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Hash oil using hexane


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#21 lambep

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Posted 01 July 2011 - 06:09 PM

how much oil get trapped in the coffee filter? I guess I mean does very much get trapped in it?

A lot got trapped and that's quite a concern here. I'm working with such small quantities that I lost a few hits (which constitute like 1/5 of the total yield) on the paper filter...

One possible way to lower the loss is by doing larger quantities. The other thing I thought about was using some kind of coffee strainer made of metal or something similar.

#22 Phineas_Carmichael

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Posted 01 July 2011 - 06:20 PM

To make the initial extract (that we end up cleaning up with hyphs tek) is it better to use hexane, naptha, acetone.

I don't think it matters that much. In fact, Hyph didn't like to talk about making hash, only purifying it, because working with these solvents can be quite dangerous. I do seem to remember him saying something about "pet ether" once though. That's Naphtha.

I'm left with the same impression about cold acetone. This doesn't sound logical because temperature shouldn't affect the fact that acetone is a ketone and thus quite polar - it's even miscible with water.

I'm not sure why acetone dissolves THC as well as it does. It is polar, but not that polar. It's dipole moment is only 2.91 Debye units. Compare that with Potassium Bromide's dipole moment of 10.5 D. Also, consider that isopropyl alcohol also dissolves THC and is slightly polar as well...

The solubility of THC isn't much affected by the temperature of the acetone, but the solubility of all the other junk is drastically affected, and that's what is being exploited in the freeze precip of waxes and such.

About the solvent to be used in the initial extract as much as I know naptha contains different alkanes (and hexane is an alkane) so they'll be able to dissolve similar amounts of THC.

Agreed. The difference between naphtha and hexane is negligible for most clandestine chemistry, especially hash-making.

#23 lambep

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Posted 01 July 2011 - 07:06 PM

...
The solubility of THC isn't much affected by the temperature of the acetone, but the solubility of all the other junk is drastically affected, and that's what is being exploited in the freeze precip of waxes and such.
...

Can you give some more detail on that?

I know everything should be less soluble in any solvent when the solution gets cooled. I suspect that different things get less soluble with different rates.

Do you know some kind of scientific explanation as to why thc would get less soluble in acetone more slowly compared to wax and other stuff when lowering the temperature of the mixture?

#24 Phineas_Carmichael

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Posted 01 July 2011 - 07:18 PM

Do you know some kind of scientific explanation as to why thc would get less soluble in acetone more slowly compared to wax and other stuff when lowering the temperature of the mixture?

It's not a question of the rate at which THC solubility decreases compared to wax solubility. It's a question of how much of each compound is soluble at any given temperature.

Based on experimental results, I'd venture a guess that wax is more soluble in room temperature solvent than THC, but less soluble in freezer-cold solvent.

I'm going to make up some numbers, for the sake of explanation.

Solubility in room temperature acetone:

THC: 100mg/mL
Wax: 250mg/mL


Solubility in freezer-cold acetone:

THC: 90mg/mL
Wax: 50mg/mL


Because the material commonly used for hash-making (leaves, stems etc) contains very little THC and very much chlorophyll and waxes, there is a lot more of them in solution in the solvent. When the temperature decreases they crash out first. I suspect that if one used high quality buds there would be little need for the dewaxing.

As to exactly why this is so, I'm afraid I couldn't say. Except for the fact that different compounds have different solubilities. Consider salt and sucrose; salt is soluble in water at 359 g/L and sucrose is soluble in water at 2000 g/L.

*EDIT* Thanks for giving me a reason to yammer on like a flaming dork, as if I needed one... :shy:

#25 Nemo Mason

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Posted 01 July 2011 - 07:22 PM

maybe it has to do with how often thc in nature gets above a certain temp. These days it seems that you hve to get natural to really get technical, but I am only offering whatever my brain feels like spitting out right now. I am only expirienced in expirimentation!

#26 lambep

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Posted 02 July 2011 - 03:41 AM

...
I know everything should be less soluble in any solvent when the solution gets cooled. I suspect that different things get less soluble with different rates.
...

Solubility is not always going down with temperature as I thought. The second statement I quoted is right.

I think so because of the following picture from http://en.wikipedia....wiki/Solubility:

Attached Thumbnails

  • SolubilityVsTemperature.png


#27 Phineas_Carmichael

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Posted 02 July 2011 - 12:15 PM

Solubility is not always going down with temperature as I thought. The second statement I quoted is right.

You happened to stumble upon one of the only compounds that has a strange solubility curve like that.

It is weird because of trapped water molecules in the crystals. Here's the solubility curve for just Na2SO4:
FileNa2SO4 solubility.png.png

And a line from the wiki article:

Sodium sulfate has unusual solubility characteristics in water. Its solubility in water rises more than tenfold between 0 °C to 32.384 °C, where it reaches a maximum of 497 g/L. At this point the solubility curve changes slope, and the solubility becomes almost independent of temperature.

