Sciencemadness Discussion Board - 16 oz of nitroethane. Buy or nah?

16 oz of nitroethane. Buy or nah?

chemist1243 - 4-6-2021 at 06:15

I found 16oz of nearly pure nitroethane in the form of brush cleaner. I know its almost pure, as ive used the same formula straight from a .5oz bottle before in the Henry reaction and everything went fine, plus MSDS confirms its at least 98%.

Should i buy it? I was able to find it on amazon and eBay, but am still nervous because..well...its a massive quantity. I’m worried if i may get a visit from some law enforcement entities after ordering such a large amount of a product who’s main component almost certainly implies drug synthesis.

I’m torn. Thoughts?

Texium - 4-6-2021 at 06:41

If you’re in the US, nitroethane is DEA list 1, so the sale info will have to be logged, and made available to the DEA on request. Buy it at your own risk. If you weren’t actually making drugs and had a more legitimate use for it, I’d say you really wouldn’t have much to worry about, but I know that isn’t the case, so yeah, probably better for you and the amateur community at large if you don’t purchase it.

chemist1243 - 4-6-2021 at 06:55

So what? Ive ordered nitroethane brush cleaner and benzaldehyde in the same month before, no visits yet. What is the chance they’ll even come?

karlos³ - 4-6-2021 at 08:58

Quote: Originally posted by chemist1243

So what? Ive ordered nitroethane brush cleaner and benzaldehyde in the same month before, no visits yet. What is the chance they’ll even come?

When they have time, and when they can be sure that a significant amount of product has been made(that half liter might would be sufficient to wake them up, no idea).
If you buy it from inside the states, better to let it be.
But if its from the outside, no worries, I got friends in the US who bought liters of nitroethane from germany with no issues.

monolithic - 4-6-2021 at 10:45

Quote: Originally posted by Texium

If you’re in the US, nitroethane is DEA list 1, so the sale info will have to be logged, and made available to the DEA on request. Buy it at your own risk. If you weren’t actually making drugs and had a more legitimate use for it, I’d say you really wouldn’t have much to worry about, but I know that isn’t the case, so yeah, probably better for you and the amateur community at large if you don’t purchase it.

The threshold for regulated transactions of nitroethane is 2.5 kg per the DEA Chemcial Handler's manual. At any rate, I'd be interested to see the product. I was under the impression that all of those nitroethane "nail removers" and "brush cleaners" were reformulated to acetone or other solvents, regardless of what the outdated MSDS claimed.

student - 4-6-2021 at 11:08

Mia Secret Brush Cleaner contained only about 5% nitroethane even though that was the only solvent listed in the ingredients.

What you need is a woman who will put your bottle with her beauty supplies!

[Edited on 4-6-2021 by student]

karlos³ - 4-6-2021 at 12:11

Yeah but that only works up to a certain amount.
3x1l of pure nitroethane definitely is too much for that excuse, speaking from experience

Fyndium - 4-6-2021 at 12:18

If you have time, you can buy stuff, put it on shelf(or deeper) and sit on it for half a year or more. If someone knocks, you know it was a problem to someone, but you don't have a problem. I read about this something like 10 years ago, when an user at a passed forum indicated that he had bought a lot of all kinds of interesting stuff and put it away, and behold, 2 months passed and he got a knock (actually a no-knock), but they found absolutely nothing, and case dried as fast as it came up. Don't know though what happened afterwards.

In Europe honeypots are not a commonplace activity because LE is generally not allowed to sell, but only buy suspected contraband, but I know several cases in US.

draculic acid69 - 4-6-2021 at 16:37

Quote: Originally posted by chemist1243

So what? Ive ordered nitroethane brush cleaner and benzaldehyde in the same month before, no visits yet. What is the chance they’ll even come?

A lot more likely now that U have announced that U r feeling sketchy about it to the world wide web.

njl - 5-6-2021 at 04:43

Quote: Originally posted by draculic acid69

Quote: Originally posted by chemist1243

So what? Ive ordered nitroethane brush cleaner and benzaldehyde in the same month before, no visits yet. What is the chance they’ll even come?

