I am trying to do headspace analyses on leather samples for any chemicals wich can course the irritation if they eveporate in the car at high temperatures. I need to start with 25 C but the programm I have got starts with 40 C. Could anybody look at the programm and tell me how to change it. It must be rather simple but I am complitely new to the instrument and would really appriciate any help.
Head space autosample programm:
Syringe 1.0 ml - HS
Sample Vol 500 micro l
Incubat Temp 35 C
Incubat time 00:20:00
Agi Speed 500 rpm
Agi on time 15 s
Agi off time 60 s
Syringe temp 35 C
Full Speed 100 microl/s
Inject Speed 250 microl/s
Syr Flushing 00:01:00
GC Run time 00:28:00
Injector temp=150 C hold=28.0 min total=28.00
Split ratio 10
Enable coolant 250 C
Coolant Time out 20
Column flow 1 mil/min
1 t=40 C hold=2.0min total 2.0 min
2 t=100 rate 5.0 hold=0 total 14.0 min
3 t=280 rate 20.0 hold 5 total=28.0
By Anonymous on Wednesday, April 10, 2002 - 05:58 am:
By Chris on Wednesday, April 10, 2002 - 06:13 am:
This reference might help:
Classification of complex gas mixtures from automotive leather using an electronic nose [Full Length Article] Analytica Chimica Acta 2000, 403:1-2:31-38
They describe a GC-MS method in this paper as well.
By Chris on Wednesday, April 10, 2002 - 06:49 am:
It looks like you are using a CTC CombiPal Autosampler. Am I correct? We like ours, but we have trouble with it breaking syringes. Have you experienced this?
By Sepúlveda on Friday, April 12, 2002 - 01:58 pm:
Wath column do yo use?
We already analyze VOC´s in Leather and plastics using a Head Space.
I recomend you 200-250 oCin the injector
200-250 oC in the FID
a PEG column is very good for the analysis (do not heat it more than 200 oC).
use a ramp of 15 oC/min
The incubation temperature at 120 oC is standar for some car manufacturers and a incubation time of 300 min.
By Anonymous on Tuesday, April 16, 2002 - 01:14 pm:
Thank you very much for all your help!
Chris, you are right, we use the same CTC CombiPal Autosampler and it had never broken any syringers before( for 2.5 years). But after reading your message, I would never beleive, it has done it today.:) It broke the syringe ( Hamilton - 10 UL.PAL,Fixed 28S style 1 - Varian Cat. N392590205 ). The worst thing is that Varian hasn't got it in stock and I need to try another supplier. It was just a bad luck!
By Chris on Tuesday, April 16, 2002 - 02:43 pm:
Try ordering directly from Hamilton, or try Leap Technology.
Didn't mean to jinx you.
By Anonymous on Wednesday, April 17, 2002 - 10:12 am:
Could you please give me the website addresses of Hamilton and Leap Technology as I am in the UK and will try to find their branches overhere.
By Chris on Wednesday, April 17, 2002 - 11:26 am:
By Anonymous on Friday, April 19, 2002 - 04:25 am:
I assume you are running the leather as a solid sample, not as a solution. If this is correct, you are wasting time agitating the vial. Agitation will speed equilibration time with liquids (which may improve precision), but it does nothing for solids.
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