Hexane Honey Oil extraction and alchemy

[Gray Wolf]

Hey Gray Wolf!
Again I am delighted with this photo, excellent color of solution!

It is a pity a little bit that there is no photo "before" for comparison.
How many percent weighed remote "paint"?

Please, you will tell in more detail about this procedure and or properties of the applied materials. It is very interesting!



PS
Such success deserves the separate special detailed illustrated report, much more valid, than a mention of it casually.
It would be very interesting to see photos not only solutions, but also the dried-up extracts "before / after", with the indication of their scales.

Here are pictures of the next whole run. The procedure involves pouring the oil, dissolved in hexane, through a column of chromatography beads to strip out the polar elements.

Included is a smaller picture showing only four of the key extracts.

After the non polar elements are collected, the column is flushed with a polar solvent, which releases all the polar elements and flushes them through. The last couple of pictures are from the polar flush and the lighter ones are the goodies.

A GC run verified that the cannabinoids are in the light extractions and the darker elements are cannabinoid free.

Alas, I'm waiting to publish the study until Oregon Medical Growers finishes packaging their proprietary column mix, and is ready to deliver product.

We mixed the beads with hexane and poured them in the column, before applying 100psi air pressure to compact them. They are then ready to drain the hexane out and ready to use.

I am planning a complete writeup, as soon as folks have some place to go for the columns. I'm pushing a little to speed things up, but am not in charge or in a position to control the schedule.

 

[squarepush3r]

Here are pictures of the next whole run. The procedure involves pouring the oil, dissolved in hexane, through a column of chromatography beads to strip out the polar elements.

Included is a smaller picture showing only four of the key extracts.

After the non polar elements are collected, the column is flushed with a polar solvent, which releases all the polar elements and flushes them through. The last couple of pictures are from the polar flush and the lighter ones are the goodies.

A GC run verified that the cannabinoids are in the light extractions and the darker elements are cannabinoid free.

Alas, I'm waiting to publish the study until Oregon Medical Growers finishes packaging their proprietary column mix, and is ready to deliver product.

We mixed the beads with hexane and poured them in the column, before applying 100psi air pressure to compact them. They are then ready to drain the hexane out and ready to use.

I am planning a complete writeup, as soon as folks have some place to go for the columns. I'm pushing a little to speed things up, but am not in charge or in a position to control the schedule.

nice fractions you got there!

 

[jump117]

The procedure involves pouring the oil, dissolved in hexane, through a column of chromatography beads to strip out the polar elements.

You wrote that the polarity of THCa is higher than THC due to the carboxyl group-COOH.

Will the chromatographic beads distinguish THCa from polar colorants and allow them to go with non-polar,
or the process works only with neutral THC?

 

[squarepush3r]

You wrote that the polarity of THCa is higher than THC due to the carboxyl group-COOH.

Will the chromatographic beads distinguish THCa from polar colorants and allow them to go with non-polar,
or the process works only with neutral THC?

yes, it should work with THCA, make sure your elutant is hexane or something else pure non-polar (not mixed).

http://www.researchgate.net/publica...sativa_using_two_flash_chromatography_systems

ABSTRACT Two isolation procedures for Δ9-tetrahydrocannabinolic acid A (THCA), the biogenetic precursor in the biosynthesis of the psychoactive Δ9-tetrahydrocannabinol (THC) in the cannabis plant, are presented. Two flash chromatography systems that can be used independently from each other were developed to separate THCA from other compounds of a crude cannabis extract. In both systems UV absorption at 209 and 270 nm was monitored. Purity was finally determined by HPLC-DAD, NMR and GC-MS analysis with a focus on the impurity THC. System 1 consisted of a normal phase silica column (120 g) as well as cyclohexane and acetone--both spiked with the modifier pyridine--as mobile phases. Gradient elution was performed over 15 min. After the chromatographic run the fractions containing THCA fractions were pooled, extracted with hydrochloric acid to eliminate pyridine and evaporated to dryness. Loading 1800 mg cannabis extract yielded 623 mg THCA with a purity of 99.8% and a THC concentration of 0.09%. System 2 was based on a reversed-phase C18 column (150 g) combined with 0.55% formic acid and methanol as mobile phases. A very flat gradient was set over 20 minutes. After pooling the THCA-containing fractions methanol was removed in a rotary evaporator. THCA was re-extracted from the remaining aqueous phase with methyl tert-butyl ether. The organic phase was finally evaporated under high vacuum conditions. Loading 300 mg cannabis extract yielded 51 mg THCA with a purity of 98.8% and a THC concentration of 0.67%.

