As long as @TheLostBiologist is okay with it, that’s an easy fix.
@Dred_pirate Since your already ahead of most of us on the subject in terms of having the issue in your lab + mitigating the issue with your sieve. Can narrowing the bandwidth on the sample containing the problem enhance the resolution during testing enough to detect the compound causing the issue in the 13x bead ran with and without the issue ? it seems to me the beads hold the answer.
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I wonder if you could have the used sieves tested somewhere
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I think the question is tested for what exactly?
as with anything from the ground up, I would believe that you need to establish a baseline and then add the contaminated 13x beads to do a contrast analysis
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I’d start with a GC/MS headspace
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left field question, Do they make a LCMS that works in subzero temps ?
or rather subzero sample temps lol
With a LC you’d have to extract it into a sample medium and run it.
You could just put the sieves directly in a headspace tube and heat.
You could even use solid phase microfiber extraction with a heated tube of sieves and run it in a normal GC
what would be the best way to collect the sample and transport it to a testing lab ?
if that 13x bead gets hot would “it” not evaporate before getting in the GC/MS
If you’re talking about the sieves, just take them out of the tube and fill a glass container that seals air tight.
So long as the vessel doesn’t blow after it’s sealed you’re transporting solid liquid and gas. The lab can super cool the jar before opening to lower pressure and recondense.
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There is an environmental group called the ‘Bucket Brigade’ who collect guerrilla air quality samples outside refineries in cancer alley for lawsuits. They pump air into plastic bags, heat seal the bag, and FedEx it to a lab in a mailer box. The bag is then run through gc/ms.
ETA: I only mention because it really doesn’t matter how you package it as long as you don’t contaminate or alter sample proportions in any way.
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Seems like that is the way to a definitive answer.
I just wonder if the compound in question is elusive or stable at rt, I run a machine similar to @Dred_pirate and our sieve is warmed so the size of the pours on the 13x beads narrow the spec at least.
For collection & transport, I think a super small diamond miner would be the best bet & just pull the bottom beads as they make the most contact with the heavies in the gas from my experience.
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Microfiber may be the way to go because you can preconcentrate the sample on the fiber. In other words you can take your sieves and seal them in a container with the fiber and heat. Volatiles will evaporate off the sieves and into the headspace to adsorb on the fiber. Wash, rinse, repeat with multiple batches of sieves using the same fiber and then run the fiber and you increase the potential concentration of whatever it is you’re trying to detect.
Plus with the microfiber you don’t need a headspace front end.
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Easier to transport too
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I have a solvent tank that has the suspected contaminant in there. I could run some of that over a bed of the 13x and see if that can be tested.
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I would also probably submit a sample of 13x beads that are clean because im sure whatever lab this ends up being tested in, will need some sort of contrast in order to get good results
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Definitely use that as a control
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Just curious: since the 13X is Na2O Al2O3 2.45 SiO2 6.0 H2O
which presents a very complicated binding-isotherm surface…
which we know effects the removal of Mystery Compound(s) X
from the butane. How would you choose your microfiber, if you do not know the id of MCX? Why would you think the loading capacity or affinity would be any better than the 13X? I think your original idea, head space analysis of 13x , might be best and simplest. Even direct APCI or ESI no GC might work. I would like to see this component identified. Of course if this work is being carried out at the picomole to nanomole level…appropriate controls are necessary, introducing additional microfiber material…simply needs additional controls.
My guess is that if the MCX is at sufficient quantity to alter boiling point and crystallization you are going to have plenty of material coming off the 13X.
@anon64373531 , I should say how would you choose your
liquid phase imbedded hollow fiber??
Still think your direct desorption method is more simple.
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I doubt you’ve ever touched a butane extractor in your life, Moronnabis.
Stop trying to armchair expert something you have no experience touching.
I’m not the only one that finds your posts bordering on absurd here. Anyone else?
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