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Hash oil techniques and solvents for non BHO hash oil?

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
The quart of Sunnyside Xylol (xylenes) arrived yesterday. The only hazard labeling was the blue ORM-D shown in the packaging picture. No signature was necessary for delivery.

I was pouring the contents of the can into a reagent bottle and noticed a grey tint, and then due to there being more than expected in the can I poured the remainder into a smaller bottle, and found the grey mass impurity, you can see globs of it in the picture. It doesn't dissolve in the xylene, and it seems to have been completely removed by simply filtering through 2.5 micron lab filter paper. There are other sources of xylene, so I won't go on further about it.

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

"Xylene is used as a solvent. In this application, with a mixture of isomers, it is often referred to as xylenes or xylol. Solvent xylene often contains a small percentage of ethylbenzene. Like the individual isomers, the mixture is colorless, sweet-smelling, and highly flammable.


Xylene is flammable but of modest acute toxicity, with LD50 ranges from 200 to 5000 mg/kg for animals. Oral LD50 for rats is 4300 mg/kg. The principal mechanism of detoxification is oxidation to methylbenzoic acid and hydroxylation to hydroxylene.

The main effect of inhaling xylene vapor is depression of the central nervous system (CNS), with symptoms such as headache, dizziness, nausea and vomiting. At an exposure of 100 ppm, one may experience nausea or a headache. At an exposure between 200-500 ppm, symptoms can include feeling "high", dizziness, weakness, irritability, vomiting, slowed reaction time.

The side effects of exposure to low concentrations of xylene (< 200 ppm) are reversible and do not cause permanent damage.

One report contained data that shows that long-term exposure to low levels of xylene led to a decrease in balance, coordination, and reaction times in participants. These are examples of how it affects the CNS.

Long-term exposure may lead to headaches, irritability, depression, insomnia, agitation, extreme tiredness, tremors, impaired concentration and short-term memory. This condition is sometimes generally referred to as "organic solvent syndrome". Unfortunately, there is very little information available that isolates xylene from other solvent exposures in the examination of these effects.

Xylene is also a skin irritant and strips the skin of its oils, making it more permeable to other chemicals.

To reduce the risk of developing health problems from occupational exposure, one must wear gloves and a mask to prevent high concentrations of inhalation and skin irritation from Xylene."


It is extremely non-polar, compare at the list my cache of solvents arranged as to polarity,

https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162


The problem with it is it has a strong odor, reminds me of the odor of felt tip markers from decades ago, you can sniff it and get dizzy. On the other hand, get some on your fingers, and at the point of complete evaporation, the odor completely disappears, happens like magic, so it might be purgeable, and for sure you'll know if you got it all out. :biggrin:


The ethyl formate is scheduled for delivery today. :woohoo:


The quart of Klean-Strip Xylol/Xylene arrived. Only the Consumer Commodity ORM-D mention on the label, no signature required, it was left at the door. The plastic cap shown in the pictures easily lifts to open, there was no inner seal. Same strong odor as Sunnyside's.
 

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G.O. Joe

Well-known member
Veteran
That's the new design they have now it wouldn't surprise me if it's not the same, some of the few products they still sell have supposedly gone crappy since the change.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
The Klean-Strip Xylol/Xylene stunk up my storage space. I placed the can in a small nylon oven roasting bag and knotted the top, 100% odor containment. Beware, these bags readily produce static electricity.

https://www.amazon.com/Roastabags-B...=1496248478&sr=8-4&keywords=oven+roasting+bag


Consolidated Chemical & Solvents LLC has reopened their Amazon Storefront. They had a fire at their facility last month.

http://www.consolidated-chemical.com

https://www.amazon.com/s?marketplac...LWP03FL&merchant=A2O5US9LWP03FL&redirect=true
 
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Hashmasta-Kut

honey oil addict
Veteran
Toluene is my next batch Blew some nice BHO today, maybe toluene batch tomorrow Very optimistic because I have read good things (what little I have) and that its polar and will get more good and less gunk.

listen to Joe who told you toluene can cause brain damage. it seems the worst thing you could use almost, at least terrible at best.
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Thanks HMK! :)

Found a trick for buying MEK, search for Barge Universal Thinner.

