secure some… (more)

▼ This study has been undertaken for two main purposes:- (1)To obtain factual information concerning the rate of growth of sucrose crystals; and (2)To secure some understanding of the operating mechanism of factors influencing crystal growth. Chapter 3 records details of the experimental method used and data gathered for actual growth rates. Associated with these in chapter 2 is set down information believed to have a significant bearing on the mechanism study. For the mechanism study growth has been looked upon as a physical rate process bearing certain analogies to chemical reactions and mathematical treatment has been carried out with this in mind, it being effectively a kinetic study in an essentially physical system. Chemical kinetics has to do with the study of rates of chemical reactions and of the influence of conditions upon these rates. The most important experimental conditions are concentrations (or pressures) of reacting substances, temperature, presence of a catalyst and radiation. In the case of sucrose crystallization the chemical reaction theory is transferred to the physical rate process. The kinetics of sucrose crystallization thus concerns the rate of crystallization of sucrose and the influence of conditions such as concentrations, temperature and impurities. Crystallization is a process in which the solute molecules move from the solution to the surface of the growing crystal and incorporate themselves into the crystal lattice. The relative influence of the crystal surface and mother liquor may then be examined in the light of rate process kinetics. The Arrhenius equation, which is the basis of kinetic studies, for chemical reactions may be stated, k = A e-E/RT where k is the velocity constant in the chemical reaction. In the current studies k is used in this equation as the velocity of crystallization of sucrose and is essentially the physical rate constant of concern in this system. A plot of log k v. 1/T is linear and the activation energy of crystallization (E) may be calculated from the slope of the line. The constant A in the Arrhenius relationship is essentially a frequency factor in chemically reacting systems and its study has been suitably incorporated in the activated complex theory of reaction rates. While some possible analogies are recognised, the full implications are not insisted upon in the present studies. The crystallization of sucrose consists of two consecutive stages, firstly, nuclei formation; and secondly, crystal growth. These current studies are essentially concerned with the latter growth process only. When studying chemically reacting systems, the chemical potential or driving force is the difference between the concentration of reacting material on the one hand and the concentration of the product on the other. In the system of crystallizing sucrose, the driving force is the difference between the concentration of the oversaturated solution and that of a saturated solution. In this thesis supersaturation (S) is defined as the ratio of the…

Subjects/Keywords: Sucrose; Crystallization

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APA (6^th Edition):

Tuck, K. E. (1968). The kinetics of sucrose crystallization. (Thesis). University of Tasmania. Retrieved from https://eprints.utas.edu.au/21790/1/whole_TuckKennethEdward1968_thesis.pdf

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Tuck, Kenneth Edward. “The kinetics of sucrose crystallization.” 1968. Thesis, University of Tasmania. Accessed March 01, 2021. https://eprints.utas.edu.au/21790/1/whole_TuckKennethEdward1968_thesis.pdf.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Tuck, Kenneth Edward. “The kinetics of sucrose crystallization.” 1968. Web. 01 Mar 2021.

Vancouver:

Tuck KE. The kinetics of sucrose crystallization. [Internet] [Thesis]. University of Tasmania; 1968. [cited 2021 Mar 01]. Available from: https://eprints.utas.edu.au/21790/1/whole_TuckKennethEdward1968_thesis.pdf.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Tuck KE. The kinetics of sucrose crystallization. [Thesis]. University of Tasmania; 1968. Available from: https://eprints.utas.edu.au/21790/1/whole_TuckKennethEdward1968_thesis.pdf

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

University of Michigan

20. Ahn, Seokhoon. Two-Dimensional Crystallization from Multicomponent Solutions.

Degree: PhD, Chemistry, 2011, University of Michigan

URL: http://hdl.handle.net/2027.42/84439

► Most crystallizations conducted in contexts from the laboratory to industrial production involve multicomponent solutions yielding one or more phases. Because of the importance of such… (more)

