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EDDIEKIRK

 

CANNABINOID CARBOXYLIC ACIDS THCA AND CBDA: THEIR POTENTIAL FUNCTIONS, APPLICATIONS, AND METHODS OF EXTRACTION
 

Wowza!  Look what Dr Kate has been up too!

 

Introduction to a cold extraction method for hash oil that preserves carboxylic acid form of cannabinoids THC and CBD

 

By Kate Welch, Pharm.D

 

http://skunkpharmresearch.com/cannabinoid-carboxylic-acids-thca-and-cbda-their-potential-functions-applications-and-methods-of-extraction/

 

 

Source: CANNABINOID CARBOXYLIC ACIDS THCA AND CBDA: THEIR POTENTIAL FUNCTIONS, APPLICATIONS, AND METHODS OF EXTRACTION

EDDIEKIRK

CANNABINOID CARBOXYLIC ACIDS THCA AND CBDA: THEIR POTENTIAL FUNCTIONS, APPLICATIONS, AND METHODS OF EXTRACTION

 

Wowza! Look what Dr Kate has been up too!

 

Introduction to a cold extraction method for hash oil that preserves carboxylic acid form of cannabinoids THC and CBD

 

By Kate Welch, Pharm.D

 

http://skunkpharmresearch.com/cannabinoid-carboxylic-acids-thca-and-cbda-their-potential-functions-applications-and-methods-of-extraction/

 

Source: CANNABINOID CARBOXYLIC ACIDS THCA AND CBDA: THEIR POTENTIAL FUNCTIONS, APPLICATIONS, AND METHODS OF EXTRACTION

EDDIEKIRK

For those of ya'll romancing a fire marshal, it may help to look at things from his perspective, to understand his motives and what he will be considering.

 

Starting with motives, he is an official paid to protect people and property, and keeps his job if he does a reasonable job of doing so, regardless of any deep love of mankind he embraces as a bonus.

 

Besides citizens and property, he also has to be concerned with the safety and welfare of his own men fighting a fire, should one occur, as well as traffic snarls and repercussions.

 

I retired about a decade ago from working regularly with fire marshals and permiting officials, but what I found is that they are trained to find what is wrong with this picture, and know the regulations chapter and verse.

 

There will always be some pathology amongst the populous, some of which will seek employment in an empowering position, but by the time a person reaches the status of fire marshal, they usually have the experience and respect of their men and superiors, as opposed to being a clerk, who will never rise above being in charge of the front thwart-the-public-desk.

 

I personally found that turning into a friendly ghost is always the best policy.

 

Friendly means treating them/their position with respect and not losing your cool when they thwart you, and turning into a ghost means not trying to outsmart them, so they don't trust you and put you under a microscope as a snake.

 

Lots of snakes, so with them under the microscope, brothers and sisters doing what they say they are going to do, fall out of focus and slide smoothly through.

 

I also found that if you use them as a resource, by involving them early on with a quick conceptual plan review, that there were fewer surprises later on, when changes are expensive to fix.

 

At any rate, here is a partial list of the NFPA standards worthy of reading, to better understand where the fire marshal will be coming from:

 

Code No**Code Name

NFPA 1 Fire Code

NFPA 3 Recommended Practice for Commissioning of Fire Protection and Life Safety Systems

NFPA 4 Standard for Integrated Fire Protection and Life Safety System Testing

NFPA 10 Standard for Portable Fire Extinguishers

NFPA 12 Standard on Carbon Dioxide Extinguishing Systems

NFPA 12A Standard on Halon 1301 Fire Extinguishing Systems

NFPA 13 Standard for the Installation of Sprinkler Systems

NFPA 13 E Recommended Practice for Fire Department Operations in Properties Protected by Sprinkler and Standpipe Systems

NFPA 14 Standard for the Installation of Standpipe and Hose Systems

NFPA 15 Standard for Water Spray Fixed Systems for Fire Protection

NFPA 16 Standard for the Installation of Foam-Water Sprinkler and Foam-Water Spray Systems

NFPA 22 Standard for Water Tanks for Private Fire Protection

NFPA 24 Standard for the Installation of Private Fire Service Mains and Their Appurtenances

NFPA 25 Standard for the Inspection, Testing, and Maintenance of Water-Based Fire Protection Systems

NFPA 30 Flammable and Combustible Liquids Code

NFPA 45 Standard on Fire Protection for Laboratories Using Chemicals

NFPA 55 Compressed Gases and Cryogenic Fluids Code

NFPA 56 Standard for Fire and Explosion Prevention During Cleaning and Purging of Flammable Gas Piping Systems

NFPA 58 Liquefied Petroleum Gas Code

NFPA 59A Standard for the Production, Storage, and Handling of Liquefied Natural Gas (LNG)

NFPA 67 Guide on Explosion Protection for Gaseous Mixtures in Pipe Systems

NFPA 69 Standard on Explosion Prevention Systems

NFPA 70 National Electrical Code®

NFPA 70E Standard for Electrical Safety in the Workplace®

NFPA 77 Recommended Practice on Static Electricity

NFPA 79 Electrical Standard for Industrial Machinery

NFPA 91 Standard for Exhaust Systems for Air Conveying of Vapors, Gases, Mists, and Noncombustible Particulate Solids

NFPA 220 Standard on Types of Building Construction

NFPA 221 Standard for High Challenge Fire Walls, Fire Walls, and Fire Barrier Walls

NFPA 290 Standard for Fire Testing of Passive Protection Materials for Use on LP-Gas Containers

NFPA 329 Recommended Practice for Handling Releases of Flammable and Combustible Liquids and Gases

NFPA 386 Standard for Portable Shipping Tanks for Flammable and Combustible Liquids

NFPA 496 Standard for Purged and Pressurized Enclosures for Electrical Equipment

NFPA 497 Recommended Practice for the Classification of Flammable Liquids, Gases, or Vapors and of Hazardous (Classified) Locations for Electrical Installations in Chemical Process Areas

NFPA 791 Recommended Practice and Procedures for Unlabeled Electrical Equipment Evaluation

 

 

 

Source: Some National Fire Prevention Association standards the fire marshal considers:Some National Fire Prevention Association standards the fire marshal co

EDDIEKIRK

Oil and fat extraction is a method we'uns will be further developing, so watch this thread.

 

Cannabinoids and the other terpenes in cannabis, are readily dissolvable in fats and oils, so fats and oils may be used for both extraction and as a menstruum.

 

When I say fats and oils, I am referring to the vegetable and nut oils, as well as clarified butter. Oils tasty enough that may be ingested with a dropper, mixed with drinks, or used in medibles.

 

Water solubility varies, but one of the advantages of using oil for extractions, is that they are for the most part non soluble in water, so they don't extract excessive water soluble constitutes, like chlorophyll.

 

There are practical limits to the potency that can be achieved extracting with oil, because as the oil becomes saturated with cannabis terpenes, they become less concentrated and their solvent action slows down to a crawl, before stopping altogether.

 

Potency can be ratcheted up somewhat through using the same oil to do multiple extractions of fresh material, but even that has limitations.

 

A key factor in achieving maximum removal rates and efficiency, is keeping the boundary layer between the un-dissolved resins and the unsaturated oils used for extraction regularly removed. The method that we used in this experiment, was simple, but through periodic stirring.

 

Sublingual oil tinctures:

 

Aside for their useful role in extraction, oils and fats may be mixed at any ratios with cannabis terpenes, if you are just mixing them together as oils. Some of them are damn tasty even taken from a dropper, though as the concentration increases, the flavor becomes less fetching and it leaves more of a lingering aftertaste.

 

Choose an Oil:

 

We haven't tried them all, but we have tried Almond, Avocado, Butter, Canola, Coconut oil, Grape Seed oil, Olive, Pecan, Sesame, and Walnut oils. They all work well, so they are a good place to start, if you are new to extraction.

 

Preparing the material:

 

We first start by drying the trim. For the most floral flavor and the highest amount of lighter terpenes, material that is hung until it reaches the small stem snap stage is best for our purposes.

 

In our experience, for best flavor and taste, freshest material works best. Older cured material loses the nuances of the floral undertones and just tastes like hash.

 

That means that the degree of drying and curing is also critical, if your goal is to maintain maximum terpene content. Not that hash has a bad flavor, but it should be a conscious choice.

 

Choosing material:

 

Oil from buds is tastier than oil from even sugar trim, because most of the terpenes are produced by the buds, and that is where they are the most plentiful. Tasty is usually not a word used to describe oil from fan leaves or stems, though effective may be.

 

The material that we used in this experiment, was donated sweet trim from Chocolate and was well dried and cured.

 

Oils used in this experiment:

 

We used Ghee (clarified butter), Coconut oil, Grape Seed oil, and Olive oil for the run, because they are commonly available and inexpensive.

 

Making Ghee:

 

To make the Ghee, we melted unsalted butter and cooked it at low temperature, until the butter fats separated from the Ghee. We then skimmed off the floating butter fats, and sucked off the Ghee, using a turkey baster, leaving the heavier butter fats in the bottom of the pot.

 

Most recipes for extraction with butter call for boiling them material in water and butter, but we studiously avoid adding water and our Ghee extraction has only the lightest tinge of green and no chlorophyll flavor.

 

Here are the three extractions taken out of the refrigerator, where they were stored between cooking and actual pressing. Note that the butter, olive oil, and the coconut extractions have a slightest green tinge, yet none actually had a chlorophyll flavor.

 

In this experiment, we didn't attempt to reach maximum saturation, but to determine what was reasonable to expect from a single batch. To reach maximum saturation, we would have simply processed more than one batch of fresh material through the oil.

 

What we did, was fill four jars 3/4 full of the trim and then added enough oil to cover it, stirred it thoroughly, and then added another inch of oil.

 

We then lightly capped the jars and set them in pot of hot water and simmered it on low for six hours, uncapping and stirring thoroughly a couple of times an hour.

 

At the end of six hours, we removed the jars from the hot water and set them aside to cool. The next day, we cooked them two more hours, stirring regularly, and the third day we cooked them another six hours, for 14 hours total, with three heat cycles.

 

Lightly capping means snug enough to allow some pressure to build, but loose enough to vent off anything excessive. Since we used cured material and didn't add water, there were little in the way of volatiles to boil off and produce pressure.

 

I left the lid off the boiling pot, so as to not force steam into the jar head space.

 

For pressing, we warmed the oils and ghee up by placing them in boiling water, this time with the lids on tight and the lid on the pot,

 

Next we cut up some rags from some surplus drape material, with approximately a 160/200 thread count, and draped it over a restaurant sized potato ricer that we scored at Hongs Restaurant Supply in Portland. By pressing it down into the potato ricer, it formed a pocket that holds approximately a quart of plant material.

 

Folding the cloth over and pressing it, produced a pristine clear oil, which was tasty enough to dropper.

 

The most flavorful, was the ghee, and possibly the fastest to uptake and produce an effect. Alas, after just testing just enough of each of them to determine their flavors, I needed a nap, so the next phase of this project, is to titrate for potency and effect, as well as flavor, using volunteer test panels.

 

We also will experiment with different ways to use the oils in medibles, so I will update this post as they occur:

 

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Copied from:

 

http://skunkpharmresearch.com/extracting-with-oils-and-fat

 

 

 

Source: Extracting With Oils and Fats

EDDIEKIRK

Kosher vegetable glycerin is an effective method for extracting cannabis concentrates directly from the plant material and produces a tasty medication that is easily ingested directly orally, or mixed with drinks and food.

 

Glycerin is a heavy, syrupy clear liquid sugar alcohol that has approximately 60% of the sweetness of sucrose, and about the same food value.

 

It is however not actually a true sugar and is often used as a sugar substitute, as diabetics are often able to use it without experienced the blood sugar rollercoaster they suffer with sucrose or other sugars.

 

Glycerin makes an extremely tasty and provocative cannabis tincture, that when made using cold extraction methods, is reminiscent of wild honey, as it preserves all the individual flavors, so that they dart off in all directions simultaneously.

 

Hot glycerin extraction also makes a tasty tincture, with the flavor more resembling a fine soup, where the individual flavors are married into one overall flavor. While not as whimsical and provocative as a cold extraction, it can be prepared start to finish in a couple days, where cold extractions take a minimum of 60 days and are commonly soaked for 120 days or longer.

 

Many of the provocative flavors and odors from cannabis are aromatic terpenoids, and the reason that they are aromatic in the first place, is that they give off molecules at room temperature.

 

Heating speeds up the rate that the accompanying terpenoids and other aromatics are vaporized off, so many are collateral damage in a hot extraction and are lost.

 

The glycerin molecule is actually only a three carbon molecule chain, with three hydroxyl groups (OH) attached, and as hydroxyl groups are hydrophilic, glycerin is hygroscopic (absorbs water) and dissolves readily (miscible) in water.

 

It has a flash point of approximately 177C (351F), and a boiling point of 290 °C (554°F).

 

It is relatively non toxic. The MSDS tells us that the LD50 Oral rat dosage is 12,600 milligrams per kilogram of body weight, which is approximately 5.7 grams per pound of body weight, or 36 ounces for a 180 pound male.

 

By comparison, acute oral toxicity (LD50) Oral Rat for sucrose sugar is 29700 mg/kg and about 7060 mg/kg for ethyl (grain) alcohol.

