[marygrace]

I put in freezer for 24h , with ice to keep the temperature as low as possible , to facilitate filtering of waxes , being solid .



a coffee filter for filtration .



I poured the oil and alcohol solution quickly and put back in the freezer for finishing filtration . This stage is crucial to keep the temperature low , to prevent fats back into solution .

What i was able to filter .

[marygrace]

The result ? A impressive clear solution .












Cheers

[mobin]

say I was going to use shake. given the nature of the initial material, would you guys recommend screening the material out to reduce lil pieces of leaf to green everything up?
or would i be better off using bubble bags then working the bubble hash? apologies if this has already been covered, ive read most of the pages here i think.

thanks to those who paved this amber road before me. its refreshing to see logical, more scientific methodology. anyone can follow a recipe....understanding what is happening and why is so so much better.

[TerpChild]

You can pour the shaky solvent mix through the 25 micron bubble bag and sqeeze the material in the bag to get all the solvent/oil out of the material, then freeze the strained solvent to let the waxes coagulate.

[SkyHighLer]

Originally Posted by jump117

Here is Sugar_Kremlin ladyboy absolute amber.

Introduction.
Firstly I have to notice the term absolute here is not about the absolute ethanol.
I’ve posted about this double extraction for several times as for the method of removing bubbles and a garbage from a primary BHO.
As was said right - a picture is worth a thousand words, thus I made a photo session to illustrate what do they (and me) mean talking about absolute and concrete.
Start from the quote to refresh.


Female plants were reversed into banana ladyboys via colloidal silver stimulation to reap 2cc+ of fem pollen yield.
Reversed flower in addition to bananas consists of a sepal and adjoining parts covered with trichomes full of resin.

View Image View Image View Image View Image View Image
Sure they are very much poorer in compare to sensimillia buds.
The flowers were prepared with a manicure scissors to open a covered resinous parts and to remove a poor fragments,
then placed into extraction pyrex teapot and chilled at -20C together with a lid.

Primary non-polar extraction.
Pre-chilled "London" butane (250 ml / 139 g, $2.35) was sprayed into the extraction teapot through the lid port (white in brown lid on photo), at outside temperature +14C (57F).
The plant matter was floated and stirred in the butane during 10 minutes, no boiling was observed.
After that solution was coffee-filtered into the evaporation teapot (with glass handle on photo)
and was placed on the top of the coffeepot, suitable by diameter and shape, filled with a hot water as the double-decker to evape butane quicker.
Plant matter is full of bananas. It was fresh frozen before the butane run, now its wet volume is 160 ml (cc).

View Image View Image View Image View Image

After evaporation of butane is over the inner surface of the evaporation teapot is covered with a transparent film of a primary non-polar extract.
It is a concrete also known as BHO.

View Image View Image

Secondary polar re-extraction.
To take it from a teapot together with secondary polar re-extraction, the ethanol 96% was added into a teapot.
EtOH doesn't dissolve everything from BHO.
Butane dissolves some waxes and fats that is insoluble in ethanol while the good resin dissolves in EtOH.
Tiny undissolved flakes were coffee-filtered off the solution.

View Image View Image View Image

The final evaporation was made on a soup-plate evaporation bowl over the boiling water.
An absolute was collected with a razor blade when it remains hot.
At room temperature it is a brittle amber. After broken in two parts it may be soldered together back with a heat of a lighter.
The coin is russian 10 копеек its diameter is 17,5mm (~0,7").

View Image View Image View Image View Image View Image
View Image View Image View Image View Image View Image

I've read a recommendation not to smoke the silver processed plants.
Probably it was said about STS and was transferred to CS unspecified, I don't know.
I hope this amber will not make any harm to the health and on the contrary will probably be a medicine against respiratory infections and against a bad weather outside.

Jump to the present, seven years.......


WINTERIZING AND DEGASSING PRIOR TO DISTILLATION

06.12.2017 winterization - degassing - decarbing - distillation Posted By Best Value Vacs

Prior to distilling oil, you should follow a winterization and degassing procedure. The winterization will remove fats, waxes, and other inactive and unwanted compounds. Degassing will remove any solvents and other inactives with low boiling points to prevent foaming during distillation. These processes are imperative to successful distillation and could be considered more important than the actual distillation itself. Always use safety equipment and have proper ventilation when working with flammable chemicals.

Winterization

The first step in your winterization procedure will be dissolving and emulsification of oil in an alcohol solvent. Alcohol is a solvent just like butane or propane but it is not a hydrocarbon. To dissolve oil in alcohol, you will need the following items:

- Hot Plate Magnetic Stirrer with either digital temperature readout or a submersible thermometer that will read up to 50C

- Alcohol: At minimum you want the highest proof alcohol you can aquire. A good starting place is 190 Proof Grain Alcohol. In most states, Everclear is available from most Liquor stores. You can also use organic alcohol purchased in bulk supply from some online retailers. If you can aquire 190 or 200 Proof Lab Grade Ethyl Alcohol, this will be the best option. Do not use denatured alcohol of any kind.

- Mixing Vessel: This will sit on the hot plate magnetic stirrer. A few options are Ball Jars, low form beakers, media bottles, or vacuum chamber pots.

Dissolving and Freezing Solution

It is recommended that you use as little alcohol as possible during this process. This will make alcohol recovery and filtration faster. A good starting place is filling a Ball jar a little more than half way full with alcohol. Place a magnetic stir bar in the Ball jar and place Ball jar on hot plate. You do not need high temps or high stir bar speeds. 40C on the hot plate and 200 RPM on the stir bar is a good place to start. Simply put oil into jar carefully and wait for it to completely dissolve. If the oil seems to become solidified, add a bit more alcohol to the mixture. Once all oil has been fully dissolved, it is time to freeze the solution.

