Thanx homie.

So I had 3 grams of uncleaned rue extract. I added it to some slightly acidic water strained ot the solids. Then combined the two jars of water and added some lye (to much lye) immediately the brown liquid turned cloudy.Let everything settle for 24 hrs then decanted all that was possible. Remainis were poured in a pyrex dish and let the rest of the water evap.Next day there was a dark tan sandy crystaly pile.So now what.Also I used alot of salt and Ican tell there is salt still in it.How would one clean further .I have no access ammonia or alcohol. I do have some acetone naptha and lye if that helps.So what should be done next.

For cleaning a rue extract I would consider adding it to acidic water, leave it in the fridge as long as you care to wait and then filtering the liquid and repeat the salting step. Repeat this until your extract looks good enough, then basify.

And try to use as little heat if any when drying.

Should work a charm.

Sorry Big Inhale ILPT didn`t get it quiet right. After one wash with basified water with sodium carbonate(ph 12)it`s ok to perform one or two washes with just distilled water, because there is some carbonate trapped in product and it`s enough to basify pure distiled water which should be added in volume 20 x to volume of precip.

Not sure about lye,lye disociate much better then sodium carbonate so maybe just one wash with distilled water after basifying should be alright.But ILPT cannot do any tests cos lye he can get is only 98% pure and definitely not food grade.
He using baked sodium bicarbonate from tesco chain. He baking 2 hours at 200C and half an hour at 250C and he has good carbonate with satisfying results.

Next time he will recrystalize both rock salt and sodium carbonate to get even better result
cos he can feel slight hint of ammonia in his sodium carbonate

I need some help. 2 grams rue extract was placed in vinegar water then strained. Then sea salt was added to the water until none dissolved then filtered the water was then basified. Clouds formed let settle for 2 days water drained off then the gunk was placed in a pyrex dish with a fan blowing over it ended up with a sparkly brownish tan dirt.But it was double the weight when weighed out.So what went wrong I can tell its salt but how do I getrid off it.

Look at step 6 from this tek:
http://dmt-nexus.me/foru...t.aspx?g=posts&t=764

All the salt will drop right out leaving the goods dissolved in the alcohol to be decanted, filtered, and evapped. I'm not sure why most people are so against doing this methyl alcohol step?

or disolve it in some water that has been slightly acidified with vinegar then slowly start adding sodium carbonate - the freebase should fall out the water - much cleaner - repeat the salting and freebasing a few times for a very very clean product.

SWIM has had a very similar problematic situation occur. It seems like that you can over-saturate the liquid with too much salt? SWIM is filtering some non-bassified rue gunk at the moment but can clearly see salt crystal on the filter... hmmmmm, SWIM will try some of the suggested procedures and see how it goes

In this point if you now how much your salt in product weight just add enough distilled water to make 10% saline solution out of it and chilled it all down, let it settle nicely and siphhone of saline. You will loose less then with multiple freebasing

Why would you when gar, salt, sodium carbonate, parboiled and distilled water all together does great job without using any fancy organic solvents.
methanol and etylalkohol are both pricey and metol is poissonous as hell (120 ml ~ 4 oz WILL KILL ANY SWIM !) and as a poison it`s a bit watched in some countries.
If ILPT has access to free methanol or ethanol he will go for it but he never would buy it for this purpose. There are other things well worthy spent money for, why would he does this

Why would you when gar, salt, sodium carbonate, parboiled and distilled water all together does great job without using any fancy organic solvents.
methanol and etylalkohol are both pricey and metol is poissonous as hell (120 ml ~ 4 oz WILL KILL ANY SWIM !) and as a poison it`s a bit watched in some countries.
If ILPT has access to free methanol or ethanol he will go for it but he never would buy it for this purpose. There are other things well worthy spent money for, why would he does this

What if I dont know?

Ok so here's the deal... it's really much simpler than people are making it out to be.

First of all, if you have excess salt in your harmaloids, simply dissolve them in an acidic solution and re-precipitate them with sodium carbonate solution, just as phlux said. Trust me this really is the easiest and best way.

As for what acid to use, swim used to use gar but now used citric acid cuz he doesn't have to huff gar fumes that way (gar is bad for the lungs).

Swim's last rue extraction used 100g of citric acid for each round on a kilo. Probly overkill but it worked GREAT, swim got super yields doing it that way (Over 50g from his first two rounds, and there's still more in there waiting for him to quit being lazy!). There was no problem when doing the salt precip, apparently the 'loids turn into hcl salts and precipitate in the presence of NaCl regardless of whether they were cooked out of the seeds as acetate salts or citrate salts.

There is absolutely no need to use lye with rue. You don't want any NaOH ending up in your final product, there's simply no reason to risk it. Sodium carbonate is the perfect base for rue. Swim used to use ammonia but has given that up since he found sodium carbonate, it's perfect for this.

Finally, there is no worry about using distilled to clean your freebase. Last time swim had some freebase that he had already cleaned twice by putting it in near-boiling water, and when he went to clean it a third time he weighed it first. It weighed out at 50g. Then he boiled some distilled h2o, killed the heat, tossed in his alkaloids, stirred, and filtered. When weighed again he still had 48g, overall he lost less than two g of weight, some of which was not alkaloids but rather impurities.

