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Broken capillary column

Posted: Thu Jul 14, 2005 3:00 pm
by Consumer Products Guy
Never had this happen in 25 years of fused-silica capillary column experience: a 30m x 0.25mm Agilent HP-5MS capillary column column installed in my GCMS spontaneously broke about in the middle after 5 months of use. The oven door had never even been opened during that time period, so it wasn't due to an operator "hand slip" or anything. Anybody else ever experience anything like this?

FYI, there was enough column so both my inlet pressure (6890) and MS tunes were still OK (my symptom was obviously no peaks at all, just air).

broken capillary column

Posted: Thu Jul 14, 2005 6:22 pm
by skunked_once
This has happened to me 2 or 3 times in about 20 years and I assumed (with no concrete evidence) that the column had a flaw or had been damaged somehow. Stuff happens :?

Only once in 15 yrs

Posted: Tue Jul 19, 2005 1:46 am
by Les
Same as you, column broke about 9m from the detector. Luckily, the column was a 100m and just connected again with little loss of retention times.

broken capillary column

Posted: Tue Jul 19, 2005 9:38 am
by Suresh Seethapathy
Never happened to me before, but happened to two of my labmates in the past six months!

suresh

Posted: Tue Jul 19, 2005 9:51 am
by WK
Hi All,
Did anyone have a column break when using an FID?
Did/would the hydrogen flow to the oven?
WK

Posted: Tue Jul 19, 2005 12:28 pm
by DR
Hi All,
Did anyone have a column break when using an FID?
Did/would the hydrogen flow to the oven?
WK
Not enough H2 going to the FID to be of much concern, if your gasses are anywhere close to correct. H2 becomes more of a safety concern when you use it as the carrier gas, so having a column break under such circumstances could lead to a problem. That's the original reason (I have been told) for magnetic oven door catches, so that an oven could blow "safely".

Re: Broken capillary column

Posted: Tue Aug 02, 2005 10:02 am
by Okkie
FYI, there was enough column so both my inlet pressure (6890) and MS tunes were still OK (my symptom was obviously no peaks at all, just air).
How can your tunes be OK, with about 100% air ???
Be carefull with these tunes, because I do think that the machine is tuned incorrectly.

Okkie

Posted: Tue Aug 02, 2005 3:11 pm
by Consumer Products Guy
I meant that my tunes were OK in terms of peak width, percent, etc., and I didn't notice the air peaks in the Tune Report because I wrongly assumed that since there was no error window on the monitor, that the Tune was OK. It was when I injected a sample that only air background was evident to me, so that's when I opened up the oven and found the broken capillary. Even I'm allowed to make a mistake sometimes !!!

Posted: Wed Aug 03, 2005 9:37 am
by Victor
Did you try to fix the column with a press-fit connector? If so, do you find these things work well?

Posted: Thu Aug 04, 2005 12:49 am
by Consumer Products Guy
Agilent sent me some, and some resin, free, but I haven't tried it yet (I installed a new back-up column).

Posted: Thu Aug 04, 2005 7:34 am
by xxx
Did you try to fix the column with a press-fit connector? If so, do you find these things work well?
We reconnected broken column with press fit connector,and works well.
You need to properly cut the column to make a leak free connection,especially for ms,where you see very small leak at the press fit connections.

Bye