merkin said:
As a follow-up, I based the gunk what dissolved below pH5.5 with sodium carb and it crashed as a brown precipitate, so it would survive the usual A/B steps.
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Harmalas extraction-syrian rue (by SAKKADELIC)
- Thread starter Sakkadelic
- Start date
As a follow-up, I based the gunk what dissolved below pH5.5 with sodium carb and it crashed as a brown precipitate, so it would survive the usual A/B steps.
michaeljohn1234m
Rising Star
Hi people
This is my first go at this Tek by SAKKADELIC
I just finished step 5,looks good. BUT has a bad taste to it.
I took some photo's an d when I zoom in you can see white stuff (caustic soda) ?
in step 4 I water washed 5 times the PH was 12.I don't know how many times two wash it
I need to know my next steps In detail
So do dissolve it in vinegar and do more water washers and how low should I go with the PH.
This is my first go at this Tek by SAKKADELIC
I just finished step 5,looks good. BUT has a bad taste to it.
I took some photo's an d when I zoom in you can see white stuff (caustic soda) ?
in step 4 I water washed 5 times the PH was 12.I don't know how many times two wash it
I need to know my next steps In detail
So do dissolve it in vinegar and do more water washers and how low should I go with the PH.
Attachments
michaeljohn1234m
Rising Star
I'm thinking of going to step 4:re basifying and water washes.but how many washers and what PH to go down to
Hi michaeljohn1234m,
these are harmala hcl crystals obtained by manske so there is no way they are contaminated with caustic soda. one very likely contamination is salt.
they are supposed to taste bitter and bad in this form. the freebase is tasteless when pure in my experience.
your results look great from the pictures :thumb_up: . what was the yield?
if you'd like to further purify it:
-dissolve in warm water and a little bit of distilled white vinegar.
-basify with sodium carbonate, after basification with only sodium carbonate the solution remains yellow, this is fine but you can add a few drops of caustic soda solution and this will complete the conversion
-top the container with water, let settle, decant. do a couple of washings. you can collect the harmalas as freebase at this point.
-if you'd like to have the hcl crystals. you can repeat the manske step.
these are harmala hcl crystals obtained by manske so there is no way they are contaminated with caustic soda. one very likely contamination is salt.
they are supposed to taste bitter and bad in this form. the freebase is tasteless when pure in my experience.
your results look great from the pictures :thumb_up: . what was the yield?
if you'd like to further purify it:
-dissolve in warm water and a little bit of distilled white vinegar.
-basify with sodium carbonate, after basification with only sodium carbonate the solution remains yellow, this is fine but you can add a few drops of caustic soda solution and this will complete the conversion
-top the container with water, let settle, decant. do a couple of washings. you can collect the harmalas as freebase at this point.
-if you'd like to have the hcl crystals. you can repeat the manske step.
michaeljohn1234m
Rising Star
Hi Sakkadelic
That's good news. I thought they were suppose to be tasteless, but that's step 6.
I got 7g from 100g of seed and it looks great.
your tek is so much easier. I did 15min microwaves. 5 times, got it all out.
I'm going to use it with DMT. So what I'd like to know is,Do I use it as is or should I go the next step and free base it, or both steps back to hcl crystals.
and thank you for all the Time you have put into this Tek and the others who contributed
That's good news. I thought they were suppose to be tasteless, but that's step 6.
I got 7g from 100g of seed and it looks great.
your tek is so much easier. I did 15min microwaves. 5 times, got it all out.
I'm going to use it with DMT. So what I'd like to know is,Do I use it as is or should I go the next step and free base it, or both steps back to hcl crystals.
and thank you for all the Time you have put into this Tek and the others who contributed
Thanks! glad it worked out well for you.
7% harmalas HCl is a very good yield! and it looks clean. it is probably contaminated a bit with salt but that is fine.
if you use it orally in capsules, it doesn't make much difference whether it's harmala salts or freebase. The freebase however is heavier so 100 mg of HCl harmalas =(in effect)= 85 mg freebase harmalas. you need to adjust your dose accordingly.
the freebase is more versatile, it can be used sublingually with minimal taste, it can be smoked on its own, infused in leaf, or used to make changa. but if it is not stored properly it degrades and turns red, the HCl harmalas is more stable and stores better.
