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Topic: cold MeOH Sampling Method  (Read 3442 times)

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cold MeOH Sampling Method
« on: August 03, 2005, 04:08:49 AM »
How can I take a MeOH sample at -72degC for analysis.  I am interested in the amount of dissolved gasses in the MeOH at that temperature.  If I sample it in a normal sample container all the dissolved gasses flash of and it makes the analysis very difficult since both phases (liquid and gas) must be contained, analyzed and the volume must be known of both the phases.  Isn’t there an easier way to do it?

Offline Dude

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Re:cold MeOH Sampling Method
« Reply #1 on: August 03, 2005, 08:03:49 AM »
There are a few ways to sample liquids that contain dissolved gases, but both involve some level of plumbing to ensure samples are caught correctly.  One method is to have a valve running from the sample collection point to a "flow through" sample cylinder (a steel cylinder, sometimes lined with Teflon for inertness) that routes back to your tank or sampling point (does not disturb tank or reactor pressure).  For GC analysis (the best way to quantify the dissolved gases), you will also need to plumb to the inlet with an HPLC like sampling valve and Teflon tubing.  Swage-lok fittings are typically used as connectors.  Samples can also be caught in something called a Welker cylinder that maintains a constant pressure on the sample.  With that cold of a temperature, you will also need to make sure that the pressure increase upon warming to room temperature will not exceed the rupture disk on the edge of the sample cylinder.  I am not aware of any insulating devices on the sample cylinders.  Restek and Parker sell sample cylinders.

Almost forgot that you might be a student.  In that case, Agilent or Hamilton sell "gas-tight" syringes that hold pressure up to about 100-200 psi.  Sample your mixture while cold (i.e. in a dry ice slurry or liquid N2) and then rapidly inject in the GC.
« Last Edit: August 03, 2005, 08:37:47 AM by Dude »

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