Personal Update: A Plea To Fellow Chemists
I am at a point of desperation that yes, I have resorted to sending a call for help into the abyss that is the internet. Will it go somewhere? Probably not, but this is just as much a vent of frustration as it is a call for help.
My group bought a GC/MS (Agilent 7820A/5975C). I had used one sparingly in my undergraduate career, but really this is what I would call my first time really using one. We’ve had it for a few months, and I can fairly easily create methods and quantitate results for solids and liquids.
Too bad someone at the lab decided they wanted me to test a gas…
This gas is CF3I with some contaminants in it of unknown origin (short chain, heavily halogenated alkanes). The experiment is trying to eliminate the contaminants, and after trying something new they want an analysis done to see what effect their efforts had. They had the first couple analyzed by a contract lab so they knew what they were looking for, and after that had one of the grad students at a university do the measurements. However, now that they supposedly have the option of getting it done on site, they want me to do it.
They told me what the 3 largest contaminants were, and I purchased bottles of those pure gases. Using those, I was able to come up with a method that would successfully separate all of them, so qualitative data isn’t a problem.
I cannot for the life of me make reliable reference gases.
Every time I think I’ve managed to make a reference gas out of one of the 3 (I’m using nitrogen as the matrix), I get a peak on my first injection, but then nothing in any subsequent injections, like the analyte mysteriously all came out of the vial in that first shot.
I in no way thought that I would be the first person to try to make a reference gas, so silly me thought I could easily find a reference somewhere on how to properly do it. Either I’m the first person to try to make a reference gas, or the other people who do it are so excited they figured it out they want to keep the secret for themselves. I can’t find help anywhere, and I have yet to find another scientist at this lab or our sister lab who measures gases.
So, if you happen to have any ounce of knowledge on measuring gases via GC/MS, for the love of all that is good in this world please share it with me. My boss and I are at the point where we look at the GC and burst into tears. Okay, we don’t actually cry, but we talk about how much we want to cry. That’s like the same thing.