7% harmalas HCl is a very good yield! and it looks clean. it is probably contaminated a bit with salt but that is fine.
if you use it orally in capsules, it doesn't make much difference whether it's harmala salts or freebase. The freebase however is heavier so 100 mg of HCl harmalas =(in effect)= 85 mg freebase harmalas. you need to adjust your dose accordingly.
the freebase is more versatile, it can be used sublingually with minimal taste, it can be smoked on its own, infused in leaf, or used to make changa. but if it is not stored properly it degrades and turns red, the HCl harmalas is more stable and stores better.
Tumupasa
Established member
Best tek so far!
I just finished this tek, though I skipped the manske, from 50g Rue, i extracted 4.4g of beige fb harmala, Im impressed by the results.
Thanks @Sakkadelic !
I just finished this tek, though I skipped the manske, from 50g Rue, i extracted 4.4g of beige fb harmala, Im impressed by the results.
Thanks @Sakkadelic !
That is awesome! I'm happy you're satisfied with the results
I'm sure it's perfectly useable as is but 8.8% yield is a bit high for harmalas 6% freebase is more typical, so if you want more accurate dosage I would suggest refining it more.
Tumupasa
Established member
Yeah, that's what I thought, probably not the cleanest fb but I'll use 1g for changa (taking into account that there may be some "undesired material") and yes, I'll refine the other 3.4 g and maybe will do a manske for storing HCl.
That sounds good!
For changa it doesn't matter much but for something like pharma where the dose per trip is much higher it becomes significant
For changa it doesn't matter much but for something like pharma where the dose per trip is much higher it becomes significant
Tumupasa
Established member
Hey, so I'm having a hard time converting to salts.
I saved approx. 3.5g freebase harmala and thought I would convert to HCl.
To do so, I dissolved the freebase in 50 ml water + vinegar solution and added the exact same amount of saturated water with non-iodized salt. As I struggled having the salts settle I left it to evaporate slowly, it took one week (!) to fully evaporate.
The result was some rocky brown crystals.
As it was obvious from the color there was a lot of impurities, I re-dissolved the salts in 50ml hot water, decanted and ended with a yellowish clear liquid, added 50ml saturated water but this time haven't witnessed any precipitation, so again I added 50ml of saturated water and still nothing happened. Now it's in the fridge but after 4 hours, still no precipitation.
At this stage I don't know what to do, any idea would be welcome!
I saved approx. 3.5g freebase harmala and thought I would convert to HCl.
To do so, I dissolved the freebase in 50 ml water + vinegar solution and added the exact same amount of saturated water with non-iodized salt. As I struggled having the salts settle I left it to evaporate slowly, it took one week (!) to fully evaporate.
The result was some rocky brown crystals.
As it was obvious from the color there was a lot of impurities, I re-dissolved the salts in 50ml hot water, decanted and ended with a yellowish clear liquid, added 50ml saturated water but this time haven't witnessed any precipitation, so again I added 50ml of saturated water and still nothing happened. Now it's in the fridge but after 4 hours, still no precipitation.
At this stage I don't know what to do, any idea would be welcome!
If you let it evaporate, the residue will have salt (NaCl) too, not only harmala salts.
How much vinegar did you add? Did the harmalas dissolve completely?
Heat the water before saturating it with salt. Add at least 10g salt per 100ml water, but you can add more (salt is soluble up to 36g/100ml at 25C). Then dissolve the harmalas in it (no need for more vinegar, they'll be in salt form already if there was enough vinegar) and let it cool off slowly outside the fridge. Then put it inside the fridge and wait, at least for 24 hours. Patience is key here.
