deeperdive36

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So I'm struggling with step 8. Seems like a lot of waste and loss for me here. I transferred extract from sep funnel added magnesium put in freezer. Now here I did the filter with vacuum. I think Buchner is way better than the setup I got as it leaked and volume is too large. So 1st when pouring into setup are you suppose to dump the whole thing in... I don't understand how to properly pour off the ether extraction without getting magnesium with it unless I don't pour all of the extract then at that point I have a lot of extract left with the magnesium what do I do with that remaining part to separate. Also I've attached pics of the leak. What do I do with this. Is this all waste . If there is magnesium that got through the filter what should I do? Basically stuck and waiting at this step
 

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Mr Good Cat

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So I'm struggling with step 8. Seems like a lot of waste and loss for me here. I transferred extract from sep funnel added magnesium put in freezer. Now here I did the filter with vacuum. I think Buchner is way better than the setup I got as it leaked and volume is too large. So 1st when pouring into setup are you suppose to dump the whole thing in... I don't understand how to properly pour off the ether extraction without getting magnesium with it unless I don't pour all of the extract then at that point I have a lot of extract left with the magnesium what do I do with that remaining part to separate. Also I've attached pics of the leak. What do I do with this. Is this all waste . If there is magnesium that got through the filter what should I do? Basically stuck and waiting at this step
deeperdive36Come on, man: you can do it. If me with my arms growing from my ass can, then you can too.
And yes! Nothing is more pleasing to my eyes than MDMA after ether washing.
AlO4WhDYHz
 

deeperdive36

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So I'm struggling with step 8. Seems like a lot of waste and loss for me here. I transferred extract from sep funnel added magnesium put in freezer. Now here I did the filter with vacuum. I think Buchner is way better than the setup I got as it leaked and volume is too large. So 1st when pouring into setup are you suppose to dump the whole thing in... I don't understand how to properly pour off the ether extraction without getting magnesium with it unless I don't pour all of the extract then at that point I have a lot of extract left with the magnesium what do I do with that remaining part to separate. Also I've attached pics of the leak. What do I do with this. Is this all waste . If there is magnesium that got through the filter what should I do? Basically stuck and waiting at this step
deeperdive36It's joanlab vacuum filter... It was cheap but the design is all wrong it allows stuff to leak on the outside... Ya I will try pours differently I read the sticky Patton wrote helpful in clarifying things a bit
 

ACAB

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It's joanlab vacuum filter... It was cheap but the design is all wrong it allows stuff to leak on the outside... Ya I will try pours differently I read the sticky Patton wrote helpful in clarifying things a bit
deeperdive36@deeperdive36 It looks like it is a ball joint which is held together with a clamp.
Have you tried greasing the ball joint with grinding grease beforehand and turning the ball until the grinding becomes clear?
That should solve your problem.
 

deeperdive36

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@deeperdive36 It looks like it is a ball joint which is held together with a clamp.
Have you tried greasing the ball joint with grinding grease beforehand and turning the ball until the grinding becomes clear?
That should solve your problem.
ACABAhhh I do remember reading somewhere about greasing it. I will try it today hopefully will fix the problem. Thanks.
 

Mr Good Cat

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@G.Patton general, does it worth to heat the water + FB solution + p.ether 40/60 up to 38-39C while ether washing is performed? probably it shall increase ether solubility and make emulsion dissolvation more easy?
 

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@G.Patton general, does it worth to heat the water + FB solution + p.ether 40/60 up to 38-39C while ether washing is performed? probably it shall increase ether solubility and make emulsion dissolvation more easy?
Policja PolskaYou can wash with something less volatile, but I don't think it's worth to heat at all if it matters.
 

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@G.Patton general, does it worth to heat the water + FB solution + p.ether 40/60 up to 38-39C while ether washing is performed? probably it shall increase ether solubility and make emulsion dissolvation more easy?
Policja PolskaI think it isn't a good idea. You can add carry out two extractions one by one and add NaCl to the water in order to separate layers easier.
 
