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Hash oil techniques and solvents for non BHO hash oil?

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
I went to grab a standard funnel to try out with some fan folded/fluted filter paper, and found something far superior.

That's an old Champion juicer loading funnel, whatever it's make of, I assume nylon, it's impervious to most solvents.

The cone is spread wide for high capacity, there's excellent flow through the large drain hole, it stays in place, and fits a wide variety of beaker style vessels, even short ones without extending into the collected solution.

If there is similar lab product, I didn't see it.

https://www.youtube.com/results?search_query=fluted+filter+paper

http://www.ebay.com/sch/i.html?_fro...nel.TRS0&_nkw=champion+juicer+funnel&_sacat=0
 

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troutman

Seed Whore
Yeah, not all plastics are safe with solvents.

I'm looking at a glass funnel from where I buy most of my laboratory glassware.

I'll probably get a Buchner funnel as well seeing I'll try reduced pressure work later on.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran

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G.O. Joe

Active member
Veteran
To check whether I was just lucky scoring HPLC grade ethyl acetate easily and inexpensively, I just bought another four liter jug, this time through Amazon Marketplace.


Ethyl Acetate, HPLC/Spectro, 4L Amber Glass (Each)
by TEDIA
$161.57

Home Depot (except in CA) (they have MEK too) (except in CA)
Ethyl acetate, 100%, gallon cans
by Klean-Strip
$25



Couldn't resist. Sorry, sorry. Carry on.
 

G.O. Joe

Active member
Veteran
This is the kind I bought a while ago on Ebay for another project and I was right I can't use it with Hexane.

Dow Corning High Vacuum Grease:


It's fine. A more likely problem if there is one is too much grease applied. Or the 204C rating is exceeded? Apiezon H has a 240C rating.
 

troutman

Seed Whore
It's fine. A more likely problem if there is one is too much grease applied. Or the 204C rating is exceeded? Apiezon H has a 240C rating.

I don't plan on applying that much heat to be honest.

Water has the highest boiling point of any solvent I plan on using in making a Cannabis extract.
Even then, I will use a separatory funnel to get rid of it. So I'm very safe. As a matter of fact
I made over a liter of distilled water a few days ago and had no issues.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Home Depot (except in CA) (they have MEK too) (except in CA)
Ethyl acetate, 100%, gallon cans
by Klean-Strip
$25

[URL=https://www.icmag.com/ic/picture.php?albumid=13921&pictureid=1725196&thumb=1]View Image[/url]

Couldn't resist. Sorry, sorry. Carry on.


I missed that, though I noticed similar commercial 100% ethyl acetate products are offered in the UK.

"M.E.K. Substitute

Klean-Strip® Methyl Ethyl Ketone Substitute is a thinner for specified coatings, including polyester and epoxy resins, ink, adhesives and contact cement. It is recommended for use when a rate of evaporation slower than acetone is desired.

Not intended for sale or use in California.

Though this product is no longer available for sale, we continue to provide the “Directions for Use” and product documentation to support Klean-Strip® customers who have previously purchased this product."

http://www.kleanstrip.com/product/m.e.k.-substitute


Tedia sent me notice:

"Dear Mr. S.......,

Thank you for placing an order with Tedia, for your high purity solvent needs. In order to ship this product, please confirm if there is a business address we can send to. We cannot ship hazardous materials into residential areas.

If there is another business location we can send to, I can change that address in our system.

If you need us to cancel this order due to the location, please confirm and I will process accordingly.

I apologize for any delays or problems this may cause.

Sincerely, SS, Tedia Customer Service"


This morning I also received an email from Amazon suggesting I open an Amazon Business Account, so I applied, as the owner and head tech of NVR Solvent Analysis. :biggrin:

One day approval process, I'll know tomorrow.
 

G.O. Joe

Active member
Veteran
You need to find the companies that sell to individuals and stick with their catalog, or at least form a LLC. One of my favorites has the 4 l HPLC grade for less than ACS at $74, but that's before at least $50 in shipping.