 

At saturation, Glycerin only hold as 33% as much cannabis oil as the same volume of ethyl (grain) alcohol, so about three times more is required per dose.

 

To reach maximum saturation however, requires processing more than one batch of fresh material through the glycerin, because as the saturation level increases, the glycerin becomes less aggressive as a solvent and the partially dissolved cannabis boundary layer interface with the solvent is also no longer at full strength and as reactive.

 

To keep the reaction from slowing to a snails pace, or even stopping, some method must be used to keep removing this stagnant layer and refreshing the boundary between the solvent and resin.

 

In addition heat dramatically affects resin dissolution rates. The hotter it is, the faster it works, up to the point of overheating.

 

As glycerin is usually used as an oral med, we also need to consider decarboxylating the cannabinoids so that they are orally active.

 

If not in excess, some water solubles add to the flavor of a glycerin tincture, and taking all of the water out of the material before processing it, makes it frangible and prone to breaking into small fragments that may be hard to remove.

 

Let's look at how these four variables can be manipulated to produce delicious and effective glycerin tinctures.

 

Drying and decarboxylation:

 

Plant material is typically dried to around 10/15% water content by weight for smoking and vaporizing purposes, which is low enough to make some delicious glycerin, but for those who prefer less water solubles in their glycerin tincture or wish to decarboxylate the material before extracting, you may add a drying and/or decarboxylation step.

 

To simply remove most of the remaining moisture, I place the plant material on a cookie sheet in a 200F oven and turn it, until it is frangible when I roll it between my finger and thumb.

 

At that point it is ready for extraction, but if you also wish to decarboxylate the plant material before making your tincture, you can then crank up the oven to 250F and after it stabilizes at the higher temperature, replace the plant material in the oven and hold it at temperature for approximately 30 minutes

 

That will add a roasted flavor to the tincture and many of the turpenoids will be lost, but it will decarboxylate approximately 70% of the existing carboxylic acids into their non acid orally active form.

 

An alternative to decarboxylating the material ahead of time, is to do it after the extraction is complete and the plant material has been filtered out. That eliminates the roasted flavor and preserves more of the turpennoids.

 

Using Temperature:

 

Elevating the temperature of the glycerin increases the rate of dissolution of the resins, especially if you raise the temperature high enough for the resins to be molten. THC, CBD and CBN are all molten at just under 180F, so we operate at that temperature.

 

The advantage of using as low a temperature as possible, is that fewer aromatic terpenoids are boiled off at that low a temperature, and it decarboxylates more slowly, so that the process doesn't pass the peak of the decarboxylation curve and start down the other side toward low THC and high CBN. As previously noted, we can finish the decarboxylation later.

 

Keeping the boundary layer removed:

 

The boundary layer is the layer of partially reacted resin and dilute solvent that forms on the surface of the resin after the initial aggressive dissolution by the solvent. The solvent at that point is dilute, as is the resin concentration, so that the reaction slows or grinds to a halt.

 

To keep the reaction operating at a reasonable rate, we need to periodically or continuously remove that boundary layer, and there are four methods that I will present here.

 

The first is to stir. Simply stir gently and thoroughly with a wooden spoon

 

The second is to shake. Simply shake a jar of glycerin and plant material by hand regularly. A paint shaker would also work for this application.

 

The third is to tumble. Placing the jar of glycerin and plant material in a rock or photo film tumbler will keep the boundaries fresh. It is an effective and gentle way to speed up the process.

 

The forth is vibration. Placing jar of glycerin and plant material in a vibratory cartridge case cleaner, or other form of vibration, creates more shear energy that tumbling and will dissolve the material the fastest of any method we have tried thus far.

 

Material selection and preparation for hot or cold processing:

 

While glycerin tincture can be made from anything from prime bud to stems, it is tastiest done from prime bud and least tasty with the stems. I usually make glycerin tincture out of the sweet trim removed from the buds during manicuring and popcorn buds.

 

It is not necessary to grind up the material, only to break it up any buds so that the material is loose enough for the glycerin to reach all the surfaces. Excessive pulverization of the material will result in color and particulate pickup that is difficult to remove. If you leave some surfaces blinded however, the resins on those surfaces won't be removed either.

 

Extracting using the cold process:

 

The cold process is the easiest and tastiest way to make glycerin tincture. We extract using the cold process, simply by soaking the plant material in glycerin at ambient temperatures and agitating it for sixty days or more. Sixty days is about the least amount of time for a cold extraction, and typically they are run 90 to over 120 days. I have one experiment with more than 365 days of soak time.

 

After the extended soak and agitation, the glycerin is poured off and pressed out of the plant material to yield quality and tasty tinctures. It can also be used with fresh material for another cycle, so as to build up more potency.

 

There are a number of ways to press out the glycerin from the plant material, and it applies to both cold and hot extraction, so I will cover that in a separate discussion at the end of extraction methods.

 

The way that I make cold process glycerin tincture, is to load a canning jar 2/3'ds full of plant material, lightly compacted and then cover with glycerin while stirring with a wooden spoon, until every surface is well coated and mixture is homogenous, and then add another inch of glycerin on top.

 

I place the jars in a cool dark place or cover to exclude light. I sometimes wrap jars with aluminum foil to exclude light.

 

Every day for the soak period days, I periodically agitate the jars, using one of the above methods and at the end I filter out the plant material for a a light golden to dark amber glycerin tincture, that is tasty and of high quality.

 

Because the aromatic terpenoids are preserved, it will have many flavors present, interacting and darting off in all directions simultaneously.

 

You can more easily filter the mixture if you warm it up to 150F or so before filtering.

 

Potency and gleaning:

 

As previously noted, to reach maximum saturation, requires processing more than one batch of fresh material through the glycerin, because as the saturation level increases, the glycerin becomes less aggressive as a solvent and the remaining partially dissolved cannabis is also no longer at full strength and as reactive.

 

In point of fact, the fresh pressed material from the above first cycle will still contain significant cannabinoids, which takes two to three cycles to get it all.

 

What I do is put the fresh pressed plant material back in the jar and refill with fresh glycerin and add fresh material to the freshly pressed glycerin for another cycle, if I desire more strength.

 

The fresh glycerin will do the best job of scavenging the remaining cannabinoids, and then can be used again with fresh material to further build up its potency. It is by this cascading technique, that we can leave little behind and yet still maintain quality and potency.

 

I should note that the most potent glycerin tincture is not necessarily the most tasty, and one cycle produces effective meds, so most of the time we do not bother to bump up the potency with cold tincture.

 

Hot glycerin extraction:

 

We prepare plant material and extract cannabis by the hot glycerin extraction process in much the same way as we do by the cold process, though we stir it instead of shaking, tumbling, or vibrating it.

 

We also use a thermal cycling process and stir regularly, rather than an extended cook as many processes call for. The expansion and contraction of the thermal cycling help break up the resins so that they dissolve more readily.

 

As with cold tincture, I load a canning jar 2/3'ds full of plant material, lightly compacted and then cover with glycerin while stirring with a wooden spoon, until every surface is well coated and mixture is homogenous, and then add another inch of glycerin on top.

 

I then set that jar in an electric fondue pot full of hot Canola oil at 200F, and stir it regularly with a wooden spoon until the mixture reaches 180F, and then I adjust the pot temperature controls to maintain 180F.

 

I stir the mixture regularly with a wooden spoon, for another thirty minutes, and then I take it out of the hot oil and allow it to cool to ambient temperature.

 

For what it's worth, I use a wooden spoon, because a light tink with a metal spoon against a hot glass jar while stirring, can break it and dump the whole mixture into the hot oil.

 

After the mixture has cooled to room temperature, I again place into 200F oil and bring it back up to 180F while stirring regularly. When it reaches 180F, after a through stir, I take it out of the hot oil and let it cool to ambient temperature again.

 

I repeat the last step about five more times and after the last cook and stir, I filter out the plant material while the mixture is still hot.

 

Filtering glycerin tincture:

 

Vegetable glycerin is thick and syrupy, so it doesn't filter quickly or easily without mechanical help. The simplest way to filter it is to heat it up so that it isn't so viscous, and pour it into a jelly bag, which you wring out by hand. That works, but leaves a lot of glycerin behind and you are limited to temperatures that you can handle with your hands.

 

A French coffee press, a potato ricer, or a jelly press can also work, and you can buy tincture presses used by the botanical extraction industry.

 

I made my own press, using a hydraulic bottle jack inside a scrap metal frame, which presses a filter bag between two stainless dog dishes, at a force of 12,000 psi, and catches the glycerin in a third stainless dog dish.

 

It presses the plant material into a hard little puck, that I have to break up to reprocess.

 

Flavoring glycerin tincture:

 

A well made glycerin tincture is a taste delight in its own right, but for those of ya'll who just like to play, here is how I've flavored glycerin that I had already infused with cannabis oil.

 

I started by adding equal parts of Bing Cherry and Blueberry raisins in a blender with enough 190 proof grain alcohol to make a soupy paste when macerated by the blender.

 

I tossed in half as much Japanese Gari and a dash of Almond extract, added another half a cup of 190 proof, and let it blend well.

 

When pureed, I poured it into a stainless mixing cup and placed it in a 180F hot oil bath. I cooked and stirred it until all the alcohol was gone, and then removed it to cool.

 

I then put a bout two tablespoons of that concentrate into each quart of infused glycerin to be flavored and place it in the 180F oil to cook for thirty minutes while stirring regularly.

 

At that point I remove it from the oil, filter out the concentrate using a filter bag and the glycerin press. The glycerin is delightfully flavored, and the chef gets to eat the concentrate from the filter bag! Ahwooooooooooooooooooooooooooooooo!!!!!!!!!! Hee, hee, hee....................

 

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Make an account now and ask us questions or just read more about extractions, (Free)

 

Source: Vegetable glycerin extraction:

EDDIEKIRK

To perform some of the desirable alchemy with cannabis essential oils, requires some sort of vacuum chamber that you can control the heat and vacuum levels in, as well as see what you are doing.

 

These are readily available as vacuum desiccators and vacuum ovens, but all are pricey, so how about just building your own?

 

We already have a glass desiccator with a hot plate inside, and picked up a new used vacuum oven, but alas the temperature controls are ineffective in the low ranges that we operate, so we are in the process of refining its controls.

 

More on that subject on a separate thread, but this thread is to show how we punted when the vacuum oven capacity that we had counted on, eluded us, with meds to process backlogged.

 

To that end, we used a old 22 quart Mirror pressure cooker that was gifted to us, and after removing the gasket, we tossed the lid.

 

I then drilled a 1/4" pilot hole through the side wall wrapper, about 2.5" below the top flange, followed by a 3/4" bit, to enlarge the hole to fit a 1/4" NPT brass bulkhead fitting.

 

I then inserted the bulkhead fitting through the side wall from the inside out, installing a gasket on the inside flange, and tightening the nut and lock washer on the outside of the pot.

 

To this I added a close nipple, a cross, with two 1/4" ball valves, and two 1/4" MPT to 1/4" flare refrigeration hose fitting. One for the vacuum pump and the other for the vacuum gauge hose.

 

As it is temporary, and we needed it immediately, we reused the existing gasket, and made a new lid out of a 1" X 16" acrylic plate. At -29.9" Hg gauge, there is about 1/16" lid deflection in the middle, so a thicker plate would be better to reduce high cyclic fatigue.

 

If it were permanent, we would have a new Viton gasket cut by Paramount, or Gaskets Unlimited and use 1 1/2" polycarbonate, for the lid.

 

Hee, hee, hee, after telling me that they didn't have any, and after having them cut the 1" acrylic plate, I found a 22" X 29" X 1 1/2" Polycarbonate remnant at Multi Craft Plastics, which I scored for $72. It has one 6" hole in one corner, but that is $2/lb for bullet proof polycarbonate panels, like those used at teller windows. Snicker, snark, snort, more projects to come!

 

Here are pictures showing how we made and how it turned out. We are able to easily control the temperature with an outside hotplate and reduce the pressure to -29.9 with one of our 6.2 cfm single stage AC vacuum pumps:

 

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Join us free on site and ask questions.

 

 

Source: DIY Vacuum Purging Chamber

EDDIEKIRK

Public opinion appears to be split on the salubriousness of including chlorophyll and other plant water solubles in our extracted oils, so this is written not to stir controversy, but specifically for those of ya'll whom do not wish ingredients other than cannabis in your extracts.

 

Those whom wish to preserve those ingredients are invited to please ignore this posting, rather that debating whether it is a mistake or even a crime against sweet Mary's natural wholeness.

 

In a nutshell, many of those non cannabinoid ingredients came along for the ride because there was water present and they are water soluble. It is easier to use a process that minimizes their extraction in the first place, but what if that is a moot point, because you already have an extraction with excessive non-active ingredients and wish to remove them?

 

Next best to a process that doesn't pick up many water soluble ingredients, is one to take them out, so let's talk about a couple processes that we use at skunk pharm:

 

If the extraction just needs final polishing, we may simply re-dissolve it in 190 proof (~95.5% azeotropic) ethanol and stick it in the freezer overnight at 0F, for the waxes to coagulate and the excess water solubles to precipitate out.

 

We then carefully decant and filter the alcohol mixture, to remove the coagulated waxes, as well as the chlorophyll, and plant alkaloids which precipitated out as sludge in the bottom of the container.