A lot more likely now that U have announced that U r feeling sketchy about it to the world wide web.

This. Your username is not a shield; it's a name just like any other. A name that is now tied to a post, on a chemistry forum, on the internet, clear for anyone who cares to see.

zed - 5-6-2021 at 05:44

It's brush cleaner. How could an innocent artist know it has some weird chemical in it? Try to order it through your local art supply store.

LE would better utilize their energies in attempting to regulate the hundreds of tons of Ephedrine, imported by the Mexican Drug Cartels every year.

Courtesy of China, India, and the Mexican Drug Cartels, the USA has been flooded with nasty drugs, at discount prices.

Nitroethane can be synthesized, but it's irksome.

[Edited on 5-6-2021 by zed]

karlos³ - 5-6-2021 at 05:45

Quote: Originally posted by njl

Quote: Originally posted by draculic acid69

Quote: Originally posted by chemist1243

So what? Ive ordered nitroethane brush cleaner and benzaldehyde in the same month before, no visits yet. What is the chance they’ll even come?

A lot more likely now that U have announced that U r feeling sketchy about it to the world wide web.

This. Your username is not a shield; it's a name just like any other. A name that is now tied to a post, on a chemistry forum, on the internet, clear for anyone who cares to see.

Nobody I know got ever in trouble because of their online activities only.

chemist1243 - 7-6-2021 at 06:49

Just got it. Its the same labeling format, brand, and formula as the regular small bottles of this brand, which are 14ml each.
I have used those .5 oz bottles in the Henry reaction and observed the correct color changes and crystallization of the nitropropene as described in literature.

I don’t think the supplier is a honey pot. There have been over 1000 orders in the past year with 96% positive reviews.

I suppose some of you found it! There are 2 less bottles available than when I checked yesterday.

It’s unlikely the DEA has any business with me. Not going into too much detail, but for undisclosed reasons it would be a waste of time and resources to prosecute me, which is more apparent after reading the conditions in which most of the negative consequences of this purchase would actually come about.

Conveniently, I actually do have other hobbies. I paint and have a very small area where I mess with perfumery stuff. I’ve always used acetone for convenience(when cleaning acrylic), but I guess it’s probably time to switch to something better.

97D93AF7-F384-4F59-9121-E7FB44DBD7C6.jpeg - 1.3MB

mr_bovinejony - 7-6-2021 at 09:05

Ohh I recognize that brand. I'm curious to know how much of a yield you get if you distill it

karlos³ - 7-6-2021 at 10:12

Well, he said he has used it as is already, so there is probably no need for that.
Anything unwanted can be removed from the nitroalkene later, I assume?
But he hasn't said anything about his henry's yields or such, so who know if that is advisable...

E: nitroethane is first on the listing, and the other things are stuff thats usually only used in minute amounts...
I would guess its pretty pure, besides the fragrance and colouring.

[Edited on 7-6-2021 by karlos³]

morganbw - 7-6-2021 at 11:25

Quote: Originally posted by zed

It's brush cleaner. How could an innocent artist know it has some weird chemical in it? Try to order it through your local art supply store.

LE would better utilize their energies in attempting to regulate the hundreds of tons of Ephedrine, imported by the Mexican Drug Cartels every year.

Courtesy of China, India, and the Mexican Drug Cartels, the USA has been flooded with nasty drugs, at discount prices.

Nitroethane can be synthesized, but it's irksome.

[Edited on 5-6-2021 by zed]

Irksome is a true description. Doable but a little mind bending.

[Edited on 6/7/2021 by morganbw]

chemist1243 - 7-6-2021 at 12:20

I always get back just a little bit more product than the amount of aldehyde I put in. So I’d say 60% on the Henry after purification when using undistilled brush cleaner. Would probably be higher if I had more experience.

The first time I did the Henry reaction, I used brush cleaner. I’ve never had to distill It for the reaction to work but I would be interested to know if it made a difference.