 

[Gray Wolf]

You wrote that the polarity of THCa is higher than THC due to the carboxyl group-COOH.

Will the chromatographic beads distinguish THCa from polar colorants and allow them to go with non-polar,
or the process works only with neutral THC?

Yes, the chromatographic beads will distinguish some the difference and the carboxylic acids come off in a different fraction than the less polar form.

I was a little brief in my description of stripping the column after passing the non polar solvent, in that instead of just dumping a non polar solvent through it, we start by running a 5% polar solution through and then a 10% etc, so as to extract the different fraction bands.

Instead of polar and non polar washes, it is more like less polar followed by more polar washes.

 

[SpaceshipNelson]

Please don't use MTBE. . . Ever. . . . .Ever ever ever. . . . EVER! . . . . .

 

[squarepush3r]

just wanted to update, I did some experiments with some fairly crude extracts (starting point about 45% THC/black color isopropyl extract) using chromatography , and refined it down to a very light color amber liquid. I tested the final amber solution, and to my surprise it was even lower THC than the starting point, leading me to believe that the extracts were terpenes/beta carotene and my method for refining THC was ineffective.

so, in summary
-45% THC crude oil/oil extract, refine/filter with silica and non-polar solvents

end up with
-very light amber solution, when solvent was removed and tested using Gas Chroma, came much lower in THC than the original crude.



So my conclusion is a lot of the THC was actually still in the silica stationary phase, even though it appears to be mostly black.

 

[RitualDelFuego]

Anyone in here know if there is any difference between n-Hexane and "Hexanes reagent ACS"??

trying to figure out if reagent grade assayed at 99.9% hexanes will be suitable for this sort of extract work? Also, if winterization is desired why not do a single solvent DeWax and simply inject the ethanol during the final purge to ensure total removal of petrochemicals??

anyone???

 

[Gray Wolf]

Anyone in here know if there is any difference between n-Hexane and "Hexanes reagent ACS"??

trying to figure out if reagent grade assayed at 99.9% hexanes will be suitable for this sort of extract work? Also, if winterization is desired why not do a single solvent DeWax and simply inject the ethanol during the final purge to ensure total removal of petrochemicals??

anyone???

Hexanes reagent ACS is a mixture of hexane isomers, plus some methylcyclopentane.

Here is an MSDS for hexane isomers, showing a typical blend of n Hexane, Isohexane, Neohexane, and Dimethylbutane.

http://www.mesagas.com/images/Hexane.pdf

Dimethylbutane is classified as an A-1 human carcinogen according to the attached MSDS.

https://www.airgas.com/msds/002683.pdf

 

[RitualDelFuego]

Sure. So we will refrain from pouring any on our morning pancakes.

I notice all isomers boil off below 170F which leads me to believe a very amount of ethanol and a diligent use of a vacuum oven might be all it takes to make it clean

the HHO i made last week seems fine , purged 48hrs in the spool then another 24 in an oven at 40C and hard vac

 

[Gray Wolf]

Sure. So we will refrain from pouring any on our morning pancakes.

I notice all isomers boil off below 170F which leads me to believe a very amount of ethanol and a diligent use of a vacuum oven might be all it takes to make it clean

the HHO i made last week seems fine , purged 48hrs in the spool then another 24 in an oven at 40C and hard vac

I try to avoid solvents identified to be a carcinogen, mutagen, or teratogen altogether, because medicating with it is a chronic exposure, and I'm uncomfortable with what that might do over time.

Attached is the FDA solvent standard list, giving the minimum levels it should be removed to as 2.9 mg/day or < 290 ppm, and placing Hexane (S) in the Class 2 group, which says:

Solvents in Class 2 (Table 2) should be limited in pharmaceutical products because of their inherent toxicity.