 

We routinely use this step to clean up extractions using Isopropyl or Methanol, because they are far more aggressive than ethanol in stripping everything, and much of the non active ingredients fall out when re-dissolved in hot ethanol and subjected to the above step.

 

It also works well to remove the minor water solubles picked up in a butane extraction, but has its limitations because alcohol is polar and 190 proof is still almost 5% water.

 

As far as filtering, I prefer a 0.45 micron or a 0.2 micron syringe filter, but got good results with a coffee filter until Joe turned us on to syringe filters. We have picked both the syringes and filters up off of E-bay, as well as from our local scientific supply store.

 

Now, if we really need to clean up an extraction, we have had good results by re-dissolving the oil in a hot highly non-polar solvent such as hexane and repeatedly washing the solution with saturated salt water until it is mint quality.

 

You can even skip the re-dissolve step, by just mixing the alcohol extraction with the highly non-polar solvent before evaporating it off, and the alcohol will leave with the first water wash, after the non-polar solvent has stolen away sweet Mary's succulent and titillating charms.

 

Salt water washing is easy, easier with a separatory funnel, but you can even do it with a few gallon Ziploc bags in pinch, or any number of ways to siphon off, blow off, etc., to achieve that purpose.

 

To use a Ziploc bag, simply hang by one corner, and clip off the lower corner to drain, pinching to control flow and shut off point. Note that low density polyethylene and Hexane are not compatible long term, showing effects after 7 days of constant exposure.

 

The way we do it is to start out by making four or five liters of saturated salt water in glass (or ceramic) containers, by mixing sodium chloride (table salt) in hot tap water with a hand mixer until no more will dissolve. We buy the salt cheap by the bag, using salt intended for water softener use.

 

The magic trick is that because the saturated salt water readily accepts the alcohol, but no longer has any room for the water solubles due to its salt saturation, they fall out of solution and are filtered off in bottom sludge or left stuck to the sides of the funnel.

 

The rest of the magic is just as predictable when you mix the polar solvent holding sweet Mary's charms and the lustful non-polar solvent that covets them deeply, given that because of her own polarity, sweet fickle Mary herself lusts after the new suitor, so participates willingly and with a passion.

 

The alcohol and water are left giggling like idiots and the sludge is probably left puzzled.

 

To perform the salt water wash of the hexane mixture, simply pour the salt water and hexane into the separatory funnel together in about equal parts and shake well, before allowing the mixture to separate out into layers.

 

After carefully bleeding off the bottom layer of water, alcohol, and sludge, we replace the salt water that we bled off and shake up the mixture again to mix well. After bleeding that salt water, et al, again, and repeating the procedure several times, the hexane mixture becomes pristine and bell clear.

 

At that point we stop washing and evaporate off the hexane. While we use HPLC grade hexane from the local science store, light naphtha will also work for this process, but get the MSDS sheet to see what it actually contains, as light naphtha designation only states that it boils between 30C and 100C. Some is Hexane and Pentane, while others contain things like Benzene, which also boil in that range.

 

To get rid of the hexane, we first evaporating off the visible liquid hexane, and then add 190 proof ethanol to the extracted oil and boil that off. We repeat that procedure several times, until there is no discernible taste or odor of hexane left.

 

That means that the remaining hexane is below about 130/22 ppm, which is (~) our sensory threshold perception level. What does that mean as far as our health means?

 

For starters, because it is a simple Alkane and relatively non toxic, hexane is used extensively in food extraction, but should not be viewed as being as salubrious as mother's milk.

 

The first clue of course, is that it doesn't come in nearly as attractive a container, and the second is the MSDS information which tells us, that in excess, N-Hexane attacks our nervous system.

 

OH MAHGAWD, but do check out at what levels this is so and note that oxygen in a breathing atmosphere greater than 75% pure will kill us dead! Poison is in the dosage, so leave us please keep N-Hexane's potential nature in perspective, which includes never losing sight of it!!!!!!

 

Despite our worst terrors, a review of the hexane Material Safety Data Sheet shows that the oral rat LD50: is relatively high at 25000 mg/kg. At that rate it would be the equivalent of about 4.5 pounds to kill 50% of a population of 180 lb men.

 

http://www.sciencelab.com/msds.php?msdsId=9927187

 

Section 8: Exposure Controls/Personal Protection

 

Engineering Controls:

 

Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective

threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location.

Personal Protection:

 

Safety glasses. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves (impervious).

 

Personal Protection in Case of a Large Spill:

 

Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing apparatus should be used to avoid

inhalation of the product. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this

product.

 

Exposure Limits:

TWA: 500 (ppm) from OSHA (PEL) [united States] Inhalation TWA: 1800 (mg/m3) from OSHA (PEL) [united States] Inhalation

TWA: 176 (mg/m3) from ACGIH (TLV) [united States] SKIN TWA: 50 (ppm) from ACGIH (TLV) [united States] SKIN TWA:

500 STEL: 1000 (ppm) from ACGIH (TLV) [united States] Inhalation TWA: 1760 STEL: 3500 (mg/m3) from ACGIH (TLV)

[united States] Inhalation Consult local authorities for acceptable exposure limits.

 

Section 11: Toxicological Information

Routes of Entry: Absorbed through skin. Dermal contact. Inhalation. Ingestion.

Toxicity to Animals:

WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. Acute oral

toxicity (LD50): 25000 mg/kg [Rat]. Acute toxicity of the gas (LC50): 48000 ppm 4 hours [Rat].

Chronic Effects on Humans:

MUTAGENIC EFFECTS: Mutagenic for bacteria and/or yeast. May cause damage to the following organs: peripheral nervous

system, skin, central nervous system (CNS).

Other Toxic Effects on Humans:

Very hazardous in case of ingestion, of inhalation. Hazardous in case of skin contact (permeator). Slightly hazardous in case

of skin contact (irritant).

Special Remarks on Toxicity to Animals: Not available.

Special Remarks on Chronic Effects on Humans:

May cause adverse reproductive effects based on animal data. May be tumorigenic based on animal data. May affect genetic

material. Passes through the placental barrier in animal.

Special Remarks on other Toxic Effects on Humans:

Acute Potential Health Effects: Skin: May cause mild skin irritation. It can be absorbed through the skin in harmful amounts.

Eyes: May cause mild eye irritation. Inhalation: May be harmful if inhaled. Inhalation of vapors may cause respiratory tract

irritation. Overexposure may affect, brain, spinal cord, behavior/central and peripheral nervous systems (lightheadness,

dizziness, hallucinations, paralysis, blurred vision, memory loss, headache, euphoria, general anesthetic, muscle weakness,

numbness of the extremeties, asphyxia, unconciousness and possible death), metabolism, respiration, blood, cardiovascular

system, gastrointestinal system (nausea) Ingestion: May be harmful if swallowed. May cause gastrointestinal tract irritation

with abdominal pain and nausea. May also affect the liver, blood, brain, peripheral and central nervous systems. Symptoms of

over exposure by ingestion are similar to that of overexposure by inhalation.

 

Don't take that as a suggestion to drink the stuff, as government hygienists have determined that the Acute Toxicity of the gas (LC50 rat): was 48000 ppm using 4 hours exposure data and the Threshold Limit Value for an 8 hour weighted average in breathing air is 500 ppm with a Permitted Exposure Limit of 1800 mg/M3 (~ppm).

 

Besides NIOSH, we also have U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER) regulating what you can use and what you can leave behind:

 

http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/ucm073395.pdf

 

They list n-Hexane as a class two solvent with 290 ppm concentration limits, and a total PDE of 290 mg/day.

 

The good news is that if you are out of the stink or taste, you are less than about .01% of TLV, but the bad news (?) is that although it is relatively non toxic, hexane still tastes like lighter fluid below toxicity levels, with our sensory threshold far below the Threshold Limit Value.

 

Not an unexpected taste treat, because as many of ya'll know, lighter fluid is in point of fact primarily a blend of pentane (5 carbon atom chain) and hexane (6 carbon atom chain).

 

Most of skunk pharm oil goes into oral or topical medications, though some is vaporized. Both the oral and the vaporization applications require residual hexane below human discernable (threshold) perception levels, so out of practicality, we standardized on zero perceptible solvent content on all our oils as just a matter of policy.

 

Lawrd knows that there are enough people kissing and licking at least some of the more provocative foxes and hunks in our folds all over, that we voted to use the same taste standard for topicals as orals.

 

The last issue, is of course residue and color, when using topicals! Besides undesirable taste, and non-active bulk in your extractions, there is the pregnant issue of how much residue they leave behind on the skin and how badly they stain our clothes.

 

Yet another reason to take care in extracting and subsequently processing our topicals, despite the ostensible threshold perception standards being lower.

 

We could also add that after we have removed the bulk of the non-active ingredients, our oil is more uniform and so our mixing ratios in our menstruums will be more precise and the results more uniform, as a bonus to not leaving a mess on our skin and clothes!

 

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Source: Getting the Green and Waxes Out Afterwards

EDDIEKIRK

My Holy Shit sublingual is actually the combining to two different research projects. In the process of learning to make canna lollipops, I discovered how much more palatable BHO or QWET was when combined with the cinnamon oil and the cinnamon oil acted to keep it liquid enough to drop.

 

I started using that as a sublingual and when the other pharmers dropped by, they often asked for some by saying, "Do you have any of that good shit?" I therefore named it GS oil, for good shit.

 

Shortly after that time, I was corroborating on the Holy Anointing Oil with Eloquentsolution and decided to add cinnamon candy flavoring oil to that that oral mixture, to take advantage of the faster uptake and improve the flavor.

 

After its success and subsequent following, I named it HS oil for holy shit!

 

I use it as my main daily med as a sublingual for pain. I highly recommend it!

 

Skunk Pharm Holy Shit recipe:

 

10 grams BHO Cannabis oil

3 grams Virgin unrefined Coconut oil

.7 grams Cinnamon Bark oil from Newdirectionsaromatics.com

.7 grams Cinnamon Leaf oil .

.3 grams liquid Myrrh Gum

1 gram cinnamon candy flavoring oil from Loranneoil.com

 

Standard pain dose for a light weight is one drop and for a high tolerance person 3 drops. Taken sublingually, some head effect is noticeable within a couple minutes, but full effect takes 45 minutes or so.

 

Titrate for dosage carefully if you are a light weight! Some lightweights have been discombobulated on one drop.

 

Heavy tolerance users on the other hand can usually tolerate six or more drops, it just doesn't relieve any more pain.

 

Source: HOLY SHIT SUBLINGUAL!

EDDIEKIRK

Just got advance copies of the May High Times, where Skunk Pharm Research was featured on pages 52 through 60.

 

Hats off to Elise for being gracious and kind in her writeup, and for being a good student in the bho and alchemy classes.

 

Some pictures of the Skywalker and Greencrack that Joe and I extracted specifically for the project, but alas the clear shots I hoped for didn't make the cut. I had a bad camera card that day and missed all of the pictures.

 

Both were extracted using denatured alcohol and dry ice for the recovery tank and the Skywalker was almost transparent, while the Greencrack looked like electric yellow stained glass. On a scraper, not so much................

 

Anyone interested in the details might pick up next May's copy and crack it to page 52, plus check out the rest of the articles and advertizements. One of the other articles is a list of strongest strains.

 

 

Source: Skunk Pharm Research in May High Times

EDDIEKIRK

Whoop, whoop, lu lu lu lu lu lu lu lu lu lu lu lu!!!!!!!!!1 Hee, hee, hee, snicker, snark, snort, don't you just love it when a plan comes together?

 

Those of ya'll who've tried to blend BHO and Vegetable Glycerin to make e-juice, know it doesn't readily happen and you are limited in the potency levels that you can reach extracting with glycerin as the menstruum.

 

You are limited even adding a surfactant like lethicin, to promote absorption, so that market hasn't taken off as readily as it might if it delivered a more potent hit.

 

At the suggestion of CAT Scientific, whom has supplied Skunk Pharm Research with equipment for testing, we tried their X-120 Homogenizer with a T-17 (N) generator shaft assembly, to see if they would not only blend, but stay blended.

 

For that experiment, we heated 250 ml of VG to 66C/150F in a 500 ml beaker, and added 6 grams of green BHO, which I've saved for several years as an example of too many washes using an open tube. Before investing any amounts of prime oil, best to see what it does with bad example show and tell samples.

 

250 ml is about the minimum that can be processed with the T-17 (N) generator, as it is high precision and relies on the liquid as its lubricant. CAT S, not only published that caveat in their supplied "destruction manual", but passed it on to us in an e-mail to make sure we read the manual before firing up the homogenizer.

 

They also provide the caveat that homogenizers don't like vortexes, for the same reason, so it can't be used in the center of the container, only around the center. That seemed fair enough, so we followed those simple instructions in the test.

 

Wowza! It made about one minutes work of fully emulsifying the BHO and VG, producing an light green opaque solution, which hasn't observably changed in 60 hours of standing, so we will be moving on to seeing just how much BHO we can mix with 250 ml of VG.

 

We will run it up to 50% BHO, in the next trial, but will start with a fresh sample so that we can field test it on patients afterwards. At CAT's suggestion, we will use a T-17 (V) generator shaft assembly, because the viscosity will be much higher.

 

I've also started dialog with an associate who is an e-juice manufacturer, whom has a market for the end product, so can test on a much larger scale. We donate our meds, but over half a liter of e-juice would far exceed current demand, while demand for the same BHO in cancer meds continues to be strong.