It’s certainly viable, great source of nitroethane. A lot of these things just pop up and die out though, so it can be a matter of keeping a good eye out for it and grabbing it ASAP when you see it.

njl - 7-6-2021 at 12:45

Quote:

I always get back just a little bit more product than the amount of aldehyde I put in

Quote:

I’d say 60% on the Henry

Can you elaborate on what this means?

karlos³ - 7-6-2021 at 13:10

Can you put this into a percentage of theoretical yield please, and say under which conditions, using what amine catalyst?
Those details are very important.

chemist1243 - 7-6-2021 at 16:10

Put 10.6g of benzaldehyde(.1mol) and 8.26g of nitroethane(.11mol) in a flask. The total weight of those 2 main reagents is 18.86g. Now let’s say I get 11g of product from a reaction using this ratio. That’s “just a little bit more product than the amount of aldehyde I put in”, just a bit more than 10.6g. (11/18.86)*100 = 58.3%

So about 60%, guess I was off a bit. That’s a confusing way to measure yield im sure. If everything had gone perfect, I’d have 16.3g of product. So the theoretical yield would be (11/16.3)*100 = 67.4%. A little high for the conditions I use, meaning I am bad at measurements and estimations ):

I’ve tried it using an adaptated mdp2np synthesis from Pihkal. I use freebase PEA as my catalyst. I’ve tried using .01mol of catalyst instead of .1mol like in the reference. I also tried using .12mols of nitroethane instead of .2

I got best results using a 1:1 molar ratio of catalyst to aldehyde and 1:2 molar ratio of benzaldehyde to nitroethane.
With a 1:10 molar ratio of catalyst to aldehyde and .12mols of nitroethane, The color only darkened to a dark yellow even after 6 hours. while using the ratios that Shulgin uses, after 2 hours of reflux it was very orange. With the ratios Shulgin uses, all the nitropropene crashed out very quickly when water was added. With the modified ratios, I could not get it to crystallize, even using seed crystals I had.

https://erowid.org/library/books_online/pihkal/pihkal100.sht...

chemist1243 - 10-6-2021 at 09:02

I found some more information on this stuff, ill also be distilling it tomorrow, which is when my new thermometers should get here.

interestingly, I found a 2 star review on ebay for the smaller bottles of this brand. the buyer said "This is expensive acetone (25%) among other chemicals other than what’s listed on the bottle.".

hmmm. so I contacted him asking how he knew this, and he simply said that another buyer did an NMR on it. bingo! so I ask if he has any contact to the person or if he can access the data. his reply? "nope". oh well, there goes that gold.

I did add a few ml of the brush cleaner to some steel wool in 31% HCl, left it for 15 minutes, then diluted with water. no overwhelming smell of ethylamine, but then again its mostly muriatic acid so it would've been salted immediately. perhaps i should add some base to neutralize the HCl and freebase he amine and then see?

also, the product floats on water. now this could be because the nitroethane is diluted with a much less dense solvent which is immiscible with water yet miscible with Nitroethane, or it could have no nitroethane in it at all and be something different entirely. i have no idea, all i know is the stuff doesnt sink, even with shaking it always floats back to the top.

i also did a burn test. now, if you take RC fuel(which is basically just MeOH, nitromethane, and lubricant), pour it on some concrete or blacktop, and light it, you will notice that it burns in an odd way. ill try my best to describe it. the flame seems to repeatedly "flash" while making a soft, quick rumbling sound, each time flaring up like that and temporarily receding back before doing it again.

so i mixed some of the brush cleaner with about 4x its volume with IPA, poured it on the black top, and set it on fire. initially, the mixture burned normally like gasoline or high proof alcohol, but as it died down it made the repeating flash/rumble just like nitromethane does.

the ebay buyer says its 25% acetone among other chemicals than whats listed in the bottle. this is vauge but could imply that those chemicals are simply among what is listed, meaning there IS nitroethane.

it does have an acetone-like smell, but after shaking with water it is more fruity. this is most likley the perfume, but still an interesting observation because it adds credibility to what this ebay buyer is saying. if the acetone smell goes away after shaking with water, it probably had acetone that went into the water.

like i said i will do a distillation ASAP and verify this brand once and for all.

