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harmine extract need help

midnight490

midnight490

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What is this black?I got this product at the last step of the extraction. I don't know if it is toxic because it is so weird.it breaks into pieces when touched and cannot be separated at all.

In the fourth picture, I stirred it. Sorry.


I used 100 grams of raw materials. I filtered it after boiling it in the first step. I used NaOH for alkalization, but I didn't wash it very cleanly in this step. Finally, I acidified the crystals with 75ml of acetic acid and heated and mixed it with 200ml65g of medical sodium chloride.I got this product at the last step of the extraction. I don't know if it is toxic because it is so weird.What is this black?it breaks into pieces when touched and cannot be separated at all.

In the fourth picture, I stirred it. Sorry.


I used 100 grams of raw materials. I filtered it after boiling it in the first step. I used NaOH for alkalization, but I didn't wash it very cleanly in this step. Finally, I acidified the crystals with 75ml of acetic acid and heated and mixed it with 200ml65g of medical sodium chloride.Cooling indoors, not in the refrigerator
 

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It's not clear to me from your write-up, but it sounds like you may have missed some filtering?

filtered it after boiling it in the first step. I used NaOH for alkalization, but I didn't wash it very cleanly in this step. Finally, I acidified the crystals with 75ml of acetic acid and heated and mixed it with 200ml65g of medical sodium chloride.
Click to expand...

So to me this reads:
Boil
Filter (keep solution)
Base
Acidify
Manske

I would approach this:
Boil
Filter (keep solution)
Base
Filter (keep precipitate)
Acidify
Filter (keep solution)
Manske

From the way your write-up reads it sounds as if you didn't filter and keep/discard the relevant bits when you based and acidified, just based your initial tea, then acidified it, then Manske'd. Is that correct?
 
Memberberries said:
It's not clear to me from your write-up, but it sounds like you may have missed some filtering?



So to me this reads:
Boil
Filter (keep solution)
Base
Acidify
Manske

I would approach this:
Boil
Filter (keep solution)
Base
Filter (keep precipitate)
Acidify
Filter (keep solution)
Manske

From the way your write-up reads it sounds as if you didn't filter and keep/discard the relevant bits when you based and acidified, just based your initial tea, then acidified it, then Manske'd. Is that correct?
Click to expand...
Sorry, omitting some details is my fault. I spend a day filtering and precipitating each step, but the crystals precipitated in the alkalinization step are dark brown because I did not wash them very clean.

I washed it twice with water before the sodium chloride precipitated, but it was still brown, but I decided it was enough and didn't continue washing it.
 
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It looks like this now, so disgusting hahaha
 

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Well, I better extract again, just to be safe. But I'm really curious about what this black one is, and I hope someone can answer it.
 
What is "medical sodium chloride"? Are you sure it doesn't have any additives?

To me it looks there is something additional there, you can do manske on unfiltered rue tea and it would still come out good, I never seen this black stuff before, doesn't look typical for rue or caapi.

It does look like you have harmala crystals there but it is not the black stuff.

I there is no toxic additive, you can try cleaning it. I think you can redissolve it in acidic water, filter, base, decant, multiple water washes, acidify and manske again using pure salt (no iodine, no additives of any kind)
 
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Sakkadelic said:
What is "medical sodium chloride"? Are you sure it doesn't have any additives?

To me it looks there is something additional there, you can do manske on unfiltered rue tea and it would still come out good, I never seen this black stuff before, doesn't look typical for rue or caapi.

It does look like you have harmala crystals there but it is not the black stuff.

I there is no toxic additive, you can try cleaning it. I think you can redissolve it in acidic water, filter, base, decant, multiple water washes, acidify and manske again using pure salt (no iodine, no additives of any kind)
Click to expand...
Well. . Medical sodium chloride is a popular method in my country. One pack of 4.5 grams of sodium chloride is used to prepare physiological saline for personal cleaning.