 

You heard it here folks, this device is a game changer in the e-juice market!!!

 

While on the spendy side for ma and pa, they could produce more e-juice in about a minute, than they would likely need in a year anyway. It is however, easily in the price range for small groups, and chump change for someone producing e-juice for the market place. In fact, for those in the market, CAT makes much larger machines than the hand held unit that we are testing.

 

Contact information for this sweetheart is http://www.catscientific.com/ and bon appetite!

 

Here is a picture of the X-120, as well as the T-17 (N) generator, as well as the 250 ml emulsion that we created three days ago:

 

GW

 

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Source: Game changer Emulsifying Vegetable Glycerin and BHO for E-Juice

EDDIEKIRK

From: ZHO Warning

 

2-13-14

Greetings Folks!

We have some exciting news. We, at Z Air Inc. developed yet another great product called MZ 12X. MZ 12X is an organic gas that is engineered to be stronger than PureZho. While MZ 12X is flammable it is NOT explosive like butane. Like any other compressed gas caution should be taken when using MZ 12X. We are confident that you will not be disappointed.

 

While we are working with potential distributors in different regions we are launching a special web promotion, so be sure to check out our website for more info. Launching of this product is scheduled to be on or before Feb 20th. Also check out our YouTube video at :

http://www.youtube.com/results?search_query=mz12x&sm=1

 

Once again we thank you for all your continuous support and enthusiasm. Have a great week and email us with any questions/comments.

 

Sincerely,

Staff at Z Air, Inc.

2-14-14

 

Ladies/Gentlemen:

 

For me to use your product, or indeed to even take you seriously, you must provide me with MSDS's sheets, which are also required by law.

 

I've requested those, as have others, but thus far to no avail.

 

Please supply me with those documents, if you plan to continue to sell your product in the US, because I will draw your failure to do so to the attention of the proper authorities.

 

Graywolf

 

PS: Nothing personal. That law is there for a reason, and if you care to research court cases of those who thought they didn't have to comply, you will find that they uniformly lost.

 

2-20-14

 

MSDS is listed on our website.

Thank you.

 

2-21-14

 

Thank you!

 

That also puts things in perspective, although your MSDS doesn't reflect it.

 

Methylene Chloride MSDS sheets by others show it to be a Class 2-B carcinogen. Perhaps you might update your MSDS sheet to include that data?

 

http://www.sciencelab.com/msds.php?msdsId=9926060

 

Peace, Graywolf

 

 

 

 

 

Source: ZHO Warning

EDDIEKIRK

BHO Safety

 

Hi ya’ll! Have ya’ll been watching the folks blowing themselves and their homes up using butane extraction techniques, thus leading you to believe that such an attempt is suicidal?

 

Thank Gawd (Great Spirit) that paying attention to details reduces the odds to limits that you might embrace, after being thus enlightened. May we discuss, before you give up all BHO extraction attempts in deference to your family and home?

 

Clearly Butane is inflammable and can be explosive, if confined in a small space and supplied with about 1.86 to 8.41 percent butane to atmospheric air content and an ignition source.

 

In addition, ignition sources come from a number of different unexpected sources, so let’s discuss that issue.

 

For starters, I never personally do a butane extraction indoors or any confined space! None at all, zero, zip, forget about it! It is important to keep it below explosive limits!

I do it all outdoors, with a non sparking plastic fan blowing, not sucking, the butane evaporation away! Butane loves self abuse and will clump together and pool, being that it is heavier than air.

 

I use three fans to keep any free butane dispersed below ignition limits of 1.86% and from it pooling and accumulating in low spots like through my basement window to my basement, chock full of ignition sources.

 

The central point is that concentration of the butane boiling off can be kept diluted below combustion limits, by blowing the accumulating vapors away using a fan.

 

Secondly, let’s talk about stupid ignition sources. Despite previous discussions, I have literally grabbed the hands of cigarette smokers poised to light a cigarette while extracting.

 

What can I say about addicts whom go on automatic pilot and forget where they are? Leave your cigarettes and lighter elsewhere.

 

Lose the lighter and cigarettes (bong?) if you are an addict! Once the pin is pulled on a 5 second grenade, it is not your friend!

 

All pretty simple, but lets talk about subtleties! How about sparks?

 

Starting simple, dragging your feet on concrete with gravel imbedded in your shoes can create a spark.

 

Wearing plastic clothing, especially socks, can also build up and discharge a static electricity spark, especially on cold dry days.

 

Unless it is an explosion proof fan, always blow, instead of suck the vapors away, not only for efficiency reasons, but because the sparks from an electric motor slip ring can ignite the vapors.

 

Always use plastic or other spark proof blades, because a grain of sand can spark when hitting a steel blade, and be propelled into the concentrated vapors.

 

Always keep a fully charged and recently inspected fire extinguisher on hand. Shit sometimes happens and less shit is better, as I see it!

 

Never had to use one at home, though I have in industry, and they can’t be beaten when they are called for!

 

If you get inadvertently sprayed with butane, stop, and go change clothes. Immolating as I sees it, is highly overrated!

 

Keep a blanket on hand, and if you do get unexpectedly ignited, immediately wrap yourself in it to extinguish the flames.

 

The good news is that none of the above has ever happened to me, or any of my friends who pay close attention and try their very best to avoid it.

 

Ohmmmmmmmmmmmmmmmmmmmmmmmm mmm!!!!!!!!!!!!!!!!!!!!!!!1

 

Butane Safety

Posted by Skunk Pharm Research,LLC.

Hi ya’ll! Have ya’ll been watching the folks blowing themselves and their homes up using butane extraction techniques, thus leading you to believe that such an attempt is suicidal?

Thank Gawd (Great Spirit) that paying attention to details reduces the odds to limits that you might embrace, after being thus enlightened. May we discuss, before you give up all BHO extraction attempts in deference to your family and home?

Clearly Butane is inflammable and can be explosive, if confined in a small space and supplied with about 1.86 to 8.41 percent butane to atmospheric air content and an ignition source.

In addition, ignition sources come from a number of different unexpected sources, so let’s discuss that issue.

For starters, I never personally do a butane extraction indoors or any confined space! None at all, zero, zip, forget about it! It is important to keep it below explosive limits!

I do it all outdoors, with a non sparking plastic fan blowing, not sucking, the butane evaporation away! Butane loves self abuse and will clump together and pool, being that it is heavier than air.

I use three fans to keep any free butane dispersed below ignition limits of 1.86% and from it pooling and accumulating in low spots like through my basement window to my basement, chock full of ignition sources.

The central point is that concentration of the butane boiling off can be kept diluted below combustion limits, by blowing the accumulating vapors away using a fan.

Secondly, let’s talk about stupid ignition sources. Despite previous discussions, I have literally grabbed the hands of cigarette smokers poised to light a cigarette while extracting. What can I say about addicts whom go on automatic pilot and forget where they are? Leave your cigarettes and lighter elsewhere

Lose the lighter and cigarettes (bong?) if you are an addict! Once the pin is pulled on a 5 second grenade, it is not your friend!

All pretty simple, but lets talk about subtleties! How about sparks?

Starting simple, dragging your feet on concrete with gravel imbedded in your shoes can create a spark.

Wearing plastic clothing, especially socks, can also build up and discharge a static electricity spark, especially on cold dry days.

Unless it is an explosion proof fan, always blow, instead of suck the vapors away, not only for efficiency reasons, but because the sparks from an electric motor slip ring can ignite the vapors.

Always use plastic or other spark proof blades, because a grain of sand can spark when hitting a steel blade, and be propelled into the concentrated vapors.

Always keep a fully charged and recently inspected fire extinguisher on hand. Shit sometimes happens and less shit is better, as I see it!

Never had to use one at home, though I have in industry, and they can’t be beaten when they are called for!

If you get inadvertently sprayed with butane, stop, and go change clothes. Immolating as I sees it, is highly overrated!

Keep a blanket on hand, and if you do get unexpectedly ignited, immediately wrap yourself in it to extinguish the flames.

The good news is that none of the above has ever happened to me, or any of my friends who pay close attention and try their very best to avoid it.

Ohmmmmmmmmmmmmmmmmmmmmmmmm mmm!!!!!!!!!!!!!!!!!!!!!!!1

 

 

Source: BHO Safety

EDDIEKIRK

BHO Safety aka "Please don't immolate or blow your self up!"

 

Hi ya'll! Have ya'll been watching the folks blowing themselves and their homes up using butane extraction techniques, thus leading you to believe that such an attempt is suicidal?

 

Thank Gawd (Great Spirit) that paying attention to details reduces the odds to limits that you might embrace, after being thus enlightened. May we discuss, before you give up all BHO extraction attempts in difference to your family and home?

 

Clearly Butane is inflammable and can be explosive, if confined in a small space and supplied with about 1.86 to 8.41 percent butane to atmospheric air content.

 

In addition, ignition sources come from a number of different unexpected sources, so let's discuss that issue.

 

For starters, I never personally do a butane extraction indoors or any confined space! None at all, zero, zip, forget about it! It is important to keep it below explosive limits!

 

I do it all outdoors, with a non sparking plastic fan blowing, not sucking, the butane evaporation away! Butane loves self abuse and will clump together and pool, being that it is heavier than air.

 

I use three fans to keep any free butane dispersed below ignition limits of 1.86% and from it pooling and accumulating in low spots like my basement, chock full of ignition sources.

 

The central point is that concentration of the butane boiling off can be kept diluted below combustion limits, by blowing the accumulating vapors away using a fan.

 

Secondly, let's talk about stupid ignition sources. Despite previous discussions, I have literally grabbed the hands of cigarette smokers poised to light a cigarette while extracting. What can I say about addicts whom go on automatic pilot and forget where they are? Leave your cigarettes and lighter elsewhere

 

Lose the lighter and cigarettes (bong?) if you are an addict! Once the pin is pulled on a 5 second grenade, it is not your friend!

 

All pretty simple, but lets talk about subtleties! How about sparks?

 

Starting simple, dragging your feet on concrete, if you have gravel in your shoes can create a spark.

 

Wearing plastic clothing, especially socks, can also build up and discharge a static electricity spark.

 

Unless it is an explosion proof fan, always blow, instead of suck the vapors away, not only for efficiency reasons, but because the sparks from an electric motor slip ring can ignite the vapors.

 

Always use plastic or other spark proof blades, because a grain of sand can spark when hitting a steel blade, and be propelled into the concentrated vapors.

 

Always keep a fully charged and recently inspected fire extinguisher on hand. Shit sometimes happens and less shit is better, as I see it!

 

Never had to use one at home, though I have in industry, but they can't be beaten when they are called for!

 

If you get inadvertently sprayed with butane, stop, and go change clothes. Immolating as I sees it, is highly overrated!

 

Keep a blanket on hand, and if you do get unexpectedly ignited, immediately wrap yourself in it to extinguish the flames.

 

The good news is that none of the above has ever happened to me, but then I do pay close attention and try my very best to avoid it.

 

Ohmmmmmmmmmmmmmmmmmmmmmmmmmmmmmmm!!!!!!!!!!!!!!!!! !!!!!!1

 

This post has been promoted to an article

 

Source: BHO/RSO Safety! Please read!

OMMP PAY IT FORWARD

DIY CO2 Extraction?
Posted by Skunk Pharm Research,LLC.
I don’t know about ya’ll, but I have been watching CO2 Super Critical Fluid (SFE) with interest and have wanted to sample some cannabis essential oils extracted by that method, but the cost of conventional SFE equipment, is outside the range of most of our finances.
For the rest of ya’ll just learning of the process, let’s quickly examine what SFE is, by looking at what Wikipedia has to say about it, followed by our kicking off our affordable DIY CO2 extractor design project:
Supercritical carbon dioxide
From Wikipedia, the free encyclopedia

