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Alkaloids not precipitating out when adding the lye - Easy Caapi Tek Options
 
behindthelight
#1 Posted : 7/24/2012 2:28:48 AM
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So I am following the tek exactly.

I did the 3 boils on the 60 grams of Caapi.

I reduced it down to about 300ml

I then added 5g of lye to 50 ml of water and stirred it up and let it clear.

Then I poured that into the caapi and nothing happened. What is going on?

Anyone have any clue?

Can it be fixed?
 

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behindthelight
#2 Posted : 7/24/2012 3:08:25 AM
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Maybe this should be in the "harmalas" forum?

Can a MOD move it over there if that is where it belongs?
 
behindthelight
#3 Posted : 7/24/2012 5:12:51 AM
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Here is a pic after I let it sit for 2 hours. It doesn't look like the picture in the Easy Caapi Tek thread. In that picture the bottom is white.

Anyone have a clue what is going on?

 
behindthelight
#4 Posted : 7/24/2012 5:03:24 PM
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Top layer is black....bottom layer is brown????? What is up?
 
SnozzleBerry
#5 Posted : 7/24/2012 6:17:41 PM

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First...no need to keep bumping your post, someone will help you out Smile.

Second, if that were my extraction, I would run it through a coffee filter, take the precipitates (the brown solids in the lower part of your bottle) that collect in the filter, redissolve them in vinegar, run the acidified solution through another coffee filter, discard the solids and re-base the liquid and proceed with the extraction according to gibran2.
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gibran2
#6 Posted : 7/25/2012 12:32:02 AM

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The bottom brown layer is your precipitate. It’s just very loosely settled.

You might want to add a bit more NaOH to ensure that everything has settled. Then either let it settle and decant/siphon the top clear layer or filter.

It’s hard to tell, but it looks like you have a good yield.
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behindthelight
#7 Posted : 7/25/2012 4:27:04 AM
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Ok guys, thanks for the input.

I'm not really sure which direction to go with this since you both gave me ideas on how to fix it.


Gibran - Why is the bottom not white like it shows in your tek?
 
SnozzleBerry
#8 Posted : 7/25/2012 12:37:33 PM

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It's not white because your alkaloids have more impurities than those gibran's pics.

If you follow gibran's advice and just decant the black water, add new water, shake it up let it settle and repeat, your alkaloids should become somewhat lighter. As you re-A/B, they will become significantly lighter Smile
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behindthelight
#9 Posted : 7/25/2012 12:43:10 PM
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SnozzleBerry wrote:
It's not white because your alkaloids have more impurities than those gibran's pics.

If you follow gibran's advice and just decant the black water, add new water, shake it up let it settle and repeat, your alkaloids should become somewhat lighter. As you re-A/B, they will become significantly lighter Smile


Alright man, thanks again. I will give it a go. Smile
 
behindthelight
#10 Posted : 7/25/2012 1:42:47 PM
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Quick update.

I siphoned off almost all of the black liquid on top. I then added in some more water and shook it up.

I then added some more lye to a about 75ml off water and then added that to the caapi mix and I am letting it settle right now. Unfortunately, I didn't really see any difference yet.
 
SnozzleBerry
#11 Posted : 7/25/2012 2:09:32 PM

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I would be willing to bet that you are already at a high enough pH, so adding more lye won't really do anything. After your alks settle again, you can repeat the decanting/washing step if you want. Personally, I don't do much washing until I've already done a couple A/B's. With gibran's method (a single A/B, I believe), given how dark your alkaloids are, I would suspect you would have to do many more washes of your precipitates, but I'd bet gibran can comment on that better than I.

Ultimately, at some point, you are going to want to collect your freebase precipitates, redissolve them in vinegar, run them through a coffee filter (anything that collects in the filter once the alks have been dissolved is plant fats/tannins and other things you don't want) and then re-base that alk-saturated liquid. When you do this, the alkaloids that precipitate should be significantly cleaner than those you have at present.
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behindthelight
#12 Posted : 7/25/2012 2:21:25 PM
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SnozzleBerry wrote:
I would be willing to bet that you are already at a high enough pH, so adding more lye won't really do anything. After your alks settle again, you can repeat the decanting/washing step if you want. Personally, I don't do much washing until I've already done a couple A/B's. With gibran's method (a single A/B, I believe), given how dark your alkaloids are, I would suspect you would have to do many more washes of your precipitates, but I'd bet gibran can comment on that better than I.

Ultimately, at some point, you are going to want to collect your freebase precipitates, redissolve them in vinegar, run them through a coffee filter (anything that collects in the filter once the alks have been dissolved is plant fats/tannins and other things you don't want) and then re-base that alk-saturated liquid. When you do this, the alkaloids that precipitate should be significantly cleaner than those you have at present.


Ok, when it comes to redissolving them in vinegar, can there still be some of that black stuff on top in there? It is pretty much impossible to decant/siphon all of it off.
 