▼ Most crystallizations conducted in contexts from the laboratory to industrial production involve multicomponent solutions yielding one or more phases. Because of the importance of such processes in purification and solid form engineering, understanding these crystallization behaviors is one of the greatest outstanding scientific challenges. Here a novel approach to studying this issue is explored, namely studying two-dimensional (2D) crystallization at the liquid/solid interface where the reduced dimensionality dramatically simplifies the system. During the course of investigations of 2D crystallization of aromatic primary amides bearing para substituents with long alkyl chains, a highly symmetric pattern was observed. This structure is in the plane group of p6 and contains rhombic voids even though the molecular symmetry of amide amphiphiles is Cs. These amide amphiphiles overcome the barrier to symmetry generation through forming an aggregate as a building block. This result demonstrates that a high symmetry pattern is achievable from a low symmetry building block through a proper combination of noncovalent interactions. Based on the hypothesis that amphiphile molecules can give rise to various aggregation modes potentially leading to different monolayers, 2D crystallization of an amide amphiphile containing a C18 alkyl-chain was conducted at the liquid/graphite interface. This amide amphiphile showed the ability to exist in six different forms: three close-packed structures and three nanoporous structures. The amide amphiphile was further employed to understand the phenomenon recently observed in three-dimensional crystallization that metastable polymorphs could be obtained during attempts to grow cocrystals with additives. The same phenomenon was able to be reproduced in two-dimensional crystallization from binary solutions while attempting to induce coadsorption. During the competition study between the amide amphiphile and other additive molecules, the formation of different metastable phases depending on the additive molecules was observed these are discussed in the context of kinetics and thermodynamics. During the competition study between the amide amphiphile and diheptadecyl phthalate, a new type of cocrystal that displays random mixing along one axis and periodic ordering along the other axis was discovered. The characteristics and formation process of this “1D-cocrystal” were examined by STM and computational models. The nature of this crystallization behavior is discussed. Advisors/Committee Members: Matzger, Adam J. (committee member), Banaszak Holl, Mark M. (committee member), Chen, Zhan (committee member), Goldman, Rachel S. (committee member).

Subjects/Keywords: Two-dimensional Crystallization; Chemistry; Science

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Ahn, S. (2011). Two-Dimensional Crystallization from Multicomponent Solutions. (Doctoral Dissertation). University of Michigan. Retrieved from http://hdl.handle.net/2027.42/84439

Chicago Manual of Style (16^th Edition):

Ahn, Seokhoon. “Two-Dimensional Crystallization from Multicomponent Solutions.” 2011. Doctoral Dissertation, University of Michigan. Accessed March 01, 2021. http://hdl.handle.net/2027.42/84439.

MLA Handbook (7^th Edition):

Ahn, Seokhoon. “Two-Dimensional Crystallization from Multicomponent Solutions.” 2011. Web. 01 Mar 2021.

Vancouver:

Ahn S. Two-Dimensional Crystallization from Multicomponent Solutions. [Internet] [Doctoral dissertation]. University of Michigan; 2011. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/2027.42/84439.

Council of Science Editors:

Ahn S. Two-Dimensional Crystallization from Multicomponent Solutions. [Doctoral Dissertation]. University of Michigan; 2011. Available from: http://hdl.handle.net/2027.42/84439

Cornell University

21. Asenath Smith, Emily. Bio-Inspired Crystallization Of Oxides In Inorganic Matrices.

Degree: PhD, Materials Science and Engineering, 2015, Cornell University

URL: http://hdl.handle.net/1813/40624

► The energy crisis facing our planet requires solutions that take an interdisciplinary approach to the improvement of existing energy systems as well as the development… (more)

▼ The energy crisis facing our planet requires solutions that take an interdisciplinary approach to the improvement of existing energy systems as well as the development of new energy sources. Moreover, the composition of the materials is important: thermally- and chemically-stable materials based on abundant, non-toxic elements are needed to support the sustainability of both the technology and our environment. Biological organisms present multiple examples of hierarchical structures that are optimized for a given function. In particular, biomineralized materials: (i) display crystallographic control across length scales; (ii) are often organic-inorganic composites due to the occlusion of components from the associated organic growth matrix; (iii) and exhibit tailored mechanical properties that are unique to their function. Of great importance to the development of advanced energy materials is the observation that biomineral architectures are built from crystallographically-defined structural elements with interfaces that span multiple length scales. Synthetically, the translation of biological mineralization strategies to oxide compounds is hindered by the low melting temperatures of biopolymer hydrogels that compose extracellular matrices. In order to successfully crystallize oxide compounds using a (bio-inspired) matrix-mediated approach, I had to identify and develop a hydrogel system with thermal stability and chemical compatibility to the growth conditions needed for the oxide. By moving to inorganic networks based on silica, I achieved a thermally-stable growth matrix. By forming these networks at low pH, I obtained a growth environment that was compatible with the crystallization of hematite. With these two features, hematite was crystallized under diffusion-limited conditions, which provided a means to to manipulate its structure and assembly from the atomic- to the microscale. By combining inductively coupled plasma atomic emission spectroscopy with Rietveld refinements to x-ray diffraction data, expansion of the hematite lattice along the c-axis was found to be correlated to increasing silicon in the crystals and the preferential growth of the coherent domains along [110] (perpendicular to the strained c-axis). Using single particle manipulation in a focused ion beam system, electron-transparent thin sections were prepared from precisely-defined geometric locations within the hematite crystals for analysis by transmission electron microscopy. Quantitative analysis on selected area electron diffraction patterns was used to unravel the net orientation of the hematite lattice with respect to the quasi-spherical form and to calculate the misorientation (mosaicity) between the coherent domains. The combined results of these analyses showed that silicon from the growth environment had consistently modified the architecture of hematite, from the atomic to the microscale, leading to microscale structures with surfaces composed of nanoscale, high catalytic activity {110} facets. With hydrogel growth as a… Advisors/Committee Members: Estroff,Lara A. (chair), Disalvo,Francis J (committee member), Gruner,Sol Michael (committee member).

