I read in some sources that adding sodium carbonate to the solution is good if an emulsion formed. Sodium carbonate reduces the solubility of water, so the free base is separated of water.
Has anybody tried this way?
Has anybody tried this way?
I had some relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, even the tests shown purity around 95. Crystallization of oversaturated water solution didn't bring any result, as well as acetone. So I decided to make an attempt with IPA as the last resort.
The report about result will come later. But I can say now, the volume of IPA mentioned by noble @G.Patton is quite excessive. I had 22 gr, so I started with 80 ml of IPA. Then, as it started boiling - 82.6C, I removed some volume down to 60 ml, and slowly added the salt. It dissolved completely without any difficulty. So I kept it on the hotplate for a while.
At the ending, as I was able to see powder rising in the beaker (but it could be some insoluble impurities as well) total volume was 71 ml. The salt itself shall take 22.0/ 1.1 = 20 ml. So IPA volume shall be 71 - 20 = 51 ml, that means 1 ml of hot boiling IPA solves at least 0.43 gr of MDMA HCl or even more, let's see.
IPA purity is >99.5.
Might be, it is better to start with 20 ml of IP per 10 gr of MDMA?
The report about result will come later. But I can say now, the volume of IPA mentioned by noble @G.Patton is quite excessive. I had 22 gr, so I started with 80 ml of IPA. Then, as it started boiling - 82.6C, I removed some volume down to 60 ml, and slowly added the salt. It dissolved completely without any difficulty. So I kept it on the hotplate for a while.
At the ending, as I was able to see powder rising in the beaker (but it could be some insoluble impurities as well) total volume was 71 ml. The salt itself shall take 22.0/ 1.1 = 20 ml. So IPA volume shall be 71 - 20 = 51 ml, that means 1 ml of hot boiling IPA solves at least 0.43 gr of MDMA HCl or even more, let's see.
IPA purity is >99.5.
Might be, it is better to start with 20 ml of IP per 10 gr of MDMA?
Last edited:
↑View previous replies…
- By Mr Good Cat
Policja Polskaprobably my hands are growing out of my ass. i did as i described above, coolled the beaker down to RT, and put it in the freezer for 2 hours. then, all I see, the whole RM is completely frozen piece of ice. is there any suggestion what to do? repeat the procedure with additional IPA in the RM?
↑View previous replies…
- By Mr Good Cat
w2x3f5It is not about color. The problem is all the RM (MDMA HCL + IPA) turned to the piece of ice (or rather a kind of dense porridge).
I even added 20 ml of IPA to increase total RM to 80 ml, and left it not in the fridge instead of freezer for a while with the same result: total RM turned into the same porridge without any chance to saperate dirty IPA from chloride.
I even added 20 ml of IPA to increase total RM to 80 ml, and left it not in the fridge instead of freezer for a while with the same result: total RM turned into the same porridge without any chance to saperate dirty IPA from chloride.
- By w2x3f5
Policja Polskaunderstood you.
if you are trying to form crystals, then slow cooling is important, scratch-free dishes, also do partial slow evaporation of alcohol at room temperature. if the solution is too saturated with salt, then the salt will fall out in flour.
if you are trying to form crystals, then slow cooling is important, scratch-free dishes, also do partial slow evaporation of alcohol at room temperature. if the solution is too saturated with salt, then the salt will fall out in flour.
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- By Mr Good Cat
w2x3f5yes, I have a feeling that the salt precipitates too quickly. may be, it could be right to leave the beaker on RT for 5-8 hour to see what is going on.
- By G.Patton
Policja PolskaIt is better to cool it down as slowly as possible at room temperature without any shaking in order to growth the crystals.
Four attempts of IPA crystallization. Fulll report with quantities, volumes and timing
or FAST IS ALWAYS BAD!
IPA purity is >99.5.
Relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, apart of the fact the tests shown purity around 95. Weight of sample - 22 gr, calculated volume of sample - 22 / 1.1 = 20 ml.
Stirring hotplate used.
All the coolings are done with the beaker hermetically closed to avoid moisture from the air catching.
1. First I prepared 60 ml of boiling IPA 82.6C on the stirring hotplate, then put the salt, that dissolved immediately. Considering such fast dissolvation, I decided, the volume of IPA was too huge and evaporated some.
The beaker was left on the hotplate to cool down to RT, that took 80 minutes approx., then moved it to the freezer.
The result came after one hour as a dense porridge without any trace of dirty IPA.
Total volume of RM after warming up to RT was 62-63 ml, that means the remains of IPA was 42-43 ml.
Result: FAULT!
2. RM was warmed up to RT, then certain IPA was added with some stirring to increase the volume of RM up to 87 ml under RT.
RM was heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the freezer.
The result was checked after 5-6 hours: dense porridge again.
Result: FAULT!
3. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the fridge.
The result was checked after 1 hours: dense porridge again.
Result: FAULT!
4. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, and left at RT for a while. As 120 minutes gone after heating was finished: some crystalls appeared at the bottom. Total volume of RM at this point was 81 ml - that means around 6 ml was evaporated while heating up.
Then I left RM at RT for 240 minutes more. As 240 minutes gone, the crystalls became pretty visible and transparent.
So, the beaker was moved to the fringe for 2 hours without any noticable changes.
With the next step the beaker was moved to the freezer to finish the process.
Result: SUCESS!
Hope, this full description will help some newbies with volume and timing estimation and let them avoid my mistakes.
Total yeld is 18.5 gr.
