info_CHEM463Zwntr10.manualv6

info_CHEM463Zwntr10.manualv6 - CHEMISTRY 463 Winter 2010...

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C HEMISTRY 463 Winter 2010 Spectroscopic Techniques for Structural Identification Dr. Tomikazu Sasaki Department of Chemistry University of Washington
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2 Table of Contents 1. Introduction Page 3 2. IR Instrumentation Page 6 3. IR Sample Preparation Page 10 4. IR Operation Page 13 5. UV Instrumentation Page 16 6. UV Sample Preparation Page 21 7. UV Operation Page 23 8. MS Instrumentation Page 25 9. MS Sample Preparation Page 32 10. MS Operation Page 33 11. NMR Instrumentation Page 42 12. NMR Sample Preparation Page 53 13. NMR Operation Page 55 14. Appendix Page 69 A: Sample Unknown Report B: Sample Preparation (quick version) C: Miscellaneous Chemistry 460 Handouts
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3 1. INTRODUCTION Chemistry 463 involves the identification of organic molecules by combining the information from nuclear magnetic resonance (NMR) spectroscopy, infrared (IR) spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, and mass spectrometry (MS). These four spectroscopies are the major tools used in the identification of chemicals. NMR, IR, and UV-Vis involve various portions of the electromagnetic spectrum. The table below shows the relationships between energy ( E ), wavelength ( ), and type of transition for several spectral regions of interest. Recall the equations: E = hv and v = c where h = Planck’s constant, c = the speed of light, and = frequency. REGION UV VIS IR RADIOFREQUENCY Energy (cal/mol) ~ 10 5 10 4 -10 5 ~ 10 3 – 10 4 <10 -3 Wavelength ( ) 200 - 400 nm 400 - 800 nm 2 - 16 m 5 X 10 7 m Type of Transition Electronic Excitation Electronic Excitation Vibrational Excitation Nuclear Spin Transition Information content conjugation functional groups connectivity Optical Spectroscopy N M R The purpose of this book is to provide the necessary information for Chemistry 463 students to acquire useful spectra from the specific instruments to which they have access. Brief background information on the theory and mechanics of operation of the instruments is also provided. For more detailed information on interpreting spectra, refer to the book by Lambert, et. al. Other textbooks of general interest are listed below.
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4 Acknowledgment: Many thanks to Jim Patterson for his assistance in preparing this manual. General References: Lambert, J.B., Shurvell, H. F., Lightner, D. A., Cooks, R. G. Organic Structural Spectroscopy. New Jersey: Prentice Hall, 1998. Pavia, D. L., Lampman, G. M., and Kriz Jr., G. S. Introduction to Spectroscopy . Philadelphia: Saunders College Publishing, 1979. Silverstein, R. M., Bassler, G. C., and Morril, T. C. Spectroscopic Identification of Organic Compounds, Fifth Edition. New York: John Wiley & Sons, Inc., 1991. Williams, D. H. and Fleming, I. Spectroscopic Methods in Organic Chemistry, Third Edition. London: McGraw-Hill, 1980. Instrumentation: Braun, R. D. Introduction to Instrumental Analysis. New York: McGraw Hill, 1987. Williard, H. H., Merrit, Jr., L. L., Dean, J. A., and Settle, Jr., F. A. Instrumental Methods of Analysis, Seventh Edition. Belmont, California: Wadsworth Publishing Company, 1988.
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This note was uploaded on 03/06/2010 for the course CHEM 463 taught by Professor Staff during the Spring '08 term at University of Washington.

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info_CHEM463Zwntr10.manualv6 - CHEMISTRY 463 Winter 2010...

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