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Formic acid class 3 solvent analysis

Posted: Thu Jan 19, 2012 7:57 am
by ATR
Morning All

just checking on the sensitivity of formic acid by headspace? I believe that the class 3 spec limit of 5000 ppm is not attainable by headspace - is this the case and I need to use LC with derivatisation for this ananlysis?

Re: Formic acid class 3 solvent analysis

Posted: Fri Jan 20, 2012 12:43 am
by chromatographer1
You would require a TCD or HID not a FID.

You would require special deactivated tubing and sample loops and sample valve.

You would also require a case of aspirin for all the cans of possible worms you would be opening.

Yeah, go LC or IC.

:D

Rod

Re: Formic acid class 3 solvent analysis

Posted: Fri Jan 20, 2012 7:48 am
by ATR
You would require a TCD or HID not a FID.

You would require special deactivated tubing and sample loops and sample valve.

You would also require a case of aspirin for all the cans of possible worms you would be opening.

Yeah, go LC or IC.

:D

Rod
I thought as much thanks Rod :)

Re: Formic acid class 3 solvent analysis

Posted: Sun Jan 22, 2012 5:44 pm
by jdezeeuw
Formic acid can be done via GC: I have found one application using a very thick-film of PDMS. Detection TCD or HID. Challenge will also be the injection as this compounds is very polar and difficult to evaporate.

It is easier done using LC

Re: Formic acid class 3 solvent analysis

Posted: Mon Jan 23, 2012 7:16 am
by Peter Apps
I get trace levels of formic acid as sharp peaks on Rtx wax and Stabilwax columns, but I have never tried to quantify it, and would not recommend it for routine QC. I would have thought that on a non-polar column PDMS it would concentration overload when the column was new, and adsorbtion tail at the first sign of column deterioration. So another vote for LC.

Peter

Re: Formic acid class 3 solvent analysis

Posted: Tue Jan 24, 2012 4:22 pm
by carlos.teixeira
Dear ATR,

Please, try reading this free application written by Dr. Wenmin Liu and Dr. Chunxiao Wang utilizing a FID-μTCD Gas Chromatography method for to determine Formic Acid as an impurity
<http://www.chem.agilent.com/Library/app ... 4456EN.pdf>:
# Column Agilent J&W DB-FFAP, 30m × 320μm, 0.25μm
# Carrier gas: He
# Constant flow: 1.5 mL/min
# Oven: 80 °C (3 min) 8 °C/min 150 °C (5 min)
# Detector μTCD: 200 °C, Reference gas: 15 mL/min,
# Makeup gas: 6.5 mL/min
# FID: 300 °C, H2: 30 mL/min; Air: 350 mL/min;
# Makeup flow (N2): 60 mL/min


Have nice elutions!!

Carlos de Souza Teixeira
teixeiracs@yahoo.com
http://br.linkedin.com/pub/carlos-de-so ... 15/7b0/125