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Mr Good Cat

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I think it isn't a good idea. You can add carry out two extractions one by one and add NaCl to the water in order to separate layers easier.
G.PattonYes, you are right, NaCl works pretty well. I tried it a couple of times in proportions 15-20 gr : 100 ml and it makes my life much easier.
But still thinking, may be proper temperature can improve the process much better.
 

Mr Good Cat

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Carry out an experiment and figure it out.
G.PattonI did try ABE with liquid kept in the freezer.
There was 50 gr of salt that shall give 42 gr of FB.
Immediately as alkaline was added, the solution was put into the freezes for 4 hours. Then p.ether previously kept in the freezer too was added.
As the result, separation done much easier with 40 gr of FB in the result. But, the color of resulting FB was not pure transparent: slightly yellowish.
I mean, slightly yellowish - not pure transparent, but still acceptable: not cola
 

Frit Buchner

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I've just read this thread. I thought to myself, " why are we going to pH 12 with the NaOh?" We didn't go to pH 2 so it's not balanced. Then I remembered an experiment I tried using oil as my non-polar. When I neutralized the HCL with NaOh, what happened? I made lye soap. Petroleum ether has factions that react to make parrifin. That is what is going on here. The parrifin is the 3rd layer, pH 12 is overkill and petroleum ether reacts with sodium hydroxide. Correct me if I'm wrong, I'm not a chemist
 

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Should we evaporate 2/3 volume DCM like we do Ether in step 9?
 

Mr Good Cat

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Another attempt of ABE.
About 300 gr of mdma hydrochloride at the beginning.
1.2L of water
85 gr NaOH
+ about 150 gr of NaCl lab grade added in process.

As NaOH added, pretty dirty black FB layer appeared in bottom layer (not top layer!!!), so i added NaCl to turn them over.

At first step 180 gr of perfect pure fb were extracted with p.ether, that is extremely low yeld.

Water leftovers left in the bottles for a week or something.

After a while, another step with 500 ml of DCM brought me 20 gr of slightly yellowish FB, that I would personally rate 9/10.

So, final yeld is 200 gr in total
Lost 50 gr
 

curlyfries

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Its almost impossible for me to dissolve amf 1/1 in water. ( tried 2times with 2diffent bad batches).
Amf is from ai/hg.
- till what temperature can we heat 1/1 water/amf solution ? ( 80*c ?)
- howmuch extra water can we add?
waited like 1 hour to dissolve 20grams of impure amf in water with magnetic stirrer ( there were some chuncks in it, will make sure its extra fine next time) .
When i somehow try filtering the solids wich didnt resolved in water, the residue left behind in buhner filter is like muchy salt structure.
 

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Note: I’m using DCM as my solvent

When adding acetone to the reaction mixture on step 10, I saw 2 separate layers form and with the addition of sulphuric acid/acetone solution i was not able to salt any powder out of the reaction mixture.

What did I do wrong? Are there specific techniques needed when using DCM instead of ether?
 

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Introduction

Purification at home condition is one of the hottest topics in the drug market. Example: you have a substance with a smell and color which is quite far from ideal. Unfortunately, it happens unacceptably often. Heavenly stuff do not come from every hellish kitchen, and we will pay special attention to the permanent giant of stimulants - amphetamine.

Amphetamine on the market is most common in various forms: sulfate and phosphate, rarely - hydrochloride. Sulfate - a salt of sulfuric acid (H2SO4) - more often. Phosphate - a salt of phosphoric acid (H3PO4) - less often. These two forms have a stable state of aggregation, do not require special storage conditions (unlike the hydrochloride salt) do not lose their properties for years, have the same presentation and, most importantly, are quite easily absorbed by the body. There is different topic about Amphetamine salts. The qualitative effect of amphetamine differs slightly between these salts. The ingredients in the synthesis of amphetamine must be balanced, only then the quality of the effects and product characteristics will be the same wherever the drug is produced.

In any synthesis, only toxic and dangerous substances are used. There are no other options. The color of amphetamine is white (a barely noticeable cream or gray tint may be present), the smell is completely absent, the taste is bitter. Fine-grained powder, dry, homogeneous, not oily, solubility in water without residue. Omitting more detailed characteristics, let's consider the most simple cleaning method "Product Washing" and the advanced method "Acid-base Extraction".


