![[personal profile]](https://www.dreamwidth.org/img/silk/identity/user.png){kind=small}
Blaaaaaaaaarg
Sep. 15th, 2010 09:52 pmToday was an incredibly busy and yet spectacularly unproductive day. John from the machine shop came up with an airtight cap for the NMR rotors and I was testing it last night on some starting material I got from another lab. (We didn't have any cheap, air sensitive starting materials with good NMR handles that weren't going to catch fire).
Well, I got in this morning and found that the spinning had gone nuts overnight. Even though it had been spinning quite stably for a couple hours when I left. Grr.
So we tried to get it spinning again by using some standards we had lying around that we knew spun well. Yeah... no. So I sighed and went to pack my standard in the next size down so we could use that probe instead. It meant that we couldn't use the fancy new cap but we had an improvised system that I knew could buy us 24 hours of the compound not dying horribly. The spinning is a bit touchier on that one, but it works once it's going. I was doing calibrations and things were going fine until I actually started trying to calibrate tin.
Yeah, one scan with the proton decoupling on "barely there" and the probe started to arc. This probe has had this problem before and John tried to fix it, but we knew his fix was just buying us time. So yeah, that time is up and we need to replace a part.
Mat got John up to try to fix the spinning on the first probe. He cleaned it and it SORTA works. Some rotors spin and some don't. So now the plan is to use that one and hope the rotor I put my sample in works.
I'm learning so much about troubleshooting spectrometer issues!
Maybe tomorrow I'll actually get data. On my third day of having the spectrometer. Yeah.
Well, I got in this morning and found that the spinning had gone nuts overnight. Even though it had been spinning quite stably for a couple hours when I left. Grr.
So we tried to get it spinning again by using some standards we had lying around that we knew spun well. Yeah... no. So I sighed and went to pack my standard in the next size down so we could use that probe instead. It meant that we couldn't use the fancy new cap but we had an improvised system that I knew could buy us 24 hours of the compound not dying horribly. The spinning is a bit touchier on that one, but it works once it's going. I was doing calibrations and things were going fine until I actually started trying to calibrate tin.
Yeah, one scan with the proton decoupling on "barely there" and the probe started to arc. This probe has had this problem before and John tried to fix it, but we knew his fix was just buying us time. So yeah, that time is up and we need to replace a part.
Mat got John up to try to fix the spinning on the first probe. He cleaned it and it SORTA works. Some rotors spin and some don't. So now the plan is to use that one and hope the rotor I put my sample in works.
I'm learning so much about troubleshooting spectrometer issues!
Maybe tomorrow I'll actually get data. On my third day of having the spectrometer. Yeah.
