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?
As 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?
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.
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.
Epsom salts - These are hydrous magnesium sulphate crystals and can be bought easily and cheaply from your local chemist such as boots (I will explain further down why these are necessary)
A smallish beaker (50 ml is good) but if that is not available then a regular kitchen glass can be utilized (a short and thin in diameter glass is good)
Filter paper (coffee filter paper is also fine for this)
something to stir the mixture with (glass rod ideally but a chopstick or metal knife is fine, just make sure if your knife has a plastic handle it doesn't come into contact with the acetone)
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.
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:
2 glass beakers (50ml is again a good size for these), unfortunately since the isopropanol needs to be heated, I cannot recommend using a normal glass to heat up the solvent as it could shatter. Fortunately, you can buy these very cheaply and without suspicion from Amazon.
Pure isopropanol (99% or above) again must not be diluted with other chemicals or water. Again, this can be bought easily and cheaply from Amazon.
Filter papers (again, coffee filter paper is fine)
Anhydrous Magnesium sulfate (the same stuff used to make the acetone anhydrous in the previous step)
Anhydrous acetone (optional)
Stirrer (wooden chopstick is fine)
Glass pipette (optional)
Overview:
Heat anhydrous isopropanol till it just starts to boil.
Use minimum amount of hot isopropanol possible to dissolve MDMA in.
Allow isopropanol solution to cool slowly to form pure MDMA crystals.
Recover extra MDMA from dirty isopropanol, then filter and dry samples.
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 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.
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.
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.
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.
Epsom salts - These are hydrous magnesium sulphate crystals and can be bought easily and cheaply from your local chemist such as boots (I will explain further down why these are necessary)
A smallish beaker (50 ml is good) but if that is not available then a regular kitchen glass can be utilized (a short and thin in diameter glass is good)
Filter paper (coffee filter paper is also fine for this)
something to stir the mixture with (glass rod ideally but a chopstick or metal knife is fine, just make sure if your knife has a plastic handle it doesn't come into contact with the acetone)
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.
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:
2 glass beakers (50ml is again a good size for these), unfortunately since the isopropanol needs to be heated, I cannot recommend using a normal glass to heat up the solvent as it could shatter. Fortunately, you can buy these very cheaply and without suspicion from Amazon.
Pure isopropanol (99% or above) again must not be diluted with other chemicals or water. Again, this can be bought easily and cheaply from Amazon.
Filter papers (again, coffee filter paper is fine)
Anhydrous Magnesium sulfate (the same stuff used to make the acetone anhydrous in the previous step)
Anhydrous acetone (optional)
Stirrer (wooden chopstick is fine)
Glass pipette (optional)
Overview:
Heat anhydrous isopropanol till it just starts to boil.
Use minimum amount of hot isopropanol possible to dissolve MDMA in.
Allow isopropanol solution to cool slowly to form pure MDMA crystals.
Recover extra MDMA from dirty isopropanol, then filter and dry samples.
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 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.
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.
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.
Hi, i make a lot of purification of shity mdma, and now i have a problem.
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%?
Hi, i make a lot of purification of shity mdma, and now i have a problem.
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%?
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.
I 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..
I 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..
I 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..
I just started re-cystallization in IPA on water bath. Let's see what I will get in the morning. The intention is to decrease temperature of water in pan 2C per 30 minutes.
But I also don't understand what is the reason to keep it under 80C for the overnight. Solubility is always the same at the same temperature: no matter how long you heat it - 10 minutes or 10 hours.
Also a question: you mentioned a flask. Do you mean Erlenmeyer flask?
Considering black MDMA, I also got strong impression, the salt degrades while heated. Every time I heat the chloride it is getting dark.
Even, when I acidify washed in ether FB, then as I heat it up to 130 it is getting dark.
Then, I wash salt is acetone in volume proportions 1:10, and re-crystallize fresh salt by heating up to 100+C it is getting dark again.