Method one: Acid-base extraction

Acid-base extraction (ABE), as a purification method, allows you to get a high-quality drug. Method is good by reason of using available reagents, tools and instruments.

Definitions:
  • Rm - reaction mass
  • NaOH - caustic soda
  • MgSO4 - magnesium sulfate
  • DCM - dichloromethane
  • amph - amphetamine
1. Dissolve amphetamine salt in water 1:1 (by weight). Complete dissolution should be achieved. It may be necessary to warm the solution, add water. Insoluble precipitate, crumbs, particles are removed by filtration.
2. Add 50% NaOH solution to pH 12 with small portions. A solution of NaOH in distilled water (room temperature) is poured by drops, depends on the volume. When pH 12 is reached, an oily layer (amphetamine free base) forms on the top surface of Rm. The amount of amphetamine base is equal to the mass of dissolved amphetamine. The color can be from amber to transparent, depending on the purity of the salt.
3. Pour petroleum ether (20% by volume) into Rm and mix thoroughly. Let the layers separate. The ether is insoluble in water, as is the free base, but the base is soluble in ether. In this way, we remove some of the water-soluble impurities from amphetamine.
4. Separate the top layer with the extract into an another container using a plastic / glass syringe or separating funnel. If DCM was used instead of petroleum ether, then we separate the bottom layer. Avoid the ingress of water into the separated extract.

5. Wash the water (the remaining lower layer) with petroleum ether three times (5% of the water volume).

6. Combine the extracts.
7. Dry the extract with anhydrous MgSO4 for 1 hour, placing it in the freezer. The glass should be hermetically sealed.

MgSO4 is added to Rm 3-20% (depends on amount of water there) of the volume of ether. Drying is necessary to remove the remaining water from the ether, which in further stages, by dissolving the amph salt in water, will lead to a lower (by weight) yield of pure product. You can wrap it with cling film for container tightness. It must be closed to avoid saturation of the solution with moisture concentrating in the freezer. If MgSO4 is not available, keep Rm in the freezer for 12 hours. Then, in case of formation of water at the bottom of the container (in a layer or drops), the ether should be carefully decanted (poured out) without touching the water.
8. We filter the extract from MgSO4 that has absorbed water using a vacuum pump connected to a Buchner funnel with a Bunsen flask and a paper filter. You can use a conventional filter without vacuum, which will slightly reduce the yield (you have to wash the filter with an anhydrous solvent). The solution should be decanted onto the filter without lifting the sediment from the bottom. MgSO4 remaining at the bottom of the beaker has to be washed with an anhydrous solvent (pour it onto a filter) and disposed of.
9. We evaporate the ether extract by 2/3 by heating it to 40 degrees using an electric stove (WITHOUT FLAME!). It is difficult to determine the pH level in ether solution with further addition of acid, so we reduce volume to a possible minimum. It doesn't be worth to heat the solution above 40 degrees, since a (albeit small) part of the free base of amphetamine can be evaporated with the ether. Evaporation should be carried out away from fire and in a well-ventilated area. Inhaling ether vapors is extremely harmful to health. In the presence of a rotary evaporator, evaporation should be carried out in it.

Important note: In no case should you evaporate the ether using a fan, directing it into the container with the extract. The extract is dry (without water) and actively absorbs moisture from the air. The fan directs the flow of air, which somehow has a percentage of moisture. A couple of minutes will saturate the ether with water, forming an aqueous phase at the bottom of the container.
10. We dilute Rm with dry cold (from the freezer) acetone (in half the volume). Acetone is needed to bind the remaining water and facilitate mixing.
11. We acidify Rm to 5.5 pH using H2SO4 solution in acetone (1:1) with thorough mixing. Additionally, we add acetone in small portions as the solution thickens.
Amphetamine salt is formed. Sulfate if H2SO4 is used or phosphate if H3PO4 is used.
12. Filter the resulting salt. Before that, tightly closing the glass, you can place it in the freezer for several hours. Low temperatures promote acceleration of crystallization.

