Hash oil techniques and solvents for non BHO hash oil?

[troutman]

I was thinking about getting a metal storage container filled with enough sand to
soak up all the liquid stored in the 1L chemical glass bottles that I would place in
it. This way even if the bottles all got broken it would minimize the amount of
flammables available to burn if most of the liquids are in the sand layer.

I'm still waiting for the mailman to deliver my last items before I can start.

 

[SkyHighLer]

I don't like plastic bottles for long term storage, everything that came in plastic is being transferred to Boston round glass bottles with PTFE lined caps.

The cyclohexane came, the odor reminds me of walking through the door of a dry cleaner's shop decades ago. Evaporates immediately.

The FDA says it needs to be completely purged if used to process food. FDA USP <467> Class 2, all the others are relatively non-toxic Class 3.

https://en.wikipedia.org/wiki/Cyclohexane

MSDS,

http://www.sigmaaldrich.com/MSDS/MS...cus=product&N=0+220003048+219853269+219853286

Notice in the pictures it came in a different grade bottle with a different cap. HDPE bottle with LDPE cone sealed cap?

 

[troutman]

I don't like plastic bottles for long term storage, everything that came in plastic is being transferred to Boston round glass bottles with PTFE lined caps.

I bought a case of 12 X 1000mL I-Chem Brand 200 Series Type III Glass Amber Boston Round Bottles,
Pre-Cleaned, With PTFE-Lined Silicone Liner on Ebay. I got the 1000mL version of these. I need to
get the smaller ones now.

http://www.ebay.com/itm/I-Chem-Bran...798598?hash=item41c13bd706:g:VUYAAOSwLnBX75IL

 

[SkyHighLer]

Those are nice!!

I bought these,

JG Finneran 9-175 Clear Borosilicate Glass Standard Boston Round Bottle with White Polypropylene Closure and 0.015" PTFE Lined, 33-400mm Cap Size, 1000mL Capacity (Pack of 12)

Price $21.70 ($1.81 / PACKAGE) + $12.50 shipping

https://www.amazon.com/gp/product/B00E35FXGE/ref=oh_aui_detailpage_o04_s00?ie=UTF8&psc=1


If you have a business account, TCI America has dimethyl carbonate and ethyl formate in stock at reasonable pricing.

http://www.tcichemicals.com/eshop/en/us/commodity/C0053/

http://www.tcichemicals.com/eshop/en/us/commodity/F0053/

 

[troutman]

There's nothing wrong with your bottles.

Its just that brown bottles protect your goodies better from light that's all.

I have one full of distilled water I made using my laboratory glass still.

Another is almost full with n-Hexane I extracted from an OTC product.
I added distilled water to this bottle to reduce the air space for safety.
I will get more N-Hexane later to fill it up properly.

I then wrapped each bottle with saran wrap to keep the dust off of them.

 

[SkyHighLer]

The benzyl alcohol feels like a very thin oil, not a solvent, it doesn't rapidly evaporate. Rub it over your hands and it's like mineral oil, massage oil, it doesn't wipe off, it doesn't disappear, I wiped them clear of it with some isopropyl

I doubt it has much possibility as a general purpose solvent for cannabis.

https://en.wikipedia.org/wiki/Benzyl_alcohol


Timer, pipettes, pump, for the visual test, the linden tea I bought for steeping should also do for preliminary extraction method tests, the juicer, french press, etc.

 

[CosmicCharlie]

SkyHighler:

I looked back a few pages and didn't see. Are you planning on trying Acetone also?

Also, are you planning on drying your solvents and testing for residues left after evaporation?

 

[SkyHighLer]

SkyHighler:

I looked back a few pages and didn't see. Are you planning on trying Acetone also?

Also, are you planning on drying your solvents and testing for residues left after evaporation?

I was at Home Depot and checked the shelf, nice 100% acetone, up to five gallon pails, everything else has been reformulated, I took notes, and checked against the Klean-Strip SDS's when I returned home.

I bought a gallon of the acetone, and I'll probably pick up another, it was only $13 plus California sales tax.


Propyl acetate, iso-butyl alcohol, n-butyl alcohol, and amyl acetate coming.

These are all from the FDA USP Class 3 solvent list except the amyl acetate, I found that myself.

https://en.wikipedia.org/wiki/Amyl_acetate

https://americandrycleaner.com/articles/using-amyl-acetate-1


I've been going over the compatibility charts for lab containers, I had to order some reagent bottles, the polypropylene caps that come with the Pyrex bottles I bought are listed as not up to withstanding pentane and methyl acetate.


Getting organized, doubling down on safety procedures, almost ready to unpack the ISO-3.

I ordered watch glasses this morning, 24 x 5cm for the evaporation test, and 12 x 12.5cm for non-volatile residue testing.


A small piece of paper towel dampened with benzyl alcohol was almost dry after twelve hours, incredibly slow for being so flammable.

The evaporation rate may be more indicative of solvent purgeability than computations from boiling point and vapor pressure figures alone.


