What's new
  • Please note members who been with us for more than 10 years have been upgraded to "Veteran" status and will receive exclusive benefits. If you wish to find out more about this or support IcMag and get same benefits, check this thread here.
  • Important notice: ICMag's T.O.U. has been updated. Please review it here. For your convenience, it is also available in the main forum menu, under 'Quick Links"!

Washing chlorophyll out with hexane: worth the trouble?

pinkus

Well-known member
Veteran
I finally decided to make some cartomizers (might not be the right term) because that is what is being bought by my former flower smoking clients.

I opted for an ethanol extraction supplemented with dry ice in a cooler. It all seemed to be going well until the first filtering. I stupidly thought that coffee filters would be sufficient. Of course as soon as I started filtering it, I became aware that getting the liquid through the filter and separate from the weed was taking way too long. Sure enough, the resulting ethanol had a greenish tint. I went ahead and put the jars in the sun for about three hours to turn the green amber.

I am also planning on thinning the oil with terpenes instead of PG or VG. I have some "pineapple express" terps and a "flavourless terp" branded as "cutter". They are both Fogg Flavours brand.

Any constructive advice and info would be welcomed.

Thanks.
:shooty:

BTW, I do have a separatory funnel. That should make a hexane wash somewhat easy.

Also, I would like any information about where to get, and the preferred types of hexane. Where I am, the local chemical supply houses won't sell to me, but a few cities that Will are within driving distance.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
1) dissolve it in some 190 proof ethanol

2) chill it down to get the unwanted waxes to drop out

3) pour off the liquid leaving the waxes behind (maybe pour off through fast filter paper if the waxes are in solution)

4) add a little water and some pentane, and shake

5) remove the pentane layer with a pipette

6) add more pentane, shake, and remove the layer

7) repeat #6 until the pentane layer is clear

8) evaporate off the combined removed pentane layers, and then vac purge at low temperature


This is the process described in Cannabis Alchemy by D Gold, Chapter 1, Step 6 with Figure 1.6 & 1.7 which can be accessed for free by clicking on the link in my ICMAG Signature below. You don't need a sep funnel for this, you're pulling off the top layer.

Everything you need to know about choosing and no hassle purchasing of solvents in the USA can be found by clicking on the Solvents listed as to polarity link also in my Signature. (Sorry, Consolidated Chemical & Solvents is closed, most likely permanently.)

Hexane is either pure n-hexane or a mixture of n-hexane and the hexane isomers, the latter is referred to as 'hexanes.'

Pentane or heptane is preferable to hexane, as hexane smells strongly like gasoline, and is more toxic than pentane or heptane. See the FDA Q3C — Tables and List Guidance for Industry,
https://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/UCM073395.pdf


"The oil from the extraction is dissolved in five times its weight of alcohol and poured into an equal volume of water in a large glass jug with a screw-on cap. All solvents used are cold or cool. A volume of petroleum ether equal to half the volume of the water used is added. The screw top is tightened and the jug is inverted. The jug is turned upright immediately, and a few seconds later, when the mixture has run down the sides of the jug, the screw cap is opened slowly to relieve the pressure. The inversion of the jug is repeated about twenty-five times, which releases the pressure each time, and then the jug is allowed to sit for about half an hour. The mixture of liquids will separate into three distinct layers. The bottom layer will contain water, alcohol, and the substances in the oil (tars and resins) that are not soluble in petroleum ether. The thin middle layer is an emulsion of waxes, ether, and air bubbles. The top layer is the purified oil dissolved in petroleum ether.

The jug is fitted with a two-holed rubber stopper, glass tubing, and rubber hose. Two pieces of glass tubing are fitted into the two-holed rubber stopper. (Injuries when cutting and fitting glass tubing are frequent—cut ends are always fire-polished and hands must be protected when any force is used in fitting the tubing.) One piece of tubing need only protrude from the stopper an inch on each side. The other tube is positioned so that when the stopper is tightly fitted to the jug, the tube extends into the mixture to a half-inch from the bottom of the ether/oil layer. The other end of the tube is attached to a length of rubber tubing to transfer the ether/oil solution to a collection jug. The end of the tubing must be lower than the end of the tube in the ether/oil solution in order to obtain a siphon action. A short piece of rubber tubing is fitted to the short glass tube, and air pressure is applied to start the siphon.