It's because none of the guides mention it that I feel strange. Maybe there is an error caused by something I didn't pay attention to. I will try to correct it. Thank you for your experience.
 
midnight490 said:
Well. . Medical sodium chloride is a popular method in my country. One pack of 4.5 grams of sodium chloride is used to prepare physiological saline for personal cleaning.


It's because none of the guides mention it that I feel strange. Maybe there is an error caused by something I didn't pay attention to. I will try to correct it. Thank you for your experience.
Click to expand...
Yes, you can make your own saline, it is easy, just mix salt and water.

Good luck!
 
Sakkadelic said:
Yes, you can make your own saline, it is easy, just mix salt and water.

Good luck!
Click to expand...


Hi, sorry to bother you. This is the result of my latest purification attempt. Starting with 100 grams of raw material (excluding components still in the sodium chloride solution and any losses), I obtained approximately 8 grams of final product. Does this yield seem correct? I think the quantity might be higher than expected.
 

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Moreover, I'm not sure whether it's due to the vinegar I used or something else, but the final product came out in this dark green color. However, I did follow the procedure.
This is a photo of the crystals formed during precipitation from the sodium chloride solution.
 

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Wait, I noticed that other people's procedures involve using sodium carbonate. Could the issue be because I didn't use it in my process?

I using sodium hydroxide as the alkaline solution
 
midnight490 said:
Hi, sorry to bother you. This is the result of my latest purification attempt. Starting with 100 grams of raw material (excluding components still in the sodium chloride solution and any losses), I obtained approximately 8 grams of final product. Does this yield seem correct? I think the quantity might be higher than expected.
Click to expand...
Oh no bother at all! I am sorry if I sounded unfriendly earlier, I didn't mean to.

sodium hydroxide is good to use but sodium carbonate is safer.

midnight490 said:
Moreover, I'm not sure whether it's due to the vinegar I used or something else, but the final product came out in this dark green color. However, I did follow the procedure.
This is a photo of the crystals formed during precipitation from the sodium chloride solution.
Click to expand...
this looks much better, nice crystals!

you can try cleaning it like this.
1. dissolve with distilled white vinegar and hot water. when things stop dissolving it is ok don't add more vinegar, even if they looked like harmalas.
2. let the solution cool down and the undissolved stuff to settle.
3. pour through cotton or coffee filter leaving the undissolved stuff behind. discard the undissolved stuff
4. base the solution with sodium hydroxide or sodium carbonate. let the harmala freebase settle in the fridge for few hours. pour the water off slowly leaving the freebase behind.
5. do water wash: top the container with distilled water, let the harmala freebase settle in the fridge for few hours again. pour off the water. repeat water wash 2 times.
6. dissolve with distilled white vinegar and hot water. filter.
7. do the sodium chloride step like you did before.

Good luck!
 
Sakkadelic said:
Oh no bother at all! I am sorry if I sounded unfriendly earlier, I didn't mean to.

sodium hydroxide is good to use but sodium carbonate is safer.


this looks much better, nice crystals!

you can try cleaning it like this.
1. dissolve with distilled white vinegar and hot water. when things stop dissolving it is ok don't add more vinegar, even if they looked like harmalas.
2. let the solution cool down and the undissolved stuff to settle.
3. pour through cotton or coffee filter leaving the undissolved stuff behind. discard the undissolved stuff
4. base the solution with sodium hydroxide or sodium carbonate. let the harmala freebase settle in the fridge for few hours. pour the water off slowly leaving the freebase behind.
5. do water wash: top the container with distilled water, let the harmala freebase settle in the fridge for few hours again. pour off the water. repeat water wash 2 times.
6. dissolve with distilled white vinegar and hot water. filter.
7. do the sodium chloride step like you did before.

Good luck!
Click to expand...


Haha, I didn’t find you unfriendly at all—being serious about chemistry is both necessary and correct. Since there’s no issue with the product being this color, that’s a relief! I was a bit worried it might have turned into something strange.
 
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