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Cleaning excess citric acid from a citrate salting. Options
 
SomewhatLost
#1 Posted : 4/11/2012 3:12:26 PM
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Hi all,

I've had some basified cactus sludge sitting around for about a month or so and I decided to try salting it again to see if I got much additional yield. After pulling with d-limonene and waiting a few days, I decanted the d-limonene and salted with what I thought was around a gram of citric acid (I foolishly didn't weigh the amount beforehand) added to about 100mls of water.

After evaporating all the water, I was left with a light amber syrupy material that had white crystals spread throughout. The yield was much more than I expected (3 grams when I expected less than 1), so I'm sure I've got a good amount of excess citric acid in it.

So, I'd like to go about removing this excess citric acid if possible. Also, if it's possible I'd like to keep all the non-mescaline alkaloids as I think I prefer my cactus trips with them present. Does anyone know a relatively simple way of doing this? Any advice would be greatly appreciated. Thanks.
 

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AlbertKLloyd
#2 Posted : 4/11/2012 10:50:45 PM

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This is tricky.

I've yet to try something like this with a solvent, but sometimes citric acid solutions of mesc have crystals precipitate before all the water has evaportated, and sometimes freezing solutions or chilling them and keeping them a few degrees above freezing also causes the same thing to happen

if you can test pH you can use a basic solution, use NP again and then only use enough citric to reach a neutral pH (6.9-7.0)

Citric acid methods can be frustrating, when it goes well it is awesome, but when it doesn't then you have this same basic issue.

Mesc citrate is often poorly soluble in very cold water, you might try rinsing with small volumes of very cold water, the citric should dissolve, but this isn't 100% effective in terms of working all the time.
 
Infundibulum
#3 Posted : 4/12/2012 12:56:38 AM

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SomewhatLost wrote:
Hi all,

I've had some basified cactus sludge sitting around for about a month or so and I decided to try salting it again to see if I got much additional yield. After pulling with d-limonene and waiting a few days, I decanted the d-limonene and salted with what I thought was around a gram of citric acid (I foolishly didn't weigh the amount beforehand) added to about 100mls of water.

After evaporating all the water, I was left with a light amber syrupy material that had white crystals spread throughout. The yield was much more than I expected (3 grams when I expected less than 1), so I'm sure I've got a good amount of excess citric acid in it.

So, I'd like to go about removing this excess citric acid if possible. Also, if it's possible I'd like to keep all the non-mescaline alkaloids as I think I prefer my cactus trips with them present. Does anyone know a relatively simple way of doing this? Any advice would be greatly appreciated. Thanks.

If you started with 1 gram of citric acid and after salting the limonene and evaporating the acidic water you ended up with 3 grams, then that reads that there are is the equivalent of 2 grams of alkaloids in there. That is, as long as you actually weighted this 1 gram of citric acid correctly.

Since as AlbertKLloid says there is no easy way to separate any contaminating citric acid, your best bet here is to perform a mini A/B, that is to dissolve your product in a small amount of water, add base, re-pull with limonene and then salt with another acid.




Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
SomewhatLost
#4 Posted : 4/12/2012 12:56:57 AM
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AlbertKLloyd wrote:
This is tricky.

I've yet to try something like this with a solvent, but sometimes citric acid solutions of mesc have crystals precipitate before all the water has evaportated, and sometimes freezing solutions or chilling them and keeping them a few degrees above freezing also causes the same thing to happen

if you can test pH you can use a basic solution, use NP again and then only use enough citric to reach a neutral pH (6.9-7.0)

Citric acid methods can be frustrating, when it goes well it is awesome, but when it doesn't then you have this same basic issue.

Mesc citrate is often poorly soluble in very cold water, you might try rinsing with small volumes of very cold water, the citric should dissolve, but this isn't 100% effective in terms of working all the time.



Thanks for the reply,

I figured it wouldn't be terribly easy. This is good information to know for the future, but for now I think I'll simply divide the dose in two for the weekend. Now that the saltings have been combined, I've got ~4 grams of very sour alkaloids, so my SO and I will take ~2 grams a piece. I figure it's a safe bet that there are anywhere from 500 to 1500 mgs of actual alkaloids a piece in those doses, so hopefully the experience won't be overpowering or terribly underwhelming. At least I've learned a good lesson as to be very mindful of the amount of citric acid I use in future saltings.
 
SomewhatLost
#5 Posted : 4/12/2012 1:16:15 AM
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Infundibulum wrote:

If you started with 1 gram of citric acid and after salting the limonene and evaporating the acidic water you ended up with 3 grams, then that reads that there are is the equivalent of 2 grams of alkaloids in there. That is, as long as you actually weighted this 1 gram of citric acid correctly.

Since as AlbertKLloid says there is no easy way to separate any contaminating citric acid, your best bet here is to perform a mini A/B, that is to dissolve your product in a small amount of water, add base, re-pull with limonene and then salt with another acid.



Thanks for the advice.

In the future, I'll do a mini A/B as you both have suggested. For now, my SO and I are going to go into the trip somewhat blind. I've only had a couple of cactus experiences so far and while I've enjoyed them both quite a bit, I wouldn't have minded if they were considerably stronger. I assume we'll have a good time Smile
 
 
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