Quote source
This happens because Na2SO4 often traps water molecules inside the crystal matrix when it crystallizes. This 32.4 *C happens to be the melting point of the decahydrate (Each molecule of Na2SO4 has trapped 10 molecules of water). When it melts it screws up normal solubility rules.

You were right the first time. With solids the general rule is when temp goes down, solubility goes down, with gases this is reversed but that doesn't matter for this discussion. There are very few exceptions, and Sodium sulphate just happens to be one of them. I did not know this until today, thanks for opportunity to learn something.

I still say this dewaxing in acetone business has little to do with the "Rate" (1st derivative of a solubility curve) at which solubility decreases with temperature and everything to do with comparing points on 2 different solubility curves.

#28 Phineas_Carmichael

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Posted 02 July 2011 - 01:33 PM

I still say this dewaxing in acetone business has little to do with the "Rate" (1st derivative of a solubility curve) at which solubility decreases with temperature and everything to do with comparing points on 2 different solubility curves.

To clarify this statement, here's a hastily drawn graph, again with made up data:
SCAN0006.JPG

The solid lines represent solubility data. The dashed lines are very crudely constructed 1st derivatives of the solubility curves. The slope of a dashed line is the "Rate at which solubility changes with respect to temperature" for that substance and the units would be "mg/mL/*C" read as "milligrams per milliliter per degree centigrade."

Yes, you're right. They have different slopes, thus different rates, but the rate doesn't tell us anything about the dewaxing in acetone procedure. The data we should be concerned with are how much THC and "oakum" (cannabis wax) is soluble in acetone at 0*C.

Based on experimental results (the fact that wax crashes out of freezer-cold acetone & thc doesn't) we can conclude that at 0*C oakum is much less soluble in acetone than THC. We're comparing points on the graph, not rates.

Edited by Phineas_Carmichael, 02 July 2011 - 01:53 PM.
Plurality agreement


#29 The Confused Man

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Posted 02 July 2011 - 03:25 PM

could a non-disposible coffee filter be used?

#30 lambep

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Posted 02 July 2011 - 03:59 PM

The Confused Man, I suppose it can be used but I bet there will be more small particles that pass through the filter.

Phineas Carmichael, thanks for the quality info :)

#31 lambep

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Posted 07 July 2011 - 06:03 PM

My imaginary dog found a bit of low grade outdoor buds hanging on a tree nearby :eusa_liar so I decided to redo the extract in this thread with some more measuring using this material.

1. I took 50g of freshly unfrozen bud (it had a bit of water in it) and ground it in a coffee grinder until it consisted of particles 1-3mm in size (in my opinion it shouldn't be made smaller). This was put in 2 jars and hexane was poured in those jars until it covered completely all the leafs and a centimeter more.
2. Both jars were stirred manually for 30 minutes the first and 45 the second and then were filtered using a coffee filter.
3. The resultant mixture was evaporated in a water bath (to be honest I once again distilled the hexane but this is irrelevant to the result IMO) until I was left with around 50-60ml (actually until I started seeing 2mm thick hash oil lines outlining where the solvent, the air and the glass meet).
4. This was then transferred to a big petri dish and further evaporated in normal temperature. I should note here something I consider relevant to quality - the petri was not left horizontal, but rather at an angle so that most waxes and similar stuff could precipitate outside/above the solution. Also the petri was covered with a paper towel to lower the amount of dust falling on the product.
5. When the resultant liquid has gotten quite thick and has stopped leaving impurities it was transferred to a small petri dish.
6. This new small dish was further evaporated in a water bath.
7. It was left again at an angle to solidify. A nice clear drop of wax or something else IDK appeared in the part of the petri that was highest and cannot be seen on the pics.

Here's a few pics (the first is the weight of the product - 3g, a few hours after the water bath, the second is done with the camera flash and the last two are done without it):
SN851942.JPG

EDIT: I'd love to hear your comments on purity based on my pics.

Attached Thumbnails

  • SN851941.JPG
  • SN851939.JPG
  • SN851940.JPG

Edited by lambep, 07 July 2011 - 07:26 PM.


#32 lambep

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Posted 09 July 2011 - 04:14 AM

Please feel free to comment on the purity based on my technique and pictures.

I really want to know what's on your mind.

#33 BuckarooBanzai

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Posted 09 July 2011 - 08:25 PM

Your results look gorgeous to me...but the true proof of an extraction is in the consumption.

Does it smoke good? Any hint of solvent? Does it burn clean or leave a black ash?

One way or the other - it looks freakin' gorgeous...

#34 lambep

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Posted 10 July 2011 - 03:47 AM

I have to admit it's quite a harsh smoke but it might be so because of the way I smoke it - I drop a big fat drop of oil, around 0.1g or even a bit more, on some tobacco, then use this tobacco on the tip of a joint (filled with only tobacco). The drop travels down as it melts and that's the most similar to a rolled weed cigarette way of smoking I've found.