Fery - 10-6-2021 at 11:43

chemist1243 - yes, nitroethane has nice fruity scent
here an useful thread concerning acetone - nitroethane separation:
http://www.sciencemadness.org/talk/viewthread.php?tid=7689

chemist1243 - 10-6-2021 at 14:15

first Ill just do a simple distillation, recording and collecting what comes over at what temperatures and how much. I should be able to identify at least one of the ingredients from doing that. if there are other boiling points matching those of known azeotropes or solvents even better.

maybe fractional distillation will be needed, but ill see when I get there.

EDIT: I have been waiting all day for my new thermometers, and I till need to see how much they're off by. I will start tomorrow.

[Edited on 11-6-2021 by chemist1243]

chemist1243 - 12-6-2021 at 18:53

RESULTS:

50ml of the brush cleaner is added to a RB flask. this is then set up for simple distillation, insulated with foil and then heated. 3 fractions were collected over period of almost 2 hours. the following time stamps, temperatures and changes to the set-up have been condensed and compiled below, being listed in that order:

T+ 0:00 | 29C | fan turned on low and directed towards setup for ventilation

T+ 0:00 - 15:00 | 29C | fan turned off |

T+ 20:00 | 58C | fan turned on again |

T+ 25:00 | 54C | fan turned off |

T+ 26:44 | 61C |

T+ 28:02 | 64C | flask switched out, distillate weighed |

T+ 30:00 - 35:00 | 65C |

T+ 40:03 - 48:29 | 64C |

T+ 51:36 - 54:39 | 60C |

T+ 56:35 | 56C | flask switched out again |

T+ 61:03 | 123C |

T+ 65:36 - 115:23 | 29C |

after 115 minutes, the distillated was stopped before reaching dryness.

the first fraction came over at 54-58C, and weighed 3.6g. this is around the the boiling point of acetone, so I think that's what it is. I will have to do more tests to be sure.

the next fraction was around 61-64C, roughly the boiling point of methanol. this was larger, weighing 5.6g. interesting.

then the largest fraction and arguably the most disappointing as well was the last. it boiled at 123 - 129C, which averages out to exactly 126; the boiling point of a commonly used solvent in brush cleaners and nail polish removers, n-Butyl Acetate. this fraction weighed 34.58.

altogether, the fractions weigh 43.75g

so the respective percentages for acetone, methanol, and n-Butyl Acetate are 8%, 13%, and 79.

maybe they are different solvents though, I still have to test that. I have some pictures too.

in the photo with the 2 flasks and beaker, the far left 50ml beaker is the first fraction, the one next to that is the second fraction, and the last is the third. the other photo is the 6g or so of remaining liquid in the main flask. I didnt want to distill to dryness for safety reasons, but I dont think its anything other than the NBA.

unfortunately, this bottle is useless. dont buy the big bottles of this brand if you want nitroethane.

mr_bovinejony - 12-6-2021 at 20:53

Do they not update the sds on their website? That's kinda shitty, although I bought some small bottle of the same brand and same name so hopefully it'll be different

njl - 13-6-2021 at 05:30

At least we know now. I suppose that also applies to this.

chemist1243 - 13-6-2021 at 09:45

yes, it applies to that; thats the bottle I distilled.

monolithic - 13-6-2021 at 14:12

I bought the same brand of brush cleaner a few years ago. I tried doing a water wash to separate the nitroethane and the water soluble crap. I instantly knew something was wrong when it formed a single layer. Tried salting out the "nitroethane" and nothing ever separated out, so I just threw it the fuck away. As far as I know there is only a single "OTC" product on the market in the United States that contains an appreciable and affordable amount of nitroethane.

[Edited on 6-13-2021 by monolithic]

chemist1243 - 14-6-2021 at 07:37

and whats that?