http://www.bargeadhesive.com/upload...baug_-_ghs_us_-_hcs_2012_v4.4english_(us).pdf

https://www.amazon.com/Original-Pur...=UTF8&qid=1496285389&sr=8-29&keywords=toluene

http://www.ebay.com/itm/Barge-All-P...hash=item1eb4f3cdb0:m:mXrIrcWwp8fymApRAKR8V9w

I went with a gallon for $34.90 total, delivered to my door. :biggrin:


Barge All Purpose Thinner is a completely different product, it's a blend of toluene, heptane, and ethyl acetate, rather than the 100% MEK of the Universal Thinner described above.

http://www.bargeadhesive.com/upload...baug_-_ghs_us_-_hcs_2012_v4.4english_(us).pdf
 
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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
https://en.wikipedia.org/wiki/Hash_oil

"A wide variety of solvents can be used for extraction, such as chloroform, dichloromethane, petroleum ether, naphtha, benzene, butane, methanol, ethanol, isopropanol, and olive oil. Currently, resinoids are often obtained by extraction with supercritical carbon dioxide. The alcohols extract undesirable water-soluble substances such as chlorophylls and sugars (which can be removed later by washing with water). Non-polar solvents such as benzene, chloroform and petroleum ether will not extract the water-soluble constituents of marijuana or hashish, and will yield a somewhat more potent oil as a result. In general, non-polar cannabis extracts taste much better than polar extracts."

:whistling:

https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
The quart of Sunnyside Xylol (xylenes) arrived yesterday. The only hazard labeling was the blue ORM-D shown in the packaging picture. No signature was necessary for delivery.

I was pouring the contents of the can into a reagent bottle and noticed a grey tint, and then due to there being more than expected in the can I poured the remainder into a smaller bottle, and found the grey mass impurity, you can see globs of it in the picture. It doesn't dissolve in the xylene, and it seems to have been completely removed by simply filtering through 2.5 micron lab filter paper. There are other sources of xylene, so I won't go on further about it.

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

"Xylene is used as a solvent. In this application, with a mixture of isomers, it is often referred to as xylenes or xylol. Solvent xylene often contains a small percentage of ethylbenzene. Like the individual isomers, the mixture is colorless, sweet-smelling, and highly flammable.


Xylene is flammable but of modest acute toxicity, with LD50 ranges from 200 to 5000 mg/kg for animals. Oral LD50 for rats is 4300 mg/kg. The principal mechanism of detoxification is oxidation to methylbenzoic acid and hydroxylation to hydroxylene.

The main effect of inhaling xylene vapor is depression of the central nervous system (CNS), with symptoms such as headache, dizziness, nausea and vomiting. At an exposure of 100 ppm, one may experience nausea or a headache. At an exposure between 200-500 ppm, symptoms can include feeling "high", dizziness, weakness, irritability, vomiting, slowed reaction time.

The side effects of exposure to low concentrations of xylene (< 200 ppm) are reversible and do not cause permanent damage.

One report contained data that shows that long-term exposure to low levels of xylene led to a decrease in balance, coordination, and reaction times in participants. These are examples of how it affects the CNS.

Long-term exposure may lead to headaches, irritability, depression, insomnia, agitation, extreme tiredness, tremors, impaired concentration and short-term memory. This condition is sometimes generally referred to as "organic solvent syndrome". Unfortunately, there is very little information available that isolates xylene from other solvent exposures in the examination of these effects.

Xylene is also a skin irritant and strips the skin of its oils, making it more permeable to other chemicals.

To reduce the risk of developing health problems from occupational exposure, one must wear gloves and a mask to prevent high concentrations of inhalation and skin irritation from Xylene."


It is extremely non-polar, compare at the list my cache of solvents arranged as to polarity,

https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162


The problem with it is it has a strong odor, reminds me of the odor of felt tip markers from decades ago, you can sniff it and get dizzy. On the other hand, get some on your fingers, and at the point of complete evaporation, the odor completely disappears, happens like magic, so it might be purgeable, and for sure you'll know if you got it all out. :biggrin:


The ethyl formate is scheduled for delivery today. :woohoo:

The quart of Klean-Strip Xylol/Xylene arrived. Only the Consumer Commodity ORM-D mention on the label, no signature required, it was left at the door. The plastic cap shown in the pictures easily lifts to open, there was no inner seal. Same strong odor as Sunnyside's.