3.5 gr are somewhere in the dirty IPA or evaporated(((
or FAST IS ALWAYS BAD!
IPA purity is >99.5.
Relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, apart of the fact the tests shown purity around 95. Weight of sample - 22 gr, calculated volume of sample - 22 / 1.1 = 20 ml.
Stirring hotplate used.
All the coolings are done with the beaker hermetically closed to avoid moisture from the air catching.
1. First I prepared 60 ml of boiling IPA 82.6C on the stirring hotplate, then put the salt, that dissolved immediately. Considering such fast dissolvation, I decided, the volume of IPA was too huge and evaporated some.
The beaker was left on the hotplate to cool down to RT, that took 80 minutes approx., then moved it to the freezer.
The result came after one hour as a dense porridge without any trace of dirty IPA.
Total volume of RM after warming up to RT was 62-63 ml, that means the remains of IPA was 42-43 ml.
Result: FAULT!
2. RM was warmed up to RT, then certain IPA was added with some stirring to increase the volume of RM up to 87 ml under RT.
RM was heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the freezer.
The result was checked after 5-6 hours: dense porridge again.
Result: FAULT!
3. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the fridge.
The result was checked after 1 hours: dense porridge again.
Result: FAULT!
4. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, and left at RT for a while. As 120 minutes gone after heating was finished: some crystalls appeared at the bottom. Total volume of RM at this point was 81 ml - that means around 6 ml was evaporated while heating up.
Then I left RM at RT for 240 minutes more. As 240 minutes gone, the crystalls became pretty visible and transparent.
So, the beaker was moved to the fringe for 2 hours without any noticable changes.
With the next step the beaker was moved to the freezer to finish the process.
Result: SUCESS!
Hope, this full description will help some newbies with volume and timing estimation and let them avoid my mistakes.
Total yeld is 18.5 gr.
3.5 gr are somewhere in the dirty IPA or evaporated(((
- By G.Patton
Policja Polska
Anyway, congratulation and thank you for your full report with "FAULT!" results. It helps people to do not repeat same mistakes.
Actually, it is acceptable color for mdma =)
I wrote in the topic Recrystallization and Hot Fltration (Lab FAQ section) that the slowest cooling have to be applied. Also, don't use freezer with -17*C. It is worth to cool down at 3-4*C in regular cooling camera of fridge.
You can evaporate IPA in mother liquor on a hot plate for about 1/2 or more and slowly cool it down to get second batch of a little bit dirtier crystals.
Anyway, congratulation and thank you for your full report with "FAULT!" results. It helps people to do not repeat same mistakes.
- By Mr Good Cat
G.PattonYes, it is acceptable. The test with methanol and ruler also shows high percentage. Any way, we are looking for the purest product. This is why all these efforts.
I did it like this a long time ago:
1 Liter of Ipa (isopropyl alcohol) 99% laboratory grade (the "drugstore" grade does not work)
1 Liter of 99% acetone ("drugstore" grade does not work and less than Mercadona)
1 glass of 1 liter
1 hot plate (but since not everyone has it, a double boiler is an option)
1 laboratory thermometer
That's all.
For each gram of Mdma we need 3.50 ml of ipa (measurements are very important!)
We put the ipa in a beaker and also a thermometer touching the ipa
We heat the ipa to 55 degrees (do not exceed 60 degrees)
Once we have that temperature, we put the Mdma and it will dissolve
Cover the glass with a piece of paper and leave it at room temperature for 4 hours.
After those 4 hours it should be in the fridge for a day
the day after freezing for another day and the crystals are already forming
First batch:
Pour the dirty ipa into another glass and put it back in the freezer.
in the beaker with the crystals we add acetone (half ipa) the beaker is so cold that the crystals dissolve and the acetone blocks it.
approximately in an hour that same acetone we overturned it in the dirty ipa glass
We let the crystals dry for a day.
Why do we add acetone to the ipa? Because there are still crystals, but we need acetone, otherwise the crystals will not form.
With the discarded acetone we add it to the dirty ipa glass from the freezer. Without the acetone, the second batch of crystals won't form!
these crystals will take longer to form, leave them in the freezer for a few days
We took out the glass and threw away the dirty ipa.
We add acetone so that the crystals do not dissolve. When the glass is at room temperature, we throw away the acetone and let the crystals dry
1 Liter of Ipa (isopropyl alcohol) 99% laboratory grade (the "drugstore" grade does not work)
1 Liter of 99% acetone ("drugstore" grade does not work and less than Mercadona)
1 glass of 1 liter
1 hot plate (but since not everyone has it, a double boiler is an option)
1 laboratory thermometer
That's all.
For each gram of Mdma we need 3.50 ml of ipa (measurements are very important!)
We put the ipa in a beaker and also a thermometer touching the ipa
We heat the ipa to 55 degrees (do not exceed 60 degrees)
Once we have that temperature, we put the Mdma and it will dissolve
Cover the glass with a piece of paper and leave it at room temperature for 4 hours.
After those 4 hours it should be in the fridge for a day
the day after freezing for another day and the crystals are already forming
First batch:
Pour the dirty ipa into another glass and put it back in the freezer.
in the beaker with the crystals we add acetone (half ipa) the beaker is so cold that the crystals dissolve and the acetone blocks it.
approximately in an hour that same acetone we overturned it in the dirty ipa glass
We let the crystals dry for a day.
Why do we add acetone to the ipa? Because there are still crystals, but we need acetone, otherwise the crystals will not form.