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Carbon dioxide pressure-temperature phase diagram
Supercritical carbon dioxide
is a fluid state of carbon dioxide where it is held at or above its critical temperature and critical pressure.
Carbon dioxide usually behaves as a gas in air at standard temperature and pressure (STP), or as a solid called dry ice when frozen. If the temperature and pressure are both increased from STP to be at or above the critical point for carbon dioxide, it can adopt properties midway between a gas and a liquid. More specifically, it behaves as a supercritical fluid above its critical temperature (31.1 °C) and critical pressure (72.9 atm/7.39 MPa), expanding to fill its container like a gas but with a density like that of a liquid.
Supercritical CO2 is becoming an important commercial and industrial solvent due to its role in chemical extraction in addition to its low toxicity and environmental impact. The relatively low temperature of the process and the stability of CO2 also allows most compounds to be extracted with little damage or denaturing. In addition, the solubility of many extracted compounds in CO2 vary with pressure,[1]permitting selective extractions.
Soooo, in us’n layman’s terms, we use plain old CO2, that we have gotten hotter than 31.1C/87.98F, while under at least 1086 pounds per square inch pressure.
In that state, the CO2 becomes a super solvent, which has higher penetration power, and can be fine tuned to focus in on specific constitutes, by varying the pressure, temperature, and by the use of co-solvents like ethanol or hexane.
Fair enough, and easy enough to accomplish several ways! Traditionally a high pressure intensifier pump is used to achieve the required pressures.
Cryo-pumping also works. You start with liquid CO2 or dry ice and heat it in an enclosed space.
My first conceptual of a system that was semi affordable, was a simple minded system using liquid CO2 and heat to run it at about 1500 PSI. That eliminated the pumps normally used and by using a liquid Dewar with a dip tube, with both a gas head and a liquid tap, the need for any liquid pumps is eliminated as well.
It is designed to use readily available Schedule 180 austenitic stainless pipe and its largest component is small enough to fit in my 7″ X 36″ lathe. My original plan was to use an existing hydraulic cylinder for my vessel, but alas, carbon steel embrittles excessively at cryogenic temperatures.
My design calls for achieving pressure by simply heating the pipe with available pipe band heaters.
Pressure was controlled using a conventional, though expensive back pressure regulator. Please note the attached conceptual, which reflects my thinking four to five years ago. I put the project on the back burner after reading the SFE CO2 patents for extracting cannabis, and noting that CO2 isn’t a very aggressive solvent and the patented processes used significant fluid exchange rates, as well as relatively long spans of time.
To compound that, reports from those testing SFE CO2 extractions reported poor taste and effects, so I put CO2 extraction on the back burner to just watch for awhile.
Within the last couple of years several folks have done some interesting work starting with dry ice. The first that I noted was able to maintain high enough pressure in a test tube to keep dry ice from sublimating as it warmed, so as to extract some Limonene from an orange peel.
That led me to question whether super critical pressures were required to extract the essential oils from cannabis that we typically extract with other solvents, and further experiments by others suggests that it is not. Some even report better results at subcritical pressures, especially with the use of co-solvents.
Sub critical extraction presents an interesting twist from a simplicity standpoint, so of course my simple mind immediately envisioned replacing the test tube with a pressure vessel containing dry ice in the bottom, and a basket of material suspended above it. Screw down lid and bring it up to temperature with a pipe clamp heater for pressure.
Flooding is achieved by simply turning it upside down to soak the material and right side up to drain. That step could be repeated back and forth, to soak the material and keep the boundary layers diminished. On setting it upright the final time, we could bleed off the liquid into an expansion chamber and then to atmosphere, leaving behind the oil.
I have decided to build a 2″ X 24″ prototype, and have acquired two resources on this project that emboldens me. One is the offer from a dear old friend, to allow me the use of his aerospace pressure and vacuum equipment manufacturing facilities for giggles and old times sake.
The other is an agreement with another old friend, who owns a cryogenic equipment manufacturing plant back east and is familiar with SFE.
We have a mutual engineering support agreement in effect, in exchange for my support on one of their projects with a former aerospace customer of mine, who is now their customer as well.
For my support interfacing their equipment with equipment of my own design and manufacture before retirement, they will support me in developing a simple minded DIY SFE system, that hopefully more of us’ns can afford to build, or have built.
So here is my first simple minded conceptual using liquid:

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Here is my simple minded conceptual starting with dry ice:
OOPs, solly, watch this space!
After working all day on the drawing, my 2002 32 bit Auto Cad program is not able to access my printer on my 64 bit processor, and I’m not smart enough to figure it out, so I have to find a computer hero or heroine first.
The way my conceptual works, is the bottom of the cylinder is filled with dry ice , on top of which sits a wire basket of plant material. Clamp on band heaters turn the dry ice to liquid, which is circulated and soaked through the material by simply turning the cylinder upside down.
After flipping it about a few times, over an extended soak, the vessel is set upright and attached to the lower expansion chamber via a hydraulic quick disconnect. The liquid is bled off, decompressed, and the oil collected from the decompression vessel via the bottom drain valve, as well as via the detachable bottom.
Lu lu lu lu lu lu lu lu lu lu lu lu lu lu lu!!!!!!!!!!!!!!!!!!!!!!!! Progress!
Well thank the Great Spirit for ex-brother in laws, who can sort out computer problems, so that I can print from virtual mode. Hee, hee, hee, kept him at tossed the sister……….
Here is my simple minded conceptual of how such a dry ice system might work. More detail prints once I have exercised some resources.
After further discussion with another experimenter, I have decided to build the system to operate at 5000 psi and below. Instead of using schedule 160 stainless pipe, I will gun grill a billet of stainless, but will keep the bore at one inch.
Posted Image
Hi ya’ll!
Been out talking to folks running commercial CO2 SFE units and would like to share some selected excerpts from their letters, to keep their identities confidential:
Hi Graywolf, here is some pics of the unit i have been running for 8+ years. Our whole thing with this unit was to have maximum fractionation capabilities.
The extraction vessel is rated to 10,000psi, and made of stainless!!
We use a basket to hold the material and I’m having a natural cloth bag made that will go into the vessel and hopefully allow me to extract 2x current volume.
There are some great graphs around the net that show the combinations of pressure and temps and the resulting density of co2. In general high pressure (we go up to 10,000psi) works well in combination with high temps (around 100c) and lower pressure around 5000 psi goes well with about 60c.
I tried high pressure and while i need to try again to confirm, there seemed to be some degradation to the overall quality and definitely the fragrance. the yield was higher and its much more efficient requiring less co2.
I already noticed on the bit of extract that i dissolved in ethanol and then winterized and filtered, the flavor is no where near what it was before going in the ethanol. I plan to try and get the waxes out with only co2.
I cant see any advantage to using either hexane or ethanol or a mixture as a co solvent?? the compounds are easily soluble in co2 and usually those types of things will help to extract more polar compounds such as chlorophyll. It all depends on what your goals are? maybe he is using that mixture to help fractionate out the waxes??
I can do a small run next week using those co- solvents and report back if i see anything magic or some beautiful separation. maybe he is just some chemical engineer using a method that was used for another project and he is trying to apply it there?
It seems really counterproductive to use co solvents and contaminate a great extract… maybe he can only do really low pressure and he requires the co solvent to help the efficiency??
I found material with a moisture content of around 10% to be fine. I don’t know what the implications of a slight amount of carbonic acid could mean?
I have heard it can make oils rancid, but have run vegetable oils at 10+% moisture and had them test very low in peroxide values in respect to oxidation and rancidity. I do not see any problems with around 10% moisture, the water sometimes comes out with the extract and is sitting on top and the few mls there can be poured off.
Posted Image
And from yet another hero!
I. Extraction was performed by sub and supercritical CO2:
Subcritical (liquid): 10-12 ºC @ 65-70 bar for approximately 6 hrs.
Supercritical (liqid/gas): 40-45 ºC @ 230 bar for approximately 4 hrs.
II. Separation of fats and sugars, by winterization, chromatography and high speed centrifugation.
This part was very critical in the purification schema and required analysis of both the anaylate and precipitate.
III. Purification, at this point one has two options, Flash Chromatography or Wiped Film Evaporation (Short-path)
I performed both and in both techniques, one can obtain purities in the range of 95-99% total THC (∆9, ∆8 and ∆6) with the purity of ∆9 ranging anywhere from 78-98% depending on the parameters set.
One last comment, probably the most important….. absolutely no petroleum derived hydrocarbon solvent was used. Except for the small amounts used for LC/MS analysis. This was my driving force to see if it could actually be pulled off.
Posted ImagePosted Image
12-21-12
We are moving this project from research to active experimentation in our FY 2013, now that the shack and Terpenators projects are a fait accompli. What I did in FY 2012, was simply research and develop resources.
It was good that I did, as further research put things in better perspective.
While I determined that my simple minded CO2 SCFE system would work, it raises a the bigger germane question of why is this trip necessary, given how effective BHO and some of the other extraction methods are. Why spend the money for this more expensive fish trap, if we already have the fish?
The answer lies in that what CO2 SFE extraction shines at, is selective extraction. By fine tuning the pressure and temperature, as well as using co-solvents, specific components may be extracted, while leaving behind everything else.
That is of less value when discussing cannabis essential oil extraction, in that it has been determined that it is the entourage effects of all the terpenes present, including the diterpene cannabinoids, that are responsible for its medicinal properties. That however doesn’t mean that we can’t specifically focus on that list of terpenes.
The other thing that my research made clear, and that is using one vessel to process the material and raise the pressure in, would result in extractions along the entire temperature/pressure curve. Woops, no selectivity there, but easily solved by bringing the liquid CO2 or dry ice up to a higher temperature and pressure in a separate vessel, and then equalizing it with the one containing the plant material! Easy, but the system complexity grows.
One of the interesting things that my research turned up during tete a tetes with brothers owning and operating commercial CO2 SCFE’s, and bumblers like myself whomping up DYI ghetto extraction equipment, is the wide range of processes that different operators have achieved a modicum of success at.
One operator simply took the valve out of a CO2 bottle and filled it with plant material and dry ice, before replacing the valve and heating the tank to SCFE ranges. He then inverted the tank and vented the CO2 into a catch container, where it left cannabis essential oils behind.
He claimed his best success using co-solvents at ~5500 psi and that his product was superior to all competing, but alas, I was never able to sample it and his spamming got him banned from the forums where we shared information.
Commercial SCFE operators report successful sub critical products as low as 350psi, and another at 850psi, but I haven’t been able to sample their successes, to confirm my own opinion of product quality. There in lies the rub of course, as there is no common measurement and each creator loves his creation.
Fortune has ostensibly smiled on us however, in that two of the operators that I have been conversing with, have agreed to work more closely with us and to supply confirmation samples. Hee, hee, hee……………………………
Even simpler DIY SCFE C02 6-2-13
Hee, hee, hee, you have to admire simplicity. Here is the system by jyndustriez which I mentioned, that simply puts the plant material in an off the shelf CO2 tank, and floods it with liquid C02 from a second off the shelf tank, before heating to achieve super critical state.
More information on how he accomplishes that at http://jyndustriez.blogspot.com/, but here are some pictures he has shared:
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8-25-2013
Progress! We got to play with a donated SCFE CO2 extraction sample and were able to heat it under vacuum and observe the effects.
As received, the sample was in a “wax” hydrate form, and was not aromatic. The flavor was mild, and the effects were good.
As it was a small sample, I was unable to winterize it to remove the waxes, but I was able to heat it to 115F, under vacuum, and observe what happened.
The sample out gassed significant CO2, even though at 115F decarboxylation was minimal, and never quite turned clear, due to the high wax content, but that isn’t unique, as BHO extracts are improved by wax removal as well.
On the surface however, the wax content seemed high, compared to our typical BHO extraction, so I look forward to a large enough sample to winterize and determine just how much.
Here is a starting and ending photo, demonstrating the ending wax content.
Posted Imagehttp://skunkpharmresearch.files.wordpress.com/2012/05/c02-sample-1-2.jpg?w=855&h=774
To add to our excitement, last week we got a guided tour of Eden Labs during our recent business trip to Seattle! What fun!!!
Patrick, one of Eden Lab’s bright new sales consultants, attended one of our BHO classes and subsequently invited us for a tour, so how could we resist, hee, hee, hee, snicker, snark, snort………………?
Always a pleasure to see how the pros from Dover do things, and I do likes the way they detail a package.
We lucked out in finding the original creator available and got our guided tour from Fritz himself. Besides his latest creation, we got to see not only his original test sled, but some of the R&D that may make great strides someday, when Fritz can find enough time to finish them, between current product demands……….
Their latest all stainless creation was in final assembly and testing, and was capable of extracting not only with subcritical and Super critical C02, but also with refrigerants like butane and propane.
It was appointed well, and used pneumatic intensifiers both for the hydrocarbon pump, as well as the SCFE CO2 pump.
It also sported a unique closure system, which simply spins close and that greatly simplifies loading, as compared to a 12 bolt flange with a torque wrench.
The vessel itself uses a Schedule 160 stainless core, but adds water jackets, so as to permit the use of a commercial heater/chiller for temperature control.
The unit that we looked at, had a $60K base price, plus the price of the hydrocarbon extraction capabilities. Not cheap, and more complicated that most folks should attempt at home, but if you need a machine capable of a quality extract, in commercial quantities, you will need to step up to a system of this caliber, which includes pumps to cycle the C02, and C02 recycle to recover it afterwards.
Fritz did note that one of the things on his list of thangs he is juggling, is a smaller lab sized unit, which fills the market window for a smaller unit that doesn’t recycle. Looking forward to see what comes up there!
From a process perspective, Fritz shared that the aromatic extractions are best done at low pressures and as the pressure goes up, so does the rate of chlorophyll extraction. Based on his and other input, I will focus on the range from 800 psi to 3500 psi. While I’ve heard operating parameters up to 9500 psi, the lower ranges sound more believable.
As unbelievable as it may sound, ah think sometimes operators shuck me, cause they are trying to protect process secrets and lead me astray.
10-27-13
Lu lu lu lu lu lu lu lu lu lu lu lu lu lu lu!!!!!!!!!!!!!!!!!!!!!!!1 The Great Spirit smiled and JYNdustriez loaned us a CO2 extraction setup and will show us how to use it, when he visits to watch Dr. Fischedick’s lecture on 11-2.
I’ve also located a local brother with an Eden Lab machine, who is amenable to experimentation, so things are heating up in the area of CO2 extraction at Skunk Pharm Research. We will have machines from both ends of the price scale to experiment with.
Sound CO2 has also extended us an invitation to visit, and they run Apeks equipment, soooo even though our CO2 project was slow getting in motion this year, it looks like it is finishing with a bang.
1-31-14
Hee, hee, hee, check out JYN’s latest link on DIY SCFE CO2 http://jyndustriezllc.com/diy-co2-extraction-crumble-wax-shatter/

EDDIEKIRK

From: Cannabis Acetate

Let's discuss cannabis acetate! To put it into perspective, it is to cannabis, as aspirin is to willow bark and heroin is to poppies.