Freeze your mixture overnight in a standard freezer. This will allow fats and waxes to coagulate and precipitate out of the solution. For ever faster coagulation, freeze and filter at different temps. I.e, freeze for 4 hours at 32F and filter through a fast speed filter. Freeze for 4 hours at 0F and filter through medium speed filter. Freeze for 4 hours at -40F and filter through slow speed filter. This will remove more and more mass from the mixture each time, making filtration faster.

What Kind of Filter Should I Use?

This question is both simple and difficult to answer. Simply put, you want the fastest filter you can aquire. For small personal use, a 600mL fritted disc Buchner Funnel will work fine. For larger amounts, a porcelain, polypropelene, or stainless steel filter such as our BVV Refinement Filter are recommended. As described in the paragraph above, a combination of all three speeds of filter paper will work most efficiently. You should also use some type of filtration aide. The most common is Celite 545. This will allow the mixture to flow at a constant speed, as well as create a vacuum seal across the whole surface of the funnel.

Filtering

Prior to filtering, if you have activated carbon, do a basic carbon scrub by filling your media bottle with activated carbon and shaking for 1-5 minutes. To prepare Buchner Funnel for filtering, place filter paper in bottom of filter and secure with ring if using a stainless filter. Create about a half inch to inch of filter aide on top of filter paper. You can also make another 2-3 inch layer of carbon on top of the filter aide if you'd prefer to pour the solution over the carbon rather than shaking it in a media bottle. Start vac pump and slowly pour solution into filter. Try to spread liquid evenly across the whole diameter of the filter.

Alcohol Recovery via Rotovap

Once you have filtered your solution, discard fats and waxes. You can reuse filter aide by rotovaping it down but this will only work for a few uses as it does not have an infinite lifespan. Begin a rotovap procedure and reduce your solution down so that there is as little alcohol in it as possible. You might need to leave a bit of alcohol in the mixture to transfer it.

Degassing

Once you have reduced your solution and recovered your alcohol, transfer your solution to a new Ball Jar or stainless steel vacuum chamber. For this example we will use a 1.5 Gallon Glass Vac. The glass lid has the best chemical resistance. If you use any other type of vacuum chamber, the lid may suffer damage from harmful degassing vapors. Place 1.5 Gallon Glass Vac on hot plate and connect to Cold Trap. Degassing will make quite a smell so it is recommended to do this under a fume hood or outside. Begin heating mixture under no vacuum. You may do this without a closed chamber or cold trap but it is recommended to have a fan blowing air over the top of the vessel to keep vapors from condensing and falling back into solution if you are not inside a fume hood. Heat the mixture to 140C. This should be a slow heat that makes the solution slightly bubble or foam. During this process you are removing solvents, unwanted compounds, and nasty terps. Once solution hits 140C, pull the vessel from the hot plate and transfer to distillation system.

Advanced Winterization

Depending on first or second pass material, you may consider repeating this process again to further refine oil or distillate. There are other chemicals that can be used to pull unwanteds from the solution. These include hexane, pentane, salt water or saline, etc. Each of these chemicals has a certain polarity and will pull residual unwanteds such as water soluble pesticides. The use of a separatory funnel will greatly add in this process. These chemicals are highly flammable and advanced winterization should only be attempted by extremely well versed indivduals with proper safety protection.

https://www.bestvaluevacs.com/blog/w...-distillation/

[cheezhead]

Thanks for that SkyHighler, as I've noticed that there are some posts in the cannabis concentrate sections with some old info. From 2010 to today we know a LOT more! Thanks for semi-updating the post.

[anasrzi]

What a invaluable thread, nice work to all involved in its creation, it's already answered a good number of questions I had, some amazing images too.

I do have one more question however, I make a good deal of bubble as I grow outdoors every year so I have a good supply of trim and air bud to work through. So I brought a set of bubble bags, 220u tea bag for all the trim and a camping washing machine to process sit all. My question is can I simply dissolve the bubble (as a powder, once dry) into a thermos of butane?

If so what kind of contact time would I need? Bearing in mind there isn't any or little green matter to consider.

Also a quick question about winterising using ethanol, is there a certain amount you need to use in order to scrub the fats out properly or is it just enough to re melt the bho and keep it good for 24-48 hours?

[Gray Wolf]

Originally Posted by anasrzi

What a invaluable thread, nice work to all involved in its creation, it's already answered a good number of questions I had, some amazing images too.

I do have one more question however, I make a good deal of bubble as I grow outdoors every year so I have a good supply of trim and air bud to work through. So I brought a set of bubble bags, 220u tea bag for all the trim and a camping washing machine to process sit all. My question is can I simply dissolve the bubble (as a powder, once dry) into a thermos of butane?

If so what kind of contact time would I need? Bearing in mind there isn't any or little green matter to consider.

Also a quick question about winterising using ethanol, is there a certain amount you need to use in order to scrub the fats out properly or is it just enough to re melt the bho and keep it good for 24-48 hours?

Extraction time should be less than 5 minutes with agitation.

48 hours at -18C/0F works. A couple of hours at -50C.

I've just set the solution aside at ambient and a month later this is what precipitated out.

[anasrzi]

thanks gray wolf for the info, sounds like a plan. Is there a exact amount of ethanol needed for winterizing the extract at all or is it about time spent in the solution?

[Gray Wolf]

Originally Posted by anasrzi

thanks gray wolf for the info, sounds like a plan. Is there a exact amount of ethanol needed for winterizing the extract at all or is it about time spent in the solution?

We use about 10:1.