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Trickster
#1 Posted : 12/27/2009 1:16:52 PM

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SWIM extracted 100g of rue and after 2 A/B cycles has got 9g of pretty clean looking extract.

For some reason SWIM could not attach the picture.
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endlessness
#2 Posted : 12/27/2009 1:59:01 PM

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did you do at least one manske step?

if not, then its not only harmalas but also the other alkaloids such as vasicine and vasicinone
 
Trickster
#3 Posted : 12/27/2009 2:29:36 PM

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endlessness wrote:
did you do at least one manske step?

if not, then its not only harmalas but also the other alkaloids such as vasicine and vasicinone


Yep. SWIM did.

Here is the process:

1. Acid (vinegar) extraction. 4h+4h+10h with a magnetic stirrer/heater.
2. Freezing for over 12 hours.
3. Decanting & filtering.
4. Manske
5. Dissolution of precipitate in warm water + a few drops of vinegar.
6. Adding NaCl
7. Collecting precipitate.
8. Dissolution of precipitate in warm water.
9. Adding Sodium Carbonate.
10. Freezing for 36 hours.
11. Decanting.
12. Drying the precipitate.

She just noticed that there is a taste of Sodium Bicarbonate in the final product. SWIM thought it should not get into the precipitating harmalas.
Trickster attached the following image(s):
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69ron
#4 Posted : 12/27/2009 2:54:29 PM

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The sodium bicarbonate taste is not a good sign.

Maybe there was too much salt present if the salted crystals before adding the sodium carbonate.

PLEASE DO NOT PM ME.
I do not answer PMs! I delete all PMs no matter who they are from, even from a good friend. I don't have time for the PMs. I have very little free time. If you have a question just post it in a threadSmile


All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
69ron
#5 Posted : 12/27/2009 2:57:13 PM

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In the past SWIM found his salted alkaloids to be as much as 20% salt. How you filter the salted alkaloids can really make a difference in salt contamination. At the freebasing stage, too much salt will prevent sodium carbonate from dissolving properly because water can only hold so much sodium, and then it starts to precipitate out of the water.

I think step 7 above wasn't done right, and lots of salt was still present and this messed up step 9.

Yields should be about 1-3%. Anything above that is suspicious. There are seeds that produce more, but they are not common. 10% is definitely not believable.
PLEASE DO NOT PM ME.
I do not answer PMs! I delete all PMs no matter who they are from, even from a good friend. I don't have time for the PMs. I have very little free time. If you have a question just post it in a threadSmile


All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
endlessness
#6 Posted : 12/27/2009 3:56:47 PM

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how can there be taste of sodium BIcarbonate if you didnt use any? you mentioned sodium carbonate being used...

also.. you say freezing, you mean literally freezing? Like, water turned into ice?

How much sodium carbonate did you use? Just enough to precipitate alkaloids or maybe so much that you super-saturated the water with it and some crashed out together with harmalas?

I would do another A/B on it....

where were the seeds from?


and ron, yes alks from manske definitely have salt contamination but if one redissolves it in water and precipitates the base, there shouldnt be any salt contamination as it would be dissolved in the water
 
burnt
#7 Posted : 12/27/2009 4:17:02 PM

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why use sodium carbonate or bicarbonate in such an extraction? SWIM doesn't see the point?
 
Phlux-
#8 Posted : 12/27/2009 4:33:49 PM

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making sodium carbonate saturated water and adding that to the water containing the harmalas can totally reduce sodium carbonate contamination.
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endlessness
#9 Posted : 12/27/2009 5:01:13 PM

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burnt wrote:
why use sodium carbonate or bicarbonate in such an extraction? SWIM doesn't see the point?


to precipitate the freebase and then collect by filtration.. what else do you suggest? Freebase is way cleaner than salt from manske, sodium carbonate/bicarbonate are safe chemicals.. I already used ammonia for this, works just as well but stinks like hell, never again!
 
burnt
#10 Posted : 12/27/2009 5:06:03 PM

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O oh ok sorry SWIM didn't realize you were collecting freebase and not salts. Nevermind wasn't paying enough attention.
 
69ron
#11 Posted : 12/27/2009 5:54:26 PM

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Let me say this again. Salt is SODIUM CHLORIDE. Sodium carbonate is a SODIUM. Both are SODIUMS. Water can only hold so much SODIUM. This is the problem.

If the initial alkaloids are contaminated with too much SODIUM chloride then adding more SODIUM carbonate will cause SODIUM to precipitate out with the harmalas.