Subjects/Keywords: Biomineralization; Crystallization; Transition Metal Oxides

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APA (6^th Edition):

Asenath Smith, E. (2015). Bio-Inspired Crystallization Of Oxides In Inorganic Matrices. (Doctoral Dissertation). Cornell University. Retrieved from http://hdl.handle.net/1813/40624

Chicago Manual of Style (16^th Edition):

Asenath Smith, Emily. “Bio-Inspired Crystallization Of Oxides In Inorganic Matrices.” 2015. Doctoral Dissertation, Cornell University. Accessed March 01, 2021. http://hdl.handle.net/1813/40624.

MLA Handbook (7^th Edition):

Asenath Smith, Emily. “Bio-Inspired Crystallization Of Oxides In Inorganic Matrices.” 2015. Web. 01 Mar 2021.

Vancouver:

Asenath Smith E. Bio-Inspired Crystallization Of Oxides In Inorganic Matrices. [Internet] [Doctoral dissertation]. Cornell University; 2015. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1813/40624.

Council of Science Editors:

Asenath Smith E. Bio-Inspired Crystallization Of Oxides In Inorganic Matrices. [Doctoral Dissertation]. Cornell University; 2015. Available from: http://hdl.handle.net/1813/40624

University of Michigan

22. Li, Zi. Manipulating Solubility and Dissolution through Multicomponent Crystallization.

Degree: PhD, Chemistry, 2016, University of Michigan

URL: http://hdl.handle.net/2027.42/133485

► Chemical entities can be arranged into different packing motifs, leading to variation in properties of solid materials. Therefore, solid form optimization is a critical approach… (more)

▼ Chemical entities can be arranged into different packing motifs, leading to variation in properties of solid materials. Therefore, solid form optimization is a critical approach to material development. Here crystallization systems with multiple components are investigated to improve performance of materials. Cocrystallization is a technique to optimize solid forms by introducing a neutral coformer to form multicomponent crystal with the target molecule; this method shows great potential to improve the dissolution of poorly soluble compounds. A novel carbamazepine /p-aminobenzoic acid 4:1 cocrystal is discovered and structurally characterized. Phase stability data demonstrate that it is a thermodynamically unstable form. According to the dissolution experiments, cocrystal stoichiometry is not the only factor that determines the dissolution rate; intermolecular interactions within the crystal play a vital role. Solid state studies of a class of nitric oxide releasing S-nitroso-N-acetyl-D-penicillamine (SNAP)-doped polymer materials are conducted to investigate the stability mechanism. Crystalline SNAP is detected in polymers and a crystallization based theory is proposed wherein SNAP molecules are partially solubilized in polymers, and the excess SNAP beyond the solubility limit crystallizes and embeds in the polymer. Solubility of SNAP in polymer has been determined by PXRD analysis. It is proposed that the lattice energy of crystalline SNAP is the key to the stability improvement, while the solubilized SNAP is more reactive that decomposes and releases NO. This crystallization based hypothesis has been tested in other SNAP/polymer composites. It is proposed that the unsuccessful cocrystallization between target compound and a poorly soluble coformer with accessible synthons can be a kinetic result of the coformer solubility limit, which favors the formation of single component crystals that compete with the hypothetical cocrystals. In order to retain a high degree of coformer supersaturation in solution favorable for cocrystallization, soluble polymeric additives were employed. It was demonstrated that solubility and metastable limit of poorly soluble compounds can be altered in presence of soluble polymers. Therefore, utilization of polymer additives is a feasible approach to adjust the metastable zone width which is a potential strategy to facilitate the growth of unattainable cocrystals. Advisors/Committee Members: Matzger, Adam J (committee member), Rodriguez-Hornedo, Nair (committee member), Biteen, Julie Suzanne (committee member), McNeil, Anne Jennifer (committee member).

