Sciencemadness Discussion Board

Cheap OTC DCM in the USA?

monolithic - 28-8-2019 at 04:04

OTC sources used to go for about $10 for a quart of 99% DCM e.g. Sunnyside #64032 paint stripper. Unfortunately, many of these sources have dried up due to the ban on DCM. I can get it for $25-30 per quart plus shipping through individual-friendly chemical suppliers (Dural, Hi Valley, Sierra Chemical, etc.), which is more than twice the cost of what it was once. Are there any cheap, OTC sources left?

[Edited on 8-28-2019 by monolithic]

[Edited on 8-28-2019 by monolithic]

CouchHatter - 28-8-2019 at 04:09

Did you search eBay?

Cheaper than when I got mine last year.

monolithic - 28-8-2019 at 04:13

Quote: Originally posted by CouchHatter  
Did you search eBay?

Cheaper than when I got mine last year.


I did see that, but I really only need a quart, especially since I recycle solvents whenever possible.

Herr Haber - 28-8-2019 at 05:49

I recently got a 5 liter can despite the ban for 28 Euros.

Check your local boating supplies shop, skate board, windsurf etc. Anything that uses fiber.
They have some interesting chemicals.

MrHomeScientist - 28-8-2019 at 07:07

Quote: Originally posted by monolithic  
Unfortunately, many of these sources have dried up

Make sure the cap is on tight! DCM is very volatile :P


I got mine from distilling paint stripper form the hardware store - check the SDS to make sure it's the right stuff. It leaves behind a lot of goop in the flask, but that's (surprisingly) easily removed with rubbing alcohol.

monolithic - 28-8-2019 at 07:52

Quote: Originally posted by MrHomeScientist  
Quote: Originally posted by monolithic  
Unfortunately, many of these sources have dried up

Make sure the cap is on tight! DCM is very volatile :P


I got mine from distilling paint stripper form the hardware store - check the SDS to make sure it's the right stuff. It leaves behind a lot of goop in the flask, but that's (surprisingly) easily removed with rubbing alcohol.


Do you remember what brand of paint stripper it was? A lot of them are moving toward formulas which completely exclude DCM.

MrHomeScientist - 28-8-2019 at 08:32

Klean Strip KS-3 Premium Stripper. Here's my video on distilling it: https://www.youtube.com/watch?v=c3ppYMTAqWM

Apparently that was 7 years ago now (damn!) so things may have changed. Searching Klean Strip's site returns a different item now, but it still lists DCM and methanol in the warnings so it may still be the same thing.

Further down the Google page, it looks like a paint store still sells the same can I used: http://www.nelsonpaint.com/S00315.html


Edit:
I rewatched my old video and I misremembered: kerosene was used to wash the goop out of the flask, then acetone removed the kerosene residue.
And then if you're interested, here's how I purified the DCM I obtained: https://www.youtube.com/watch?v=ZcsHZVydZds

[Edited on 8-28-2019 by MrHomeScientist]

TD64209 - 28-8-2019 at 11:51

Some "Goof Off" (sprayable) is methanol, DCM, and shit that gums up on contact with water. So not as easy as a simple water wash but 50-60% DCM.

monolithic - 28-8-2019 at 14:24

Quote: Originally posted by TD64209  
Some "Goof Off" (sprayable) is methanol, DCM, and shit that gums up on contact with water. So not as easy as a simple water wash but 50-60% DCM.


A good source of DCM but it's discontinued per the manufacturer's website. Looks like Klean Strip Premium Stripper and specialty products at boat shops is the best option in 2019.

[Edited on 8-28-2019 by monolithic]

monolithic - 18-9-2019 at 03:57

Just to update, apparently Klean Strip changed the formula of Premium Stripper sometime in 2018. It's no longer DCM, it's now DMC (dimethyl carbonate) which is great if you want to perform methylation reactions but bad if you want a chlorinated solvent...

2018 MSDS: https://images.homedepot-static.com/catalog/pdfImages/4c/4cc...
2015 MSDS: http://www.kleanstrip.com/uploads/documents/GKS3_SDS-4015.34...

I believe the 2018 and later production runs will advertise "Non-Methylene Chloride" on the front of the bottle/can, so it should be easy to tell if you see any old stock on the shelves of your hardware store. They also make a California compliant old stock version which omits DMC, see: https://images.homedepot-static.com/catalog/pdfImages/f2/f2f...