 

In all cases, the acetylization results in the active ingredients passing the blood brain barrier more readily than cannabis oil, salicylic acid, or opium, the raw extracts.

 

In the case of cannabis, the effects come on so rapidly, that in his book, Marijuana Chemistry, Michael Starks proffers 3X potency. I don't embrace that theory, but instead think that it comes on so quickly that it feels that way.

 

We've been making it for awhile, trying to sort out the process. We looked at Starks procedure, which seems to be based on making heroin out of opium, but after counting molecular weights, decided to start with the general procedure for making aspirin out of salicylic acid.

 

Sooo, let's talk about the progress that we've made here in those experiments, now that we have had an opportunity to make this enough times to get repeatable results.

 

Here is the process, probably not refined as far as it will be, but works and produces reliable results.

 

We started by dissolving 10.4 grams of BHO into 16.5 grams of hexane, to remove it from the storage container with an unknown tare, so as to not waste any left behind in films and to get an accurate weight. We warmed the mixture in a hot water bath to increase dissolution rate.

 

When dissolved, we decanted into a beaker with a known tare and weighed the total amount, from which we subtracted the beaker tare and the weight of the hexane to get the BHO weight of 10.4 grams.

 

We then poured that into a one liter boiling flask. To that we added 25 ml of acetic anhydride and 1.25 ml of 98% sulfuric acid.

 

We placed the boiling flask on a combination hot plate stirrer, and added a stirring bar to the mixture.

 

We added an Alhin condenser to the flask, through which we pumped ice water, and reflux boiled the mixture for one hour while stirring.

 

After refluxing for one hour, we added 40 ml of water to react the remaining acetic anhydride, and another 40 ml of hexane. We poured that into a separatory funnel, which we finished filling with saturated salt water.

 

After shaking well, we allowed the layers to separate and bled off the lower water emulsion layer, only to refill with salt water again and repeat the procedure until we had run about 4 liters of salt water through the mixture.

 

After bleeding off the salt water one last time, we bled the hexane mixture into a beaker and after filtering through a 0.2 micron syringe filter, we boiled off the hexane using the hot plate stirrer, with the beaker sitting in a larger beaker half full of water.

 

Just before the hexane was gone, I refilled the beaker to the half way mark with 190 proof ethanol and boiled that off using a 250F hot oil bath.

 

I repeated the alcohol wash three times to insure the removal of the rest of the hexane.

 

When the alcohol was all purged, I took the attached picture.

 

As you note, the resulting acetate is of a lighter color than the original oil and of lower viscosity.

 

Here are some pictures:

 

Starting solution

 

Startingsolution.jpg

 

 

Acetic Anhydride

 

AceticAnhydride.jpg

 

 

Cannabis acetate equipment

 

Cannabisacetateequipment.jpg

 

 

Adding salt water

 

Addingsaltwater-1.jpg

 

 

Washing with saline solution

 

Washingwithsalinesolution.jpg

 

 

filtration

 

filtration-1.jpg

 

 

Separatory funnel

 

Separatoryfunnel.jpg

 

 

Final product

 

Finalproduct.jpg

 

 

Source: Cannabis Acetate

EDDIEKIRK

Butane Honey Oil extraction, or BHO, is one of the methods used to extract cannabis oleoresins and oils using butane as the solvent. There are many theories on the best way to accomplish this, but here is the formula the skunk pharm uses to extract the crude oleoresin and refine it into a pristine absolute.

 

As most of our extracted oil goes into oral meds, we also decarboxylate ours. This process is based on the 252F curve shown in the attached graph, which I copied from Jump 117.

 

Butane performs one of the cleanest extractions of cannabis, because it a relatively non polar solvent, and therefore extracts few water solubles. It however produces a lower yield than alcohol extraction, because of being more circumspect in what it extracts.

 

N-Butane, also known as R-600 refrigerant, is non toxic enough to be used as a food propellant. Those who have been led to believe that it is highly toxic, owe it to themselves to compare the MSDS on Google to drinking ethanol.

 

One does have to be selective as to source however, as all butane stove fuel must by law have methyl mercaptan added for leak detection. Besides adding odor, Methyl mercaptan adds an unpleasant taste and has a sensory threshold of only 2 parts per billionth, so it difficult to impossible to eliminate once it is present.

 

R-600 refrigerant or cigarette lighter fuel butane is therefore normally used, as they do not have mercaps added. There are none the less a plethora of wives tales surrounding lighter fuel butane, for the most part designed to separate the unwary from their money.

 

Specifically, there is much controversy surrounding the number of times the butane has been refined and the level of contamination present. The contamination present is in the form of oleaginous waxes, which in butane is paraffin. Paraffin is non toxic enough that the MSDS doesn’t even list an LD-50 rating and it is used to seal jelly jars.

 

The refining to get it out has nothing to do with toxic properties, but the fact that expensive lighters have small orifices that are easily clogged by wax. The number of times the butane has been refined also says nothing about how much wax is left, so it means absolutely nothing. Just Madison Avenue verbiage to sell the same product for more money.

 

One supplier cleverly added the title “Near Zero Contamination” to all the brands that they produce, and it certifies that the residual contamination is less than 50PPM. In point of fact, they actually measure less than 15 PPM contamination, as does many competitive brands with less ostensible refining.

 

Skunk pharm uses Lucienne 4X butane because it tests under 15 ppm, same as the “Near Zero Contamination” 5X brands and we can purchase it for under $25 a case of (12) 300 ML cans.

 

Butane is highly flammable, so let us next talk about safety. It goes without saying that smoking around a butane extraction is asking for a disaster, but I have literally grabbed the hand of folks starting to light up because they “forgot” where they were at and what they were doing. May I suggest that you leave your lighter and smokes somewhere else when you are doing extractions.

 

Same with your cell phone!

 

Wear no synthetic fabrics, including your socks, because static electricity sparks probably ignite more butane unintentionally than bone headed smokers.

 

We use a fan to disperse the butane rapidly so as to keep it from pooling. Butane is heavier than air and will collect in low spots given its own devices. We use a plastic fan so that no sparks are created by a piece of gravel or other hard material passing through the fan blades.

 

In dry cold conditions, we add a grounding strap to our cans, so as to not draw static electricity sparks between the can and the column.

 

As most of our extracted oil goes into oral meds, we also decarboxylate ours. This process is based on the 252F curve shown in the attached graph; I copied from Jump 117 on ICMag’s forum.

 

The first question is why use a BHO technique to extract the resins, instead of just boiling the material in alcohol to get the greatest amount of extracted material?

 

The answer to that is that because butane is relatively non polar, it doesn’t extract the water solubles like chlorophyll and plant alkaloids, as well as the plant waxes and vegetable oil. Butane produces one of the cleanest extractions, albeit at the lowest yield.

 

On average we have extracted about 18% oil by weight from bud, but as low as 12% and as high as 25%.

 

The first wash will usually extract 75 to 80%, leaving the balance for the second after repacking the column. The second extraction will be more sedative and less heady. If you use a hand microscope, you can easily see when the trichome heads are gone and the stalks look like wet fur.

 

The first step in the process is to get as much water as possible out of the material.

 

A fresh material BHO is possible, and is hands down the most flavorful extraction tested by the panel thus far, but this procedure covers both fresh and cured material that has been cured to about 15% water content. 15% is a lot of water, so unless we reduce the water content even further, we will be extracting some water solubles, despite butanes low polar activity.

 

We dry our cured material even further by spreading it on a cookie sheet and baking it in a 200F oven until just frangible when rolled between the finger and thumb. We then scrub it through a wire mesh pasta strainer, using a leather gloved hand and firm pressure, so as to minimize the amount of fine particles generated.

 

The stems will be left behind, which I encourage you to save for a different extraction, and make a killer topical out of them. If you leave them in the extraction, they will leave some of their flavor behind.

 

We never, ever, use a blender or coffee grinder to reduce material, because it produces a lot of ultra fine powder that makes it through conventional filters.

 

Next, while it is still warm, we seal the material in a jar or baggy until loaded in a column.

 

If we are running fresh material, we simply cut it from the mother plant and freeze it as is. That ties up the water as ice. We take it out of the freezer and place it in a plastic bag, which we pummel to break into small pieces. We load those pieces into an extraction tube and return to the freezer. We also place the butane in the freezer and process the material, once both the plant material and the butane stabilize at 0.0F.

 

If it is cured, desiccated, and reduced material, we simply load it into a column and do not bother to freeze it.

 

Sooo, let us talk about columns. A column is a long narrow containment that allows a solvent to be passed though it using either gravity or pressure. In the case of a butane column, we do both.

 

If you Google Cole-Palmer, you will note that n-butane is not compatible with all of the materials available to build a column from. Some plastics like PVC are not suitable for instance because the butane leaches out the constitutes, which we prefer to not have in our meds, but in some part because of impurities in the butane that may attack them given extended usage.

 

Glass and borosilicate (Pyrex) work well, as does 300 series stainless steel, and as does copper, with the caveat that the column must be meticulously kept clean of copper oxide, which produces fume fever when welders weld copper based alloys with insufficient respiratory protection. If you do not have the time or inclination to keep the extraction column pristine, glass or stainless is a better choice.

 

Our local cost for borosilicate columns from the local scientific glass blower is only a buck an inch, plus five bucks to flare one end and close to an orifice on the other end.

 

As many of you have already no doubt noticed, there are also battle lines drawn around the use of plastic in a column. Some truth, but all plastics are not created equal.

 

HDPE, UHMW, XLPE, and PPE plastics are compatible with butane, but not PVC or CPVC. I strongly advise against using PVC for that reason.

 

When loading the material in the tube, we use a wooden dowel to keep it uniformly and firmly, but not tightly packed.

 

Before loading the tube, we wad up a coffee filter and stuff it in the injection port end, to diffuse the butane as it enters and so that no plant material blow back out into your extraction, should you need to release butane pressure in the middle of the process for any reason.

 

Having loaded the material in the column, which is essentially a tube with an open end and one closed except for the butane injection orifice, we need to close off the open end. Lots of ways to do that, but we use a double layer of coffee filter, plus a patch of 65/35% 160 threads to the inch (~80 micron) bed sheet, as blow out protection.

 

We hold those in place with a heavy rubber band, wrapped around enough times to hold the filters tightly in place. Because of the cold temperatures involved, these rubber bands may be used for more than one extraction, but not sequentially. I just toss them aside and sort through them later to see which ones might be suitable for a second extraction,

 

I also take a pair of scissors and trim away all extra filter material, so as to minimize the oil soaked up during the process. I find that if I am careful removing the filter after an extraction, that I can reuse it multiple times, so as to further minimize losses.

 

Skunk pharm use of a column is pretty unremarkable as compared to general practice. It is only our collection and processing techniques that divert from the norm. We simply support the column full pulverized plant material over a collection vessel and inject butane through it. The butane passes through the material in the column and dissolves the trichomes as it does so.

 

The cannabis oils in the trichomes remain dissolved in the butane as it passes out the bottom of the column into the collection dish, so when the butane subsequently evaporates off, it leaves the extracted cannabis oil behind.

 

As previously mentioned, we use a collection vessel for the butane cannabis oil mixture as it passes from the column and there is more than one choice. Because of space constraints, I will only cover two, which specifically are large surfaced open container like a 10” Pyrex pie dish using vacuum or conventional evaporation to minimize CBN conversion, and a smaller Bain Marie stainless container, which will be cooked off to decarboxylize and produce oral meds.

 

If discharging into a pie plate or a Bain Marie, we always place the receiving vessel in a hot water bath, to not only boil off the butane faster, but to also minimize water pickup from the humidity in the air. The heavier butane will keep the water laden atmosphere at bay until it is mostly boiled off.

 

When the stream of solvent running out of the bottom runs clear, we cease injecting butane and insert a basket ball pump needle into the injection hole and blow out any remaining liquid. A modified butane can nozzle adapter will adapt the needle to seal the hole.

 

After collecting and boiling off the butane with hot water, our process diverges, depending on our intended usage of the extract.

 

If it is to be only vaporized or smoked, we wash the butane extraction out of the 10” Pyrex pie dish with 190 proof ethanol and allow the mixture of alcohol and cannabis oil to evaporate off naturally, or vacuum it off. See attached pictures of simple glass jar vacuum reduction, as well as using a pressure cooker for a vacuum vessel, and attempts at vacuum distillation.

 

As most of ya’ll know, medications that will be subsequently smoked or vaporized, do not require up front decarboxylation, as it happens during the ingestion process.

 

If it is to be ingested orally, we simply wipe off the water from the original container and place it in a 240/250F hot oil bath in an electric fondue cooker with sensitive temperature controls. Some fry cookers also have sensitive enough temperature controls, but some have extremely wide dead bands in that range, as they are mostly produced to cook at around 375F.

 

Make sure that the container is sitting on something that suspends it up off the bottom of the oil pot. I throw four jar lids in the bottom of my electric fondue pot and use it for that purpose.

 

Never trust the numbers on the dial and use a good thermometer to set temperatures. We use either a mercury lab thermometer, or a digital one. Good temperature control is key to the process.

