This week has been mainly devoted to attempting to determine if liquid cell 1 and or 2 is working properly, i.e. see if thermal fluid is leaking into the liquid cells. As I talked about in last week summary (there is some crossover between weeks) we changed out the Teflon caps for both 1 & 2 and lowered the level of the thermal fluid in hopes that this would prevent the thermal fluid from leaking in. We ran a KCl solution in liquid cell 2 and found contamination of thermal fluid after a 5-85C run after 24h, and then we ran a DI water solution in liquid cell 1 for the same 5-85C run and after 24h found no contamination. This gave us some hope and I prepared another KCl solution in hopes to calibrate liquid cell 1. I ran liquid cell 1 with the KCl solution, but found, 24h later, that there was an error with the ministat so I reran the solution the next day, letting the liquid cell sit for a total of 48h. I found that upon removal that liquid cell 1’s solution was contaminated with thermal fluid. On the possibility that both liquid cells are non-operational, Allison has decided to intervene and determine for herself if liquid cell 1 is out of order.
In the mean time I have been looking into Karl-Fischer titrations and prepared an operation procedure for the vacuum oven.