The quart of MG Chemicals Xylol/Xylene arrived, minimal labeling, no signature required.

Same grey particulate as I found in the Sunnyside, it could be in the Klean-Strip also, I couldn't see through the small opening of the plastic top to check. Filtered with 2.5 micron filter paper, and as with the Sunnyside, it's easily catchable, see the pictures.


I employ high flow rate, positive pressure, forced ventilation of my work area, and am prepared for spills, etc., otherwise I'd be outside with this much solvent exposed.
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Thanks HMK! :)

Found a trick for buying MEK, search for Barge Universal Thinner.

http://www.bargeadhesive.com/upload...baug_-_ghs_us_-_hcs_2012_v4.4english_(us).pdf

https://www.amazon.com/Original-Pur...=UTF8&qid=1496285389&sr=8-29&keywords=toluene

http://www.ebay.com/itm/Barge-All-P...hash=item1eb4f3cdb0:m:mXrIrcWwp8fymApRAKR8V9w

I went with a gallon for $34.90 total, delivered to my door. :biggrin:


Barge All Purpose Thinner is a completely different product, it's a blend of toluene, heptane, and ethyl acetate, rather than the 100% MEK of the Universal Thinner described above.

http://www.bargeadhesive.com/upload...baug_-_ghs_us_-_hcs_2012_v4.4english_(us).pdf

The Barge Universal Thinner (MEK) arrived, Priority Mail 1-Day, no labeling, it was left in the mail locker.

I also recognize this one all the way back to childhood, the butterscotch odor is high and pleasant.

"Butanone, also known as methyl ethyl ketone (MEK), is an organic compound with the formula CH3C(O)CH2CH3. This colorless liquid ketone has a sharp, sweet odor reminiscent of butterscotch and acetone. It is produced industrially on a large scale, and also occurs in trace amounts in nature. It is soluble in water and is commonly used as an industrial solvent."

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


MEK is listed as FDA USP <467> Residual Solvents Class 3, it's one of the least toxic 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."

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


The MEK made a mess of the label, so I spent over an hour removing it. :laughing:
 

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SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
:whee:

Amazon shipped me a 500ml bottle of ethyl formate. I have another order for three more, they're supposed to ship next week.

Here's the link, you order and wait,

https://www.amazon.com/gp/product/B00DYO8LAK/ref=oh_aui_detailpage_o03_s00?ie=UTF8&psc=1


Ethyl formate is an ester formed when ethanol (an alcohol) reacts with formic acid (a carboxylic acid). It is also known as ethyl methanoate because formic acid is also known as methanoic acid. Ethyl formate has the characteristic smell of rum and is also partially responsible for the flavor of raspberries. It occurs naturally in the body of ants and in the stingers of bees.

Exposure
Ethyl methanoate is generally recognized as safe by the U.S. Food and Drug Administration.

https://www.accessdata.fda.gov/scripts/cdrh/cfdocs/cfcfr/CFRSearch.cfm?fr=184.1295


According to the U.S Occupational Safety and Health Administration (OSHA), ethyl formate can irritate eyes, skin, mucous membranes, and the respiratory system of humans and other animals; it is also a central nervous system depressant. In industry, it is used as a solvent for cellulose nitrate, cellulose acetate, oils, and greases. It can be used as a substitute for acetone; workers may also be exposed to it under the following circumstances:

during spray, brush, or dip applications of lacquers
during the manufacture of safety glass
when fumigating tobacco, cereals, and dried fruits (as an alternative to methyl bromide under the U.S. Department of Agriculture quarantine system)

OSHA considers a time-weighted average of 100 parts per million (300 milligrams per cubic meter) over an eight-hour period as the permissible exposure limit. The U.S. National Institute for Occupational Safety and Health (NIOSH) also considers a time-weighted average of 100 ppm over an eight-hour period as the recommended exposure limit.

In space
Astronomers have identified ethyl formate in dust clouds in an area of the Milky Way galaxy called Sagittarius B2. The astronomers, from the Max Planck Institute for Radio Astronomy in Bonn, Germany, used the 30 metre IRAM radiotelescope in Spain to analyse the spectra of radiation emitted from hot regions near a new star. It is among 50 molecules identified by the astronomers.

