Need Help Polishing With Hexane

[welder]

Hello fellow farmers. Long time reader and farmer. First time joining and posting. Im a legal WA patient. I normally stomp around in a local forum we have here but I needed to start tapping and networking with a larger group of knowledge.

I have been banging my head against the wall trying to figure out how to polish with hexane. I have wasted a lot of oil, material and, solvents and its time to ask for help. I must have spent countless hours reading skunkpharms site (and then some) and Im just not getting the same results.

My problem is that the hexane will not lighten up no matter how many times I wash it.

I have tried using ethanol, ISO and Denatured for the alcohol/water wash. Nothing. Just dumping a lot of alcohol down the drain. Gets spendy with the ethanol.

I have also tried the saturated saline / hexane wash. I accidentally used salt with iodine. Didnt work.
Got new table salt that has not had iodine added. Didn't work.
The iodized salt has sodium silicoaluminate, soduim thosufate listed in the ingredients.
The non-iodized salt has calcium silicate list as an ingredient for anticaking agent.
Maybe these are the reasons its not working. When I mix the hexane with the saline, shake and burp it... some of the salt precipitates out and falls to the bottom of my sep funnel.

The only thing I can think that it may be is the hex. Something has to be displacing that salt and causing it to precipitate out like that right? Ill tell ya its not the stuff I want out.

Here is the Hexane I am using. It says on the label that it leaves less than 1 ppm after evaporation. I also noticed that when I try to do an extraction with it, it slightly picks up chlorophyll. After I post this I will be chilling some hexane and material with dry ice and seeing what I can get from a 3 min wash. I prob create a thread on it with my results.
http://i58.invalid.com/2wmmhkl.jpg
Product Specifications
TESTSPECIFICATION
For Laboratory,Research,or Manufacturing Use
FID-Sensitive Impurities (as 2-Octanol) Single Impurity Peak (ng/mL)<= 5
ECD Sensitive Impurities (as Heptachlor Epoxide) Single Peak (pg/mL)<= 10
ECD-Sensitive Impurities (as Ethylene Dibromide) - Single Impurity Peak (ng/mL)<= 5
Assay (Total Saturated C₆ Isomers) (by GC, corrected for water)>= 99.5 %
Assay (as n-Hexane) (by GC, corrected for water)>= 95 %
Color (APHA)<= 10
Residue after Evaporation<= 1.0 ppm
Substances Darkened by H₂SO₄Passes Test
Water (by KF, coulometric)<= 0.05 %
MEETS SPECIFICATIONS WITHIN THE EXPIRATION PERIOD

Here is the MSDS on it

I would very much appreciate any help you guys might have. Graywolf?

 

[welder]

I tried to put a pic of label up but it keeps changing the url to invalid. I used tinypic and photobuket. ???

 

[Graywolf]

Polishing with Hexane removes the water soluble ingredients, but doesn't remove some of the darker polar elements. The easiest way we've found to do that, is to dissolve it in hexane and run it through silicon bead chromatography column.

Here is a picture of the different fractions as they were stripped. Almost no cannabinoids in the first, and last three jars. Most of the cannabinoids are in the light yellow to whiskey colored fractions.

 

[welder]

Thank you for the info. I was off reading / watching videos about colum chromatography. It looks easy enough and it seems you can recover almost all the yield. From the looks of how it works. I imagine it would also separate CBD from THC to an extent. I bet it would take a lot of hexane. Im glad I invested in a 2 liter distilling kit. I have been able to recover almost all of my hexane.

Off topic and speaking of recovering hexane -
I would like to use hexane for my extractions and came up with an idea to recover it all. The losses (hex/oil) seem to be what is left on the material after straining it.
My first idea was to build a steel container that I could heat the spent material and distill it off that way. The safety aspect of that killed that idea. (big vapor container on heat) plus it would not address the oil still on material.

Finally I came up with using a 12 cup stainless french press. After extraction, put the wet material in the french press and fill it with water. Agitate it until the hexane forms on top. Push the material down with the press and let it sit and then remove the top layer of hexane (with the good stuff)

 

[Graywolf]

Hee, hee, hee, good idea!