ferrocene lab - David Grauer November 5 2007 CHM 371...

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David Grauer November 5, 2007 CHM 371 – Ferrocene Synthesis and Physical Properties of the pi-bonded organometallic compound: Ferrocene Introduction : This lab was centered on the compound ferrocene and its oxidized twin, ferrocinium. It was essentially split into two parts, synthesis of the two compounds and physical analysis of the two to determine their similarities and differences. Physical analysis was performed using FT-IR, UV-Vis and NMR spectroscopies as well as magnetic susceptibility. Please refer to the lab notebook pages 1-2 for Synthesis pre-lab. Instrumentation Pre-Lab NMR: We prepared six sample tubes each with varying concentrations of ferrocene and ferrocinium to determine the exchange constant between the two. Our data came in the form of different peak widths and shift values. These were used in the rate constant equation along with the varying solution concentrations. A diagram of the 300 MHz NMR machine follows. UV-Vis: UV-Vis spectroscopy samples were prepared for both ferrocene and ferrocinium. UV- Vis allows for the determination of a molecular orbital scheme. The EM radiation causes electronic transitions, which; in the data correspond to absorbances at specific wavelengths of light. A diagram of the UV-Vis spectrometer follows.
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FT-IR: We did not prepare our own IR samples. The IR data allows for the identification of functional groups in a sample by using the vibrational transitions induced by IR radiation. In our case, IR allowed to differentiate ferrocene from ferrocinium as well as identify any potential contaminants. A diagram follows. Magnetic Susceptibility: The magnetic susceptibility machine allows one to see if a sample is paramagnetic or diamagnetic based on whether it responds to a magnetic field. In our case, ferrocene was shown to be diamagnetic (all paired electrons) while ferrocinium responded to a magnetic field and was therefore paramagnetic. A diagram follows. Reaction Apparatus 1: This apparatus is a distillation apparatus essentially. It was used to heat the dicyclopentadiene splitting it into two cyclopentadienes. Once the dimer was split, removal of the methylene proton could proceed. A diagram follows. Reaction Apparatus 2: This apparatus was used for the removal of the proton as well as the coordination of iron with the two Cp rings. The apparatus isolated the reactions from the air so that side reactions were limited. This apparatus supplied us with ferrocene. A diagram follows.
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Sublimation Chamber: The sublimation chamber was used to purify the crude ferrocene synthesized beforehand. The ferrocene was heated then crystallized on the sides of the sublimation chamber. A diagram follows. Data Collection: Partner: Anna Deroo Mass error ~ +/- .1 mg FT-IR Spectrum : (error ~ +/- 5 cm -1 ) Ferrocinium 50 55 60 65 70 75 80 85 90 95 100 0 500 1000 1500 2000 2500 3000 3500 4000 Ferrocene 70 75 80 85 90 95 100 0 500 1000 1500 2000 2500 3000 3500 4000
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Ferrocene Observed: Peaks (cm -1 ) Strength 3100 S 1700 Broad, M 1450 S 1100 S 1000 S 800 S 490 S Ferrocene Expected Peaks (cm -1 ) Strength 3085 S 1758 M 1720 M 1411 S 1108 S 1002 S 811 S
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