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.

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Posted on February 15, 2012, in Personal and tagged , . Bookmark the permalink. 3 Comments.

  1. Sadddd… the last time I did GC/MS was in undergrad… I wish I knew how to help you… That sounds so frustrating… Where did it go?! How can you not get any more peaks? Can it be getting stuck on the column or something (I don’t see how…)? My only advice is to check the scale on the readout because I have a friend who was doing HPLC and the scale was set really weird. So it looked like she had no peaks except at the injection point… It’s probably terrible advice but that’s all I got. 😦 Boooo reference gases… Why are you sad?

    • Yeah, absolutely no explanation for the disappearing peak. I don’t think it can be a scale problem since it wouldn’t show up to being with then, and I spent most of today trying to prove that the container leaks so after I puncture it to take a sample the the rest just kind of leaks out (but instead I proved those suckers are air tight…).

      It’s incredibly frustrating because this is the first project outside of our group who asked for help, and I’m still bumbling around like an idiot because I can’t calibrate the instrument since I can’t make a stupid reference. They have to think we’re just stupid or something.

      Thanks for the support 🙂

      • Boooo… Sorry it’s so complicated. I hate it when people ask you for help and then it turns out to be ridiculously hard… I know the feeling. My cells kept dying when I was trying to do some experiment for this other lab and they must have thought I was stupid too… I was just like whyyyyyyy do you dieeeee?!?!?!?! Arggggh. I hope you figure out the problem soon.

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