With the discarded acetone we add it to the dirty ipa glass from the freezer. Without the acetone, the second batch of crystals won't form!
these crystals will take longer to form, leave them in the freezer for a few days
We took out the glass and threw away the dirty ipa.
We add acetone so that the crystals do not dissolve. When the glass is at room temperature, we throw away the acetone and let the crystals dry
Attachments
- By Mr Good Cat
Mdp2pAs I understand, MDMA solubility in boiling IPA is around 1.4 ml of IPA per 1 gr of chloride.
May be, you can specify what is MDMA solubility in IPA at RT and frozen IPA?
May be, you can specify what is MDMA solubility in IPA at RT and frozen IPA?
- By Mr Good Cat
Policja PolskaI empirically found interesting fact. Solubility in IPA depends on purity.
I had two batches, one after ABE, pure white, another one brownish after crystallization in water.
Both batches were solved by weight in IPA from the same bottle under T=65C.
Chloride weight - 70 gr
IPA weight - 193 gr
First flask dissolved completely.
Second flask got a problem with dissolvation: I had to add 9 gr of IPA to solve it completely. IPA weight was adjusted at the point of complete dissolvation in order to replenish the evaporated.
Also, as crystallization run, chloride flakes were seen floating on the surface in second flask. That wasn't noticed in first. Obviously density is different due to contaminants.
I had two batches, one after ABE, pure white, another one brownish after crystallization in water.
Both batches were solved by weight in IPA from the same bottle under T=65C.
Chloride weight - 70 gr
IPA weight - 193 gr
First flask dissolved completely.
Second flask got a problem with dissolvation: I had to add 9 gr of IPA to solve it completely. IPA weight was adjusted at the point of complete dissolvation in order to replenish the evaporated.
Also, as crystallization run, chloride flakes were seen floating on the surface in second flask. That wasn't noticed in first. Obviously density is different due to contaminants.
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Introduction.
As all of us know, ecstasy pills can be admixtured by enormous number of drugs and adulterants. In the ecstasy assessment protocol which I've described, you may familiarize with them.
So to begin with some background information on MDMA purity. The crystal form of MDMA that we all know is MDMA.hcl (i.e. it's a salt of MDMA). A common misconception that I see around forums is that if it's brown and smells like aniseed/liquorice, then it is pure MDMA - This is incorrect, as pure MDMA*HCl is an odorless white transparent crystal. This brown appearance and sometimes oily texture, coupled with the distinctive aniseed like smell, are actually precursors and by-products that have not been cleaned off after the synthesis. I won't go into details as to what they are but some, such as safrole, are potential carcinogens whilst others have unknown activity but, either way, it's probably not a good idea to be ingesting them. Another problem that this causes is that these impurities can make up a significant proportion by weight of the sample (up to 50% impurities!) and so skew what people consider to be a good dose. As the level of impurities will vary from sample to sample, the ability to be able to consistently know a good dose for yourself becomes impaired which of course is very problematic in terms of safety and having a satisfying effect.
The described below process will rid your drugs of impurities and cuts such as caffeine, dye, and other pesky contaminants. It should be clear that this process is to separate the polar material from the non-polar material. If there are polar adulterants along with your MDMA (other amphetamines for example) they will remain with the cleaned MDMA. While it's useful for inactives and caffeine, it does not mean you're off the hook from having to test it. That being said, if you have washed and tested MDMA you can be as certain of your dose as anyone possibly could be (short of lab testing, of course). Also, this process works for extracting MDMA out of ecstasy tablets.The Actual acetone wash is very straightforward after doing this:
For the acetone wash, you will need:
- Pure acetone (crucially not mixed with water or anything else like in some nail polish removers) - This can be bought easily and cheaply on amazon without suspicion.
Procedure of purification.
Firstly, you need to make anhydrous acetone [caution: acetone is extremely flammable, so keep away from sources of ignition]. MDMA is very soluble in water and acetone is hygroscopic, meaning that it attracts water. You will lose a very large quantity of your sample if your acetone is not anhydrous before use. This is where the Epsom salts come in: first, you bake your Epsom salts (you will want to use a fairly large quantity) in the oven at 200-250 degrees centigrade for 2-3 hours. This will yield a dusty white powder which is anhydrous magnesium sulfate. Next you just add the anhydrous magnesium sulfate you have made to your acetone until a snow-globe type of effect happens when you swirl the liquid around (the presence of free-flowing magnesium sulfate indicates the acetone is dry, when there is water in your acetone the magnesium sulfate will clump together and sink to the bottom of the solution). After you reach this point, give the acetone a good shake and chill in the freezer for a few hours before use. This should ensure that it's dry for use.
Important.
Over time, anhydrous acetone will absorb moisture from the air. It's pretty much inevitable, but you can always add more magnesium to make it right again. Never leave the acetone exposed to the air. Keep the jar, filter and bottle covered as much as possible.
Step 1: Crush your MDMA/ecstasy tablet to dust - same procedure as if you were going to take a line of it, the finer you crush it the better the acetone wash will work to remove impurities. Here is a photo of my sample to give you an idea of how fine it should be.The sample shown here has been reagent tested and purity tested by the EZ semi-quantitative kit and is of about 60-70% purity, it feels a little oily and has a very strong aniseed smell.
