Ian Salveson: Research Log

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June 15, 2016

Determine the effect of flow rate on product formation. Figure 1 below shows similar reactions with differing flow rates.

Figure 1

This figure shows flow rate has a small effect on product formation. This experiment was done at 2 additional concentrations with similar results.

June 16, 2016

Concentration of acetaminophen is increased in preparation for Flash Chromatography. Figure 1 below shows the effect of increasing concentration on product formation.

Figure 1

It appears that at higher concentrations, the reaction will begin to form polymeric material, despite relatively low concentrations of Hydrogen Peroxide.

Sample B will be separated using Flash Chromatography.

It is important to note that we have reached the max absorbance of our instrument.

Figure 2 below shows a set of samples under identical conditions as Figure 1 except with a flow rate of 2 ml/min.

Figure 2

The chromatography on this figure is faulty, specifically the changing retention time. The results also contradict what may have been expected of a faster flow rate. These samples should be run again if the data is deemed significant.

June 20, 2016

Sample C from June 16th was Lyophilized and reconstituted in a solution of 90% water and 10% ACN. This solution was filtered and analyzed once more using the HPLC see if any product was lost.

Prepped-APAP062016.jpg

June 22, 2016

Peformed flash Chromotography on the prepped APAP sample from 6/20. Was able to collect a nonstandard peak. Below is a chromatogram of the complete mixture shown with the peak collected through flash.

APAP Flash 062216.jpg

There appear to be two impurities which are unaccounted for in the complete mixture.