Because SODIUM carbonate is less water soluble than SODIUM chloride, then SODIUM carbonate precipitates out, so you'll get harmala alkaloids that taste like SODIUM BICARBONATE because there's sodium carbonate in it.

It's simple chemistry. Water can only hold so much sodium. If there’s too much sodium chloride, added sodium carbonate will not dissolve.
PLEASE DO NOT PM ME.
I do not answer PMs! I delete all PMs no matter who they are from, even from a good friend. I don't have time for the PMs. I have very little free time. If you have a question just post it in a threadSmile


All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
Trickster
#12 Posted : 12/27/2009 8:57:47 PM

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69ron wrote:
In the past SWIM found his salted alkaloids to be as much as 20% salt. How you filter the salted alkaloids can really make a difference in salt contamination. At the freebasing stage, too much salt will prevent sodium carbonate from dissolving properly because water can only hold so much sodium, and then it starts to precipitate out of the water.

I think step 7 above wasn't done right, and lots of salt was still present and this messed up step 9.

Yields should be about 1-3%. Anything above that is suspicious. There are seeds that produce more, but they are not common. 10% is definitely not believable.


SWIM did not filter precipitate at all. She just put the salted liquid in the fridge until the it's become completely transparent and then very carefully decanted it. After that she just added warm water and some vinegar to the remaining goo (step 8 ).
Do not seek the truth, just drop your opinions.
 
Trickster
#13 Posted : 12/27/2009 11:22:01 PM

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69ron wrote:
Let me say this again. Salt is SODIUM CHLORIDE. Sodium carbonate is a SODIUM. Both are SODIUMS. Water can only hold so much SODIUM. This is the problem.

If the initial alkaloids are contaminated with too much SODIUM chloride then adding more SODIUM carbonate will cause SODIUM to precipitate out with the harmalas.

Because SODIUM carbonate is less water soluble than SODIUM chloride, then SODIUM carbonate precipitates out, so you'll get harmala alkaloids that taste like SODIUM BICARBONATE because there's sodium carbonate in it.

It's simple chemistry. Water can only hold so much sodium. If there’s too much sodium chloride, added sodium carbonate will not dissolve.


Some questions:

1. I presume by Sodium you mean Sodium ions?

2. SWIM would prefer to exclude any guesswork from the process but she is still looking for exact quantities of chemicals. Do you happen to know them?

3. Is SWIM right thinking that when Sodium Carbonate reacts with water it changes to Sodium Bicarbonate?

4. SWIM understands that Sodium Bicarbonate is completely harmless, so why bother cleaning the final product?

5. If there is a reason, how would SWIY clean it?
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69ron
#14 Posted : 12/28/2009 1:37:09 AM

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Trickster wrote:
69ron wrote:
In the past SWIM found his salted alkaloids to be as much as 20% salt. How you filter the salted alkaloids can really make a difference in salt contamination. At the freebasing stage, too much salt will prevent sodium carbonate from dissolving properly because water can only hold so much sodium, and then it starts to precipitate out of the water.

I think step 7 above wasn't done right, and lots of salt was still present and this messed up step 9.

Yields should be about 1-3%. Anything above that is suspicious. There are seeds that produce more, but they are not common. 10% is definitely not believable.


SWIM did not filter precipitate at all. She just put the salted liquid in the fridge until the it's become completely transparent and then very carefully decanted it. After that she just added warm water and some vinegar to the remaining goo (step 8 ).


That's the problem I’m sure. Because it was decanted and not filtered, there was a lot of salt present. The salt prevented the sodium carbonate from dissolving properly.

You cannot easily dissolve sodium carbonate in a solution of salt. Water can only hold so much sodium.

You also cannot easily dissolve sodium carbonate in a solution sodium acetate. If you added vinegar, you created sodium acetate when the sodium carbonate was added. So this is another problem.
PLEASE DO NOT PM ME.
I do not answer PMs! I delete all PMs no matter who they are from, even from a good friend. I don't have time for the PMs. I have very little free time. If you have a question just post it in a threadSmile


All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
Phlux-
#15 Posted : 12/28/2009 5:49:49 AM

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hey ron -

"Let me say this again. Salt is SODIUM CHLORIDE. Sodium carbonate is a SODIUM. Both are SODIUMS. Water can only hold so much SODIUM. This is the problem.

If the initial alkaloids are contaminated with too much SODIUM chloride then adding more SODIUM carbonate will cause SODIUM to precipitate out with the harmalas.