Step 2: Pour MDMA into a beaker/glass, then pour in the anhydrous acetone that you made earlier. Use an amount that will give you a decent head of solvent that can be decanted off without pouring out your MDMA as well. Stir vigorously for two minutes and leave to settle until the residue will be obtained (you can gently tap the side of the beaker/glass to speed this up). You should now have the MDMA sunk to the bottom and a layer of discolored acetone at the top containing the impurities as shown here.Now decant off the dirty acetone carefully without pouring out the MDMA with it (this part is made easier by a pipette, but is not necessary). Repeat this step until the acetone on the top layer stays clear (usually about 3-5 washes).Step 3: Filter the MDMA out of the acetone using filter paper. Fold your filter paper into 4 times and then pop it out in to a cone shape (3 of the folds will be on 1 side and 1 on the other side), then pour your mixture through the paper. The easiest way to do this is, to stir the solution, so the crystals are flowing around with acetone then quickly pouring the mixture into the filter paper, this makes it easier to get the MDMA out of the beaker without having to scrape it off. Any remaining MDMA in the beaker can be mobilized like this using a small volume of acetone and is then poured into the filter paper. Make sure the filter paper is either held stable by you or a filter funnel while pouring! You cannot drop the filter paper accidentially and loose all your hard work.Step 4: Dry your crystals. Acetone is very volatile (evaporates easily) so this can be done easily using a hairdryer. Simply wrap up your crystals in the filter paper, so there are nowhere the crystals can be blown out from, and dry using a hair dryer till the paper and crystals inside are dry to the touch and don't smell of acetone. If you are going to recrystallize with isopropanol afterwards, your crystals do not need to be fully dry. Also, if you don't have a hairdryer, you can dry your sample in the oven at a low temperature (50-60 degrees centigrade).
That's it, you are all done! This procedure can be used to wash other substances such as cocaine and mescaline and to extract the MDMA out of pills. This is what my sample looked like after the acetone washes. It would be brighter, but it was still wet at this stage. You can continue to recrystallize your stuff, or end up there. Now wait 24 hours, or until all the acetone has evaporated from the dish and crystals. Once the smell is gone, you're good to go.Recrystallization Using Isopropanol:
In order to attempt this, it's advisable to understand how this works. Recrystallization works by dissolving your sample in hot (near boiling) solvent (isopropanol in this case) as solubility increases with temperature. This allows you to dissolve all of your sample in a relatively small amount of solvent (1g of MDMA will dissolve easily in 10 ml of hot isopropanol). Now all of your sample, including the impurities that were trapped inside the crystal, are now in solution. This is why it is better than an acetone wash as no matter how finely you grind the crystals up there will always be some impurities trapped in the crystals that the acetone cannot remove. Also, as you are heating up the isopropanol, some harder to dissolve impurities will be soluble in it. Then allow the heated solution to cool as slowly as possible. The pure MDMA crystals will start to precipitate out from the solution when the temperature decreases. This is because the MDMA is less soluble in cold isopropanol. By doing this slowly, it allows the MDMA crystals to form whilst the impurities stay dissolved in the isopropanol (along with a small amount of MDMA crystals). By cooling the solution too fast (i.e. putting it immediately in the freezer after dissolving your sample in the isopropanol) other impurities crash back out of the solution along with the MDMA, so the product is not as pure, also the crystals that form will be smaller and not as pretty as a result of the lower purity.What you will need:
How to carry out procedure.
Step 1: Pour some isopropanol into a glass beaker. It's better to use more than you need, as you will be heating it and some will evaporate. For 10 g's of MDMA use around 30 ml to dissolve it but heated up 40 ml. Then you can stack a saucepan on the surface of a frying pan over the hob to heat up the isopropanol. Isopropanol is also extremely flammable, so should never be directly exposed to the flame from the hob. By using the set-up of the saucepan on top of a frying pan, the isopropanol is buffered from the flame directly, so the risk of it igniting is minimal. Place the beaker of isopropanol onto the saucepan and heat it up to when it just starts to boil. Use the extractor hood above your hob if you have one during this, if not at least open a window to help ventilate the room better.
Step 2: Get your beaker containing your MDMA crystals ready. Now, once the isopropanol has just reached boiling, pour in a small volume into the beaker containing your MDMA (not the whole volume you planned to use). The top of the beaker should be cool enough to touch as long as the beaker is not completely full, but you can use insulating gloves/cloth if you prefer. Swirl the isopropanol around to mix it with the MDMA. Now place the Beaker with your MDMA and isopropanol onto the saucepan as we'll to keep it hot. Keep adding small amounts of hot isopropanol to your MDMA until it just dissolves. Let me repeat this in clearer words: you want to add the smallest volume of isopropanol possible to dissolve the MDMA, if you add too much isopropanol the MDMA will not precipitate from the solution once you cool it down or if it does your yield will be very poor. If you accidentally add too much, you can boil some off to reduce the volume once the MDMA has all been dissolved. Keep swirling/stirring the solution with the MDMA in it whilst adding isopropanol to help it dissolve. Once everything is dissolved, you should be left with a discolored solution with everything dissolved that looks similar to this picture.
As you can see, even after acetone washing my sample, there were still lots of the brown colored impurities that have dissolved into the isopropanol.Note 2: From the image above, you can see that I am using just a frying pan to heat the isopropanol and not a saucepan in a frying pan. This is quicker to heat up the isopropanol, but also carries more risk of ignition and overboiling your solvent. I do this because I have lots of experience handling chemicals in a lab, I would recommend that someone with little to no experience with lab work/handling solvents use the set-up I suggested.
Note 1: If there are impurities that are insoluble in isopropanol, for instance, if your sample is contaminated with table salt or talcum powder, they won't dissolve in the isopropanol at all. They will be left over once all the MDMA and other impurities have dissolved, and you can simply filter the solution using filter paper to remove them and then let the solution cool down as normal.
