C5380 Special Laboratory Techniques

Faculty of Science
Autumn 2013
Extent and Intensity
1/0/0. 1 credit(s) (fasci plus compl plus > 4). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
Teacher(s)
RNDr. Miloš Černík, CSc. (lecturer)
Guaranteed by
RNDr. Miloš Černík, CSc.
Department of Chemistry - Chemistry Section - Faculty of Science
Supplier department: Department of Chemistry - Chemistry Section - Faculty of Science
Timetable
Tue 15:00–15:50 C12/311
Prerequisites
C1100 Introductory Chemistry Lab
Succesful completion of basic courses in inorganic, organic and physical chemistry.
Course Enrolment Limitations
The course is also offered to the students of the fields other than those the course is directly associated with.
fields of study / plans the course is directly associated with
Course objectives
This lecture covers special techniques intended for the syntesis and characterization of air-sensitive, highly corrosive or thermally unstable compounds, including high-vacuum line, inert-atmosphere bench-top technique and preparative cryochemistry methods. In addition, the high pressure/temperature synthetic chemistry, sonochemistry, photochemical and electric-discharge syntheses are briefly surveyed. At the end of this course, students should understand the principles of various inert-atmosphere laboratory techniques and have a basic knowledge of their technical background. They should be able to choose an appropriate technique or procedure for the manipulation of a selected air-sensitive compound and decide, how to properly and safely handle substances with diverse properties, e.g. reactive gases, moisture-sensitive compounds or volatile and pyrophoric reagents.
Syllabus
  • 1. Manipulations of air-sensitive compounds in an inert atmosphere. Inert gases and their purification. Detection of moisture and oxygen.

    2. Inert atmosphere glove boxes. Basic dry box construction. Attainment and maintenance of inert atmosphere. Working inside a dry box. Polyethylene glove bag.

    3. Components of air-less glassware. Ground-glass joints and stopcocks. Vacuum greases and their physical and chemical properties. Greaseless joints and glass/teflon valves. O-rings elastomers and their chemical compatibility.

    4. Vacuum in the chemical laboratory. Rotary oil-sealed pumps and diaphragm vacuum pumps. Diffusion pump and its attaching to a vacuum system. Theory of pumping. Vacuum gauges. Leak detection and location.

    5. Bench-top techniques. The inert gas/vacuum double manifold. Principles of Schlenk techniques. Schlenk type glassware. Syringe and cannula techniques.

    6. Apparatus constructed from Schlenk glassware. Basic operations under an inert atmosphere: measuring out reagents, transferring solvents, magnetic and mechanical stirring, filtration, distillation, sublimation, Soxhlet extraction.

    7. General design and function of the high-vacuum line. The pumping station and the main vacuum manifold. The working manifold. Pressure gauges.

    8. Operations on the high-vacuum line. Manipulation of condensable gases and volatile liquids. Transfer and quantitative measurement of noncondensable gases. Separation of volatile compounds. Determination of vapor pressures, melting points and molecular weights.

    9. Manipulation of corrosive fluorides and other highly reactive compounds. Chemical compatibility of construction materials. Metal and plastic valves and tubing joints. Vacuum systems for manipulation of volatile fluorides. Sampling of corrosive compounds in IR, Raman and NMR spectroscopy.

    10. Solvents and reagents. Purifying and drying of solvents. Safe handing of compressed gases. Generation and purification of reagent gases. Liquefied gases as solvents.

    11. Matrix isolation spectroscopy - a technique for the study of reactive species. Matrices materials and their properties. Preparation of matrices with unstable particles. Spectra of matrix - isolated species.

    12. Principles of preparation cryochemistry. Classification of gaseous particles suitable for cryochemical experiments. Construction of cryochemical reactors. Cryochemical synthesis with metal vapour. Cryochemistry of high-temperature generated molecular species.

    13. Specialized equipment and techniques in inorganic synthesis. High pressure reactions. Sonochemistry. Electric-discharge synthesis. Photochemical reactions with UV radiation. Selective stimulation of chemical reactions by infrared laser.
Literature
  • PŘÍHODA, Jiří a Miloš ČERNÍK a Slávka JANKŮ a Jaromír LITERÁK. Laboratorní technika. Příručka pro začínajícího chemika. 1. vydání. Brno: Masarykova univerzita, 2012. 221 s. ISBN 978-80-210-5820-0
  • Errington R. J.: Advanced Practical Inorganic and Metalorganic Chemistry, Blackie Academic and Professional, London 1997.
  • Shriver D.F., Drezdzon M. A.:The manipulation of air-sensitive compounds, 2nd Edn., Wiley, New York 1986..
  • Wayda A. L., Darensbourg M.Y.,Eds.: Experimental Organometallic Chemistry, ACS Symposium Series 357, American Chemical Society, Washington, DC 1987
  • Plesch P. H.: High vacuum techniques for chemical syntheses and measurements, Cambridge Univ. Press, New York 1989, ISBN 0-521-25756-5.
  • Jolly W.L., The synthesis and characterization of inorganic compounds, Prentice-Hall, Inc., Englewood Cliffs, N. J. 1970
  • Moskovits M., Ozin G.A., Eds., Cryochemistry, John Wiley and Sons. Inc., New York 1976.
Teaching methods
Lectures
Assessment methods
Oral examination
Language of instruction
Czech
Further Comments
The course can also be completed outside the examination period.
The course is taught annually.
The course is also listed under the following terms Autumn 2007 - for the purpose of the accreditation, Autumn 1999, Autumn 2000, Autumn 2001, Autumn 2002, Autumn 2003, Autumn 2004, Autumn 2005, Autumn 2006, Autumn 2007, Autumn 2008, Autumn 2011, Autumn 2011 - acreditation, Autumn 2012.
  • Enrolment Statistics (recent)
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