Swim has recently found a brand of drinking water called Evamor that is ph9. From now on he plans on using this to clean his alkaloids. But distilled works fine, he knows this from much experience.

The ideal tek for getting harmaloids is as follows:

1. Boil seeds in citric acid solution, reduce to simmer, simmer for ~45min.

2. Strain.

3. Add 100g NaCl per litre of solution. Add directly to solution, heating if necessary to help it dissolve.

4. Refridgerate overnight

5. Pour off liquid from the top (you can save it if you wanna get the other alkaloids out by precipping with sodium carbonate, but be careful with these as they are somewhat toxic. Do not give them to pregnant women unless they want an abortion as they are uterotonic). Filter mush (by the way, I really like the syringe idea! BRILLIANT!)

6. Redissolve the mush in boiling distilled water. Alkaloids are already in salt form so no need to use an acid for this. Filter to remove any insoluble crud. Cotton balls work well for this stage of filtration, much quicker than paper filtering.

7. Use saturated sodium carbonate solution to precip fb alkaloids. Add until color stabilizes, then add a little more for good measure.

8. Pour off liquid from the top, and filter.

9. Bring distilled water, or better yet Evamor, to a boil. Kill the heat and let it cool just a little, then toss in your alkaloids. Stir briefly and filter.

10. Repeat step 9 until your wash water is clear to your satisfaction.

11. Enjoy!

Also, if you wanna separate harmine and harmaline, there is no need to use any nasty solvents as burnt suggested. One need only basify to roughly ph8, and the harmine will precip while the harmaline stays dissolved. One tek calls for adding ammonia dropwise to reach the desired pH, but sodium carbonate solution should work just as well with less stinkiness. Then after filtering out the harmine, basify the rest of the way to get harmaline.

That's really all there is to it. No need for any solvents, lye, alcohols... all you need is citric acid and sodium carbonate. It's that simple.

Much Love,
SyZ

Overall best tek for harmalas I seeing here so far(sorry if I missed something)
However ILPT has some comments to this post:

One has fume hood, no ?


...this rose wave of DISAGREEMENT in the ILPT`s household. You can boil off gar whilst you cannot boil off citric acid.He using parboiled tap water(which is pretty much hard=slightly basic) in the initial extractions and boiling down pretty much too. pH changing a lot. You not mentioned pH at all like others before you. ILPT taking it as ignoracy towards chemistry which is behind all this There is other advantage of acetic acid he will talk about later...

Absolutely! NaOH or NH4OH (NH3.OH exactly ) has not place in this extraction.
Sodium carbonate is great, bicarbonate can be use to some point too. But one will try some untraditional tek where powers of Ca(OH)2will be tested


Well, there is a worry. distilled water has no solubles in and has pH of 7.Parboiled Tap water is everywhere slightly different .... not comparable at all
why rushing with freebasing ????? One you have mixed harmalas hydrochlorides just take advantage of their insolubility in saline solution. Boiled with solution distilled water and NaCL (10% is surely safe, but less concentrated saline will be tested )let cool down and settle, siphone off dirty saline...and again...until clean hydrochlorides obtained.Freebasing would be the very last step. One wouldn`t loose virtually anything... Did you think about this?

NOTHING is ideal, neither this tek



Very true Syz, but one should not forget that his "harmine" could be contaminated up to 20 % with harmaline when "roughly" precip at pH 8, but that`s not a real contamination

SWIM followed these directions up to step 8 and seems to have achieved a relatively satisfactory result. The only problem that was encountered was that while adding the saturated sodium carbonate to begin precipitation SWIM was unsure when to stop adding once the color had stabilized so SWIM believes that there may have been too much saturated sodium carbonated solution added. Is it possible to add too much?

SWIM reports that the final dried substance looks similar to what was described earlier in this thread and is very soft and almost like talc powder... SWIM did get a little on his hands and when it was washed it felt very baseish...

SWIM is a little hesitant to try and wash it with water at the moment to remove any further impurities.. but will try it and see how it goes...

It`s good to have pH papers for this ...

SWIM sometimes use a ph meter, but it seems unreliable and the readings tend to fluctuate... time for a new probe or something SWIM thinks... SWIM will get a bunch of ph papers

After just reading the above post by soulfood it has been noticed that heat is not recommended during the drying phase. SWIM in his usual impatient manner decided to dry the filter papers in the oven on a very low setting. maybe >60C or so... will this damage the harmaline/harmine at all? if so what exactly will happen to it?

SWIM finished the final wash and filter and has ended up with about 3/4 of what he had before the wash. So from 50g of Rue SWIM has ended up with about .75g of whiteish/grayish powder, and there is more settling in the fridge at the moment waiting to be worked on.

Overall this is a great tek that is safe and easy. Even if you are sloppy like swim and dont really pay attention to weighing stuff, or ph or whatever (just leaving it up to intuition, hehe) you can still get a relatively satisfying amount.

Thanks to phlux- and to everyone who has contributed knowledge to this thread, it has been very helpful

Any pics of very very clean product?

well look at page one - u see it as it comes out - brown - then to light brown - then to creme, each time its washed it gets so much cleaner.

another wash was done and swim was happy with the product.