[Edited on 9-18-2019 by monolithic]

artemov - 18-9-2019 at 05:25

Is DCM that toxic? Now I'm a bit worried ...

https://www.msn.com/en-us/news/us/epa-ban-on-popular-toxic-p...

"Rosenman said methylene chloride directly affects the brain and acts similarly to alcohol toxicity when someone drinks too much – but just a little of this chemical, can kill quickly. Methylene chloride in paint strippers can be inhaled as fumes breach the air and it can also be absorbed through the skin.

"Between those two ways, just a tablespoon is enough to kill you," he said"

monolithic - 18-9-2019 at 05:51

Quote: Originally posted by artemov  
Is DCM that toxic? Now I'm a bit worried ...

https://www.msn.com/en-us/news/us/epa-ban-on-popular-toxic-p...

"Rosenman said methylene chloride directly affects the brain and acts similarly to alcohol toxicity when someone drinks too much – but just a little of this chemical, can kill quickly. Methylene chloride in paint strippers can be inhaled as fumes breach the air and it can also be absorbed through the skin.

"Between those two ways, just a tablespoon is enough to kill you," he said"


Sure, it's toxic but if you aren't acting recklessly (drinking it, working in a poorly ventilated area without a fume hood, spilling hundreds of milliliters on yourself, etc.) you'll likely be fine. I'm guessing it was banned from the OTC realm because it's not very environmentally friendly to be a significant constituent in paint stripper which is sold by the quart or gallon, and the fact that most people are idiots who will strip paint indoors with no ventilation.

PirateDocBrown - 18-9-2019 at 13:48

https://www.carolina.com/catalog/detail.jsp?prodId=875970&am...

PirateDocBrown - 18-9-2019 at 13:54

That said, I'm surprised the possible terror applications of dimethyl carbonate have not been attended to by the authorities.

Though I suppose that phosgene production via HCl isn't much simpler than producing it by direct reaction of CO with Cl2.

[Edited on 9/18/19 by PirateDocBrown]

monolithic - 21-1-2020 at 16:29

For anyone wondering, Dural will not ship DCM to a residential address. Man of Ohm will not ship DCM to a residential address, either. With regard to over the counter products, I believe Caseway acrylic cements (they have a number of them) still contain DCM. I believe SCIGRIP and TAP Plastics acrylic cements also still contain DCM.

earpain - 15-4-2020 at 17:02

I was wondering about this as well. I've been steam distilling flavor/essence compounds. Some like to phase out bellow water, not above it. Or just having a very non-polar, and very volatile solvent handy is so universal. But diethyl ether, chloroform , and now DCM are becoming scarce. Are there any solvents still OTC that somewhat have these characteristics?

Dr.Bob - 16-4-2020 at 07:47

If anyine wants DCM in the NC area, I can give or sell you used material that you can distill. I have lots left over from stripping some paint and varnish a few years back, just too lazy to distill it.

Bob

clearly_not_atara - 16-4-2020 at 10:27

Chloroform is easily synthesized if hypochlorites are available. However, its instability and toxicity make it a rather undesirable choice.

Isopropyl formate is relatively nonpolar and has a boiling point of 68 C and melting point -80 C. Its water solubility is about 2% w/w or 0.235 M according to the EPA:
https://comptox.epa.gov/dashboard/dsstoxdb/results?search=DT...

Unlike other esters, formates can be obtained simply by the reaction of isopropanol and formic acid with no catalysts. Formate esters are aprotic solvents but react with nucleophiles, including amines, and decompose in the presence of strong acids. However, I think they might be acceptable solvents for organozinc or organomanganese reagents which do not usually react with esters.

Ethyl formate is obtained similarly but has a higher water solubility of about 9%.

Some papers indicate that attempting to esterify ethanol with oxalic acid accidentally produces ethyl formate. In particular this occurs because of decomposition of the intermediate half-ester. It seems like it should be possible to obtain a good yield of isopropyl formate by heating isopropanol with oxalic acid in a 1:1 molar ratio, so that principally half-esters are obtained and they decompose to the desired formate. Anhydrous oxalic acid should be used rather than the dihydrate.

earpain - 16-4-2020 at 11:07

Quote: Originally posted by clearly_not_atara  
Chloroform is easily synthesized if hypochlorites are available. However, its instability and toxicity make it a rather undesirable choice.