Most companies have this problem with residential addresses and residential customers, yet when shipped from the same big company through some intermediary in their name to your residential address, the problem magically goes away.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
"business-to-business-address-verification@amazon.com Today at 2:44 AM
To
j......................

Hello,

We have been unable to verify the information provided in your business account registration. To help us verify your account, upload the following documents using the link below:

https://www.amazon.com/bb/registration/pending

1. One of the following official documents that contains your valid/active Federal Tax ID or sole proprietor status for NVR Solvent Analysis:

-- EIN Verification document from IRS
-- Business license
-- State documents which contain the state seal

AND

2. A document from your business confirming employment for J... E..... S....... (printed on company letterhead with logo, when possible).

If you would like to change the above contact information, please respond to this email with the information you would like displayed in your Amazon Business account. If the legal name of your business differs from the name you are doing business as (DBA), please include both business names.

If you have enrolled or wish to enroll in the Amazon Tax Exemption Program (ATEP), please go to the ATEP help page: https://www.amazon.com/gp/taxExemption. ATEP enrollment is not part of this process. Do NOT include ATEP documents with the documents requested above.

We will reply within 1 business day of receiving your information. In the meantime, to avoid delays, do not open new business accounts.

If you have questions or concerns, contact Business Customer Service: https://www.amazon.com/gp/help/contact-us/b2b-help.html. For your security, we restrict business account access to a team of account specialists, who will only be able to confirm that Amazon sent this request. They can provide no additional details.

Thank you for your interest in Amazon Business.

Sincerely,

Account Specialist"


I played it out and now I know.

What irks me is Tedia out and out trolled me when I was searching for ethyl acetate at Amazon, created a product offering just for me, and flashed it like a whore.



To satisfy my curiosity I just bought this from eBay to check out, $55.99 plus $4.20 CA sales tax, free shipping and handling.

"Ethyl Acetate 99% - Technical Grade - Gallon (4 Quart Cans)

Ethyl acetate (systematically, ethyl ethanoate, commonly abbreviated EtOAc or EA) is the organic compound with the formula CH3-COO-CH2-CH3. This colorless liquid has a characteristic sweet smell

(similar to pear drops) and is used in glues, nail polish removers, decaffeinating tea and coffee, and cigarettes (see list of additives in cigarettes). Ethyl acetate is the ester of ethanol andacetic acid; it is

manufactured on a large scale for use as a solvent.

This item is in compliance with United States Postal Service Publication 52 guidelines.

This material is flammable (class 3 hazardous material) and is packaged accordingly to meet Fedex Ground guidelines and ships as a consumer commodity ORM-D.

Shipping will comply with all USPS regulations. Item will be shipped ORM-D Fedex Ground."

http://www.ebay.com/itm/121507721202?_trksid=p2060353.m2749.l2649&ssPageName=STRK:MEBIDX:IT



I assume this small house still has the same policies as when I used to live nearby, cash and carry with just a CA drivers license for ID. Is there a trick for doing an online search for other friendly brick and mortar retailers?

http://www.amicosci.com
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Not a low boiler, but I couldn't resist, the other solvent in nail polish, butyl acetate.

Three quarts for $50 plus $9.49 shipping from Amazon, similar deal at eBay.

https://www.amazon.com/gp/product/B017Q2LPT4/ref=oh_aui_detailpage_o00_s00?ie=UTF8&psc=1

"Nail polish consists of a film-forming polymer dissolved in a volatile organic solvent. Nitrocellulose that is dissolved in butyl acetate or ethyl acetate is common."

"The most common (nail polish) remover is acetone. This can be harsh on skin and nails, and can also remove artificial nails made of acrylic or cured gel. A less harsh nail polish remover is ethyl acetate, which often also contains isopropyl alcohol. Ethyl acetate is usually the original solvent for nail polish itself.

Acetonitrile has been used as a nail polish remover, but it is more toxic and potentially carcinogenic. It has been banned in the European Economic Area for use in cosmetics since 17 March 2000."

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



Also ordered a liter of butanol/n-butyl alcohol.


Still avoiding acetone, MEK, and MIBK... already searched for MTBE, expensive with limited availability.


