Yellow Liquid K crystallization

[bobby1]

So... I have liquid k which is yellow and have done some research and figured out that DCM and pentene ether added to it will finalize the yellow liquid k before drying it. Anyone know if this is right? how to do the procedure properly if it is right...the yellow liquid is at a pH level of 5.0-6.0 so it is pretty acidic. Any advice or input into what to do would be much appreciated.. Cheers!

 

[Oxide]

We don't SWIM here. I'm going to stick this question in Psychedelic Discussion, though.

 

[Solipsis]

Finalize? What?

There is petroleum ether and there is pentene, and there is pentene-ether as a name for a mixture of pentene and ether. All of them including DCM are of course solvents. I'm not saying they are unable to react with other compounds, not at all... but when it comes to a ketamine solution (liquid K) don't expect any of them to change anything about ketamine itself.
But forget that, I guess you are talking about a wash. And you saw this in Merck and Clarke or quoted on BL:

Ketamine FB: Properties: Crystals from pentane-ether, mp 92-93°.

pKa 7.5. pH of 10% aq soln 3.5.

Ketamine HCl from the Merck: White crystals, mp 262-263°. Soly in water: 20 g/100 ml.

Clarke's: HCl: Soluble 1 in 4 of water, 1 in 14 of ethanol and 1 in 6 of methanol; sparingly soluble in chloroform; practically insoluble in ether.

If you choose a solvent or mixture of solvents that dissolve the yellow but not the ketamine, then you will flush out the yellow and upon letting your K dry. You probably lose a little ketamine this way using DCM but with ether you shouldn't lose any. Not sure what makes you think the yellow is soluble in non-polar solvents though, do you understand what you talk about doing?

The pH sounds about right, it is normal for liquid K to be acidic like that. You don't want it more alkaline or neutral because it will freebase a part of the K which will then be soluble in non-polar solvents.

 

[bobby1]

the solution is a thick yellowish color unlike most liquid k's, has a very strong smell, currently at the state which the solution is in, it will not crystallize or harden when heated any way. A little bit or research was done and was believed that the yellow solution was at this phase in the process, Acidic extract is basified and extracted with DCM.Solvent is removed giving the product as an oil that quickly crystallizes. It can bee purified by recrystallization from pentane/ether or hexane/ether. Would this allow the yellow solvent to dry and crystallize? the person that the solution was acquired from also said that 2 solutions need to be added to the yellow solution and heated and then placed in a water bottle lightly stirred and crystallization will occur inside of the water bottle. If these 2 solutions are incorrect what solutions would work?
Thanks guys, cheers!

 

[greenmeanies]

I think you got ripped off. I would not do any acid/base extractions in a water bottle for fear of dissolving the plastic with my nonpolar solvent. And it will not crystallize inside the bottle if you attempt an extraction. How do you plan on siphoning? Have you ever performed an acid/base extraction? Why do you seek freebase K? I thought the HCl form is the one that gets insufflated....

 

[bobby1]

The acid/base extraction is done in a pot. Once complete you are left with a thick oily liquid which is then poured into a water bottle and allowed to cool off. While cooling, the water bottle is lightly stirred. Small crystals will begin to apear in the water bottle.

It is not clear whether the two liquids which need to be used are DCM (methylene chloride) and pentane ether or if other chemicals would be better suited?
Has anyone come accross yellow liquid K before?
My friend has seen yellow liquid k be crystalized before. It is much more potent than regular clear liquid k.

What needs to be added to the yellow liquid to allow it to crystalize?

 

[greenmeanies]

That is NOT how an acid/base extraction is performed.

Nothing needs to be added to the yellow liquid--- in fact water must be removed! You said this yellow solution is acidic, so there is probably Ketamine HCl in solution. Adding DCM or pentane will NOT crystallize the ketamine, and it will NOT cause the ketamine to enter the nonpolar phase!