Step 3: Once everything has dissolved, turn off the hob and allow the solution to cool on the saucepan, this will ensure that it cools down slowly. Once it reaches room temperature, you can put it in the freezer to allow the crystals to fully form. If you have added a minimal volume of the isopropanol after leaving the beaker in the freezer for 20-30 mins, the crystals should be forming pretty obviously. Sometimes the crystals start to precipitate out once the solution has reached room temperature, this is also okay. As I said before, the slower you cool it, the purer the crystals are. Some people will leave the beaker at room temperature overnight then leave it in the fridge for 4 hours, then in the freezer overnight to obtain incredibly pure and large crystals. Personally, I find this to be excessive and have achieved excellent results with leaving the beaker to cool down for one hour to room temperature, then to leave it in the freezer for 2-3 hours. Occasionally, crystallization has to be induced once the sample has cooled down. If you think you have used the right volume of isopropanol to dissolve your MDMA, but after cooling down in the freezer no crystals have appeared, you can scratch the bottom of the beaker with something like a glass rod or a metal fork. This will often induce crystallization, and the crystals will start to appear right before your eyes. When successfully done, you will have a beaker containing your crystals at the bottom and a head of excess discolored isopropanol at the top, which you will want to keep. This is what my MDMA looked like once I had poured off the dirty isopropanol.If you do not have anhydrous acetone available, then you will want to keep the dirty isopropanol in a beaker with your MDMA, then dislodge the crystals from the bottom of the beaker using a chopstick or metal knife, swirl the mixture to mobilize crystals and then pour into a filter paper to collect your MDMA crystals and keep the dirty isopropanol in another beaker. If you have anhydrous acetone, then you can simply pour off the dirty isopropanol into another beaker and use the acetone to help dislodge the crystals, and then pour the mixture through a filter. This is my batch whilst being filtered.The MDMA you have collected in the filter paper is now very close to 100% pure, I have achieved purifies of greater than 95% with this method. It can now be dried in the same way using a hairdryer as described earlier. If you have used acetone to help get the MDMA out of the beaker, it will be quicker to dry than if you have just poured the MDMA out with the dirty isopropanol.
Step 4: This is not compulsory, but is highly advised to improve your yield.
In the dirty isopropanol you have collected. There is still some MDMA. This can be extracted by boiling off the dirty isopropanol until there is only a tiny volume left (approximately 5 ml). Then you just let it cool down slowly again to allow the MDMA to precipitate from the dirty isopropanol. This will be a smaller but still significant amount of product. From the batch I have shown, there was around a whole gram extracted from the dirty isopropanol. The MDMA formed from this will not be as pure as the main batch of crystals but will still be very pure compared to the starting product. You can separate the crystals from the dirty isopropanol the same way as described above.
The beaker on the right is the purest main batch and on the left is the recovered batch.Here is the result of the EZ purity test for the purified batch. It corresponds to the color in the bottom-right corner of the chart, which indicates a similar purity to a 100% pure sample of MDMA.You have just made some near 100% pure MDMA. Here is what the batch looked like after all manipulations.
Hi, i make a lot of purification of shity mdma, and now i have a problem.Introduction.
As all of us know, ecstasy pills can be admixtured by enormous number of drugs and adulterants. In the ecstasy assessment protocol which I've described, you may familiarize with them.
So to begin with some background information on MDMA purity. The crystal form of MDMA that we all know is MDMA.hcl (i.e. it's a salt of MDMA). A common misconception that I see around forums is that if it's brown and smells like aniseed/liquorice, then it is pure MDMA - This is incorrect, as pure MDMA*HCl is an odorless white transparent crystal. This brown appearance and sometimes oily texture, coupled with the distinctive aniseed like smell, are actually precursors and by-products that have not been cleaned off after the synthesis. I won't go into details as to what they are but some, such as safrole, are potential carcinogens whilst others have unknown activity but, either way, it's probably not a good idea to be ingesting them. Another problem that this causes is that these impurities can make up a significant proportion by weight of the sample (up to 50% impurities!) and so skew what people consider to be a good dose. As the level of impurities will vary from sample to sample, the ability to be able to consistently know a good dose for yourself becomes impaired which of course is very problematic in terms of safety and having a satisfying effect.
The described below process will rid your drugs of impurities and cuts such as caffeine, dye, and other pesky contaminants. It should be clear that this process is to separate the polar material from the non-polar material. If there are polar adulterants along with your MDMA (other amphetamines for example) they will remain with the cleaned MDMA. While it's useful for inactives and caffeine, it does not mean you're off the hook from having to test it. That being said, if you have washed and tested MDMA you can be as certain of your dose as anyone possibly could be (short of lab testing, of course). Also, this process works for extracting MDMA out of ecstasy tablets.The Actual acetone wash is very straightforward after doing this:
For the acetone wash, you will need:
- Pure acetone (crucially not mixed with water or anything else like in some nail polish removers) - This can be bought easily and cheaply on amazon without suspicion.
Procedure of purification.