After the water bath there was no hint of solvent at least in the smell.

It leaves no ash. I tried evaporating a drop of around 0.1g on a teaspoon over an alcohol lamp and all it left was brown coloring that doesn't evaporate. Also it first evaporated the hash oil (judging by the smell) and after that something else, far harsher to the lungs. This to me means it's less pure than I thought... Also obviously the brown color I always wanted in hash oil is not the best - the brown colorant was left on my spoon. Now I think that the color of hash oil should be reddish as in hyph's thread mentioned above.

I'll have to try the acetone method to further improve my extract.

I think evaporating hash oil on a teaspoon is the most effective way of smoking it I found so far.

#35 lambep

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Posted 25 July 2011 - 03:24 AM

I made another batch of honey oil using hexane and 50g bud.

When I evaporated the hexane I got 3g product. The honey oil was than put in a jar of almost boiling water and the water was shaken vigorously. After this cooled the extract was quite hard so it was easy to remove the water. This was dissolved initially in room temperature acetone which dissolved all of the coloring and a bit of the waxes so I had to heat it to dissolve everything. This mix was left to cool, than was put in the freezer. Even in room temperature waxes precipitate from the acetone solution and I'm not sure if freezer temperature is necessary. Anyway, the freezer cold mix was than filtered through a paper coffee filter. Until this moment everything was going as expected.

At this point I added 20g powdered pharmaceutical activated charcoal. This made the solution pitch black. After about 24 hours the mix was still absolutely black (the charcoal didn't fall to the bottom) so I decided to use paper coffee filters again. Unfortunately quite a lot of charcoal passed through so I got desperate and tried using a paper towel with the coffee filter as a filter. This worked very well (in removing the charcoal) and the solution that was left was crystal clear with no color whatsoever. This was than evaporated and left something fatty looking, colorless, clear and smelling like some herb (not weed) and totally not smelling like hash oil. This weighed around 0.5g. As it looked so wrong I couldn't make myself bioassay it. I suppose I used too much activated charcoal of the wrong size.

I made another batch similar to above using 75g. I washed this mass twice with hexane (which I never did before), the first wash gave around 5g and the second around 3g. This was combined and water purified as above. Next hot acetone was used to dissolve everything (I had to use around 700ml!). After that I cooled down (including in the freezer) the acetone and filtered the waxes. I moved around 100ml of this mix to another jar to try cleaning with granulated activated charcoal and evaporated everything else which left 5g product. The jar with the charcoal hasn't changed its appearance for 12 hours now. I'll leave it another 12h and will filter the charcoal and evaporate everything else.

#36 mimosadmtastronaut

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Posted 27 July 2011 - 02:06 PM

I'm quite curious to see how it will turn out after another 12hrs. This is a great thread, if
only I had accces to the right lab equipment now.... sigh

#37 Defiance

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Posted 27 July 2011 - 06:07 PM

We've moved waaay past this, but baking trim before doing an extraction probably isn't necessary. The carboxyl group is polar but it probably won't cause THCA to fall out of solution during an extraction (Just a Guess based on structure). It will decarboxylate during smoking.

I think it's only necessary to bake off the trim if you're going to eat the extract, not smoke it.

Phin, you're awesome in this thread. lambep, you're awesome too. :thumbup:

#38 lambep

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Posted 01 August 2011 - 01:48 PM

The hash oil, acetone and granulated charcoal mixture was left at room temperature until now. It lost most of its green and some of its brown coloring and now looks like the pics in hyph's thread, but noticeably browner.

I'll leave this mix for a few days in the refrigerator and if that doesn't make it less brown I'll remove the charcoal, evaporate some of the solvent and put some fresh charcoal.

mimosadmtastronaut and defiance, thanks for the encouragement!

#39 lambep

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Posted 15 August 2011 - 04:07 AM

The time in the refrigerator (around 10 days) removed some more of the colorants. A few days ago I filtered out the granulated charcoal and yesterday I evaporated the acetone.

A few posts back I used some powdered charcoal in an attempt to purify my product. This left a clear, colorless product smelling like some herb and not hash like (sorry I can't explain that better) which I discarded as I thought it was not what I was going after. Well the current purified (by granulated charcoal) product I'm working on has the same smell although it's not colorless and clear.

I'll probably try it with a friend in about an hour and at some point later I'll share with you my personal experience.

Here's how 1.5g of this looks like:

Attached Thumbnails

  • SN851968.JPG


#40 lambep

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Posted 15 August 2011 - 04:32 AM

Well, we're smoking it right now and I've got to say it's got a very nice mild taste - the best taste of a thc product IMO after good quality buds. I'm impressed with the taste and the high is high quality too :)

That's it for now.

P.S. The product has a low odor and the taste is not as noticeable as with hash, not-so-pure hash oil and buds. Also the taste and the smell are both totally not hash-like unlike the effect. One more thing - I think that's the least harsh thc product I've ever tried.




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