 

That means the device that you use to control the oil temperature must have a narrow dead band, so that the temperature control is stable.

 

I paid about $60 for a Quisinart fondue pot that was designed to heat sensitive sauces like chocolate and has excellent control throughout its temperature range. There are a couple of Revels in our group that are slightly larger and work well, plus cost only about $30, though they have a slightly larger dead band.

 

Some fry cookers have sensitive enough controls, but many deep fryers designed to primarily run at 375F, lack control sensitivity and have large dead bands at 250F.

 

When the pool of cannabis oil becomes almost quiescent, we remove it from the bath and continue with further processing. Studies suggest that 70% decarboxylation is the point of diminishing returns, so pool activity down to a few remaining small C02 bubbles is the signal that it is ready for further processing.

 

 

 

 

Either boil or distill off the alcohol until the liquid is reduced to a pool of oil and all but minor bubbles cease rising at the edges and then add at least ten volumes of alcohol and wash out the whole pot by swirling it and washing off any resin stuck to the sides.

 

Using a funnel, pour that liquid into a jar or bottle, seal it, and place that in the freezer.

 

I usually leave it at least overnight, but have pushed it to a couple hours. The liquid will lose its clarity and become slightly cloudy, primarily from plant waxes flocculating out.

 

Filter that liquid one more time, and you will have a bell clear extract, which is ready to reduce down one more time.

 

Place in a suitable container for return to the oil bath. Since you have much less material, a smaller one may be used.

 

At this point I put them in small stainless cups with their tare engraved on their sides or about a 250 ml beaker. The smaller container reduces the surface area that will be coated with oil when I cook it down the last time and knowing the cups tare weight allows me to take it directly from the oil bath and place it on a scale after simply wiping the exterior.

 

Since I know the tare, I then know the extracted weight, and exactly how much other ingredients to add. Once adding those ingredients, I place the cup back in the oil bath, where I stir it until well mixed and then decant into its final container.

 

Since the added ingredients include things that lower the cannabis oils viscosity, very little is left as a film in that container.

 

If I plan to use the oil as is, without adding any other ingredients, I extract it from the container using a pipette, so as to not leave a streak of material in the vessel. After I have extracted all that I can using a pipette, I wash the container and pipette out with hot alcohol, and save the wash for the next run.

 

Nothing is wasted or left behind.

 

Dryingleaf.jpg Borosilicatetubes001-1.jpg Extractionblowdown.jpg Injectingbutane.jpg Extractioncomponents.jpg

 

Purginganddecarboxylating.jpg Extractionbutaneboiloff.jpg Borosilicatetubes4-1.jpg Purginginhotoilbath.jpg Sievingleaf.jpg 945gramBHOrun-1.jpg

 

 

Be sure and make a free account here so you may ask questions from us, (takes two min)

 

Source: BHO OIL EXTRACTION

EDDIEKIRK

 

Oil and fat extraction is a method we'uns will be further developing, so watch this thread.

 

Cannabinoids and the other terpenes in cannabis, are readily dissolvable in fats and oils, so fats and oils may be used for both extraction and as a menstruum.

 

When I say fats and oils, I am referring to the vegetable and nut oils, as well as clarified butter. Oils tasty enough that may be ingested with a dropper, mixed with drinks, or used in medibles.

 

Water solubility varies, but one of the advantages of using oil for extractions, is that they are for the most part non soluble in water, so they don't extract excessive water soluble constitutes, like chlorophyll.

 

There are practical limits to the potency that can be achieved extracting with oil, because as the oil becomes saturated with cannabis terpenes, they become less concentrated and their solvent action slows down to a crawl, before stopping altogether.

 

Potency can be ratcheted up somewhat through using the same oil to do multiple extractions of fresh material, but even that has limitations.

 

A key factor in achieving maximum removal rates and efficiency, is keeping the boundary layer between the un-dissolved resins and the unsaturated oils used for extraction regularly removed. The method that we used in this experiment, was simple, but through periodic stirring.

 

Sublingual oil tinctures:

 

Aside for their useful role in extraction, oils and fats may be mixed at any ratios with cannabis terpenes, if you are just mixing them together as oils. Some of them are damn tasty even taken from a dropper, though as the concentration increases, the flavor becomes less fetching and it leaves more of a lingering aftertaste.

 

Choose an Oil:

 

We haven't tried them all, but we have tried Almond, Avocado, Butter, Canola, Coconut oil, Grape Seed oil, Olive, Pecan, Sesame, and Walnut oils. They all work well, so they are a good place to start, if you are new to extraction.

 

Preparing the material:

 

We first start by drying the trim. For the most floral flavor and the highest amount of lighter terpenes, material that is hung until it reaches the small stem snap stage is best for our purposes.

 

In our experience, for best flavor and taste, freshest material works best. Older cured material loses the nuances of the floral undertones and just tastes like hash.

 

That means that the degree of drying and curing is also critical, if your goal is to maintain maximum terpene content. Not that hash has a bad flavor, but it should be a conscious choice.

 

Choosing material:

 

Oil from buds is tastier than oil from even sugar trim, because most of the terpenes are produced by the buds, and that is where they are the most plentiful. Tasty is usually not a word used to describe oil from fan leaves or stems, though effective may be.

 

The material that we used in this experiment, was donated sweet trim from Chocolate and was well dried and cured.

 

Oils used in this experiment:

 

We used Ghee (clarified butter), Coconut oil, Grape Seed oil, and Olive oil for the run, because they are commonly available and inexpensive.

 

Making Ghee:

 

To make the Ghee, we melted unsalted butter and cooked it at low temperature, until the butter fats separated from the Ghee. We then skimmed off the floating butter fats, and sucked off the Ghee, using a turkey baster, leaving the heavier butter fats in the bottom of the pot.

 

Most recipes for extraction with butter call for boiling them material in water and butter, but we studiously avoid adding water and our Ghee extraction has only the lightest tinge of green and no chlorophyll flavor.

 

Here are the three extractions taken out of the refrigerator, where they were stored between cooking and actual pressing. Note that the butter, olive oil, and the coconut extractions have a slightest green tinge, yet none actually had a chlorophyll flavor.

 

In this experiment, we didn't attempt to reach maximum saturation, but to determine what was reasonable to expect from a single batch. To reach maximum saturation, we would have simply processed more than one batch of fresh material through the oil.

 

What we did, was fill four jars 3/4 full of the trim and then added enough oil to cover it, stirred it thoroughly, and then added another inch of oil.

 

We then lightly capped the jars and set them in pot of hot water and simmered it on low for six hours, uncapping and stirring thoroughly a couple of times an hour.

 

At the end of six hours, we removed the jars from the hot water and set them aside to cool. The next day, we cooked them two more hours, stirring regularly, and the third day we cooked them another six hours, for 14 hours total, with three heat cycles.

 

Lightly capping means snug enough to allow some pressure to build, but loose enough to vent off anything excessive. Since we used cured material and didn't add water, there were little in the way of volatiles to boil off and produce pressure.

 

I left the lid off the boiling pot, so as to not force steam into the jar head space.

 

For pressing, we warmed the oils and ghee up by placing them in boiling water, this time with the lids on tight and the lid on the pot,

 

Next we cut up some rags from some surplus drape material, with approximately a 160/200 thread count, and draped it over a restaurant sized potato ricer that we scored at Hongs Restaurant Supply in Portland. By pressing it down into the potato ricer, it formed a pocket that holds approximately a quart of plant material.

 

Folding the cloth over and pressing it, produced a pristine clear oil, which was tasty enough to dropper.

 

The most flavorful, was the ghee, and possibly the fastest to uptake and produce an effect. Alas, after just testing just enough of each of them to determine their flavors, I needed a nap, so the next phase of this project, is to titrate for potency and effect, as well as flavor, using volunteer test panels.

 

We also will experiment with different ways to use the oils in medibles, so I will update this post as they occur:

 

Oils-1-1.jpg

 

Leafmaterialforextraction-1-1.jpg

 

Boilingjarsofoil-1-1.jpg

 

Commercialricer-1-1.jpg

 

Dumpingjars-1-1.jpg

 

Foldovercloth-1-1.jpg

 

Pressing-1-1.jpg

 

Extractedoils-1-1.jpg

 

Copied from:

 

http://skunkpharmresearch.com/extracting-with-oils-and-fat

 

Ask questions of Graywolf and the other Pharmers by making an account today free.

 

Source: Extracting With Oils and Fats

EDDIEKIRK

For ya’ll brothers and sisters doing serious extraction and alchemy requiring a stirring hotplate, heads up, cause we’ve been testing a CAT MCS 66 that bears your attention and investigation.

We use a stirring hot plate for various things and have gotten by using our aging Thermolyne, but have never been able to maintain accurate even heating in the low ranges between 18C/85F and 46C/115F, so it requires constant monitoring.

We’ve tested the CAT MCS 66 in a variety of different applications, both in the lower ranges, as well as above 100C/212F, and it adds new meaning to the word steady.

For instance, it kept a solution at 46.C for two days without ever flickering to 45.9 or 46.1C.

Wanna talk about stirring ability? How about spinning a stir bar in cold vegetable glycerin through a stainless steel bain marie container? Hee, hee, hee…………..

Check out this vortex with water at less than half throttle……..

 

cat-scientific-hot-plate-at-46c-1-1.jpg

Those of ya’ll who like to play with buttons, will love the digital LCD display, and array of membrane button choices. Besides individual on/off buttons for overall power, there are individual controls for the plate power and the stirring motor. There are two up down buttons, and selection buttons for setting plate temperature, stirring motor rpm, container volume, how fast a ramp up, timer, upper limits, and monitoring the temperature of an emersion thermocouple that plugs in to the base.

The thermocouple monitors the actual temperature of your solution, separate from monitoring set point and hot plate surface temperature. With water, at 36C set point, the hot plate held steady at precisely 36C, and the 500 ml of water came up to and stabilized at a rock steady 28.5C.

cat-s-hotplate-1-1.jpg

 

read and ask questions

http://skunkpharmresearch.com/cat-scientific-mcs-66-stirring-hotplate-test/

EDDIEKIRK

The Mk IVA Phoenix Terpenator
Posted December 7, 2013 by Skunk Pharm Research,LLC in Projects. 7 Comments
Behold the Mk IV Phoenix, risen from the ashes of the Chimera and embracing everything that we’ve learned to this point.
This prototype has a 10″ X 12″ lower spool and a 4″ X 36″ column. I put that size column on it for a January shoot out in Seattle, but it will accept anything from a 2″ X 24″ column up to a 4″ X 36″ column.
One of the things that we’ve learned and which has been addressed in the Mk IVA, and that is that stainless to stainless threaded fittings can be problematic, so the IVA uses welded manifolds, rather than manifolds assembled out of pipe fittings.
It has two sight glasses to monitor what is going on, and has a thermocouple in the tank, to monitor the internal temperature during processing.
Read more at http://skunkpharmresearch.com/the-mk-iva-phoenix-terpenator/:
Posted ImagePosted Image

See more

EDDIEKIRK

A05Bapothecary.jpg

APOTHECARY JAR'S & BOTTLES:
(BULK CONTAINERS)

While glass containers (bottles etc.) existed well before the 19th century, one must always keep in mind that until the latter part of that century, the glass container could easily cost more than the product that was being sold inside it. Given that cost factor, it was expected that once empty, the bottle would be cleaned and reused. It was expected and normal for the druggist to take an apothecary jar off the shelf and simply fill or refill the customer's container.

Picture Gallery of Veterinary Products S02Apothecary.jpg S03Apothecary.jpg S05Apothecary.jpg S06Apothecary.jpg S10Apothecary.jpg S12Apothecary.jpg S13Apothcary.jpg S14ACannabisTin.jpg S15Apothcary.jpg Sbesjar.jpg SFake.jpg S16Apothcary.jpg S18Apothcary.jpg S11Apothecary.jpg SC02Apothecary.jpg S89_3.jpg SApothcary.jpg S10BulkCabinet.jpg S03ABulkTin.jpg http://antiquecannabisbook.com/images/SShowGlobe.jpg


3.0- Apothecary (Cannabis) Containers:

3.1 - About Apothecary Containers:
Like all so many other collectors before me, I mistakenly used to think of these old pharmaceutical containers (whether ceramic jar or glass bottles) as being analogous to some of those old decorative glass cake & pie stands, that can still be found on many a mom & pop restaurant counter. They act as advertisements to remind one of dessert. They beautify the pies, make them look more desirable and, I suppose, more saleable, but other than that have absolutely nothing to do with the pies themselves. And even ignoring the fact that the pies are being oxidized, actually ruining their taste, it still makes for a lot of work just to keep them clean and maintained.

However, the more one delves into the subject, the more impressed one becomes. Some of these old apothecary containers (the show-globe's) were more than just pretty advertisements; they even served as one of our first national heath alert systems. According to the California Pharmacists Association:

"Upon entering a western frontier town, visitors would look to the [apothecary] show-globe in the drug store window to see which color liquid it contained. Red indicated the town was besieged by an epidemic."

In order to truly appreciate the importance of apothecary containers, one must remember that while glass containers (bottles etc.) existed well before the 19th century until the latter part of that century, the glass container itself could easily cost more than the product that was being sold inside it. Given that cost factor, it was expected that once empty, the bottle would be cleaned and reused. It was also expected and normal for the druggist to take an apothecary jar off the shelf and simply fill or refill the customer's container.