Properties :good:
Chemical formula: C3H6O2
Molar mass: 74.08 g·mol−1
Appearance: colorless liquid
Odor: fruity
Density: 0.917 g/cm3
Melting point: −80 °C; −112 °F; 193 K
Boiling point: 54.0 °C (129.2 °F; 327.1 K)
Solubility in water: 9% (17.78°C)
Vapor pressure: 200 mmHg (20°C)

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


97% reagent grade at Sigma-Aldrich, 500ml/$48 plus shipping and Hazmat fees,

http://www.sigmaaldrich.com/catalog...Insite-_-prodRecCold_xviews-_-prodRecCold10-3

http://www.sigmaaldrich.com/Graphic...PEC/11/112682/112682-BULK_______SIAL_____.pdf

(it will require a signature at the door, and if you don't have a business account forget about it)

versus HiMedia's 97% @ 500ml/$27 total, delivered via Amazon to the general public without hassles.

http://www.himedialabs.com/TD/GRM2185.pdf


Notice how it compares to my other solvents listed as to polarity,

https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162


The chemist at Manofohm said it was very popular when he had it in stock.


Pictures of another solvent from HiMedia delivered via Amazon,

https://www.icmag.com/ic/showpost.php?p=7922415&postcount=143

I'll post up pics of the ethyl formate when it arrives.

Icy, ethereal to the nose, and evaporates completely in seconds, nothing but the clear ether odor as it dissipates.


I hope everyone can get some. It says one to two month wait at Amazon, and they still haven't sent me my other three bottles, but the ad hasn't changed to unavailable, so I encourage you to make an order and give it a chance, they don't charge you until it ships. :)


Best overall solvent so far.

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


Bezoomny Bezos is sending me more outer space solvent!!!


They hit my card, it's shipping,

"HiMedia GRM2185-500ML Ethyl Formate, 500 mL
Be the first to review this item
Price: $27.00 & FREE Shipping. Details
Only 3 left in stock (more on the way).
Want it Sunday, June 11? Order within 3 hrs 14 mins and choose Standard Shipping at checkout. Details
Ships from and sold by Amazon.com. Gift-wrap available.
New (1) from $27.00 & FREE shipping. Details

Specifications for this item

Part Number GRM2185-500ML
Number of Items 1
Brand Name HiMedia
EAN 8902729529997
Model Number GRM2185-500ML
UNSPSC Code 41116105"

https://www.amazon.com/gp/product/B00DYO8LAK/ref=oh_aui_detailpage_o01_s01?ie=UTF8&psc=1


$88.08 total ($7.08 CA sales tax) for three 500ml bottles.
 
Last edited:

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Woke up this morning to find all three indeed shipped, and Amazon still states:

"Only 3 left in stock (more on the way)"

https://www.amazon.com/HiMedia-GRM2...&qid=1496847662&sr=8-1&keywords=ethyl+formate

Solvents are the basis of Alchemy, and this is one of the basic bests you're never going to come across otherwise (unless you have a business account with a major chemical supply house, and even then try and beat the price!!)


Btw, I have two more solvents ordered and awaiting shipment, the four liter jug of isopentane from Right Price Chemicals, and two 500ml bottles of ethyl propionate from HiMedia via Amazon.

I have a reason for holding off on the testing, please bear with me. :)
 
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stoned-trout

if it smells like fish
Veteran
Culinarysolvent....yeehaw.....and ya can drink it if your man enough...the 190 kicks my ass.......got to love Maine...imiss it.....Brewer lol
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
Nice one!

http://www.culinarysolvent.com/store/c1/store



Attached:

"Section 3: Chart showing scoring outcomes for full 154 solvent dataset, sorted by chemical class"


From:

Electronic Supplementary Information for:

Updating and Expanding GSK’s Solvent Sustainability Guide

Catherine M. Alder, John D. Hayler, Richard K. Henderson, Anikó M. Redman, Lena Shukla, Leanna E. Shuster, Helen F. Sneddon.


Found here:

http://www.rsc.org/suppdata/c6/gc/c6gc00611f/c6gc00611f1.pdf


I don't think the generalized ranking of solvents ('Composite Colour') is valuable, but otherwise the factors/data are clearly presented for one to make their own conclusions.
 