Because SODIUM carbonate is less water soluble than SODIUM chloride, then SODIUM carbonate precipitates out, so you'll get harmala alkaloids that taste like SODIUM BICARBONATE because there's sodium carbonate in it.

It's simple chemistry. Water can only hold so much sodium. If there’s too much sodium chloride, added sodium carbonate will not dissolve.
PLEASE DO NOT PM ME."


Thanks for that man - i didnt think about that b4, makes a load of sense - so shotto chap.
antrocles wrote:
...purity of intent....purity of execution....purity of experience...

...unlike the "blind leading the blind". we are more akin to a group of blind-from-birth people who have all simultaneously been given the gift of sight but have no words or mental processing capabilites to work with this new "gift".

IT IS ONLY TO THE EXTENT THAT WE ARE WILLING TO EXPOSE OURSELVES OVER AND OVER AGAIN TO ANNIHILATION THAT WE DISCOVER THAT PART OF OURSELVES THAT IS INDESTRUCTIBLE.


Quote:
‹Jorkest› the wall is impenetrable as far as i can tell


Quote:
‹xtechre› cheese is great


He who packs ur capsules - controls your destiny.

 
Trickster
#16 Posted : 12/28/2009 9:12:57 AM

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69ron wrote:

That's the problem I’m sure. Because it was decanted and not filtered, there was a lot of salt present.


How SWIM could have filtered salt out if both excessive salt and alkaloids were in solid phase?

She decanted the liquid several times over a couple of days, so finally there was less than 1/20th of the original amount of liquid in the remaining precipitate. You may as well say that it has been filtered, only the solids were wet.


69ron wrote:
The salt prevented the sodium carbonate from dissolving properly.

You cannot easily dissolve sodium carbonate in a solution of salt. Water can only hold so much sodium.


She has been adding sodium carbonate while checking how it dissolves in the water. Every now and then she stopped the stirrer to see if there is any undissolved sodium carbonate. There seemed to be none.

69ron wrote:
You also cannot easily dissolve sodium carbonate in a solution sodium acetate. If you added vinegar, you created sodium acetate when the sodium carbonate was added. So this is another problem.


Somebody suggested earlier to add a few drops of vinegar. That's what SWIM did. She wishes she knew more specific amount of vinegar, or pH of the solution.

Now, what would be the best way to clean the product?
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burnt
#17 Posted : 12/28/2009 9:20:31 AM

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Quote:
2. SWIM would prefer to exclude any guesswork from the process but she is still looking for exact quantities of chemicals. Do you happen to know them?


Check the solubility of NaCl and sodium carbonate in water and use less then that.
 
Trickster
#18 Posted : 12/28/2009 3:44:22 PM

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burnt wrote:
Quote:
2. SWIM would prefer to exclude any guesswork from the process but she is still looking for exact quantities of chemicals. Do you happen to know them?


Check the solubility of NaCl and sodium carbonate in water and use less then that.


SWIM is not a chemist. Anybody ever did that?
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burnt
#19 Posted : 12/28/2009 3:53:01 PM

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Its general chemistry stuff. You can find solubilities on wiki.

You could also experimentally determine. Just add salt into regular distillated water until it precipitates. Keep track of weights. Then add sodium carbonate until it precipitates. You might need to use like half NaCl of saturation point. Maybe something like this would work.

Numbers will vary slightly depending on how much from the rue stuff dissolves in the water too. This will change solubility as well. Its good to get estimates anyway from the chemical properties of NaCl and sodium carbonate.
 
69ron
#20 Posted : 12/28/2009 6:54:23 PM

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Trickster wrote:
Now, what would be the best way to clean the product?


Trickster, the best solution at this point is to put the product in cold water with a little ice, and mix it for a few minutes. Then filter it until all the water and ice filter through. The sodium carbonate should dissolve and wash away. Harmine is insoluble in water, harmaline is very slightly soluble in cold water. Some loss of harmaline will be had, but no matter what you do, that’s going to happen. Even when you precipitate the alkaloids using salt water, some loss of harmaline occurs. Pretty much at every step in this process, there’s loss of harmaline.

Repeat if there's still some sodium carbonate taste left.

The are other options, but this is the easiest.
PLEASE DO NOT PM ME.
I do not answer PMs! I delete all PMs no matter who they are from, even from a good friend. I don't have time for the PMs. I have very little free time. If you have a question just post it in a threadSmile


All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a fictional character based on other people) either obtained a license for said activity, did said activity where it is legal to do so, or as in most cases the activity is completely fictional.
 
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