The glass tube is spaced a bit above the emulsion layer; any ether/oil solution not removed will be recovered later. The ether/oil solution in the collection jug is saved. Another volume of fresh petroleum ether is added to the extraction by inverting, separating, and collecting the ether solution, which is added to the first ether/oil solution. This process is repeated until the ether layer remains clear after inverting. This indicates that the ether-soluble oil is totally extracted from the alcohol-and-water layer."


The petroleum ether referenced is the low boing point ~35-60C cut containing mostly pentane with some hexane. Imo, it's best to avoid the hexane altogether if possible, therefore the pentane or heptane recommendation.
 

Attachments

  • Screen Shot 2018-07-25 at 9.04.52 AM.jpg
    Screen Shot 2018-07-25 at 9.04.52 AM.jpg
    44.4 KB · Views: 49
  • Screen Shot 2018-07-25 at 9.04.16 AM.jpg
    Screen Shot 2018-07-25 at 9.04.16 AM.jpg
    35.3 KB · Views: 54
Last edited:

pinkus

Well-known member
Veteran
Thanks for all the info.


Is it worth it to go to the trouble with slightly more than a slight amount of chlorophyll? I am NOT very experienced with modern cannabis concentrates.

:bandit:
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Pentane's a good investment, low odor, nearly as non-toxic as butane or propane, and it can be purged easily without vacuum if necessary with just low heat like from a seedling heat mat (<120F) and a little fan blowing over it spread out in a thin film in a Pyrex casserole dish.

Try a small scale extraction using pentane alone, you don't even need to chill the pentane much, it's extremely non-polar like butane or propane. The main reason for the two step process with alcohol is economics - ethanol is cheaper and more readily available, so loosing some in the initial extraction and filtering of the plant material is ok, while the second stage pull off requires only a relatively little amount of pentane.

Heptane is also a nice one step non-polar extraction solvent, but it's higher boiling point means a long purge off using just a seedling heat mat and fan. Available in pure enough form ubiquitously at very reasonable prices, everyone should pick up a quart and become familiar with it.


A pippete pump provides 100x the control of a rubber bulb on a pipette, smooth, really smooth. You don't want to disturb the other layers when doing the pull off, and the rubber bulb is a herky-jerky mess.

https://www.amazon.com/gp/product/B00191BXTG/ref=oh_aui_search_detailpage?ie=UTF8&psc=1
 

Attachments

  • P1030458.jpg
    P1030458.jpg
    106.9 KB · Views: 39
  • P1030461.jpg
    P1030461.jpg
    91 KB · Views: 36

pinkus

Well-known member
Veteran
I am curious about your thoughts as to why the siphoning setup would be preferable to using a sep funnel?

Thanks!
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
I am curious about your thoughts as to why the siphoning setup would be preferable to using a sep funnel?

Thanks!


I honestly can't figure out how one would use a sep funnel to remove the upper non-polar solvent layer.

I have a suspicion very few have actually tried the non-polar wash as described in Cannabis Alchemy, instead most everyone's described doing repeated saline washes of the non-polar solution which does indeed work best with a sep funnel.

The Cannabis Alchemy process results are dramatic, follow the instructions exactly, and you'll have some nice oil.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
But then you have to return the bottom layers to add more non-polar solvent and repeat the process, repeat the process...

And the pristine non-polar solvent/oil layer is being dragged through the area of the sep funnel that is coated with residuals from the bottom two layers. You do not want water in your non-polar solution, it'd be a hassle to purge compared to pentane, and it might lead to waxing up before you get it out.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Highly recommended reading,

THE ORGANIC CHEM LAB SURVIVAL MANUAL
A Student’s Guide to Techniques
JAMES W. ZUBRICK

Free download of the ninth edition,

https://b-ok.xyz/book/2172555/352514

Chapters 13-16 are specifically pertinent, 15 very much so.

