|Phosphorylation Lab||Main project page|
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A silica gel column was prepared to purify the crude ruthenium complex. Glass wool was used to plug the bottom of the column (with a little bit of water). After the water had been drained, about 1 cm of sand was poured into the flask so that the glass wool was completely covered in sand. 300mL silica gel was mixed with ~400mL acetonitrile-sodium nitrate saturated solution. After the mixture had reacted and settled, the gel mixture was poured into the column. The column material was allowed to settle. When no significant change had occurred, the stopcock was opened and air (pressure) was added to help the packing settle. The liquid was drained so that the top was dry. The sample was then added to the column followed by about 1 cm of sand. The column was filled with acetonitrile (saturated with sodium nitrate) solution. The acetonitrile solution was used until the large band appeared to have stopped moving. Pressure (air) was used to run the column efficiently while also using a little less liquid. Then, 90% acetonitrile solution was used until the large dark-orange band was collected. The column was then dried by draining all the liquid and adding pressure (air) for a few hours. The ruthenium band that was collected was rotovapped.
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