Tumupasa
Established member
Thanks for the answer @blig-blug
Ok, sounds logical!
about 1 part vinegar to 3 parts water, but only when I dissolved my freebase. Ihaven't added more vinegar, when I dissolved my brownish salts, just hot water
So, you're suggesting adding even more salt to my heated harmala water, even though I already added 2 times 50ml saturated solution?
Yeah, maybe I'll wait a little bit more before adding more salt. I think my confusion is due to the fact I'm expecting for an immediate precipitation as it does when freebase precipitates, but it seems that it's not always the case with salts.
If it dissolved fully, then it was enough. It was just to make sure.
How saturated was it? Don't rely on it apparently just not dissolving anymore, if you didn't heat it up it can be hard to saturate. And at it was a small volume, I suppose it was not easy to stir. When I have done the manske, I have always done it to just slightly less than 1L, and it has worked well. What matters is the saturation, the total amount of salt is not relevant. So it's better to measure it and make sure there are at the very least 10g/100ml. And that concentration should be the minimum for the whole volume, not just what you add to it. For this reason, I would add the salt directly to the harmala solution instead of saturating water and mixing it in later.
I wonder also if, as a smaller volume cools down faster, that could make it harder for crystals to form. A larger volume should work without issues. If you look at other people's pictures, most people are using larger volumes than 100ml total.
In this step (manske) crystals don't precipitate out suddenly, but form very slowly. In my case it always takes them hours to start forming. Once the first small needles appear, they grow quite fast.
One thing you can do is base it and see if the harmalas are still there, retreive the freebase, and redo the manske. When you say yellowish clear, do you mean its color is yellow like or a dilute yellow? It should have a strong color especially in just 50 ml.
Instead of evaporating what you should have done is reheat the solution to near boiling in a double boiler until things redissolve, then just leave it as is in the hot water to fully cool on it's own, that helps form bigger crystals. I like my manske to always start from a near boiling temperature. A very concentrated solution is also not ideal, the crystals won't have enough room to grow and they won't settle well.
And since your 8.8% yield was on the high side, there should have been a good amount of undissolved stuff when you acidifed and dissolved the freebase, 1.5g or more. Did you observe that and filtered it out?
Tumupasa
Established member
@blig-blug and @Sakkadelic , thank you guys, I will troubleshoot this week end, I'll get back to you when I figure out what is/was going wrong 
Tumupasa
Established member
Hey, so, I retrieved the freebase (which means I still have harmalas in the soup), dissolved again in hot water and vinegar, ended up with 180ml,, warmed it, I added 180ml of saturated hot water (there were salt crystals remaining at the bottom, left it to cool down at room temp for 4 hours then stored it in the fridge. Now it's been 18 hours and as you can see in the photo nothing seems to be happening.
I've been struggling with it for weeks now, so I'm starting to think I will retrieve freebase again and work with this... unless someone here have an idea...
I've been struggling with it for weeks now, so I'm starting to think I will retrieve freebase again and work with this... unless someone here have an idea...
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Did you measure how much salt you added? I'm asking because it always takes me a long time to dissolve it. But if there's enough salt for sure we can discard that as a problem.
I don't think there should be a problem working with freebase. So that's an option. I always store it as freebase.
Another option if you really prefer salt form would be to just mix the freebase in water, add enough vinegar for it to dissolve completely (slowly, in order to not add too much), and boil it until some kind of goo-ish residue remains. It should be less easy to handle than crystals, but still doable, and if it's for changa it shouldn't matter much.
Yet another option would be to dissolve the freebase in Ethyl Acetate and salt it out with citric acid, as described here, in the "salting" step: Ethyl Acetate Approach Harmala - DMT-Nexus Wiki
Tumupasa
Established member
Yes, 65g for 180ml water
Sure, this time, i wanted salt for taking sublingually or dissolved in water, so oral use. but if freebase can also wok for these purposes, i'll maybe stick to this.
That should definitely be enough. No idea then of what could be happening.
For that specific use you can just either dissolve it in water with some vinegar (tastes very bad but works), or in some acidic juice. When taking oral, extracted harmalas I always dissolve my freebase in orange juice. The acid converts it into salt form.