Isopropyl formate is relatively nonpolar and has a boiling point of 68 C and melting point -80 C. Its water solubility is about 2% w/w or 0.235 M according to the EPA:
https://comptox.epa.gov/dashboard/dsstoxdb/results?search=DT...

Unlike other esters, formates can be obtained simply by the reaction of isopropanol and formic acid with no catalysts. Formate esters are aprotic solvents but react with nucleophiles, including amines, and decompose in the presence of strong acids. However, I think they might be acceptable solvents for organozinc or organomanganese reagents which do not usually react with esters.

Ethyl formate is obtained similarly but has a higher water solubility of about 9%.

Some papers indicate that attempting to esterify ethanol with oxalic acid accidentally produces ethyl formate. In particular this occurs because of decomposition of the intermediate half-ester. It seems like it should be possible to obtain a good yield of isopropyl formate by heating isopropanol with oxalic acid in a 1:1 molar ratio, so that principally half-esters are obtained and they decompose to the desired formate. Anhydrous oxalic acid should be used rather than the dihydrate.


Interesting infromation, thank you!

It seems that these reagents, would still be a bit too reactive to be considered 'general use solvents'. My main use for a non-polar really would be acid/base extractions, perhaps crystallizations.

I have made chloroform before, and I'm aware of how and why it should be stored in amber glass, and that it is psychoactive, etc. The issue was I couldn't find any non aq. form of a hypochlorite, so making just 50ml requires a car trunk full of NaOCl 5% bottles.

I have -attempted-, and epically failed at EtOH + H2SO4 -> diethyl ether. I'm certain it was due to lack of equipment. In particular, no way of dripping ethanol in slowly as the reaction progressed, and inadequate column + subsequent condenser set up, likely I formed SOME diethyl ether but at 130C in the reaction flask, I'm sure it was on it's way to the sky long before i would have even noticed a drop of it

[Edited on 16-4-2020 by earpain]

monolithic - 16-4-2020 at 13:55

Quote: Originally posted by earpain  
I was wondering about this as well. I've been steam distilling flavor/essence compounds. Some like to phase out bellow water, not above it. Or just having a very non-polar, and very volatile solvent handy is so universal. But diethyl ether, chloroform , and now DCM are becoming scarce. Are there any solvents still OTC that somewhat have these characteristics?



Ether can be sourced quite easily from starter fluids. Biggest concern is adding peroxide inhibitors (BHT, etc.)

Chloroform can be made quite easily from acetone and bleach in good yields. I have done this myself recently, if you buy pool cleaner grade bleach (10% w/w sodium hypochlorite) then the cost to synthesize a liter of chloroform isn't too bad, somewhere around $30-35/liter.

DCM is unfortunate in that it is incredibly useful but almost impossible to synthesize or source. I ended up buying a liter from a scientific supplier that sells to individuals for something like $45 after shipping. Expensive but oh well, not like there's an alternative.

[Edited on 4-16-2020 by monolithic]

earpain - 16-4-2020 at 14:08

Quote: Originally posted by monolithic  
Quote: Originally posted by earpain  
I was wondering about this as well. I've been steam distilling flavor/essence compounds. Some like to phase out bellow water, not above it. Or just having a very non-polar, and very volatile solvent handy is so universal. But diethyl ether, chloroform , and now DCM are becoming scarce. Are there any solvents still OTC that somewhat have these characteristics?



Ether can be sourced quite easily from starter fluids. Biggest concern is adding peroxide inhibitors (BHT, etc.)

Chloroform can be made quite easily from acetone and bleach in good yields. I have done this myself recently, if you buy pool cleaner grade bleach (10% w/w sodium hypochlorite) then the cost to synthesize a liter of chloroform isn't too bad, somewhere around $30-35/liter.

DCM is unfortunate in that it is incredibly useful but almost impossible to synthesize or source. I ended up buying a liter from a scientific supplier that sells to individuals for something like $45 after shipping. Expensive but oh well, not like there's an alternative.

[Edited on 4-16-2020 by monolithic]


Maybe I just haven't looked, or maybe it's because I live in a snowwy area where people rarely have their own pooles, but I've never seen a 10% hypochlorite solution sold.

Though I think when I used 5%, the H2O to Chloroform ratio was almost comical. Like I had to use a plastic bin large enough to put a person in.