Awaiting the iso-octane, and maybe ethyl formate and dimethyl carbonate.

 

[CosmicCharlie]

Cool. Thanks.


How are you planning on proceeding with the extractions?

Will you use the solvents as they are right out of the bottle?

It may be of some use to dry your solvents to eliminate any possible water contamination like anhydrous acetone attracts water and people use baked Epsom Salts (which turn into Magnesium Sulfate) to get rid of any possible water contamination since opening the bottle of acetone will allow it to pull some water from the air.

Of course this may not matter much since THC isn't water soluble but any water in the solvent could pull some other things that you don't want in your extraction.

Also, how long of wash times were you planning on using?

Thanks.

 

[SkyHighLer]

I ordered a set of seven precision glass light liquid hydrometers, 0.650 to 1.000 specific gravity. $110.

These,

H-B DURAC B61891-1400 0.950/1.000 Specific Gravity ASTM 108H Hydrometer for Light Liquids

https://www.amazon.com/B61891-1400-...1381&sr=1-18&keywords=light+liquid+hydrometer

 

[SkyHighLer]

Attached:

"Table A-1. Compilation of one-hundred important organic solvents together with their physical constants, arranged in order of decreasing ETN value, as empirical parameter of solvent polarity."

Solvents and Solvent Effects in Organic Chemistry, 4th, Updated and Enlarged Edition

Christian Reichardt, Thomas Welton
ISBN: 978-3-527-32473-6
718 pages
December 2010

http://www.wiley.com/WileyCDA/WileyTitle/productCd-3527324739,subjectCd-CH82.html

Follow the link, click on "LEARN MORE" at "Digital version available through Wiley Online Library." Check out the unlocked chapters, in particular, "Appendix A. Properties, Purification, and Use of Organic Solvents (pages 549–586)" Sorry, Wiley doesn't allow direct links in.

I bought a hardcopy from Amazon for $150.

 

[SkyHighLer]

Amazon has dimethyl carbonate in stock!! I have three cans on back order...

https://www.amazon.com/MG-Chemicals...=1492864970&sr=8-1&keywords=dimethyl+carbonat

https://en.wikipedia.org/wiki/Dimethyl_carbonate


I also made a test order of MG Chemicals' ethyl acetate and butyl acetate from Amazon.

 

[G.O. Joe]

I bought a hardcopy from Amazon for $150.

WILEY-VCH Verlag GmbH & Co. KGaA thanks you for your support of the science cartels.

Those who prefer science in pdf form can get books and articles from alternate outlets below publisher cost.

 

[SkyHighLer]

It downloaded instantly, thank you.


pages 455-461

Table 7-3. Empirical parameters of solvent polarity, ET(30) [cf. Eq. (7-27)] and normalized ETN values [cf. Eq. (7-29)], derived from the long-wavelength UV/Vis charge-transfer absorption band of the negatively solvatochromic pyridinium N-phenolate betaine dyes (44) and (45), measured at 25 C and 1013 hPa, for a selection of 288 solvents, taken from reference [293].

:yay:

 

[SkyHighLer]

The iso-octane and dimethyl carbonate should ship this week, the ethyl formate is back ordered at Amazon Marketplace.

Listed as to increasing polarity using the table from the previous post,

cyclohexane C6H12 110-82-7 0.006
https://en.wikipedia.org/wiki/Cyclohexane

iso-octane C8H18 540-84-1 ????
https://en.wikipedia.org/wiki/2,2,4-Trimethylpentane

n-pentane C5H12 109-66-0 0.009
https://en.wikipedia.org/wiki/Pentane

propyl acetate C5H10O2 109-60-4 0.210
https://en.wikipedia.org/wiki/Propyl_acetate

ethyl acetate C4H8O2 141-78-6 0.228
https://en.wikipedia.org/wiki/Ethyl_acetate

dimethyl carbonate C3H6O3 616-38-6 0.232
https://en.wikipedia.org/wiki/Dimethyl_carbonate

n-butyl acetate C6H12O2 123-86-4 0.241
https://en.wikipedia.org/wiki/Butyl_acetate

methyl acetate C3H6O2 79-20-9 0.253
https://en.wikipedia.org/wiki/Methyl_acetate

n-amyl acetate C7H14O2 628-63-7 ????
https://en.wikipedia.org/wiki/Amyl_acetate

ethyl formate C3H6O2 109-94-4 0.315
https://en.wikipedia.org/wiki/Ethyl_formate

iso-propyl alcohol C3H8O 67-63-0 0.546
https://en.wikipedia.org/wiki/Isopropyl_alcohol

iso-butyl alcohol C4H10O 78-83-1 0.552
https://en.wikipedia.org/wiki/Isobutanol

acetone C3H6O 67-64-1 0.355
https://en.wikipedia.org/wiki/Acetone

n-butyl alcohol C4H10O 71-36-3 0.586
https://en.wikipedia.org/wiki/N-Butanol

benzyl alcohol C7H8O 100-51-6 0.608
https://en.wikipedia.org/wiki/Benzyl_alcohol

n-propyl alcohol C3H8O 71-23-8 0.617
https://en.wikipedia.org/wiki/1-Propanol

ethyl alcohol C2H6O 64-17-5 0.654
https://en.wikipedia.org/wiki/Ethanol

 

[SkyHighLer]

Iso-octane is not the correct name for 2,2,4-trimethylpentane, but is often used as I did in the above list.