G.O. Joe :thank you: Way too funny.....
 
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G.O. Joe

Active member
Veteran
Is there a trick for doing an online search for other friendly brick and mortar retailers?

Anything is possible locally. There's usually something somewhere at a site that lets you know how they feel about residences. Strike's second book Sources is almost 20 years old and your Amico is in there - maybe something listed in CA still works out. pdf at bookzz.org or wherever if interested.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran

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troutman

Seed Whore
I just ordered a Friedrichs Condenser and should be ready to rock once I get that. :woohoo:

Mind you, I keep thinking my shopping is over and it never is. :laughing:
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Not a low boiler, but I couldn't resist, the other solvent in nail polish, butyl acetate.

Three quarts for $50 plus $9.49 shipping from Amazon, similar deal at eBay.

https://www.amazon.com/gp/product/B017Q2LPT4/ref=oh_aui_detailpage_o00_s00?ie=UTF8&psc=1

"Nail polish consists of a film-forming polymer dissolved in a volatile organic solvent. Nitrocellulose that is dissolved in butyl acetate or ethyl acetate is common."

"The most common (nail polish) remover is acetone. This can be harsh on skin and nails, and can also remove artificial nails made of acrylic or cured gel. A less harsh nail polish remover is ethyl acetate, which often also contains isopropyl alcohol. Ethyl acetate is usually the original solvent for nail polish itself.

Acetonitrile has been used as a nail polish remover, but it is more toxic and potentially carcinogenic. It has been banned in the European Economic Area for use in cosmetics since 17 March 2000."

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



Also ordered a liter of butanol/n-butyl alcohol.


Still avoiding acetone, MEK, and MIBK... already searched for MTBE, expensive with limited availability.


G.O. Joe :thank you: Way too funny.....

Butyl acetate
From Wikipedia, the free encyclopedia

n-Butyl acetate, also known as butyl ethanoate, is an ester which is a colorless flammable liquid at room temperature. Butyl acetate is found in many types of fruit, where along with other chemicals it imparts characteristic flavors and has a sweet smell of banana or apple. It is used as a synthetic fruit flavoring in foods such as candy, ice cream, cheeses, and baked goods. Butyl acetate is often used as a high-boiling solvent of moderate polarity.

The other three isomers of butyl acetate are: isobutyl acetate, tert-butyl acetate, and sec-butyl acetate.


Occurrence in nature

Apples, especially of the Red Delicious variety, are flavored in part by this chemical. The alarm pheromones emitted by the Koschevnikov gland of honey bees contain butyl acetate.

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


Extremely sweet, and evaporates quickly. I'm tempted to give it a taste. :biggrin:


The packaging was impeccable, and the label nicely laminated.
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Preliminary test of the butyl acetate.

About a 0.1g of flower tops crushed between my fingers, the seeds weren't included.

Soaked three times in about 2ml of butyl acetate, each time filtered through the same filter into the same collection glass.


To determine if there was green tint yet to be extracted I soaked twice more, this time using 99% isopropyl alcohol.

All the soaks were about ten minutes each. The butyl acetate was at about 65F, the isopropyl alcohol at room temperature.


The cannabinoid and terpene dissolving power of the butyl acetate was checked against 99% isopropyl alcohol by how quickly each dissolved some BHO, each took a moment, and then cut it completely without hesitation.


Pics of the end result tomorrow.
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
I put a fan on it this morning and the remainder blew off immediately.

Then I vacuumed it down three times with the cordial liquor glass at room temperature.

The fragrant odor of the butyl acetate still was coming through, though I'm sure raising the temperature to 115-120F during vacuum purge would make a significant difference, we'll see when I do an actual run.

The tint looks promising to me, a quick soak with ice cold solvent should help.



I intend on doing a preliminary test of ethyl acetate next.

Q & A under Responses @ https://skunkpharmresearch.com/simple-alkanes-alcohols-and-ethers/


Posted by tilopa88 on June 9, 2012 at 2:41 PM

What about Ethyl Acetate? Is that not a better thc solvent than any of the Simple Alkane Alcohols?