For my purposes chloroform and DCM would be interchangeable, i suppose you are using it as a reagent.


All of the branded starter fluid spray formulations in my area seem to have maybe 10% diethyl ether now. the SDS shows usually 7 or 8 rather flammable substances, besides ethanol the others are rather exotic. Based on a few distillations while watching the thermometer, although certaintly not 'analytical' grade care and attention , Something like 10% - 15% seemed to be the content.

Only some ghetto gas stations with very generic looking can of starter fluid still have 50% diethyl ether and 50% hexane

[Edited on 16-4-2020 by earpain]

monolithic - 16-4-2020 at 17:44

Quote: Originally posted by earpain  
Quote: Originally posted by monolithic  
Quote: Originally posted by earpain  
I was wondering about this as well. I've been steam distilling flavor/essence compounds. Some like to phase out bellow water, not above it. Or just having a very non-polar, and very volatile solvent handy is so universal. But diethyl ether, chloroform , and now DCM are becoming scarce. Are there any solvents still OTC that somewhat have these characteristics?



Ether can be sourced quite easily from starter fluids. Biggest concern is adding peroxide inhibitors (BHT, etc.)

Chloroform can be made quite easily from acetone and bleach in good yields. I have done this myself recently, if you buy pool cleaner grade bleach (10% w/w sodium hypochlorite) then the cost to synthesize a liter of chloroform isn't too bad, somewhere around $30-35/liter.

DCM is unfortunate in that it is incredibly useful but almost impossible to synthesize or source. I ended up buying a liter from a scientific supplier that sells to individuals for something like $45 after shipping. Expensive but oh well, not like there's an alternative.

[Edited on 4-16-2020 by monolithic]


Maybe I just haven't looked, or maybe it's because I live in a snowwy area where people rarely have their own pooles, but I've never seen a 10% hypochlorite solution sold.

Though I think when I used 5%, the H2O to Chloroform ratio was almost comical. Like I had to use a plastic bin large enough to put a person in.

For my purposes chloroform and DCM would be interchangeable, i suppose you are using it as a reagent.


All of the branded starter fluid spray formulations in my area seem to have maybe 10% diethyl ether now. the SDS shows usually 7 or 8 rather flammable substances, besides ethanol the others are rather exotic. Based on a few distillations while watching the thermometer, although certaintly not 'analytical' grade care and attention , Something like 10% - 15% seemed to be the content.

Only some ghetto gas stations with very generic looking can of starter fluid still have 50% diethyl ether and 50% hexane

[Edited on 16-4-2020 by earpain]


If you're using the USA, Wal-Mart and Home Depot carry 10% bleach.

https://www.walmart.com/ip/Pool-Essentials-Chlorinating-Liqu...
https://www.homedepot.com/p/HDX-128-oz-Chlorinating-Liquid-3...

Yes I checked and most of the starter fluids are now 20-30% ether, even the premium versions, with the rest being heptanes. That sucks.

clearly_not_atara - 17-4-2020 at 08:40

20-30% ether I think you could work with... 10% sucks. Ether can dissolve in seventeen parts water, and might thereafter be salted out.

earpain - 19-4-2020 at 07:13

Quote: Originally posted by clearly_not_atara  
20-30% ether I think you could work with... 10% sucks. Ether can dissolve in seventeen parts water, and might thereafter be salted out.


monolithic, thanks! Hmm, I wonder if my local home depot would actually stock that. There's definitely no 'pool' section.

clearly_not_atara I am 110% sure that the difference in those percentages is explained by my casual lab technique whenever it was that I did conclude 10%.

I really need to get better at making cooling baths.

Actually after some perusing of amazon and ebay, in the US, I think semi-OTC (does not require customer to be a business) n-hexane, ethyl acetate, are pretty ok options for ok prices. there's still toluene at the hardware stores, though I would distill it first for sure.

I have glassware coming that should make it possible to succeed at the dehydration of ethanol via H2SO4 to diethyl ether.

And don't worry everyone, once collected I would have some KOH flakes in the container. Dessicate/salt out / peroxide protection all in a few flakes. Store in freezer with mechanical clamping on the stopper.

clearly_not_atara - 19-4-2020 at 09:13

Quote:
Hmm, I wonder if my local home depot would actually stock that. There's definitely no 'pool' section.


A number of hardware stores have an in-store locator you can use online, which saves a lot of time.