For instance when you search Right Price Chemicals store for iso-octane/isooctane you find no results, but when you search for 2,2,4-trimethylpentane they indeed carry it, and subtitle it isooctane.

http://www.rightpricechemicals.com/buy-2-2-4-trimethylpentane-online.html


I sent them an email requesting to cancel my order for a liter so I could increase my order to a four liter jug at a better price point, and their response was to send me notice of shipment of the liter!! I'd gone ahead and ordered the four liter jug (the shipping was a very reasonable $21,) and will let both orders stand.

The liter requires signature at delivery, the box is going to be covered with hazard stickers, I'll post pictures when it comes.


Waiting to see if Amazon will actually ship the MG Chemicals solvents today as promised.

 

[troutman]

This morning I received my laboratory stand support with flask clamps and ring supports in the mail.

Just need to buy one more chemical or two locally and I should be ready to rock soon enough.

 

[SkyHighLer]

I think I found another relatively non-toxic solvent, ethyl propionate.

https://en.wikipedia.org/wiki/Ethyl_propionate

https://pubchem.ncbi.nlm.nih.gov/compound/7749#section=Top

HiMedia GRM2197-500ML Ethyl Propionate, 500 mL
Price: $35.40 FREE Shipping for Prime members once available
Usually ships within 1 to 2 months.

https://www.amazon.com/HiMedia-GRM2...d=1493058913&sr=8-1&keywords=Ethyl+propionate

I ordered two 500ml bottles as I didn't see it offered to the general public anywhere else.

 

[SkyHighLer]

Amazon sent me three 945ml cans of dimethyl carbonate!!!

https://www.amazon.com/gp/product/B06XSGX8TW/ref=oh_aui_detailpage_o01_s00?ie=UTF8&psc=1

Dimethyl carbonate's melting point of 36-39F limits how cold you can extract with it, otherwise it seems nearly perfect.

https://en.wikipedia.org/wiki/Dimethyl_carbonate


Still waiting to see if Amazon will ship MG Chemicals' butyl acetate and ethyl acetate.

 

[SkyHighLer]

Cool. Thanks.


How are you planning on proceeding with the extractions?

Will you use the solvents as they are right out of the bottle?

It may be of some use to dry your solvents to eliminate any possible water contamination like anhydrous acetone attracts water and people use baked Epsom Salts (which turn into Magnesium Sulfate) to get rid of any possible water contamination since opening the bottle of acetone will allow it to pull some water from the air.

Of course this may not matter much since THC isn't water soluble but any water in the solvent could pull some other things that you don't want in your extraction.

Also, how long of wash times were you planning on using?

Thanks.

For those interested in keeping their solvents anhydrous I ran across this article, quick, interesting, and to the point,

"Drying of Organic Solvents: Quantitative Evaluation of the Efficiency of Several Desiccants"
D. Bradley G. Williams* and Michelle Lawton
August 12, 2010

https://pdfs.semanticscholar.org/ec7d/d3c01b54535f93d48187980c11e0f789f47f.pdf

"Various commonly used organic solvents were dried with several different drying agents. A glovebox bound coulometric Karl Fischer apparatus with a two-compartment measuring cell was used to determine the efficiency of the drying process. Recommendations are made relating to optimum drying agents/conditions that can be used to rapidly and reliably generate solvents with low residual water content by means of commonly available materials found in most synthesis laboratories. The practical method provides for safer handling and drying of solvents than methods calling for the use of reactive metals, metal hydrides, or solvent distillation."


"Methanol and Ethanol

Lower alcohols are typically dried by heating over iodine- activated magnesium with a magnesium loading of 0.5- 5.0 g/L.1 Several other desiccants, including KOH, BaO, and CaO,1,3 have also been recommended. KOH and Mg/I2 are found to provide methanol with a water content of 33 and 54 ppm, respectively (Table 5). Molecular sieves (3 A ̊ ) were efficient at drying this solvent only when present at a loading of 10% m/v or higher and when the solvent was left to stand over the sieves for a minimum period of 72 h. Optimum drying is obtained with storage of the methanol over 20% m/v 3 A ̊ molecular sieves for 5 days, by which time the water content reduces to about 10 ppm.

Ethanol behaved similarly, requiring a minimum of 10% m/v of activated 3 A ̊ molecular sieves before efficient drying is noted, optimally also after a period of 5 days over 10% or 20% m/v of the sieves, under nitrogen (Table 6). Powdered KOH proved a rather active desiccant for methanol, and ethanol and may be used in a predrying step prior to storage over activated 3 A ̊ molecular sieves to provide ultimate drying efficiency."


The lower portion of the article contains the previous work they're quantifying.