Posted by Skunk Pharm Research,LLC on June 10, 2012 at 10:02 AM

Ostensibly so!


Isobutyl alcohol and propyl acetate ordered.
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Methanol is a FDA USP Class 2 solvent, my purpose is to expand the field of known to be effective Class 3 solvents.

From Cannabis Alchemy,

There are several solvents that work well. Their properties, and the advantages and disadvantages of each, are discussed below:

1. Methyl alcohol, methanol, wood alcohol (boiling point 64°C). This solvent is commonly employed and, if used correctly, does a fine job. Methanol is available at many pharmacies and in larger quantities at industrial chemical supply companies. It is also available as paint thinner, but it is seldom very pure in this form. Methanol fumes are toxic and explosive. Inhalation of these fumes makes one sick, with pronounced body ache. Continued inhalation of even small amounts may cause permanent damage. Any traces of the solvent remaining in the oil product will be hazardous to the consumer. Methanol evaporates at a uniform temperature (approximately 190°F) and does not extract a lot of the water-soluble tars, which are not psychoactive. A method for removing traces of the solvent will be discussed later.

2. Rubbing alcohol (most rubbing alcohol is 70% isopropyl alcohol and 30% water). There are several advantages to using isopropyl rubbing alcohol. It is available in many stores at a low price and is much less toxic and explosive than methanol. Unfortunately, because it contains water, many of the water-soluble, non-psychoactive substances are also extracted. The oil yield using rubbing alcohol is twice that of methanol, and is proportionally less potent. Water-soluble tars may also give the oil undesirable taste and burning qualities. If the oil is to be re-extracted later with a more selective solvent, however, it matters little what it is like at this point. The water in the mixture also causes it to evaporate at a much higher temperature than methanol. Once the alcohol is completely evaporated, the water that was in the solvent remains with the oil. This takes a long time to evaporate in a boiling water bath. An oil bath may be used. The temperature of the oil in the bath is kept slightly higher than the boiling point of water. Water that gets into the oil bath may spatter; this is a hazard.

3. Ethanol, ethyl alcohol, pure grain alcohol (boiling point 78.5°C). This is a very desirable solvent. It has extraction properties very similar to methanol, but is not as toxic. It is very difficult to obtain, however, as it is a major active ingredient in liquor and is heavily taxed. Pure ethanol may be produced from either liquor or fermented material. Denatured ethanol, which is available in hardware stores and pharmacies, contains non-removable poisons which evaporate at the same temperature as pure ethanol. This makes the ethanol unfit for drinking.

4. Petroleum ether (boiling point 30—60° C). Petroleum ether is a light solvent much more selective than any of the alcohols. Extracting with petroleum ether produces an oil that is twice as potent by weight as oil extracted with alcohol. The cannabis material may be extracted directly with ether but, due to petroleum ether’s highly explosive nature, the oil is first removed from the plant material with alcohol and then re-extracted with ether. This requires a much smaller amount of the dangerous solvent. Petroleum ether is usually available only through chemical supply companies.

http://calgarycmmc.com/E-books/E Books A-B-C/Cannabis Alchemy - D. Gold.pdf


"Class 2 residual solvents (Table 2) should be limited in drug substances, excipients, and drug products because of the inherent toxicities of the residual solvents."

"Class 3 residual solvents (Table 3) may be regarded as less toxic and of lower risk to human health than Class 1 and Class 2 residual solvents. Class 3 includes no solvent known as a human health hazard at levels normally accepted in pharmaceuticals. However, there are no long-term toxicity or carcinogenicity studies for many of the residual solvents in Class 3. Available data indicate that they are less toxic in acute or short-term studies and negative in genotoxicity studies."

http://www.usp.org/sites/default/files/usp_pdf/EN/USPNF/generalChapter467Current.pdf
 

troutman

Seed Whore
I don't have any ethanol over 40% yet.

I think the easiest and cheapest way for me to get 90+% would be to buy vodka and distill away.

I could make 100% dry ethanol if I really wanted to. But it would be overkill for most uses.
 
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