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Dr.Terp

New member
:tiphat: Anyone ever played with Paris III software? "Program Assisting Replacement of Industrial Solvents" It can be downloaded for free from EPA, but needs to be unpacked and tweaked for proper operation on your particular OS. it is basically open source ;) so you can get inside and easily alter code, expand its library and calculations to guide mixture development for performance before you even test it in lab.
:peacock:
PM and I can possibly share what my collegue craked for me. Also I wanna share another good source you can get off SciHub --->>http://www.springer.com/us/book/9783662436271 Good book, but a bit outdated from 2014, but does discuss difficulties with first gen (no-so) "GreenSolvents".
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
:tiphat: Anyone ever played with Paris III software? "Program Assisting Replacement of Industrial Solvents" It can be downloaded for free from EPA, but needs to be unpacked and tweaked for proper operation on your particular OS. it is basically open source ;) so you can get inside and easily alter code, expand its library and calculations to guide mixture development for performance before you even test it in lab.
:peacock:
PM and I can possibly share what my collegue craked for me. Also I wanna share another good source you can get off SciHub --->>http://www.springer.com/us/book/9783662436271 Good book, but a bit outdated from 2014, but does discuss difficulties with first gen (no-so) "GreenSolvents".

Thanks for the link! I ordered a copy!
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
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.

Thanks for the link! I ordered a copy!


Bookmark G.O. Joe's two resources for downloading books and papers.

Link to downloading the suggested book, Alternative Solvents for Natural Products Extraction,

http://gen.lib.rus.ec/search.php?re...open=0&view=simple&res=25&phrase=1&column=def
 

SkyHighLer

Got me a stone bad Mana
ICMag Donor
Veteran
:whee:

Amazon shipped me a 500ml bottle of ethyl formate. I have another order for three more, they're supposed to ship next week.

Here's the link, you order and wait,

https://www.amazon.com/gp/product/B00DYO8LAK/ref=oh_aui_detailpage_o03_s00?ie=UTF8&psc=1


Ethyl formate is an ester formed when ethanol (an alcohol) reacts with formic acid (a carboxylic acid). It is also known as ethyl methanoate because formic acid is also known as methanoic acid. Ethyl formate has the characteristic smell of rum and is also partially responsible for the flavor of raspberries. It occurs naturally in the body of ants and in the stingers of bees.

Exposure
Ethyl methanoate is generally recognized as safe by the U.S. Food and Drug Administration.

https://www.accessdata.fda.gov/scripts/cdrh/cfdocs/cfcfr/CFRSearch.cfm?fr=184.1295


According to the U.S Occupational Safety and Health Administration (OSHA), ethyl formate can irritate eyes, skin, mucous membranes, and the respiratory system of humans and other animals; it is also a central nervous system depressant. In industry, it is used as a solvent for cellulose nitrate, cellulose acetate, oils, and greases. It can be used as a substitute for acetone; workers may also be exposed to it under the following circumstances:

during spray, brush, or dip applications of lacquers
during the manufacture of safety glass
when fumigating tobacco, cereals, and dried fruits (as an alternative to methyl bromide under the U.S. Department of Agriculture quarantine system)

OSHA considers a time-weighted average of 100 parts per million (300 milligrams per cubic meter) over an eight-hour period as the permissible exposure limit. The U.S. National Institute for Occupational Safety and Health (NIOSH) also considers a time-weighted average of 100 ppm over an eight-hour period as the recommended exposure limit.

In space
Astronomers have identified ethyl formate in dust clouds in an area of the Milky Way galaxy called Sagittarius B2. The astronomers, from the Max Planck Institute for Radio Astronomy in Bonn, Germany, used the 30 metre IRAM radiotelescope in Spain to analyse the spectra of radiation emitted from hot regions near a new star. It is among 50 molecules identified by the astronomers.

Properties :good:
Chemical formula: C3H6O2
Molar mass: 74.08 g·mol−1
Appearance: colorless liquid
Odor: fruity
Density: 0.917 g/cm3
Melting point: −80 °C; −112 °F; 193 K
Boiling point: 54.0 °C (129.2 °F; 327.1 K)
Solubility in water: 9% (17.78°C)
Vapor pressure: 200 mmHg (20°C)

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


97% reagent grade at Sigma-Aldrich, 500ml/$48 plus shipping and Hazmat fees,

http://www.sigmaaldrich.com/catalog...Insite-_-prodRecCold_xviews-_-prodRecCold10-3

http://www.sigmaaldrich.com/Graphic...PEC/11/112682/112682-BULK_______SIAL_____.pdf

(it will require a signature at the door, and if you don't have a business account forget about it)

versus HiMedia's 97% @ 500ml/$27 total, delivered via Amazon to the general public without hassles.

http://www.himedialabs.com/TD/GRM2185.pdf


Notice how it compares to my other solvents listed as to polarity,

https://www.icmag.com/ic/showpost.php?p=7933632&postcount=162


The chemist at Manofohm said it was very popular when he had it in stock.