13. Without removing the filter, rinse the salt three times with small portions of acetone.
Optionally, you can additionally recrystallize the amphetamine salt from alcohol or vodka according to classical methods.

Discussion

The number of impurities in amphetamine can reach a very high percentage. An indicator can be not only the presence of any smell, shades of color, salt moisture, but also poor solubility in water. Read Amphetamine assessment protocol. Contaminants may be deposited, in an insoluble layer or solid particles, depends on their nature of origin. The final yield of pure amphetamine obtained by ABE can reach both 80% and 5% of the original weight.

For one of the examples of a possible case, let's take a sample (Sample No. 2) from the next part of the article.
Initially, the amphetamine salt had a light orange color, with a characteristic pungent odor and a moist, oily consistency, and was washed with dry acetone (or IPA). Having become almost white and having lost a significant number of impurities in weight, the salt almost lost its smell and became a loose consistency.
We achieved a good result with help of Product Washing procedure (second part). But it is not. The subsequent biotest (zero tolerance) subjectively showed extremely low (at the placebo level) activity of the substance at nasal dosages of 130 mg and 80 mg (four subjects in different weight categories). Side effects are expressed slightly. Further, the ABE of this amphetamine salt was carried out.
The mixture began to thicken, forming fine whiskers after complete dissolution in water (Rm = 6 pH) after approximately five minutes. Further separation of the phase with the extract was difficult because the solution turned into a porridge.
The addition of water volumes to Rm did not have a significant effect on solubility - the mass tended to occupy the entire space. Filtering an aqueous solution through a paper filter is difficult (the paper disintegrates), and the Schott filter has not been tested. Nevertheless, it was possible to complete the extraction, but with an extremely low percentage of pure amphetamine in the yield. Its biotests showed high activity in dosages of 60 mg.


Method Two: Product Washing

Drug washing is an essential and final part of almost any synthesis. Sometimes repeated several times. The method is available to anyone, does not require skills, can significantly improve the quality of product and presentation. The method is Ideal for small quantities. Washing is indicated for residues of P2NP, alkalis, acids and so on. Washing will not remove contaminants (acetaminophen, caffeine, etc.) and mercury salts.

The most accessible, and therefore easier, is to wash amphetamine with isopropyl alcohol (IPA). More difficult to use is anhydrous acetone. IPA does not contain water, and therefore it does not dissolve amph salt. The key to the process success is the lack of water. It is needing for avoiding amph from dissolution with pollutants because they will be thrown out.

We take our amphetamine and put it into a beaker. Thoroughly grind into a dust and add IPA ~5-10 volumes of powder. After mixing, let it stand for 5-10 minutes. The alcohol (or acetone), impurities and amphetamine in the beaker now. It is necessary to apply a filtering method to separate them. From improvised means for squeezing the mass, a white dense fabric is suitable. You can also simply draw a fraction with pollutants with a syringe. If the amount to be purified is less than half a gram, then it is more convenient to carry out the entire procedure in a Petri dish. After allowing to settle, carefully drain the solvent (alcohol or acetone), leaving the amphetamine. Removing the solvent with impurities should leave the amphetamine to drying to a constant weight (and no smell). In the pictures we can see the whole simple process.

We will consider two samples
  • Sample number 1, although it seems white, but only in comparison with the second sample. Light beige color. Distinct odor of amphetamine free base.
  • Sample number 2 has an oily texture, a pronounced orange color and a strong smell of vinegar. The smell of vinegar and color indicate the absence of even primary cleaning. With a probability of 100%, this sample contains impurities (salts of mercury, aluminum, P2NP, etc.).
For the curiosity sake, after placing the samples in the IPA and letting it settle, we will measure the pH.
  • Sample No. 1 - pH not less than 8. This indicates that the crystallization step (adding acid to a solution of amphetamine free base in acetone) was not completed. A strong burning sensation while consuming is guaranteed.
  • Sample No. 2 - pH is ideal, equal to 6.

