We are analysing samples for N2/Ar ratios using a modified version of the An and Joye (1997) method: He carrier gas, stripping and cryogenic trapping of gases, Ca-chabazite packed column at 30C, GC-TCD.
We are seeing two peaks, rather than the expected three (Ar, O, N2): the first peak seems to be a combination of Ar and O; the second peak is N2. Because this method requires a ratio between N2 and Ar, we must separate the Ar and O peaks.
Are there any suggestions for how to 1) increase/obtain peak separation of Ar and O (e.g., via modification of oven/detector temperature, carrier flow rate, ?) or 2) remove oxygen (but not Ar and N2) from the sample after cryogenic trapping?
Any assistance will be much appreciated!
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By MC Schwartz on Monday, May 31, 2004 - 12:38 am:
We have had some subsequent success in separating the Ar and O peaks by baking the column at 380-400 deg C for 12-24 hours (i.e., following the initial conditioning protocols outlined in An and Joye (1997) and Maroulis and Coe (1989)).