Proper acid-base extraction using a glass seperatory funnel (or a glass container and a glass pipette for removing the lower layer):
1. Combine your acidic aqueous phase (water+drug) with a small amount of your nonpolar solvent (DCM) This is the prewash for removing impurities that are soluble in DCM but not in acidic water. Agitate gently by rolling or swirling-- do not create a milky emulsion!
2. Separate the two layers. Discard the DCM, as it has no drug in it, only impurities.
3. Using ammonia or sodium hydroxide solution (be careful, will burn skin and eyes), basify the aqueous layer until it shows pH 10 or greater.
4. Add a fresh measure of DCM to your separatory funnel. Agitate gently. At this point your drug should be in freebase form (nonsoluble in water) and will migrate into the DCM phase. Separate the two layers and reserve the DCM phase. Repeat this step twice more with fresh DCM to ensure you have extracted all of the freebase drug.
5. Combine these DCM extracts in a wide pan and evaporate in a well-ventilated area. You should be left with relatively clean freebase drug crystals. Dunno what you would do with them, because they will burn the holy hell out of your nose (caustic base) and will definitely NOT dissolve in water for any kind of injection.
6. Alternatively, mix up a fresh batch of acidic water using distilled water and some muriatic acid (HCl). Use this acidic water to extract the drug-laden DCM (instead of evaporating) and you will have a fairly clean Ketamine HCl solution that you should be able to "cook down" into ketamine HCl crystals.

Again I ask, do you fully understand the chemistry of what you plan to do? How do you plan on consuming this ketamine? If you have tried boiling the yellow solution and have not gotten crystals to form, I seriously think you might have been ripped off.

 

[Solipsis]

Apart from the possibility of being ripped off, it is a bad situation for you to not know what kind of liquid you have... what kind of composition, and no apparent understanding of finding out. Hmm on the other hand if you refrain from ingesting it unless you are successful in yielding colorless crystal product little harm can be done other than unproper handling of chemicals/solvents.

You say the liquid has a strong smell, but can you place it? Do you have experience that can tell you whether it is a solvent you smell or not, is it familiar to you? Is the liquid aqueous: is it mostly water, does it behave like water? Well it must I guess, because it has pH.
You talk about the use of solvents like DCM and ether and basic alkane/hydrocarbon solvents such as pentene... but it does not sound like you know much about this, can you get whatever chemical you want for purification? Otherwise all this talk is useless anyway.

Good luck with the extraction if you have the means and the understanding to get it done. If the yellow impurity can be protonated like ketamine there is a good chance it gets carried along with the extraction and it will not work. Then you cannot separate it that way (unless IIRC the pKa is even higher than you basify).

You mention cooling down, am I to understand that you try to recrystallize from hot solvent? Maybe you get some crystals but it will only work for a good quantity if you add the correct solvent to the mixture that does not allow ketamine to be in solution.

What is the use of ketamine freebase? You cannot dissolve it in water so it cannot be in liquid K for shooting. Actually I would not inject any product you get considering it doesn't sound like you really know what you are doing. And I don't think you can snort it either - again because it cannot dissolve in the water (in your body/blood/nose). It does not matter that the freebase is slightly more potent than the salt because if you make the HCl, it slightly increases in quantity proportionately.

And there is no way that any ketamine is more 'potent' than normal liquid K of pharmaceutical quantity, it can only be more concentrated - more ketamine per milliliter (per unit).
If you know of ketamine that is extracted and recrystallized it may seem superior to you because it is not cut like other powder/crystal K you may have come across.

I don't really feel comfortable going on and on about this if we're not on the same level. But right now I guess it's your thread and who knows - perhaps you can just follow the instructions and get fine product out of it.
If you know a friend who processed "yellow liquid K" successfully why don't you go ask him about it? At least he seems to know what the hell it is and what the hell makes it yellow.

 

[sekio]

Ketamine HCl should xtallize nicely if you just boil the water off (reduce it) to a very small volume and then chill the solution.

Another option would be shaking with decolourising carbon, or doing an A/b extraction.

 

[Solipsis]

What makes you think activated charcoal absorbs (or adsorb in this case) the yellow impurity but not the ketamine?

 

[bobby1]

Will a charcoal filter allow the solution to crystalize?

I tried heating up the solution and then cooling it off but that did not work.

Something needs to be added to the yellow liquid to allow it to crystalize.

 

[Solipsis]

If anything charcoal will catalyze crystallization, in my rationalization of theory, but not in a way you would appreciate. You see part of crystallization is that you need it to be seeded i.e. there has to be a starting point for a crystal to start forming. Two things that serve as seeds (that may work the same way) are something that on a microscopic level is very very jagged so absolutely the opposite of a smooth surface. Erratic sharp shapes on an almost molecular level then function as a peg for in this case ketamine to start grabbing on and growing as a crystal by stacking molecules onto one another. A second one is scraping an instrument like a glass rod on the container of your solution. This probably also immediately creates disturbances on the material that also is used as a peg to seed crystals.
Activated charcoal is extremely jagged, there are all types of caverns and holes and bumps and tunnels in the surface structure. Anyway with charcoal this would suck because basically in every ketamine crystal formed there would be charcoal in the center. Highly impractical to say the least. Though you could do that, filter, redissolve in pure solvent and achieve some separation from impurity at least. Filter it again to get the clumps of charcoal out, then let it stand to evaporate to yield crystals once again.
FYI, activated charcoal is not the same as normal charcoal. It is treated with oxidators at high temperature to create those jagged surface structures. Normal coal does not have this and is useless for the application.