I just started re-cystallization in IPA on water bath. Let's see what I will get in the morning. The intention is to decrease temperature of water in pan 2C per 30 minutes.
But I also don't understand what is the reason to keep it under 80C for the overnight. Solubility is always the same at the same temperature: no matter how long you heat it - 10 minutes or 10 hours.
Also a question: you mentioned a flask. Do you mean Erlenmeyer flask?
Considering black MDMA, I also got strong impression, the salt degrades while heated. Every time I heat the chloride it is getting dark.
Even, when I acidify washed in ether FB, then as I heat it up to 130 it is getting dark.
Then, I wash salt is acetone in volume proportions 1:10, and re-crystallize fresh salt by heating up to 100+C it is getting dark again.
Policja PolskaI've heard this black color is a common issue with MDMA made from PMK..
Today I think the best way is to acidify FB with 37% HCl in cold acetone: no heating, and powder in result is pure white.
Probably slow re-crystallization in IPA from 60C down to RT is also more gentle for unstable molecule inclined to degrade.
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.
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.
Now 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. View attachment 27148
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.
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.
G.Pattonyeah, product is ok.
this medium layer also looks more dark not because excess of contaminants, but due to such funny crystals formation.
i think it is due to different modes of temperature control.
@G.Patton , general, IPA is very good to remove certain compounds (side products of synth) from mdma. But my real pain in the ass is huge volume of hydrochloride left in IPA that I need to recover. Now I think if using ethanol I can get bettter result? Is there any well known route for mdma hcl washing in ethanol?
@G.Patton , general, IPA is very good to remove certain compounds (side products of synth) from mdma. But my real pain in the ass is huge volume of hydrochloride left in IPA that I need to recover. Now I think if using ethanol I can get bettter result? Is there any well known route for mdma hcl washing in ethanol?
G.PattonI'm also thinking about glicerol usage in purification process as a triple-atomic alcohol it may work. Will come back to the work in a couple of days and post the report.
@G.Patton general, just curious if you have any idea about different solvents for mdma purification by base extraction like pro and contra: hexane, dcm, petroleum ether?
My personal observation is that ether dissolves quite a bit of base. As my experience says, to dissolve 1 gr of base you need about 3 ml of ether. But I'm interested not only in volume (and cost) but in minimal solubility of side impurities as well.
I guess hexane used for base extraction is cas 64742-49-0 (isohexane)?
@G.Patton general, just curious if you have any idea about different solvents for mdma purification by base extraction like pro and contra: hexane, dcm, petroleum ether?
My personal observation is that ether dissolves quite a bit of base. As my experience says, to dissolve 1 gr of base you need about 3 ml of ether. But I'm interested not only in volume (and cost) but in minimal solubility of side impurities as well.
I guess hexane used for base extraction is cas 64742-49-0 (isohexane)?
@G.Patton general, just curious if you have any idea about different solvents for mdma purification by base extraction like pro and contra: hexane, dcm, petroleum ether?
My personal observation is that ether dissolves quite a bit of base. As my experience says, to dissolve 1 gr of base you need about 3 ml of ether. But I'm interested not only in volume (and cost) but in minimal solubility of side impurities as well.
I guess hexane used for base extraction is cas 64742-49-0 (isohexane)?
Mr Good CatVacuum distillation of free base with a reflux condenser and separation of the dissolved product into fractions depending on the boiling point will give you maximum purity and minimal loss of substance.
Hello friends, thanks for the contribution, it works very well but I have a doubt, when crystallizing (crystals precipitate very very well) I do not get crystals like the typical ones of mdma, it is something more similar to snowflakes, to ice frost in a glass on a snowy day, it is glass but very fragile. Why can't I get strong glass? Thank you and greetings
Hello friends, thanks for the contribution, it works very well but I have a doubt, when crystallizing (crystals precipitate very very well) I do not get crystals like the typical ones of mdma, it is something more similar to snowflakes, to ice frost in a glass on a snowy day, it is glass but very fragile. Why can't I get strong glass? Thank you and greetings