Fantasma4500 - 15-6-2021 at 08:08

its lucky they havent realized the energetics potential of NE, its very damn close to NM.

student - 15-6-2021 at 12:58

I checked one of these 16 oz bottles and have a theory about what is going on. My bottle looks tampered with, having label residue on the cap and no seal. The contents are colorless despite the official ingredients including blue coloring. It smells like an ester, and the smell is much stronger than pure nitroethane. I ran the Henry reaction on a small scale with benzaldehyde and it turned dark orange, so nitroethane seems to be present. Diluting the cold reaction product with water causes a brown oil to precipitate that smells like benzaldehyde, consistent with a low concentration of nitroethane in the cleaner.

I will try distilling it. When I distilled Mia Secret brush cleaner, which was also missing the blue dye and gave an identical result with the Henry reaction, it gave 15 mL of distillate between 110°C and 120°C from 110 mL of cleaner. So there may be 10% nitroethane in it, making it not cost effective as a source.

We have been speculating that these products are getting reformulated out of concerns for user safety or misuse of the product. But the observations above suggest that there is a middleman intercepting the bottles and replacing their contents with reformulated solvent. The incentive would be to then sell the nitroethane on the black market.

One question I have for the OP - when the bottles give a proper yield of nitrostyrene, is the brush cleaner blue or colorless?

mr_bovinejony - 15-6-2021 at 16:09

Where are you buying these bottles from where a middleman gets ahold of them? Seems like from Amazon or from the supplier themselves, they shouldnt be able to be tampered with

student - 16-6-2021 at 06:22

Quote: Originally posted by mr_bovinejony

Where are you buying these bottles from where a middleman gets ahold of them? Seems like from Amazon or from the supplier themselves, they shouldnt be able to be tampered with

I've bought from Amazon and eBay. The fact that this exact same counterfeiting is happening with different brands means that any "middleman" is involved early in the supply chain, maybe just an employee at a bottling factory. I don't know that the counterfeit product is identical between brands, but the OP's distillation results sound equivalent to my own.

chemist1243 - 16-6-2021 at 10:23

ive only ever used the small bottles, which were colorless. I never did a reduction to amphetamine using what I believe is the desired nitropropene, just to note.

we could of course contact the owners about the issue: https://cuccio.com/index.php?main_page=contact_us

but I think our cries would fall on deaf ears.

I tried the henry reaction using the stuff from 16oz bottles and it turned dark orange after only 15 mintes of reflux. thats oddly fast to me. for some reason the color change is happening but there seems to not be any nitroethane in the brush cleaner.

[Edited on 16-6-2021 by chemist1243]

karlos³ - 16-6-2021 at 10:57

Quote: Originally posted by chemist1243

I never did a reduction to amphetamine using what I believe is the desired nitropropene, just to note.

You could have said the same with "I wasn't one of the cool kids" in fewer words

Just kidding of course.

By the way, in a good henry reaction, you aim not to have much color change at all, that defies the thought the way you carry it out.

[Edited on 16-6-2021 by karlos³]

chemist1243 - 16-6-2021 at 15:55

amphetamine is SOOOO last weekend, get with the times! ;D

I think in a good henry reaction, yes, piss-yellow is ideal. but I know strong coloration is definitely a good indicator that somethings happening.

Monoamine - 25-6-2021 at 12:26

Quote: Originally posted by chemist1243

I found 16oz of nearly pure nitroethane in the form of brush cleaner. I know its almost pure, as ive used the same formula straight from a .5oz bottle before in the Henry reaction and everything went fine, plus MSDS confirms its at least 98%.

Should i buy it? I was able to find it on amazon and eBay, but am still nervous because..well...its a massive quantity. I’m worried if i may get a visit from some law enforcement entities after ordering such a large amount of a product who’s main component almost certainly implies drug synthesis.

I’m torn. Thoughts?

So if it's a brush cleaner then why not just check if your local arts and crafts store has it an pay wirh cash? Technically you're using it for art too after all...

macckone - 25-6-2021 at 13:59

All that distillation it actually sounds easier to go the bromoethane/sodium nitrite route.