SnozzleBerry
#13 Posted : 7/25/2012 2:26:49 PM

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I just glanced at gibran's pictorial and it looks like he does multiple A/B's too, so that would also go towards explaining why yours and his are not identical. No worries, you are on the right path.

With regards to redissolving, you have two options. If you have a coffee filter, you can collect your alks and remove them from the solution entirely. You could then redissolve them in vinegar. Basing the vinegar solution would then give you cleaner alks than those you currently have.

Alternatively, if you don't have coffee filters or don't want to go that route for another reason, you could just add vinegar to your current jar. Personally, I would advise against this as I believe you will need more vinegar than if you removed the alks. I'm not sure how much more you would need, but with the presence of the basified water, it will take more to neutralize the solution and convert your freebase alkaloids into salt form. It's not a huge deal, but you may wind up with a significantly larger quantity of liquid by the time you are done, compared to straining out the alks and just redissolving them.
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behindthelight
#14 Posted : 7/25/2012 5:05:36 PM
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Ok, thanks again. I think I will try the coffee filter method.

Can't wait to get this done, I want to see some results. Smile

I appreciate all the help.
 
SnozzleBerry
#15 Posted : 7/25/2012 5:12:09 PM

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Don't forget to filter the vinegar solution after all the alks have dissolved. This is what results in a huge amount of cleanup. I think in gibran's tek he decants the acidified solution off of the precipitates that appear when you acidify it. Either way works as long as you don't re-base those unwanted fats/tannins.
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behindthelight
#16 Posted : 7/25/2012 5:31:32 PM
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Ok, so let me just list the steps that I am going to do and let me know if I am missing something:

1. Take my current solution and filter that. This will leave behind the alkaloids.

2. Dissolve these alkaloids in vinegar.

3. Run this solution thru a filter.

4. Now base by adding lye to this new solution. I think I am suppose to add like 200ml of water also at this point?

5. Now, correct me if I am wrong, but at this point I should be able to pic up Gibrans Tek at the part where it says "Remove Soluble Impurities"
 
SnozzleBerry
#17 Posted : 7/25/2012 5:55:16 PM

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Close...

1. Take my current solution and filter that. This will leave behind the alkaloids (in the filter).

2. Dissolve these alkaloids in vinegar.

3. Run this solution thru a filter. = gibran's pictorial: Remove insoluble impurities

4. Now base by adding lye (I recommend adding lye-water rather than straight lye) to this new solution. I think I am suppose to add like 200ml of water also at this point? The water you are adding is to repeat the washing of the freebase alkaloids, like you did earlier . You decant the water off of your alks, add new water, agitate it and let the alks settle again. You can do this several times and you will notice the water should get lighter each time.

After step 4, depending on how clean your alkaloids are, you have two options. You can either go back to step 1 and repeat 1-4, or you can go on to the section of gibran's entitled "Remove Excess NaOH, Salts, Etc."

Hope that's clear (some parts it seemed like you understood, but I added some more details for clarity's sake), please let me know if anything isn't Wink
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behindthelight
#18 Posted : 7/26/2012 2:23:55 AM
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yes...yes...yes.......that is what I needed.......thanks soooooooo much..!
 
behindthelight
#19 Posted : 7/27/2012 9:39:18 PM
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Hey Snozzle...I am a little confused.


So, I did the filtering using the coffee filter to get the alks and then dissolved in vinegar.

So, I put everything back into that glass bottle and have filled it up with water....let it settle...siphoned of the water...and repeated this a few times....the water is getting lighter every time. Then I added some lye water and nothing happened...do I just keep adding water and then getting rid of it and repeating?

What to do now? Am I done? Are the alkaloids in the bottom of the jar ready?

They never turned white like in Gibran's pictures.
 
SnozzleBerry
#20 Posted : 7/27/2012 11:50:39 PM

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behindthelight wrote:

So, I did the filtering using the coffee filter to get the alks and then dissolved in vinegar.

So, I put everything back into that glass bottle and have filled it up with water....let it settle...siphoned of the water...and repeated this a few times....the water is getting lighter every time. Then I added some lye water and nothing happened...

So, my understanding at this stage is that you redissolved the alks in vinegar and then "washed" those alks while they were still in salt form.

You have to base the alkaloids before you can wash them, otherwise you are just adding water to alkaloid saturated water and any water you remove from there will contain alks (i.e. if you did this and discarded the water, you threw away your alks).

When your alkaloid solution was acidified, you could have either filtered it and discarded the insoluble stuff that the filter collected (as described above) or you could have decanted the alkaloid solution off of the insoluble impurities (as in gibran's tek). It is through filtering the matter that is insoluble in acid that you do the majority of the cleanup of your product. Essentially, you filter out the unwanted things that precipitate when acidified so that they are not there to dirty up your alks when you basify them.

If this is what happened, the reason you did not precipitate any alkaloids when you based the solution was because there were no (or very few) alkaloids to precipitate. If this is not what happened, please clarify and I'll do my best to help figure out what's going on.
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