Firstly, you need to make anhydrous acetone [caution: acetone is extremely flammable, so keep away from sources of ignition]. MDMA is very soluble in water and acetone is hygroscopic, meaning that it attracts water. You will lose a very large quantity of your sample if your acetone is not anhydrous before use. This is where the Epsom salts come in: first, you bake your Epsom salts (you will want to use a fairly large quantity) in the oven at 200-250 degrees centigrade for 2-3 hours. This will yield a dusty white powder which is anhydrous magnesium sulfate. Next you just add the anhydrous magnesium sulfate you have made to your acetone until a snow-globe type of effect happens when you swirl the liquid around (the presence of free-flowing magnesium sulfate indicates the acetone is dry, when there is water in your acetone the magnesium sulfate will clump together and sink to the bottom of the solution). After you reach this point, give the acetone a good shake and chill in the freezer for a few hours before use. This should ensure that it's dry for use.
Important.
Over time, anhydrous acetone will absorb moisture from the air. It's pretty much inevitable, but you can always add more magnesium to make it right again. Never leave the acetone exposed to the air. Keep the jar, filter and bottle covered as much as possible.
Step 1: Crush your MDMA/ecstasy tablet to dust - same procedure as if you were going to take a line of it, the finer you crush it the better the acetone wash will work to remove impurities. Here is a photo of my sample to give you an idea of how fine it should be.The sample shown here has been reagent tested and purity tested by the EZ semi-quantitative kit and is of about 60-70% purity, it feels a little oily and has a very strong aniseed smell.
Step 2: Pour MDMA into a beaker/glass, then pour in the anhydrous acetone that you made earlier. Use an amount that will give you a decent head of solvent that can be decanted off without pouring out your MDMA as well. Stir vigorously for two minutes and leave to settle until the residue will be obtained (you can gently tap the side of the beaker/glass to speed this up). You should now have the MDMA sunk to the bottom and a layer of discolored acetone at the top containing the impurities as shown here.Now decant off the dirty acetone carefully without pouring out the MDMA with it (this part is made easier by a pipette, but is not necessary). Repeat this step until the acetone on the top layer stays clear (usually about 3-5 washes).Step 3: Filter the MDMA out of the acetone using filter paper. Fold your filter paper into 4 times and then pop it out in to a cone shape (3 of the folds will be on 1 side and 1 on the other side), then pour your mixture through the paper. The easiest way to do this is, to stir the solution, so the crystals are flowing around with acetone then quickly pouring the mixture into the filter paper, this makes it easier to get the MDMA out of the beaker without having to scrape it off. Any remaining MDMA in the beaker can be mobilized like this using a small volume of acetone and is then poured into the filter paper. Make sure the filter paper is either held stable by you or a filter funnel while pouring! You cannot drop the filter paper accidentially and loose all your hard work.Step 4: Dry your crystals. Acetone is very volatile (evaporates easily) so this can be done easily using a hairdryer. Simply wrap up your crystals in the filter paper, so there are nowhere the crystals can be blown out from, and dry using a hair dryer till the paper and crystals inside are dry to the touch and don't smell of acetone. If you are going to recrystallize with isopropanol afterwards, your crystals do not need to be fully dry. Also, if you don't have a hairdryer, you can dry your sample in the oven at a low temperature (50-60 degrees centigrade).
That's it, you are all done! This procedure can be used to wash other substances such as cocaine and mescaline and to extract the MDMA out of pills. This is what my sample looked like after the acetone washes. It would be brighter, but it was still wet at this stage. You can continue to recrystallize your stuff, or end up there. Now wait 24 hours, or until all the acetone has evaporated from the dish and crystals. Once the smell is gone, you're good to go.Recrystallization Using Isopropanol:
In order to attempt this, it's advisable to understand how this works. Recrystallization works by dissolving your sample in hot (near boiling) solvent (isopropanol in this case) as solubility increases with temperature. This allows you to dissolve all of your sample in a relatively small amount of solvent (1g of MDMA will dissolve easily in 10 ml of hot isopropanol). Now all of your sample, including the impurities that were trapped inside the crystal, are now in solution. This is why it is better than an acetone wash as no matter how finely you grind the crystals up there will always be some impurities trapped in the crystals that the acetone cannot remove. Also, as you are heating up the isopropanol, some harder to dissolve impurities will be soluble in it. Then allow the heated solution to cool as slowly as possible. The pure MDMA crystals will start to precipitate out from the solution when the temperature decreases. This is because the MDMA is less soluble in cold isopropanol. By doing this slowly, it allows the MDMA crystals to form whilst the impurities stay dissolved in the isopropanol (along with a small amount of MDMA crystals). By cooling the solution too fast (i.e. putting it immediately in the freezer after dissolving your sample in the isopropanol) other impurities crash back out of the solution along with the MDMA, so the product is not as pure, also the crystals that form will be smaller and not as pretty as a result of the lower purity.What you will need:
How to carry out procedure.
Step 1: Pour some isopropanol into a glass beaker. It's better to use more than you need, as you will be heating it and some will evaporate. For 10 g's of MDMA use around 30 ml to dissolve it but heated up 40 ml. Then you can stack a saucepan on the surface of a frying pan over the hob to heat up the isopropanol. Isopropanol is also extremely flammable, so should never be directly exposed to the flame from the hob. By using the set-up of the saucepan on top of a frying pan, the isopropanol is buffered from the flame directly, so the risk of it igniting is minimal. Place the beaker of isopropanol onto the saucepan and heat it up to when it just starts to boil. Use the extractor hood above your hob if you have one during this, if not at least open a window to help ventilate the room better.