PDEs are given to the nearest 0.1 mg/day, and concentrations are given to the nearest 10 ppm.

The stated values do not reflect the necessary analytical precision of determination. Precision should be determined as part of the validation of the method.

We've had our best results purging n-Hexane, using ethanol and cold boiling it away under vacuum.

Hexane smells and tastes like gasoline, and most people can detect it at around 130 ppm, with trained threshold perception around 22 ppm.

If you can't smell or taste it, with average sensory perception, it is ostensibly below those levels.

 

[JamesFarmer]

I still have visible scars from my last chemistry class 30+ years ago....

 

[Old Gold]

I still have visible scars from my last chemistry class 30+ years ago....

Care to explicate?
I've seen someone hand over a hot metal rod by the heated end, after removing from a Bunsen burner. So injuries are injuries, not inherent faults in the solvent/reagent use.
Scars from what? Hexane fume inhalation?

 

[corky1968]

I can't wait to try this Hexane stuff as I find butane and pentane too dangerous for nothing

I found a reasonably pure source of OTC N-Hexane.
I'll be cleaning it up with a separatory funnel that I
still have to buy and my glass still once I get going.

I'm even looking at getting a soxhlet extractor.
I'm going to run a second condenser on top to
really make sure no N-Hexane escapes at any time.

I'll be recycling and repurifying my N-Hexane at
each usage to avoid wasting it and cutting costs.

 

[Gray Wolf]

I can't wait to try this Hexane stuff as I find butane and pentane too dangerous for nothing

I found a reasonably pure source of OTC N-Hexane.
I'll be cleaning it up with a separatory funnel that I
still have to buy and my glass still once I get going.

I'm even looking at getting a soxhlet extractor.
I'm going to run a second condenser on top to
really make sure no N-Hexane escapes at any time.

I'll be recycling and repurifying my N-Hexane at
each usage to avoid wasting it and cutting costs.

Pentane is still liquid until around 36C/97F, so not in the same category as Methane, Ethane, Propane, and Butane.

Hexane is the next simple Alkane after Pentane, which sadly our livers turn into 2.5 Hexanedione.

https://en.wikipedia.org/wiki/Hexane-2,5-dione

That makes it imperative that it be purged below FDA standards for Pharmaceuticals. Note that Hexane is a Class 2 solvent, while Pentane is a Class 3 in the attached list.

 

[corky1968]

Pentane is still liquid until around 36C/97F, so not in the same category as Methane, Ethane, Propane, and Butane.

Hexane is the next simple Alkane after Pentane, which sadly our livers turn into 2.5 Hexanedione.

https://en.wikipedia.org/wiki/Hexane-2,5-dione

That makes it imperative that it be purged below FDA standards for Pharmaceuticals. Note that Hexane is a Class 2 solvent, while Pentane is a Class 3 in the attached list.

I know about Pentane. But when the average room temperature is 20-25°C already.
It's doesn't give you much leeway before things start boiling. Also to purify it from
an OTC substance that I can get would take a lot more work.

This why I'm going with my OTC N-Hexane source.

Although, I'll probably purify some N-Pentane anyways later on to say I have some as well.

 

[einsteinlady]

If you are rotovaping hexane under vacuum what temperature would you set water bath to?

 

[Gray Wolf]

About 25C.

 

[G.O. Joe]

Depends on the condenser load which depends on all the other variables. And maybe your desire to keep low boilers in the extract. Both the evaporator and condenser are set for the temperature where all the condensation is in the first 2/3 of the condenser, given whatever you've got going on especially vacuum-wise. If you have a vacuum controller and enough vacuum it depends on your ability to condense.

 

[Gray Wolf]

Depends on the condenser load which depends on all the other variables. And maybe your desire to keep low boilers in the extract. Both the evaporator and condenser are set for the temperature where all the condensation is in the first 2/3 of the condenser, given whatever you've got going on especially vacuum-wise. If you have a vacuum controller and enough vacuum it depends on your ability to condense.

Good point, all systems are not created equal,

If you max out your chiller and flow to the condenser, you can tweak the temperature up or down to keep the vapor 2/3rd up the condenser.