Subjects/Keywords: crystallization; solubility; dissolution; Chemistry; Science

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Li, Z. (2016). Manipulating Solubility and Dissolution through Multicomponent Crystallization. (Doctoral Dissertation). University of Michigan. Retrieved from http://hdl.handle.net/2027.42/133485

Chicago Manual of Style (16^th Edition):

Li, Zi. “Manipulating Solubility and Dissolution through Multicomponent Crystallization.” 2016. Doctoral Dissertation, University of Michigan. Accessed March 01, 2021. http://hdl.handle.net/2027.42/133485.

MLA Handbook (7^th Edition):

Li, Zi. “Manipulating Solubility and Dissolution through Multicomponent Crystallization.” 2016. Web. 01 Mar 2021.

Vancouver:

Li Z. Manipulating Solubility and Dissolution through Multicomponent Crystallization. [Internet] [Doctoral dissertation]. University of Michigan; 2016. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/2027.42/133485.

Council of Science Editors:

Li Z. Manipulating Solubility and Dissolution through Multicomponent Crystallization. [Doctoral Dissertation]. University of Michigan; 2016. Available from: http://hdl.handle.net/2027.42/133485

23. Prabu marachen, A. Studies on the crystallization and characterization of thiourea and its complexes;.

Degree: 2015, Manonmaniam Sundaranar University

URL: http://shodhganga.inflibnet.ac.in/handle/10603/38409

►

The search for nonlinear optical materials has been of great interest because of their significant impact on laser technology optical communication and optical data storage… (more)

Subjects/Keywords: characterization; crystallization; physics; thiourea

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APA (6^th Edition):

Prabu marachen, A. (2015). Studies on the crystallization and characterization of thiourea and its complexes;. (Thesis). Manonmaniam Sundaranar University. Retrieved from http://shodhganga.inflibnet.ac.in/handle/10603/38409

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Prabu marachen, A. “Studies on the crystallization and characterization of thiourea and its complexes;.” 2015. Thesis, Manonmaniam Sundaranar University. Accessed March 01, 2021. http://shodhganga.inflibnet.ac.in/handle/10603/38409.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Prabu marachen, A. “Studies on the crystallization and characterization of thiourea and its complexes;.” 2015. Web. 01 Mar 2021.

Vancouver:

Prabu marachen A. Studies on the crystallization and characterization of thiourea and its complexes;. [Internet] [Thesis]. Manonmaniam Sundaranar University; 2015. [cited 2021 Mar 01]. Available from: http://shodhganga.inflibnet.ac.in/handle/10603/38409.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Prabu marachen A. Studies on the crystallization and characterization of thiourea and its complexes;. [Thesis]. Manonmaniam Sundaranar University; 2015. Available from: http://shodhganga.inflibnet.ac.in/handle/10603/38409

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Stellenbosch University

24. Matthews, Megan Esme. Crystallisation behaviour of commercial polyethylenes: a fundamental study.

Degree: PhD, Chemistry and Polymer Science, 2018, Stellenbosch University

URL: http://hdl.handle.net/10019.1/104839

►

ENGLISH ABSTRACT: Commercial films are generally made of polyolefins, often using a blend of two different polyolefins. Specifically, low density polyethylene (LDPE) and linear low… (more)

▼

ENGLISH ABSTRACT: Commercial films are generally made of polyolefins, often using a blend of two different polyolefins. Specifically, low density polyethylene (LDPE) and linear low density polyethylene (LLDPE) are blended due to the mechanical strength of LLDPE and the processability of LDPE. However the behaviour of these blends is unpredictable due to the lack of understanding of the underlying processes which determine the final properties. This study focused on developing an understanding of the interactions between LDPE and LLDPE in the blended form through the crystallisation behaviour of the blends. The criteria for co-crystallisation are presented and systematically investigated in order to determine whether the blends meet the criteria. By analysing the blend miscibility in the melt, the crystal structure of the individual blend components as well as the crystallisation kinetics, conclusions can be made about the co-crystallisation potential of LDPE/LLDPE blends. Melt miscibility was investigated by using fluorescent labelling of both polymer components and tracking their movements after the blending process. No isolated domains could be detected with fluorescence microscopy indicating that phase separation did not occur during the melt blending process. However, differential scanning calorimetry (DSC) displayed a number of different crystalline environments which implied that phase separation occurred during the crystallisation process. DSC was also used to verify this through kinetics and showed that the LLDPE crystallised at a faster rate than the LDPE, making co-crystallisation unlikely. Solid state nuclear magnetic resonance (SS NMR) was used to probe the phase separation within the blends and was used to identify a number of different regions which had formed within the amorphous and interfacial areas which seemed to be the cause of the interactions. This disproved the hypothesis that the difference in rate and extent of crystallisation directly affected the ultimate blend properties but rather showed that the amorphous and interfacial regions determine blend behaviour.