Heating a solution and cooling it down won't achieve anything. It has a solubility at the cool starting temperature, so a limit of K that it can contain... it only increases when you heat it allowing more ketamine to be in it. Then cooling down to the starting temperature you are again back where you started. Nothing changed.
You may be confused becaused you think cooling down will start crystallization. This is only useful is your starting temperature is actually higher than where you end up, and during the process you need to pass a point of saturation. Saturation means that the solution reaches the maximum of something dissolved in it that it can contain.
Think of it like a balloon that has objects in it. Heating it up inflates the balloon and allows more objects in it and they can move around more. Cooling down shrinks the balloon and restrains the movement. When you pass the saturation point the balloon simply becomes too small for the objects it stores, they are forced out or rather they clump together in the form of precipitation: so crystals form. You can think of the balloon size as a function of energy by the way.
So you see, blowing up a balloon and shrinking it to it's original state does not force out anything in it. Also to make the analogy more accurate, contained in the balloon is not only the objects (like marbles or balls) of ketamine but also the objects of the solvent itself. If you cool down the liquid and the balloon shrinks enough, in the case of the solvent itself the balls (molecules) also clump and this is what we normally call freezing over.

When extracting DMT, what you can do to crystallize it from your solvent is cool it down from room temperature. You can put it in the freezer. It takes very very low temperatures to freeze over the non-polar solvent used, but before that the solubility of the DMT drops so far that it is forced out of the liquid as crystals. It just so happens that there is a significant difference in how much DMT the solvent can contain between those temperatures. It doesn't necessarily have to be true that this is the same for your solvent with the ketamine. And if you have a watery solution, the water will freeze to ice before anything else. If you have a solvent like ether that readily dissolves your ketamine freebase if you basified it to high pH, freezing it won't do anything because it is just able to contain a LOT of ketamine so nothing is forced out even by cooling to minus 20 centigrade. Don't try to put ether in the freezer, it could blow up from an electric spark because it keeps evaporating. Other non-polar solvents like Coleman fuel / naphtha should be OK. I did that a number of times.

Also please remember that the solubility is measured in an amount of material (here it is ketamine) in VOLUME of liquid. So if you have a lot of liquid/solvent, nothing will happen either way because there is enough 'room' anyway for the K. So if your balloon is huge, shrinking it won't matter a bit.

Now, about adding a second solvent, I would have to adjust my analogy. It would mean adding a different type of object to it, let's say they are magnets added to balls. The magnets disturb the stacking of all those things which can lead to the ketamine not being able to fit in it anymore because the magnets cannot be stacked together with it, they push it away. I just said ether can hold FREEBASE ketamine. But it pushes away ketamine salt (ketamine HCl). Assuming you have a watery liquid with ketamine HCl in it now, ether would be opposed to the ketamine. The problem is, water and ether do not mix. So you cannot just add that for crystallization.

As is said before: you need to do an acid/base extraction to pull this off. Meaning you have to change your ketamine salt to the freebase and back to the salt again. An acid turns it into the salt, lye turns it into freebase. The salt wants to be in water and is okay somewhat in alcohols, but the salt does not want to be in ether or pentane. The freebase is virtually the other way around. That way if you swap it around two times you can get it to separate from the junk you want to leave behind.

You do this separation by forming two layers of solvents: ether floats on top of water, you can see a vague line between the two liquids sitting on top of each other. You call those liquids different phases or layers if they do not mix.

So make the two phases, then change the pH. You can imagine the ketamine travelling to the other phase or layer. Then you change the pH back again and it will travel back to the other layer. Only you don't use the same liquid, you throw away what used to contain the K and replace it with new liquid.


OK, so I explained a few basics. Hopefully you like the science lesson but if you wanted a simple tip or trick and have a hard time understanding the rest then I'm sorry. And I won't continue trying to teach you anymore because it just doesn't work that way. Either you can learn the practical chemistry and do this, or you do not and should forget about it. If that is the case, sorry. The thread won't have a very bright future.

 

[sekio]

I tried heating up the solution and then cooling it off but that did not work.

Something needs to be added to the yellow liquid to allow it to crystalize.

Try boiling off ~2/3 the (presumably water) instead of just heating and cooling it? And read up on your chemistry as soli suggested.