Step 2: Get your beaker containing your MDMA crystals ready. Now, once the isopropanol has just reached boiling, pour in a small volume into the beaker containing your MDMA (not the whole volume you planned to use). The top of the beaker should be cool enough to touch as long as the beaker is not completely full, but you can use insulating gloves/cloth if you prefer. Swirl the isopropanol around to mix it with the MDMA. Now place the Beaker with your MDMA and isopropanol onto the saucepan as we'll to keep it hot. Keep adding small amounts of hot isopropanol to your MDMA until it just dissolves. Let me repeat this in clearer words: you want to add the smallest volume of isopropanol possible to dissolve the MDMA, if you add too much isopropanol the MDMA will not precipitate from the solution once you cool it down or if it does your yield will be very poor. If you accidentally add too much, you can boil some off to reduce the volume once the MDMA has all been dissolved. Keep swirling/stirring the solution with the MDMA in it whilst adding isopropanol to help it dissolve. Once everything is dissolved, you should be left with a discolored solution with everything dissolved that looks similar to this picture.As you can see, even after acetone washing my sample, there were still lots of the brown colored impurities that have dissolved into the isopropanol.Note 2: From the image above, you can see that I am using just a frying pan to heat the isopropanol and not a saucepan in a frying pan. This is quicker to heat up the isopropanol, but also carries more risk of ignition and overboiling your solvent. I do this because I have lots of experience handling chemicals in a lab, I would recommend that someone with little to no experience with lab work/handling solvents use the set-up I suggested.
Note 1: If there are impurities that are insoluble in isopropanol, for instance, if your sample is contaminated with table salt or talcum powder, they won't dissolve in the isopropanol at all. They will be left over once all the MDMA and other impurities have dissolved, and you can simply filter the solution using filter paper to remove them and then let the solution cool down as normal.
Step 3: Once everything has dissolved, turn off the hob and allow the solution to cool on the saucepan, this will ensure that it cools down slowly. Once it reaches room temperature, you can put it in the freezer to allow the crystals to fully form. If you have added a minimal volume of the isopropanol after leaving the beaker in the freezer for 20-30 mins, the crystals should be forming pretty obviously. Sometimes the crystals start to precipitate out once the solution has reached room temperature, this is also okay. As I said before, the slower you cool it, the purer the crystals are. Some people will leave the beaker at room temperature overnight then leave it in the fridge for 4 hours, then in the freezer overnight to obtain incredibly pure and large crystals. Personally, I find this to be excessive and have achieved excellent results with leaving the beaker to cool down for one hour to room temperature, then to leave it in the freezer for 2-3 hours. Occasionally, crystallization has to be induced once the sample has cooled down. If you think you have used the right volume of isopropanol to dissolve your MDMA, but after cooling down in the freezer no crystals have appeared, you can scratch the bottom of the beaker with something like a glass rod or a metal fork. This will often induce crystallization, and the crystals will start to appear right before your eyes. When successfully done, you will have a beaker containing your crystals at the bottom and a head of excess discolored isopropanol at the top, which you will want to keep. This is what my MDMA looked like once I had poured off the dirty isopropanol.If you do not have anhydrous acetone available, then you will want to keep the dirty isopropanol in a beaker with your MDMA, then dislodge the crystals from the bottom of the beaker using a chopstick or metal knife, swirl the mixture to mobilize crystals and then pour into a filter paper to collect your MDMA crystals and keep the dirty isopropanol in another beaker. If you have anhydrous acetone, then you can simply pour off the dirty isopropanol into another beaker and use the acetone to help dislodge the crystals, and then pour the mixture through a filter. This is my batch whilst being filtered.The MDMA you have collected in the filter paper is now very close to 100% pure, I have achieved purifies of greater than 95% with this method. It can now be dried in the same way using a hairdryer as described earlier. If you have used acetone to help get the MDMA out of the beaker, it will be quicker to dry than if you have just poured the MDMA out with the dirty isopropanol.
Step 4: This is not compulsory, but is highly advised to improve your yield.
In the dirty isopropanol you have collected. There is still some MDMA. This can be extracted by boiling off the dirty isopropanol until there is only a tiny volume left (approximately 5 ml). Then you just let it cool down slowly again to allow the MDMA to precipitate from the dirty isopropanol. This will be a smaller but still significant amount of product. From the batch I have shown, there was around a whole gram extracted from the dirty isopropanol. The MDMA formed from this will not be as pure as the main batch of crystals but will still be very pure compared to the starting product. You can separate the crystals from the dirty isopropanol the same way as described above.
The beaker on the right is the purest main batch and on the left is the recovered batch.Here is the result of the EZ purity test for the purified batch. It corresponds to the color in the bottom-right corner of the chart, which indicates a similar purity to a 100% pure sample of MDMA.You have just made some near 100% pure MDMA. Here is what the batch looked like after all manipulations.
I make the acetone washe, was nice i color not too bad.
Then disolve in hot IPA (very nice color clear) a crash crystals ,filter and dry.
Disolve again in IPA I want to make big crystals ( i do a lot of times) in hot satured IPA and seed the solution, this time i let the solution in the hot plate at 80 celcius all the night, the other day when i was going to start the slow ramp down temp for the grow... i see all The solution Dark! very nasty. i shut off the heat and let cool. Ends worse than when it started the really dirty shity sugared crystals. I let dry and make other acetone wash.. and have a looooot of oil when i evap the acetone from the second washes..! !
What the fuck is the redish dark oil? is soluble in water/alcohol/acetone
Maybe the heat can degrade MDMA hcl, or some impuritis?
PD: What you think about the antisolvent crash with acetone/ipa? when is better?