Start the cleaning procedure

1. Sample No. 1 is placed in a syringe with IPA and mixed thoroughly. After settling, you can see a crystalline sediment at the bottom. Probably dealer added impurities. Drain the liquid fraction.
2. Compare the sample with the original by drying the washed sample to constant weight. It became lighter and lost its smell. Approximately 4% weight loss.
1. Sample No. 2 is placed in a beaker with IPA. Mix it thoroughly. Letting it settle, drain the IPS. You can also squeeze out amphetamine with a cloth. The image shows that the sample has a denser fraction at the bottom and a less dense fraction above.
2. The procedure was repeated 8 times with this sample, only then the amphetamine became significantly lighter.
Approximately 25% weight loss.
We compare the result after drying these fractions separately to constant weight. We didn't receive the white sample. As you can see, the fractions have a gray tint - these are organic impurities that do not dissolve and are not removed by washing. This amphetamine is still unusable. To thoroughly clean it up, it is necessary to carry out an acid-base extraction (ABE).
Summarizing, we can once again be convinced of the importance of such a stage as washing the final product with anhydrous acetone or IPA. The use of amphetamines of various colors can cause serious harm to the body and psyche.

Conclusion

The amphetamine originally sold was not only of the lowest quality, but could also cause significant harm to the health of a user. In particular, it affected those who use the drug intravenously (i.v.). After dissolution of the powder in water for injection (if this could be achieved at all), the solution thickened in the syringe, making it difficult to inject into the bloodstream. Ignorance of consumers is used (intentionally or not) by sellers in the sale of defective drugs batches, harming the body and psyche of the consumers, and bringing profit to sellers. In conclusion, it is important to note that the lack of experience with pure drugs leaves the buyer incompetent in assessing the quality of the product purchased.

G.PattonThanks a lot i will try the first Method

I often did the Method 2 but i just filtered it with Coffee paper filtre and think with Acetone better results.
 

garro

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First, ty to everyone sharing your knowledge.

Second, i fucked up the A/B extraction and need some advice on whether what I have is recoverable or not.

I'm using
1) Lye
2) Sulphuric Acid (Drain cleaner)
3) VMP Naptha
4) ~3g meth

Everything was going well. I extracted the freebase layer and froze to remove any water. Then I think I over acidified. I tried to recover it and caused more of a mess. I currently have two layers, one water(PH ~2) and one naptha There was also some particulate matter which has either been filtered out or dissolved in the water layer.

I also diluted the sulphuric acid with water, not acetone. I believe this was a mistake, please correct me if I'm wrong.

Few questions:
1) Is it possible to recover any product from this? If so what steps would you recommend?
2) In the future, If I over acidify, what should I do to recover the current process, or reset back to start (amph in distilled water)
3) Can I do the A/B w/o ether/spirits layer? As I understand the process, this would leave water soluable cuts, but just want to verify.
 

EmilioE66

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Hello i have a question. Whats ideal PH for Amphetamin (liquid Form Mixed with methanol) when adding sulfuric Acid ? The Amphetamine 1:2 with methanol has ph 12.
 

EmilioE66

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When the Amphetamin has ph12 i have to put sulfuric Acid Till it reachs ph 6 Right?
 

kinkyfeet1

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Hi General Patton, I cant find any resource that shows the final production of the pink adderal pills. If i want to make the pink adderal pills, do i have to follow this instruction specific?Thank you for your time and help.
 

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Hi General Patton, I cant find any resource that shows the final production of the pink adderal pills. If i want to make the pink adderal pills, do i have to follow this instruction specific?Thank you for your time and help.
kinkyfeet1Are you interested in the pink color or the composition of the admiral, which includes different salts of amphetamine and dextroamphetamine?
 

kinkyfeet1

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Are you interested in the pink color or the composition of the admiral, which includes different salts of amphetamine and dextroamphetamine?
HIGGS BOSSONArent all adderal pills pink color on the market? sorry for my naive question, but i want to look into the production of adderal, and how can i start on that?
 

kinkyfeet1

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Are you interested in the pink color or the composition of the admiral, which includes different salts of amphetamine and dextroamphetamine?
HIGGS BOSSONI have taken one before and it was super helpful for me to focus. it was a pink pill and 20MG written on it I think. is there anyway i can produce the same thing at home or even in a lab with the right resources?
 
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