Pictures of another solvent from HiMedia delivered via Amazon,

https://www.icmag.com/ic/showpost.php?p=7922415&postcount=143

I'll post up pics of the ethyl formate when it arrives.

Icy, ethereal to the nose, and evaporates completely in seconds, nothing but the clear ether odor as it dissipates.


I hope everyone can get some. It says one to two month wait at Amazon, and they still haven't sent me my other three bottles, but the ad hasn't changed to unavailable, so I encourage you to make an order and give it a chance, they don't charge you until it ships. :)


Best overall solvent so far.

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

Bezoomny Bezos is sending me more outer space solvent!!!


They hit my card, it's shipping,

"HiMedia GRM2185-500ML Ethyl Formate, 500 mL
Be the first to review this item
Price: $27.00 & FREE Shipping. Details
Only 3 left in stock (more on the way).
Want it Sunday, June 11? Order within 3 hrs 14 mins and choose Standard Shipping at checkout. Details
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Specifications for this item

Part Number GRM2185-500ML
Number of Items 1
Brand Name HiMedia
EAN 8902729529997
Model Number GRM2185-500ML
UNSPSC Code 41116105"

https://www.amazon.com/gp/product/B00DYO8LAK/ref=oh_aui_detailpage_o01_s01?ie=UTF8&psc=1


$88.08 total ($7.08 CA sales tax) for three 500ml bottles.


The three 500ml bottles of ethyl formate arrived, see the quoted posts, follow them back for the pictures that accompany them.


The first bottle I received had an expiration date of February 2021, the labels on these state April 2021.
 

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SkyHighLer

Got me a stone bad Mana
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There are a few solvents that seam interesting, but upon further inspection are unsuitable for essential oil extractions. Some have melting points at or below room temperature, and some have disagreeable odors, this post concerns those that form explosive peroxides.


Peroxide Forming Solvents

A significant number of laboratory solvents can undergo autoxidation under normal storage conditions to form unstable and potentially dangerous peroxide by-products. This process is catalyzed by light and heat and occurs when susceptible materials are exposed to atmospheric oxygen. Molecular structure is the primary factor relating to a material’s potential for hazardous peroxide formation.

Most overviews of potential peroxide-forming chemicals classify various materials into three categories, on the basis of peroxide formation susceptibility, each with general handling and use guidelines.1 The two categories relevant to solvents are defined as solvents that pose a peroxide related safety risk without having to be pre-concentration (see Group A, next section) and solvents that necessitate pre-concentration in order to form peroxides (see Group B, next section). Storage time guidelines for perviously opened containers is provided in the section following this paragraph (Potential Peroxide-Forming Solvents*). Please note that the storage time indicated below are based on these solvents continually being stored in opaque containers and under inert atmospheric gases.


Potential Peroxide-Forming Solvents*

Group A: Chemicals that form explosive levels of peroxides without concentration
Severe peroxide hazard after prolonged storage, especially after exposure to air.
Test for peroxide formation before using or discard after 3 months.

Isopropyl ether

Group B: Peroxide hazards on concentration
Test for peroxide formation before distillation or evaporation. Test for peroxide formation or discard after 1 year.

Acetal
Acetaldehyde
Benzyl Alcohol
2-Butanol Dioxanes
Chlorofluoroethylene
Cumene(isopropylbenzene)
Cyclohexene
2-Cyclohexen-1-ol
Cyclopentene
Decahydronapthalene(decalin)
Diacetylene(butadiyne)
Dicyclopentadiene
Diglyme
Diethyl ether
Ethylene glycol ether acetates
Furan
4-Heptanol
2-Hexanol
Methyl Acetylene
3-Methyl-1-butanol
Methyl-isobutyl ketone
4-Methyl-2-pentanol
2-Pentanol
4-Penten-1-ol
1-Phenylethanol
Tetrahydrofuran
Tetrahydronapthalene
Vinyl Ethers
Sec. Alcohols

* Materials other than those listed may form peroxides. Applies only to pure materials.


