also using a huber cc902
SooâŚ.youâve got a Huber on your solvent tank, but no thermal probe in there (right?), which means you donât actually know what is going on in your solvent tank.
I highly recommend solving that. you can use pressure to figure temp, but you have to make some assumptions that are often invalid. Eg no N2, or âknown blendâ.
If it is moisture in your chiller fluid, and circulation has slowed because âslushâ, chiller will read same temps as always, but solvent wonât be getting as cold.
Itâs often easier to implement a temp probe on the solvent injection side. also recommend. Such a sensor may have alerted you to the issue sooner.
A refractometer will at least tell you where your heat transfer fluid is. Unless of course youâre going the MeOH/EtOH route, which I advise against. I suggest you let the system thaw then circulate for a bit before sampling.
You might also just try a flow test. open the system at the return line and time a bucketful. The chill and repeat. Possibly at various temps. You would then know what ârightâ was and could check that off the list next time this happensâŚ
Edit:
For $35k it should list flowâŚand raise its hand if things get slushy. Are you using Huberâs fluid? Not certain the refractometer will solve it. youâll have to dig that part up.
Unless you have lost the lid, it should take quite some time to pull water into that chiller. Still sounds like the most likely explanation.
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LMFAO I agree with you on everything and yes no probe to actually know my temp of actual solvent and solvent tank. And yes temp on chiller kept reading same temp so I was confused. I also have been using the fluid I got from huber. I was wanting to get more of it but its pretty expensive going through them.
also how would I go about adding a probe to injection side? And any ones youâd recommend?
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You can just add a T inline with a thermo probe on one port. If you are running swagelok parts we have all the pieces available including probes and readers. You may need adapters with other types of fittings but itâs all pretty painless to source.
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thank you @BizzybeeTeam: exactly who I was gonna call inâŚ
see also: Any Way to Measure Actual Inline Solvent Temp?
âŚand this (tee) is how I got at solvent and collection temps via the 1/2" compression fittings on the bottoms of the tanks. NOT a stock swagelok part.
you can purchase bored through fittings for thermocouples from a variety of vendors. eg
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That fitting is awesome! We typically run reducers but thatâs nice and sleek.
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Yeah, reducers like this absolutely have their place (almost anywhere!!)
you can get the 1/8â compression x npt for less $, so where I was taught (chemistry machine shop), you either drilled and tapped or machined then welded the fitting anywhere the researcher wanted to put a probe. Usually as a retrofit.
for the fancy tee above, I think I used a 1/4 x 1/8 reducer similar to the 1/2x1/8 in my hand. Machined a flat spot, drilled a 1/4â hole. shortened the fitting on the lathe, then handed them off to my mentor to weld.
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Thatâs super cool, really clean execution also! Thatâs such a great background to have for this industry. You sir, are a boss!
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Damn you guys are awesome! Im gonna run through some options and see what I come up with.
These guys have good gear at good pricesâŚand they will answer your questions.
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When nitro makes its way into the solvent tank, you gain pressure. Either bleed the nitro from collection before recovering or crack a bleed on the solvent tank you are recovering into until the nitro has all passed.
Only other thing I can think, is you donât have enough cooling(condensing coil or chiller) to keep up with the faster recovery thus some tane is coming over as gas, thus building pressure.
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