Stuck d8 conversion

We use an alk beam test and run the reaction until it shows no purple. It usually takes 4-12 hrs. I have a run that is on hour 36 that is still showing dark purple indicating CBD. I keep adding more ptosic and 4a beads to no avail (currently about 20grams of ptosic and a few ounces of beads). The mixture has been dark red since the first few hours of reacting which is usually a sign of conversion. The reaction temp is 88c.

The distillate I am using is wfe residue reclaim (I ran wfe residue back through wfe to recapture lost material and then ran it 2-3 more times to increase purity) the distillate was clear and a pretty good color before reaction.

I’m wondering if anyone has ideas about what could be preventing conversion. Maybe something in the reclaimed distillate creating side reactions?
Thanks

@Photon_noir ,@anon93688 what’s your hunch on this ?

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At what temp ?

Saturated beads ?

Did you check the distillate with GC to make sure you were starting with cbd? Maybe it was high in CBN and it’s got a side reaction occurring.

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It’s ocbd hemp genetics with the alk beam test showing heavy CBD via color change so farly confident it’s over 75% CBD probably 80% with a couple points d9

Beads get saturated with water at some point approx 20% of their weight is all they can hold
Maybe the beeds alter the ph ?

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I ran the reaction under vacuum for the first day
with no beads thinking maybe water interferes with the reaction or the catalyst plus water gets stuck in the beads. The reaction did not finish (as per alk beam) so day 2 I turned off vacuum and added beads as I’ve been doing normally. I wonder if the complete lack of water because of vac purge is preventing a reaction? No water no pH? (Although I always assumed this was a hydrophobic solution/reaction)

Man I wish I had de knowledge to help you out :frowning:
Truth is I can t @ScoobyDoobie might know @Krative @QGA @Rastan

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You’re using the 3a beads for a catalyst bed right?

Maybe water is competing for space in your media, slowing down the reaction?

@MagisterChemist you got any ideas?

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Using 4a beads because they were referenced in several patents. Dont have a bed per say but using a stirred reactor with a small amount of beads floating in the solution (several cups beads)

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4Å Beads were very likely specified because ptosic acid is probably too big a molecule to fit into a 3Å pore.

Bubbles could just be a sign of the pores of the beads filling up with liquid and expelling the gases trapped.

How are you adding the p tosic acid?

Next time around try to dry the shit out of your beads and see if that helps.

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If you have a well calibrated and accurate thermometer I d imagine
That the heating of the beads can be measured once in contact with water in your crude :thinking:

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Just powdering the ptosic acid crystals and pouring them into the reactor while agitating. Usually I only need to add 5 grams for a liter. This time I kept adding 5 grams ptosic a day with a half cup of beads or so (currently about 20g ptosic, 2.5 cups beads) because it was not finishing.

The beads are brand new, you think they could have water from the air? Thanks!!

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What is the data i am looking to observe with the heating of the beads? I use distillate instead of crude, which should be low water content. Thanks again

Molecular sieves will generally need to be activated before you use them. They usually ship them with some moisture content, I’m not sure if theres a reason theyre shipped like that or if they pick up water content during transit.

Maybe it’s to add some strength to beads so they dont get crushed as easily?

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The absorbing of water by a4 beads creates heat so would imagine several beads and a few drops of oil might give a temperature reading

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A molecular sieve bead will generate heat as the water molecules adsorb to its surface, the amount of heat is directly related to the amount of water in the sample.

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Did you active the MS correctly? 8 h under vacuum at 160*C for 12 hours is the norm.

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I wouldn’t be able to speak on exactly why that’s your problem, but my crude guess is that the water content is reducing the active surface area of your media.

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