Can be a good one... free base the MDMA extract with diethyl ether and recrash with a few ml of chlorid acid 37%?
thanks boss
- By G.Patton
Macondor
Read more about Recrystallization and hot filtration
Hello, your MDMA reacted with oxygen in air. What a sense of heating at 80*C at night? I guess, all IPA was evaporated and your product was heated in a beaker at 80*C. You need to heat the solvent in order to increase MDMA solubility in the minimum amount of the solvent. Then, cool down it slowly in order to grow crystals.
Read more about Recrystallization and hot filtration
↑View previous replies…
- By Macondor
G.PattonThe IPA was not evaporated because was in a seal flask with pressure, i do this a few times and grow big crystals, maybe it was lucky...?
So MDMA hcl react with oxigen and degrade to what? what is the oxidation product?
i think that MDMA was really heat resistent.
thanks
So MDMA hcl react with oxigen and degrade to what? what is the oxidation product?
i think that MDMA was really heat resistent.
thanks
Last edited:
- By Macondor
G.PattonAfter the acetone wash and one recrystallization in ipa can still be an excess of hcl? can you explain me more please?
There was a strong sweet aroma when i promt the second hot recrystallization when the red oil appeared, very strong. Now whats is left i wash with acetone like 6 times o 7 for clean again.. was a pain in the ass but.. lets see whats happen in a normal Recrystallization.
What do you think about an a/b metod for purification? Disolve in water Base with hidroxysodium and extract with diethyl ether and precipitate with hcl like shulgin in pikhal or bubble hcl gas.
thanks!!!
There was a strong sweet aroma when i promt the second hot recrystallization when the red oil appeared, very strong. Now whats is left i wash with acetone like 6 times o 7 for clean again.. was a pain in the ass but.. lets see whats happen in a normal Recrystallization.
What do you think about an a/b metod for purification? Disolve in water Base with hidroxysodium and extract with diethyl ether and precipitate with hcl like shulgin in pikhal or bubble hcl gas.
thanks!!!
- By G.Patton
Macondor
No, there is no acid for sure. What a reason of your manipulations with boiling in IPA? I really don't understand your motivation. You are telling me that you've already washed your product and recrystallized. Doesn't your product testify you after this?
I posted the topic about a/b extraction of amphetamine. Here is same procedure with HCl gas instead of sulfuric acid.
- By Macondor
G.PattonI dont understand why dont crash white the crystals.. crash a litlle brown..and i make the second rex. i will do a 3 . Maybe is a reaction that start and can be stoped? When i heat the IPA for the second recrystallizations start to dark a litlle again
The method of adding drops of hcl 37% solution to the ether, will not work well? is more easy too me now,,
Is for grow big crystals..i do this a few times and work.. and with piperine to, at 70 celcius.. satured solution ,seeding cap the flask (are that ones for sterilzation and can hold pressure) and then slow down the temp in one or two days...only for fun i love see big crystals.
i do this a few times..and no problem.. maybe is something more in the product before the purification that react
thanks man sorry all questions..
The method of adding drops of hcl 37% solution to the ether, will not work well? is more easy too me now,,
Is for grow big crystals..i do this a few times and work.. and with piperine to, at 70 celcius.. satured solution ,seeding cap the flask (are that ones for sterilzation and can hold pressure) and then slow down the temp in one or two days...only for fun i love see big crystals.
i do this a few times..and no problem.. maybe is something more in the product before the purification that react
thanks man sorry all questions..
- By Mr Good Cat
G.PattonNow I have 100% evidence long time exposure of MDMA at high temperature affects the color.
I use different crystallization methods and it is not a problem for me to get pure white crystals. Normally it doesn't take a lot of time for heating, and crystals are perfect white.
But this time I tried to do something new for me just to make crystals bigger and more transparent: "Per aspera ad astra".
I used the same batch of pure white powder after ABE, as solution was ready it had the same color as usually, transparent slightly brownish. I left it on the hotplate for 10 hours, T mostly 40-70C.
Unfortunately, I did a mistake in my calculations, and my expectations were not met. As the result I had to re-crystallize all this batch. As I made my solution ready for re-crystallization, it was much worse then before.
Still it is open question, what it is. It could be carbon of carbolic acid. Also it could be a natural property of salt to get dark while heated: jewelers ofter use it, and heat stones for long time to change the color.
But I noticed the solution of MDMA HCL that was not purified with base extraction gets much more dark brown and even much more fast.
So, I believe, still there is presence of some side product (not a lot, may be 1-2%) that turns black while heated.
I use different crystallization methods and it is not a problem for me to get pure white crystals. Normally it doesn't take a lot of time for heating, and crystals are perfect white.
But this time I tried to do something new for me just to make crystals bigger and more transparent: "Per aspera ad astra".
I used the same batch of pure white powder after ABE, as solution was ready it had the same color as usually, transparent slightly brownish. I left it on the hotplate for 10 hours, T mostly 40-70C.
Unfortunately, I did a mistake in my calculations, and my expectations were not met. As the result I had to re-crystallize all this batch. As I made my solution ready for re-crystallization, it was much worse then before.
Still it is open question, what it is. It could be carbon of carbolic acid. Also it could be a natural property of salt to get dark while heated: jewelers ofter use it, and heat stones for long time to change the color.
But I noticed the solution of MDMA HCL that was not purified with base extraction gets much more dark brown and even much more fast.
So, I believe, still there is presence of some side product (not a lot, may be 1-2%) that turns black while heated.
Last edited:
- By G.Patton
Mr Good CatHi, a lot of organic compounds have tendency to become darker after heating. Air oxygen reacts with it under increased temperature well. Also, dimerization may take place to be.
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