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Microwave Spectroscopy of Complexes

A puzzle of many pieces
by

Maria Javier

on 15 January 2013

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Transcript of Microwave Spectroscopy of Complexes

Synthesis of Deuterated Propiolic Acid, C-D Propiolic Acid Microwave Spectroscopy Spectrometer 3 Synthesis of 3 Deutero Ortho-Difluorobenzene (ODFB) SCHS Maria Javier http://www.colorado.edu/physics/2000/waves_particles Electromagnetic Radiation Microwave Spectroscopy of Complexes D Obj.1. Synthesize deuterated Propiolic Acid, C-D Propiolic Acid. Purification with Na2SO4 anhydrous Acetylene dicarboxylic acid monopotassium salt in deuterated water (D2O) under N2 (vacuum distillation) Work up with HCl, dH2O, and solvent extraction with ether Synthesis of C-D Propiolic Acid. Obj.2. Use microwave spectroscopy to detect lines and transitions for the C-D Propiolic Acid. Lines were observed at different frequencies and modes from the synthesized propiolic acid. Some Spectral Frequencies of C-D Propiolic Acid Day 3 Day 2 Day 1 Spectrometer 3 Assembly and Testing Troubleshooting continued
System pumped
Pressure readings Troubleshooting Problem: Mirror does not slide back
Lubricate 3 shafts
Adjust cylinder beads
Tighten screws
Add spring Assembly
Vacuum (forepump and vacuum gauge)
Thermostat gauge (pressure inside chamber)
Hoses (cold water inlet and outlet to prevent overheating
System Test wtt-pro.nist.gov Signals found using frequencies
6716.627- difuorobenzene (main isotopologue)
6706.122- 1,2 difluorobenzene
6634.865- 4, 5 difluorobenzene
Signal not found at frequency 6618.543 in 10000 shots for
3,6 difluorobenzene Difluorobenzene Runs Day 6 Day 5 Day 4 Spectrometer 3 Assembly and Testing Testing
Cable check
Connections check Troubleshooting continued
Parts assembly
System pumped
System good Troubleshooting Continued
System disassembly
Parts cleaning Day 8 Day 7 Day 9-11 Spectrometer 3 Assembly and Testing Testing
Run Difluorobenzene Troubleshooting continued
Parts assembly
System pumped
System good Testing
Argon attached
System go Obj. 3. Assemble and
Test Spectrometer 3. Synthesis of Para Deuterofluorobenzene D D OR Obj.4. Synthesize 3 deutero orthro-difluorobenzene (ODFB). Dry with silica gel; perform Nuclear Magnetic Resonance Prepare sodium methoxide Synthesize ODFB (Hine and Langford) Synthesis of 3 Deutero Ortho-Difluorobenzene D Obj.5. Synthesize para-deuterofluorobenzene using Grignard reaction. Run para deuterofluorobenzene in microwave spectrometer 1 and 3 Prepare DCl (Bak, Christensen, Tannenbaum) Synthesize para deuterofluorobenzene (Mg and parabromofluorobenzene to produce Grignard reagent) Synthesis of Para Deuterofluorobenzene
Deborah Kimball
Peggy Humbert
Dr. Lisa Elfring
Dr. Silvia Ronco Dr. Stephen Kukolich
Dr. Ming Sun
Brian Sargus
Greg Porter
Erik Mitchell
SpencerCarey Acknowledgements Paperwork/
Processes Group Meeting Microwave Spectroscopy Classes/NMR Training Practice Lab Techniques Peroxidizable Compounds vacuum distillation; vacuum sublimation; dry box utilization (operation and substance transfer) Base Bath safety training; University forms (DSV);
CAT card and key acquisition progress report on present project; next step lecture on microwave spectroscopy; homework involving calculations (e.g. center of mass, moment of inertia, rotation constants, etc.); NMR testing of several organic compounds for formation of peroxides neutralization for disposal; make up new batch; cleaning glassware Maintenance, practice, and processes Other Lab Activities + D2O
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