So actually what we are discussing is an extraction, not a wash.
 
Last edited:

troutman

Seed Whore
If you used hexane alone as your primary solvent you wouldn't have this chlorophyll problem I bet. ;)

I had lots of fun playing with methanol as my primary solvent last time.
Talk about a green mess of an extract. :biggrin:
I won't use any alcohol as a primary solvent again.

My next try will be using dry n-hexane as my primary solvent.
This will then be distilled and finally purged using dry ethanol.
Distillation of the ethanol should give me a nice product.
 

Mengsk

Active member
Lots of good info from the experts here. Moving right along :) Funny theme, 'stoners' 'potheads' idk did anyone else ever cut class? But there is good chemistry here in this thread, as in the best chemists might not get the best grades they might not even kiss ass or buy apples for the teacher but get the job done.


I have used the QWISO method and as long as you keep everything in the freezer (most utensils, whatever will be in contact with the flower) or even better dry ice and a large cooler it's pretty simple and works well. Cold and fast contact with solvent (whether using a press, or hand-wringing, coffee filters and a thick string and gloves, cheesecloth). The good info is here in the thread, such as coffee filters and a vacuum funnel helping but it doesn't really matter because you can decant or pour off the solids that fall to the bottom. With a washing step, it's easy to pipette off and use more than enough solvent so what little you miss is a small percentage. Pipette almost looks easier than separatory funnel either way. My careful extractions at home are (at least) on par with the stuff at the clubs although it isn't the same as live resin. I don't want to guess but some of the bho is like clear gum almost.


My experience is that the Fogg terpene (for flavor not dilution) at ~10% is nice. Instructions will say not to dilute your concentrate more than 50% or so for loading the cartridges. However I have found that some potent flower shatter might have to be diluted with polyethylene glycol 400 (or maybe other cannabis terpenes?) more than 50% to match the consistency that I think the cartridges were designed for. Some fine tuning here, because doing a butane (or propane like Hank Hill?) run on fresh frozen chopped up flowers especially a very large batch, could come out with a considerably different yield (and strength and color?) than small batch, cured potent flowers, very little ice cold lab grade solvent contact and cold vacuum purge.
 
Last edited:

pinkus

Well-known member
Veteran
Thanks for contributing Mengsk.

I went ahead and ordered Fogg's "cutter", which is claimed to be a "nonaromatic" terpene or terpenes. I will be using that in addition to the Pineapple Express blend.

I realize that it is overkill in many people's eyes, but I went ahead and ordered fuel line tubing for the procedure.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
In addition to Right Price Chemicals, I presume these are no hassle sources of pentane,

Xtractor Depot, $350 for five gallons,

https://xtractordepot.com/collections/new-arrivals/products/pentane-tank

Summit Research, $275 for five gallons, $2,000 for fifty-five gallons,

http://summit-research.tech/chemicals/


Fuel line should be ok if you first wash it thoroughly with hot soap and water, rinse, dry, and then final rinse with a small amount of pentane.


I'm sure everyone would appreciate some pics when the time comes!!
 

pinkus

Well-known member
Veteran
Oh yeah, I also ordered a few PTFE cap liners. I don't want any nasty surprise moments of panic!

:bandit:
 

troutman

Seed Whore
Oh yeah, I also ordered a few PTFE cap liners. I don't want any nasty surprise moments of panic!

:bandit:

Last year, I order a case of 12 Boston glass chemical bottles with PTFE lined caps.

I just ordered some more specialized laboratory glassware to help with my honey oil projects. :)
 

pinkus

Well-known member
Veteran
I will FINALLY be proceeding with this. The fuel line is STILL in transit, but glass pipette tubes should be here tonight.

Doubtful on the pictures SkyHighLer. It's all a fantasy. :shooty:
 
Top