AFRIKAANSE OPSOMMING: Kommersiële films bestaan hoofsaaklik uit poliolefiene en meestal uit ‘n samestelling van twee verskillende poliolefiene. Spesifieke verwysing word gemaak na die samestelling van lae digtheid poliëtileen (LDPE) en liniêre lae digtheid poliëtileen (LLDPE) as gevolg van die meganiese sterkte van LLDPE en die verwerkbaarheid van LDPE. Die werkverrigtinge van hierdie samestellings is onvoorspelbaar as gevolg van ‘n gebrek aan begrip oor die onderliggende prosesse wat die finale eienskappe daarvan bepaal. Die fokus van hierdie studie is om begrip te ontwikkel van die interaksie tussen LDPE en LLDPE in ‘n samestellende vorm, deur die kristallisasie van die samestellings. Die kriteria vir ko-kristallisasie word voorgelệ en sistematies ondersoek om te bepaal of die samestellings aan die vereistes voldoen. ‘n Ontleding van die mengbaarheid van die samestelling in die smeltsel, die kristalstruktuur…

Advisors/Committee Members: Van Reenen, Albert, Stellenbosch University. Faculty of Science. Dept. of Chemistry and Polymer Science..

Subjects/Keywords: UCTD; Polyethylene; Crystallization; Polyolefins

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Matthews, M. E. (2018). Crystallisation behaviour of commercial polyethylenes: a fundamental study. (Doctoral Dissertation). Stellenbosch University. Retrieved from http://hdl.handle.net/10019.1/104839

Chicago Manual of Style (16^th Edition):

Matthews, Megan Esme. “Crystallisation behaviour of commercial polyethylenes: a fundamental study.” 2018. Doctoral Dissertation, Stellenbosch University. Accessed March 01, 2021. http://hdl.handle.net/10019.1/104839.

MLA Handbook (7^th Edition):

Matthews, Megan Esme. “Crystallisation behaviour of commercial polyethylenes: a fundamental study.” 2018. Web. 01 Mar 2021.

Vancouver:

Matthews ME. Crystallisation behaviour of commercial polyethylenes: a fundamental study. [Internet] [Doctoral dissertation]. Stellenbosch University; 2018. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10019.1/104839.

Council of Science Editors:

Matthews ME. Crystallisation behaviour of commercial polyethylenes: a fundamental study. [Doctoral Dissertation]. Stellenbosch University; 2018. Available from: http://hdl.handle.net/10019.1/104839

University of Johannesburg

25. Thandiswa Florence, Bodoza. The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation.

Degree: 2012, University of Johannesburg

URL: http://hdl.handle.net/10210/5357

►

M.Tech.

The study into the effect of additives used in nickel powder precipitation by sodium hypophosphite has been carried out. Reduction experiments were conducted in… (more)

▼

M.Tech.

The study into the effect of additives used in nickel powder precipitation by sodium hypophosphite has been carried out. Reduction experiments were conducted in a 10 L stainless steel batch reactor fitted with 3 baffles, 4-bladed axial impeller, heating element, thermocouple and thermostat. Nickel seed was used to initiate the reduction process, sodium hypophosphite was used as a reducing agent, and ammonia solution was used to adjust pH, poly(ethylene-comaleic anhydride) (EMA) was used as the first additive and poly(acrylic acid) (PA) as the second additive. Reduction experiments were conducted at a temperature between 60 °C to 70 °C, pH around 8 and a reaction time of 3 min. Synthetic nickel sulfate solution and sodium hypophosphite solutions at concentration of 0.5 g/L were used as nickel feed solution and reducing agent, respectively. Additives were investigated at high and low concentrations of 5 mg/L and 10 mg/L. The effect of additives on reduction behavior of nickel was investigated by studying the evolution of the volume distribution, moments, specific surface area, and rate of reduction and purity of the powder product. EMA was found to be a growth promoter and PA was found to be a growth inhibitor. The highest reduction rate was observed in the presence of EMA and the lowest in the presence of PA. The SEM micrographs of the powder obtained in the presence of EMA and PA showed that the powder was spherical shaped, open, dentritic and more porous compared with that of the seed particles. Both additives were found to increase the pore size of the powder particles. The presence of particle fragments observed in the scanning electron micrographs confirmed breakage as one of the major particulate process. The addition of additives significantly affected the volume distribution at lower concentrations of 5 mg/L. The extent of aggregation increased with increasing dosages of PA and decreased with increasing dosages of EMA. The highest specific surface area was obtained in the presence of 5 mg/L of EMA.

