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How to tell the difference between KOH/NaOH crystals and DMT crystals? Options
 
rudder
#1 Posted : 12/29/2012 5:24:21 AM
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So I took the extract from two N-heptane pulls of ~600g of Acacia mearnsii bark powder, and put it in a shotglass and recrystallized with N-heptane.

I'm fairly certain I inadvertently pulled some KOH/NaOH in the two pulls. (I used this for a base: http://www.scotchcorp.co...grease-drain-opener.html ). It also seems like the KOH/NaOH is present in the N-heptane that I decanted from the recrystallization.

How can one be sure the cloudy residue left behind on the glass tray (both, after pulls, and after recrystallization) is spice and not KOH/NaOH?

Sidenote: Whatever my extract is composed of, there is not a very large volume of it, considering it came from ~600g of bark.
 

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rudder
#2 Posted : 12/29/2012 5:27:47 AM
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Here's the MSDS on that drain cleaner in case anyone is curious: http://www.scotchcorp.co...loads/MSDS%201969-70.pdf
 
Jin
#3 Posted : 12/29/2012 11:11:16 AM

yes


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perhaps washing your freebase with water ( drop by drop) is a good idea , koh/naoh shoul dissolve in the water leaving freebase intact ,place your freebase on a filter papar and add water from a dropper drop by drop ,

i am just assuming this in the case if recrystalization did'nt help , or recrystalize a few more times , perhaps that can help

the water cleaning can be tricky so .....
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endlessness
#4 Posted : 12/29/2012 11:55:39 AM

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NaOH and KOH do not dissolve in non-polar solvents like naphtha, so unless your separation was very sloppy and you brought some droplets of the bottom layer across, you should be fine.

You can always just recrystallize, any NaOH/KOH will not dissolve in the non-polar solvent and stay below. You can also do a sodium carbonate wash after you redissolved in naphtha. FAQ has instructions

You can also wash with water as poster above mentioned, dmt will not dissolve but the bases will (sounds a bit more messy way of doing it though)

If you put a bit on a spoon or clean glass surface and warm it up, the dmt will vaporize but NaOH/KOH would stay solid since they have very high melting point, so thats another way to check if theres anything there.

Personally I guess id just recrystallize, and next time be more careful and/or wash before freezing or evaping the solvent
 
rudder
#5 Posted : 1/3/2013 4:54:55 PM
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endlessness wrote:
NaOH and KOH do not dissolve in non-polar solvents like naphtha, so unless your separation was very sloppy and you brought some droplets of the bottom layer across, you should be fine.

You can always just recrystallize, any NaOH/KOH will not dissolve in the non-polar solvent and stay below. You can also do a sodium carbonate wash after you redissolved in naphtha. FAQ has instructions

You can also wash with water as poster above mentioned, dmt will not dissolve but the bases will (sounds a bit more messy way of doing it though)

If you put a bit on a spoon or clean glass surface and warm it up, the dmt will vaporize but NaOH/KOH would stay solid since they have very high melting point, so thats another way to check if theres anything there.

Personally I guess I'd just recrystallize, and next time be more careful and/or wash before freezing or evaping the solvent


I did recrystallize. That's what my post is about. I put the original N-heptane pulled, dried extract into the bottom of a shotglass, added a small amount of water (just enough to submerge the extract) and then nearly filled the rest of the shotglass with N-heptane.

Then I submerged the shotglass in near boiling water until it heated up significantly, then I stirred the extract around to mix it up with the warmed N-heptane. Then I took the shotglass out of the hot water and set in on a table for a minute and then began to decant the N-heptane using an eyedropper..

I guess I'll have to try the warming test to see if it vaporizes. Would using a spoon and touching the bottom of the spoon with a bic flame work? Or would that also vaporize KOH/NaOH?
 
 
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