Use and Storage of Peroxide-Forming Solvents

The solvents most commonly used in the laboratory solvents, such as diethyl ether, tetrahydrofuran, cyclohexene, glycol ethers, decalin and 2-propanol are shown in Group B of the previous section. These compounds produce organic peroxides that are significantly less volatile than the solvent in which they are formed, as a result, evaporative concentration or distillation can produce dangerous levels of peroxides. In fact, most Group B solvents are sufficiently volatile that multiple openings of a single container can result in significant and dangerous peroxide concentration. The next section contains a list of key aspects to consider when handling peroxide-forming solvents.


General Handling Considerations for Peroxidizeable Solvents:

All peroxide-forming solvents should be checked for the presence of any peroxides prior to distillation or evaporation.
Solvents containing low levels of free radical scavengers such as BHT should be used whenever the presence of the stabilizing species does not interfere with intended application.
Uninhibited materials should be stored with care and frequently checked for peroxide formation.
Peroxide-forming solvents should be purchased in limited quantities and older material in inventory should be preferentially selected for use.
Materials should be stored away from light and heat with tightly secured caps and labeled with dates of receipt and opening.
Periodic testing to detect peroxides should be performed and recorded on previously opened material.

For more information, it is recommended that the reader review the articles referenced below by Kelly2 and/or Clark3


Peroxide Detection

A variety of methods are available to test for the presence of peroxides in organic solvents with the two most common tests described below. At present, 100 ppm is widely used as a general control point with respect to minimum hazardous peroxide concentration in a solvent, however, this value lacks scientific validation and is likely too liberal or conservative depending on the solvent in question and intended application.2 If there are visible crystals, visible precipitate or an oily viscous layer present in the material, these are visual indicators of dangerous high peroxide levels, immediately contact your company's EH&S (Environmental, Health and Safety) department or its equivalent, to manage this hazardous situation and to dispose of this material.

Quantofix® Peroxide Test Strips (Sigma-Aldrich Part # Z249254 and Z101680)
In the presence of hydrogen peroxide the test paper turns blue. Quantofix® Peroxide test sticks can also be used for the determination of peracetic acid and other organic and inorganic hydroperoxides. To test for hydroperoxides in organic solvents, the test zone is wetted with one drop of water after evaporation of the solvent.

Interferences: In the pH range of 2-9, the accuracy of the determination is independent of the pH of the test solution. Buffer strongly acidic solutions with sodium acetate and adjust alkaline solutions to about pH 5-7 with citric acid. Falsely positive results can only be caused by strong oxidizing agents.

Storage: Avoid exposing the sticks to sunlight and moisture. Store unopened packs in refrigerator (+2 °C to +8 °C). Opened packs: store container in a cool and dry place.


Potassium Iodide Indicator

Add 0.5-1.0 ml of the sample solvent to an equal volume of glacial acetic acid containing about 0.1 g of sodium iodide or potassium iodide crystals. A yellow color indicates iodine formation via iodide oxidation by sample peroxide; a brown color indicates high concentration. A blank determination should be made particularly when color development is faint since iodide/acetic acid mixtures will, over time, turn a yellow - brown color due to air oxidation.

A more sensitive variation of the above method adds one drop of a saturated, aqueous starch solution to the sample solution. Starch and iodine combine to form a bright blue complex that is more easily visualized than the yellow color generated by iodine alone. Dark blue solution color would be indicative of high peroxide concentrations.


References
Jackson, H.L., McCormack, W.B., Rondestvedt, C.S., Smeltz, K.C., and Viele, I.E. Control of Peroxidizable Compounds, J. Chem. Educ., 1970, 46 (3), A175.
Kelly, R.J, Review of Safety Guidelines for Peroxidizable Organic Compounds, Chemical Health and Safety, 1996, 3 (5), 28-36.
Clark, D.E., Peroxides and Peroxide - Forming Compounds, Chemical Health and Safety, 2001, 8 (5), 12-21.


https://www.sigmaaldrich.com/chemistry/solvents/learning-center/peroxide-formation.html


And that's why I did't purchase tetrahydrofuran and a few others.

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

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