Subjects/Keywords: Crystallization; Nickel powder precipitation

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APA (6^th Edition):

Thandiswa Florence, B. (2012). The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation. (Thesis). University of Johannesburg. Retrieved from http://hdl.handle.net/10210/5357

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Thandiswa Florence, Bodoza. “The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation.” 2012. Thesis, University of Johannesburg. Accessed March 01, 2021. http://hdl.handle.net/10210/5357.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Thandiswa Florence, Bodoza. “The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation.” 2012. Web. 01 Mar 2021.

Vancouver:

Thandiswa Florence B. The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation. [Internet] [Thesis]. University of Johannesburg; 2012. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10210/5357.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Thandiswa Florence B. The effect of poly (crylic acid) and poly (ethyleneco-maleic anhydride) on nickel powder precipitation. [Thesis]. University of Johannesburg; 2012. Available from: http://hdl.handle.net/10210/5357

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

University of Toronto

26. Naeini, Alireza Tabatabaei. Visualization of the Crystallization in Foam Extrusion Process.

Degree: 2012, University of Toronto

URL: http://hdl.handle.net/1807/33701

►

In this study, crystal formation of polypropylene (PP) and poly lactic acid (PLA) in the presence of CO2 in foam extrusion process was investigated using… (more)

Subjects/Keywords: Visualization; Crystallization; Foam Extrusion; 0548

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APA (6^th Edition):

Naeini, A. T. (2012). Visualization of the Crystallization in Foam Extrusion Process. (Masters Thesis). University of Toronto. Retrieved from http://hdl.handle.net/1807/33701

Chicago Manual of Style (16^th Edition):

Naeini, Alireza Tabatabaei. “Visualization of the Crystallization in Foam Extrusion Process.” 2012. Masters Thesis, University of Toronto. Accessed March 01, 2021. http://hdl.handle.net/1807/33701.

MLA Handbook (7^th Edition):

Naeini, Alireza Tabatabaei. “Visualization of the Crystallization in Foam Extrusion Process.” 2012. Web. 01 Mar 2021.

Vancouver:

Naeini AT. Visualization of the Crystallization in Foam Extrusion Process. [Internet] [Masters thesis]. University of Toronto; 2012. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1807/33701.

Council of Science Editors:

Naeini AT. Visualization of the Crystallization in Foam Extrusion Process. [Masters Thesis]. University of Toronto; 2012. Available from: http://hdl.handle.net/1807/33701

Cape Peninsula University of Technology

27. Tchibouanga, Remi Rolland Ngoma. Salts and cocrystals of substituted phenylacetic acids .

Degree: 2018, Cape Peninsula University of Technology

URL: http://etd.cput.ac.za/handle/20.500.11838/2857

► The prediction of the single crystal structure that will form due to the combination of two or more compounds to form a multicomponent crystal is… (more)

▼ The prediction of the single crystal structure that will form due to the combination of two or more compounds to form a multicomponent crystal is one of the important areas of research in crystal engineering. Since these compounds display different properties when combined as a single crystal, knowledge of synthesis and design of the resulting compound is essential. The formation of a multicomponent crystal, such as a salt or a cocrystal generally depends on the complementarity of the functional groups present on both components. This means that basicity and acidity of the functional groups present on the selected compounds need to be considered. This study investigated salts and cocrystals of 3-chloro-4-hydroxyphenylacetic acid (CHPAA) using the ΔpKa rule. The calculated ΔpKa values were recorded and correlated with the experimental analysis in predicting the outcome of the crystallisation experiments ie. salt or cocrystal formation. This was further confirmed by the analysis of the C-O bond lengths found in the crystal structures. Salts were obtained by combinations of CHPAA with several organic bases (co-formers) such as diethylamine, dibutylamine, 2-aminopyridine, 2-amino-4-methylpyridine, 2-amino-6-methylpyridine and 4-dimethylaminopyridine. The calculated ΔpKa values were within the range of salt formation. Furthermore, the experimental analysis also showed that all resulting compounds were salts. Cocrystals were obtained by reactions of nicotinamide, isonicotinamide, phenazine and 4,4’-bipyridine with CHPAA. Again, the calculated ΔpKa values predicted cocrystals as the new solid forms. Experimental analysis carried out also confirmed cocrystal formation. For all resulting compounds, the comparison of intermolecular interactions as well as supramolecular synthons were reported. All compounds were synthesised by slow evaporation techniques using various organic solvents and characterised by single crystal X-ray diffraction, powder X-ray diffraction, thermal analysis and Fourier transformer infrared spectroscopy. From the structural analysis, it was found that all resulting structures displayed strong N-H•••O and O-H•••O intermolecular interactions including weak interactions of C-H•••Cl, C-H•••O and C-H•••π for a few of the structures. Furthermore, comparison of the crystal structures showed that no packing arrangement similarity existed between the compounds. Advisors/Committee Members: Jacobs, Ayesha, Prof (advisor).

