Process of Precipitation and Crystallization

NAME OF THE COURSE Process of Precipitation and Crystallization

Code

KTA321

Year of study

3.

Course teacher

Assoc Prof Dražan Jozić

Credits (ECTS)

3.0

Associate teachers

Type of instruction (number of hours)

P S V T

30

0

0

0

Status of the course

Elective

Percentage of application of e-learning

0 %

COURSE DESCRIPTION

Course objectives

Students acquire the basics of the different crystalline states and their arrangements as well as the fundamentals of the processes of nucleation, precipitation and crystallization under different experimental conditions (water solution and melts). The knowledge acquired to allow students applying acquired knowledge in composing reaction mixtures as well as control of the experimental conditions for obtaining the final materials required physical and chemical properties.

Course enrolment requirements and entry competences required for the course

Enrolled in or passed the course Exercises in Process of Precipitation and Crystallization

Learning outcomes expected at the level of the course (4 to 10 learning outcomes)

After passing the exam the student will be able to:
- Able to choose on the base of the physical and chemical properties suitable solvent
- Can choose a suitable precipitant agent for providing the process of precipitation
- Know the basic methods and procedures of dissolutions, precipitation and crystallization
- Known procedures and methods of recrystallization and purification of the product
- Basic knowledge about the industrial equipment for the crystallization process

Course content broken down in detail by weekly class schedule (syllabus)

1. Week. The crystalline state (Liquids crystals, Crystalline solids, Crystal symmetry, Crystal systems, Miller indices)
2. Week. Space lattice, Solid state bonding, Isomorphs and polymorphs, Enentiomorphs and chirality,
3. Week. Cristal habit, Dendrites, Composite crystals and twins, Imperfections in crystals
4. Week. Physical and thermal properties (Density, Viscosity, Surface tension, Diffusivity, Refractive index, Electrolytic conductivity),
5. Week. Physical and thermal properties (Crystal hardness, Unit of heat, Heat capacity, Thermal conductivity, Boiling freezing and melting points, Enthalpies of phase change, Heats of solution and crystallization, Size classification of crystals)
6. Week. Solution and solubility (Solutions and melts, Solvent selection, Expression of solution composition, Solubility correlations, Theoretical crystal yield, Ideal and non-ideal solutions, Particle size and solubility,),
7. Week. Solution and solubility (Effect of impurities on solubility, Measurement of solubility, Prediction of solubility, Solubility data sources, Supersolubility), Phase equilibria (The phase rule, One-component systems, Two-component systems, Enthalpy-composition diagrams, Phase change detection)
8. Week. The First colloquium
9. Week. Phase equilibria (Three-component systems, Four-component systems, Dynamic phase diagrams)
10. Week. Nucleation (Primary nucleation, Secondary nucleation, Metastable zone widths, Effect of impurities, Induction and latent periods, Interfacial tension, Ostwald’s rule of stages),
11. Week. Crystal growth (Crystal growth theories, Growth rate measurements, Crystal growth and dissolution, Crystal habit modification, Polymorphs and phase transformations, Inclusions),
12. Week. Recrystallization (Recrystallization schemes, Resolution of racemates, Isolation of polymorphs, Recrystallization from supercritical fluids, Zone refining, Single crystals),
13. Week. Industrial techniques and equipment (Precipitation, Crystallization from melts, Sublimation, Crystallization from solution),
14. Week. Crystallizer design and operation (Crystal size distribution, Kinetic data measurement and utilization, Crystallizer specification, Fluid-particle suspension)
15. Week. The Second colloquium

Format of instruction:

Student responsibilities

Class attendance at the lecture in the amount of 70% to 100%, and to experimental work of 100% from total hours.

Screening student work (name the proportion of ECTS credits for eachactivity so that the total number of ECTS credits is equal to the ECTS value of the course):

Class attendance

1.0

Research

0.0

Practical training

0.0

Experimental work

0.0

Report

0.0

0.3

Essay

0.0

Seminar essay

0.0

 

 

Tests

0.6

Oral exam

0.6

 

 

Written exam

0.5

Project

0.0

 

 

Grading and evaluating student work in class and at the final exam

The exam can be finished over the two tests during the semester. Minimum for successful tests is the limit of the 50% resolved test. Each test in assessing participates with a share of the 40% of the final grade. Presence at lectures 70-100% participates with a share of the 5% of the final grade while the presence of the laboratory exercises from 100% participates with a share of the 15% of the final grade. The examination periods there is a written and oral exam. Minimum for successful written exam is the limit of the 50% resolved test. Passing one test (previous activity) is valuable in the summer semester examination period with a share of the 15% of the final grade. Written exam has a share of the 25% and verbal has a share of the 40% of the final grade. Students who have not passed any tests during the semester they take the examination through written and oral exams in the regular examination period. Minimum for successful tests the limit of the 50% resolved test. Written part of exam and oral part of exam participates with a share of the 50% of the final grade.
The final grade: 50%-61% - sufficient, 62%-74% - good, 75%-87% very good, 88%-100% - excellent.

Required literature (available in the library and via other media)

Title

Number of copies in the library

Availability via other media

J.W. Mullin, Crystallization, Fourth Edition, University of London, Butterworth-Heinemann, Linacre House, Jordan Hill, Oxford, 2001.

0

van V. Markov, Crystal growth for beginners, Fundamentals of Nucleation, Crystal Growth and Epitaxy, Word Scientific Publishing Co.Pte.Ltd. London, 1995.

0

C.M.Van t Land, Industrial Crystallization of Melts, Marcel Dekker, New York, 2005.

0

Optional literature (at the time of submission of study programme proposal)

Selected articles from journals recommended by lecturer

Quality assurance methods that ensure the acquisition of exit competences

Tracking suggestions and reactions of students throughout the semester
Student survey

Other (as the proposer wishes to add)