It should also be noted that in the 19th century, and even into the early part of the 20th century, it was common practice for pharmacists to manufacture at least some of their own medicines. The pharmacist (who in many cases was also the local town general store owner) would simply ask local farmers to grow Indian Hemp (among other herbs) for them. Cannabis (the flower tops of the hemp plant) thus obtained would then be prepared and either stored in apothecary jars until sold in bulk (solid or powder) form or taken to the back room and brewed into tinctures or other medicines.

And while, realistically speaking, most of these bulk preparations would end up in the back room (most likely stored in bins and old boxes) at least those placed by the front counter would be stored in apothecary containers.

But still after all is said and done, it must be remembered that the apothecary jar's main purpose was as an early form of advertising. The more beautiful the container the better the sales. And this, at a time before brand-name products and Madison Avenue, was no small feat.


3.2 - APOTHECARIES - (A Time Line):
Leaving aside Tin's and Box containers; In general, apothecary containers can be subdivided into ceramic jars (used to store solid or powdered Cannabis flower tops) and glass bottles (used mostly for liquid tinctures). The jars normally had large lids to allow for a hand to reach in, and the glass bottles used for tinctures would have smaller bottlenecks, for poring.

Apothecary containers can range anywhere from beautifully crafted multicolor vessels to the cheapest glass jars with only a label to distinguish them. They could have been custom built in glass houses, or originally meant for other purposes (say to store peach preserves), and simply utilized for this purpose because of their size. Note: Pharmaceutical wholesale books were full of pre-printed labels for sale, just for this purpose.

I myself put the golden age for Cannabis apothecary containers between 1840 and 1910. And while Cannabis was still well in use into the 1930's, it must be remembered that by the late 19th century "brand-name drugs" slowly began to replace locally grown products. People wanted the security and presumed superior quality that a "brand name" could give them.

As more and more pre-packaged medicines made their way unto store shelves, the age of the apothecary came to an end. By the late 1930s, old apothecaries were more likely to hold candy than medicines.


3.3 - HEMP SEED OIL:
As can be seen by the photos [see Pictures], the flowering tops were not the only medical parts of the Hemp Plant that was sold in apothecary shops. [see Chapter 19 -- On Medical Hemp Seed Oil.] Although, it is unclear from the label whether this container was used to store plain Hemp Seeds or actual Hemp Seed Oil.


3.4 - APOTHECARY / BULK CONTAINER:
Not all pharmacists stored their Cannabis (as well as other bulk medicines) in Apothecary jars. As can be seen by the photos, [see Pictures] some simply used multi-drawer wooden cabinets. These cabinets looked pretty much like the ones found today in Chinese herb shops. [Reference should be made to Chapter 5 -- Cannabis Bulk Containers]


3.5 - CERAMIC JAR APOTHECARIES:
While Large (Display) Glass Bottles worked fine for liquid (Cannabis) Tinctures and such. They were impractical for use with the solid (loose-leaf) medical products also sold in bulk by pharmacies. Simply put, the bottle tops simply weren't practical (or big) enough for the job.

Thus (for obvious reasons) Ceramic Jars also found there way onto the sheaves of most apothecary shops. Like their glass bottle counterparts, they were attractive (some being hand painted works of art) and thus served as a good advertising tool, but most important of all, they had BIG lids, which allowed the proprietor to stick his/her hand in and scoop up the product.


3.6 - BULK TIN CONTAINERS:
[see Chapter 5 -- Cannabis Bulk Containers]
When dealing with antique Cannabis Tin Containers, the main problem the antique collector quickly finds is that their really aren't that many of them still around today. While Glass and Ceramic containers are still abound, Tin Containers (Mostly due to their ugliness I feel) simply weren't kept.


3.7 - PRICES AND FRAUD WARNINGS:
One would assume that as a rule of thumb the well-crafted custom-built ones, which seem to have been used mostly by pharmacies on the east coast, and in many cases were imported, would carry the most value. And to some extent that is true.

But the market is kind of crazy right now, with no rhyme or reason. So long as the label "Cannabis" can still be seen, even the cheapest lousiest-looking things are going for outrageous prices.

Prices at the present time are outrageous. If the apothecary says "Cannabis," as opposed to, say, belladonna, then be prepared to add a zero to the price tag. Even cheap glass containers (as long as the label "Cannabis" is still readable) are going for hundreds of dollars and the custom-built ones going for over $600. I myself will not even try to give a price range for them right now. As a rule of thumb, find a similar container, add a zero to the price and multiply by two, but again that is just a rule of thumb.

But if the warning "let the buyer beware" ever applied, this is it. We are dealing with a product where (in many cases) only a label stands between an old piece of junk glass and a hundred-dollar apothecary antique. And if that label reads "Cannabis," then the price goes up a couple of hundred dollars or more. And the problem is that many of those old labels are still lying around out there waiting to be used.

Without any proof, I would say that at least 50% of the cannabis apothecary jars now in circulation are out-and-out fakes. And because of the high demand we can expect that figure to grow.

Even the crafted custom apothecaries can be deceiving; I've seen one that looked so beautifully well preserved that its label could have been painted just a few years ago---and after a close examination, I would say that it was.

Only the label under glass (where the label was sandwiched between two layers of glass) type seem to be reproduction-free for now. But given the interest and steadily raising demand and increasing prices, I feel it's only a matter of time.

In general (and with great sadness) I would advise the first-time collector to avoid the area of apothecary containers altogether, until a certain degree of expertise is developed. Rule of thumb; if you can't figure out how to fake one, don't buy it.

EDDIEKIRK

Decarboxylation

Decarboxylation

Posted by Skunk Pharm Research,LLC.

Cannabis produces phyto cannabinoids in a carboxylic acid form that are not orally active at least at the CB-1 receptor sites, because they don’t readily pass the blood brain barrier in their polar form.

To enable them to pass the blood brain barrier, they must first be decarboxylated, to remove the COOH carboxyl group of atoms, which exits in the form of H20 and CO2.

Decarboxylation occurs naturally with time and temperature, as a function of drying, but we can shorten the amount of time required considerably, by adding more heat. The more heat, the faster it occurs, within reasonable ranges, and in fact occurs spontaneously when the material is burned or vaporized.

There is another mechanism at play however, which suggests that we need to control the decarboxylation temperatures carefully.

When we heat cannabis to convert the THCA and CBDA into THC and CBD, we are also converting THC to CBN at a faster rate. At about 70% decarboxylation, we actually start converting THC to CBN at a faster rate than we are converting THCA to THC, so as you can see by the following graph, after about 70% decarboxylation, the levels of THC actually start to fall sharply.

That of course means that the CBN also begins to rise and the medication is becoming more sedative.

Thank you Jump 117 for this excellent graph!

decarboxylation-graph-1-11.jpg?w=855&h=861

Decarboxylation graph

Another fly in the ointment, is that we can never know for sure exactly what the starting state of decarboxylation is, so the times at temperature shown on the graphs are an average.

We can’t expect dry material placed in an oven at any given temperature to be that uniform temperature throughout instantly upon placing it in a heated oven, nor know for sure the state of decarboxylation by simple observation.

Decarboxylating plant material, also alters the taste (roasted/toasted), which some find less agreeable, and of course decarboxylating also evaporates away the smaller Monoterpenes and Sequiterpenes alcohols, phenols, ketones, aldehydes, ethers, and esters.

The good news is that it is dirt simple to monitor the state of cannabis oil decarboxylation placed in a 121C/250F hot oil bath, because you can watch the CO2 bubble production.

Just like the curves suggest, CO2 bubble production will proceed at its own observable rate. By keeping the puddle of oil lightly stirred on the bottom and in the corners of the pot (I use a bamboo skewer), so as to keep the bubbles broken free and floating to the top, you can tell exactly when the bubble formation suddenly tapers off at the top of the curve.

That is the point that we take it out of the oil for maximum head effect, and we leave it in until all bubbling stops, if we want a more sedative night time med.

Here are a couple pictures of what oil looks like when boiling off the residual butane. Residual butane or alcohol produces larger, randomly sized bubbles, and is fully purged, when they cease.

I am seemingly missing the middle picture of the CO2 bubbles, so I will add it later, but the second picture shows what fully decarboxylated oil looks like.

purging-in-hot-oil-bath1.jpg?w=450&h=302

Residual solvent bubbles above:

quiescent-oil-1-11.jpg?w=855&h=572Quiescent oil.

 

Join us here on the site to talk with the Pharmers today.

EDDIEKIRK

Sold out and over booked

Posted October 27, 2013 by Skunk Pharm Research,LLC in Projects. Leave a Comment

Hi ya’ll!

The response to our classes this year has been nothing short of phenomenal, with most classes ending up overbooked. Sorry to ya’ll that didn’t make it, but except for truffle making, our public classes are all overbooked for the rest of the year and we have stopped accepting applications. Please watch for our class offerings next year.

We are also sold out for Dr. Fischedick’s 11-2 lecture on Cannabis Terpene Profiles, but will film his presentation, and his lecture will subsequently be available on DVD.

 

http://skunkpharmresearch.com/2013/10/27/sold-out-and-over-booked/

EDDIEKIRK

 

For those of ya'll wishing to vacuum distill your butane to remove any heavier components, before using it for extraction, here is a design for the cold trap that we will be using as a test sled, to not only vacuum distill the butane, for further polish filtering it through a Bentonite, zeolite, etc, column.

 

The way it works, is that the butane is injected into the cold trap as a liquid and pumped off as a vapor, leaving behind those things with a higher boiling point.

 

I set my cold trap in 85F water. You can do it without setting the trap in warm water, but as the butane boils off under vacuum, the transition from liquid to vapor, liberates the heat of vaporization, and plunges the temperature of the pool of butane to below its boiling point, so the process moves in starts and stops.

 

The next Alkane boils at about 36.1C/98.6F, at atmospheric pressure, so it is important to not heat the pot much beyond about 85F. The thermometer in the cold trap lid will tell you at what temperature your butane pool is during the cycle.

 

It is also important to not recover the butane below where the compound pressure gauge reads zero pressure, zero vacuum, or 14.7 PSIA.

 

PSIA is pounds per square inch absolute, which starts at absolute zero, without the weight of the atmosphere (at full vacuum). The atmosphere weighs 14.7 pounds per square inch, which is what a 1" column of mercury 29.92" tall weighs.

 

We do this operation outside and recommend that everyone do the same. Even though it is ostensibly a fully enclosed system, what if there is a leak or something goes wrong, goes wrong, goes wrong..........?

 

I recommend that you read and heed the thread on Butane Safety, before embarking on this journey. http://skunkpharmresearch.com/butane-safety/

 

Pull a full vacuum on the empty 50# refrigerant recovery tank for the first time, and valve it off.

 

Attach the pressure gauge to the cold trap via 1/4" refrigerant hose and pull a full vacuum on the trap, and valve it off, before assembling the system.

 

To vacuum distill using the cold trap, attach a 1/4" refrigerant hose to the inlet of the cold trap, and the other end to either an LP-5 tank of n-Butane, or to a can tapper, preferably with a ball valve attached at the tapper.

 

Attach the 1/2" outlet hose to the top of the filter section and the other end goes to the inlet of a refrigerant recovery pump.

 

We've used a couple of inexpensive brands for this purpose, namely the Appion G-5 twin and the CPS T-21, but neither are not rated by the manufacturer for butane, because they are not explosion proof should a leak occur.

 

Our larger commercial sized Mk V Terpenator will have the more expensive Caresaver Universal, or a Haskell pneumatic refrigerant recovery pump as an option, that are rated for flammable refrigerants, such as R-600 (n-Butane).

Depending on your situation, you should pick an option that fits your needs and safety needs.

 

The other hose goes to the red liquid dip tube valve on the 50# refrigerant recovery tank, which is sitting in an ice bath. If you really want to fly, set it in a denatured alcohol bath, with chunks of dry ice dropping the temperature to -70F or so.

 

Start the refrigerant recovery pump and the open the red valve on the refrigerant recovery tank, as well as the outlet valve on the cold trap.

 

If you are using an LP-5 tank of n-Butane, set the tank on a refrigerant scale and weigh it. Record the weight and push tare on the scale.

 

Open the inlet valve on the cold trap slowly and transfer about two liters of butane, or about 1146 grams, 2.5 lbs. Close the inlet valve.

 

The pressure gauge will have gone from -29.92" Hg vacuum, to positive pressure in the range of 10 to 30 psi. Watch until the pressure gauge drops to zero pressure, zero vacuum, and then load another 2 liters for distillation.

 

If you are using canned butane and a can tapper, close the valve at the can tapper, and open the inlet valve on the trap fully.

 

Tap the can and open the ball valve at the tapper. The pressure will rise from zero, to positive pressure. When the recovery pump lowers the pressure back to zero pressure, zero vacuum, close the valve at the tapper and tap a new can.

 

Open the valve to drain that can as well, and continue this cycle until all cans are empty.

 

Once you have emptied the LP-5 or the cans, when the pressure reaches zero again, close all valves and turn off the recovery pump.

 

Disconnect the hoses from the trap and open all valves to let it breath.

 

Remove the lid to the cold trap to remove the materials removed from the butane, and clean the trap with denatured alcohol for the next batch of butane.

 

 

 

 

 

 

Source: Vacuum distilling butane

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