Subjects/Keywords: Phenylacetic acid; Crystallization; Salts

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APA (6^th Edition):

Tchibouanga, R. R. N. (2018). Salts and cocrystals of substituted phenylacetic acids . (Thesis). Cape Peninsula University of Technology. Retrieved from http://etd.cput.ac.za/handle/20.500.11838/2857

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Tchibouanga, Remi Rolland Ngoma. “Salts and cocrystals of substituted phenylacetic acids .” 2018. Thesis, Cape Peninsula University of Technology. Accessed March 01, 2021. http://etd.cput.ac.za/handle/20.500.11838/2857.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Tchibouanga, Remi Rolland Ngoma. “Salts and cocrystals of substituted phenylacetic acids .” 2018. Web. 01 Mar 2021.

Vancouver:

Tchibouanga RRN. Salts and cocrystals of substituted phenylacetic acids . [Internet] [Thesis]. Cape Peninsula University of Technology; 2018. [cited 2021 Mar 01]. Available from: http://etd.cput.ac.za/handle/20.500.11838/2857.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Tchibouanga RRN. Salts and cocrystals of substituted phenylacetic acids . [Thesis]. Cape Peninsula University of Technology; 2018. Available from: http://etd.cput.ac.za/handle/20.500.11838/2857

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

28. Krawczynski, Michael J. Experimental studies of melting and crystallization processes in planetary interiors.

Degree: 2011, MIT and Woods Hole Oceanographic Institution

URL: http://hdl.handle.net/1912/4837

► Melting and crystallization processes on the Earth and Moon are explored in this thesis, and the topics of melt generation, transport, and crystallization are discussed… (more)

Subjects/Keywords: Crystallization of water; Magmas

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Krawczynski, M. J. (2011). Experimental studies of melting and crystallization processes in planetary interiors. (Thesis). MIT and Woods Hole Oceanographic Institution. Retrieved from http://hdl.handle.net/1912/4837

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Chicago Manual of Style (16^th Edition):

Krawczynski, Michael J. “Experimental studies of melting and crystallization processes in planetary interiors.” 2011. Thesis, MIT and Woods Hole Oceanographic Institution. Accessed March 01, 2021. http://hdl.handle.net/1912/4837.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

MLA Handbook (7^th Edition):

Krawczynski, Michael J. “Experimental studies of melting and crystallization processes in planetary interiors.” 2011. Web. 01 Mar 2021.

Vancouver:

Krawczynski MJ. Experimental studies of melting and crystallization processes in planetary interiors. [Internet] [Thesis]. MIT and Woods Hole Oceanographic Institution; 2011. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/1912/4837.

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

Council of Science Editors:

Krawczynski MJ. Experimental studies of melting and crystallization processes in planetary interiors. [Thesis]. MIT and Woods Hole Oceanographic Institution; 2011. Available from: http://hdl.handle.net/1912/4837

Note: this citation may be lacking information needed for this citation format:
Not specified: Masters Thesis or Doctoral Dissertation

University of Houston

29. Bandara, Randeniya Adikaram Mudiyanselage Subhani Samanmali 1983-. Developing a strategy to enhance protein crystallization using metal chelate complexes.

Degree: PhD, Biochemistry, 2014, University of Houston

URL: http://hdl.handle.net/10657/1642

► The ability to solve the structures of important proteins can be enhanced by increasing the probability of obtaining suitable crystals. Co-crystallization of the proteins with… (more)

