Showing posts with label chromatography. Show all posts
Showing posts with label chromatography. Show all posts

Saturday, September 16, 2006

Plumbing better than Mario and Luigi

Instead of dealing with large green pipes you have to jump into,



I have to deal with peristaltic pump tubing.

These little tubes are used to carry liquids into the mass spec. Other people use them too, such as chemists who use HPLC, IC, and SFA.

About twice a month, I have to run an analysis called FIAS or TTRA. Too make a long expanation short, the samples are mixed with buffer (pH 5.5) and internal standard (Y, In, Tb) all "online", then pushed through a column with an affinity resin that grabs the transition metals and lets the group I metals pass through. Then, the column is washed with acid, which rinses the transition metals into the mass spec which sorts them and counts them.



The way the literature describes to do this was unecessarily complicated. It explained using a sample loop and employing a water line to wash the column. It involved two valves, two pumps, four peristaltic pump lines, a double six-way valve, and finally the column.That's the way I did it and it worked for a while, but eventually it stopped working properly and I couldn't fix it. So instead of spending multiple days troubleshooting, I decided to just completely start over and re-think the whole thing.

I re-plumbed it much more simple and straight forward. Both valves, half of the double six-way valve, and the water line ended up being unnecessary. Now, loads of para-film were no longer needed to prevent leaks in the peristaltic pump tube connections. Also, less sample is used.



Tuesday, May 23, 2006

Backwards chromatography with Mass Spec


I've been trying to run the FIAS analysis for three days now, the column just doesn't seem to be doing its job. I think the problem might be that I have it backwards. I believe the way the flow should be is into the large end and out the small end. This way, the front of the column will bind the most metals, then, when the flow reverses to rinse the metals off the column with dilute acid, the metals will be at the end of the column, so they come off together.