▼ The ability to solve the structures of important proteins can be enhanced by increasing the probability of obtaining suitable crystals. Co-crystallization of the proteins with metal-chelate complexes (MCCs) show promise in achieving this goal. In this study, six lanthanide ligand complexes, [Tb(HDPA)3]3- , [Tb(DPA)3]3-, [Tb(HDPA)3-n(DPA)n]n=0-3, [Gd(DTPA)]2-, [Eu(DOTA-4Amc)]- and [Tm(DOTP)]5- were used in crystallization trials with eight test proteins, concanavalin A, glucose isomerase, beta amylase, alpha lactalbumin, thermolysin, lipase B, lysozyme and streptavidin under customized grid screens to observe their ability to enhance crystallization of the proteins. A new crystal form of the streptavidin-biotin complex (C222) was facilitated by co-crystallization with [Tb(DPA)3]3- under conditions that were not previously reported for the protein. The crystal composed of sheets of streptavidin molecules held together by [Tb(DPA)3]3- complexes along the vertical 2-fold axes. Likewise this type of symmetric, rigid complexes can favor the bridging of symmetry related protein molecules and provide a symmetry point for the crystal on which to build. Also, it is evident that the [Tb(DPA)3]3- complexes are involved in interactions important to expand the lattice in the third dimension. Similarly a novel crystal form for concanavalin A was obtained in the presence of [Tb(HDPA)3]3- in the tetragonal space group P43212. The 4-hydroxyl groups of the ligands in [Tb(HDPA)3]3- could allow these complexes to interact with each other in addition to protein molecules. These inter-complex Interactions formed a network of [Tb(HDPA)3]3- complexes in the concanavalin A crystal, providing a stronger surface for the protein molecules to interact with and to build into a lattice. In addition, [Tb(HDPA)3-n(DPA)n]n=0-3, [Gd(DTPA)]2-, [Eu(DOTA-4Amc)]- and [Tm(DOTP)]5- promoted crystallization of the proteins under conditions, different from that of previously reported crystal structures. Co-crystallization with the metal-chelate complexes has the added advantage of incorporating lanthanides, which are strong anomalous scatterers that can be used to solve the structure by anomalous dispersion. Additionally, fluorescence microscopy could be used to separate protein crystals from small molecule crystals of certain MCCs. In conclusion, the lanthanide chelate complexes can enhance protein crystallization via introducing crystal contacts and/or by promoting nucleation. Advisors/Committee Members: Fox, Robert O. (advisor), Briggs, James M. (committee member), Williams, Cecilia M. (committee member), Gilbertson, Scott R. (committee member).

Subjects/Keywords: Proteins; Crystallization; Metal-chelate complexes

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Bandara, R. A. M. S. S. 1. (2014). Developing a strategy to enhance protein crystallization using metal chelate complexes. (Doctoral Dissertation). University of Houston. Retrieved from http://hdl.handle.net/10657/1642

Chicago Manual of Style (16^th Edition):

Bandara, Randeniya Adikaram Mudiyanselage Subhani Samanmali 1983-. “Developing a strategy to enhance protein crystallization using metal chelate complexes.” 2014. Doctoral Dissertation, University of Houston. Accessed March 01, 2021. http://hdl.handle.net/10657/1642.

MLA Handbook (7^th Edition):

Bandara, Randeniya Adikaram Mudiyanselage Subhani Samanmali 1983-. “Developing a strategy to enhance protein crystallization using metal chelate complexes.” 2014. Web. 01 Mar 2021.

Vancouver:

Bandara RAMSS1. Developing a strategy to enhance protein crystallization using metal chelate complexes. [Internet] [Doctoral dissertation]. University of Houston; 2014. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/10657/1642.

Council of Science Editors:

Bandara RAMSS1. Developing a strategy to enhance protein crystallization using metal chelate complexes. [Doctoral Dissertation]. University of Houston; 2014. Available from: http://hdl.handle.net/10657/1642

Boston University

30. Stevens, Carl Alden. Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers.

Degree: PhD, Philosophy, 1961, Boston University

URL: http://hdl.handle.net/2144/19149

Subjects/Keywords: Transducers; Crystallization

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6^th Edition):

Stevens, C. A. (1961). Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers. (Doctoral Dissertation). Boston University. Retrieved from http://hdl.handle.net/2144/19149

Chicago Manual of Style (16^th Edition):

Stevens, Carl Alden. “Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers.” 1961. Doctoral Dissertation, Boston University. Accessed March 01, 2021. http://hdl.handle.net/2144/19149.

MLA Handbook (7^th Edition):

Stevens, Carl Alden. “Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers.” 1961. Web. 01 Mar 2021.

Vancouver:

Stevens CA. Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers. [Internet] [Doctoral dissertation]. Boston University; 1961. [cited 2021 Mar 01]. Available from: http://hdl.handle.net/2144/19149.

Council of Science Editors:

Stevens CA. Consideration of certain vibrational modes of polarized multi-resonant barium titanate transducers. [Doctoral Dissertation]. Boston University; 1961. Available from: http://hdl.handle.net/2144/19149

Open Access Theses and Dissertations