Author Topic: new additive in OTC acetone, others  (Read 467 times)

iknowjt

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new additive in OTC acetone, others
« on: January 08, 2010, 10:08:45 PM »
I've encountered first in one brand of acetone, than an another, and now in naphtha.  I believe it's a surfactant intended to either slow down evaporation or inhibit accidental combustion.  It really messes up crystal formation, A/B, washing.  Distilling it solves the problem.

Anybody else?

Methyl Man

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Re: new additive in OTC acetone, others
« Reply #1 on: April 21, 2011, 12:28:15 AM »
Does this additive show itself as a residue left behind in test evaporations of small amounts? Seems like a surfactant shouldn't be able to evaporate very quickly.
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psychexplorer

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Re: new additive in OTC acetone, others
« Reply #2 on: April 21, 2011, 03:02:33 AM »
Yeah, OTC acetone is a mixed bag like the rest of our hardware store solvents. Definitely start with an evap on glass.

The manufacturing of all this stuff is questionable at best. We think and hope in terms of ACS reagent grade prepared by chemists, meanwhile the stuff is probably dispensed out of a giant vat labeled "SALVE?T" by somebody who couldn't tell the difference between a salt and a ketone.

I always distill. That's one less variable I have to drive myself crazy thinking about when wondering what went wrong. Those who can't repeatedly deal with solvent vapors while working with glass should start with an evaporation test, a density measurement, and a boiling range. Anything too bad to be used straight probably will flunk at least one of the three.

pyramid

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Re: new additive in OTC acetone, others
« Reply #3 on: April 21, 2011, 05:05:14 AM »
Acetone obtained from a hardware store or paint store should always be refluxed with potassium permanganate and then distilled, preferably fractionally distilled. Read more about this elsewhere as it is covered in lots of detail.
 There is not only surfactants and water but also ketones and who knows what else. If making products intended for eventual consumption (but who would do such a thing) then it must be purified properly. Yu might have made a great pure salt of some compound, then once you wash it with acetone you have introduced all sorts of shit simply because it was not purified properly. This should not be acceptable to anyone.

Methyl Man

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Re: new additive in OTC acetone, others
« Reply #4 on: April 21, 2011, 06:22:56 PM »
How about the (claimed to be) 99.5% pure acetone from the pre-eminent biodiesel supply site (starts with a "D")? I imagine that for biodiesel making, it's a similar thing---impurities in solvents could screw things up.

I have hope that theirs is actually 99.5% as they say... it's $10 more (and then shipping!) than hardware store acetone, but perhaps it's worth it. I know I don't want to do any more distillations than I have to.
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pyramid

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Re: new additive in OTC acetone, others
« Reply #5 on: April 21, 2011, 06:24:48 PM »
My rule is if it does not have a COA then take nothing said about it as truth, and at least distill once. But I think that would be better than the hardware stuff, for sure.

Methyl Man

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Re: new additive in OTC acetone, others
« Reply #6 on: April 21, 2011, 08:03:12 PM »
If making products intended for eventual consumption (but who would do such a thing) then it must be purified properly. You might have made a great pure salt of some compound, then once you wash it with acetone you have introduced all sorts of shit simply because it was not purified properly. This should not be acceptable to anyone.

I agree, and it certainly seems reasonable, but just to show how crazy this world and this chemistry stuff can be, I want to tell you something. Back 10 years ago or so, when "I" (stepping into the fictional internet character Methyl Man here) was doing this before, I was not so mindful of solvent purity and used regular hardware acetone for my recrystallizations. I'm almost certain the brand was Klean-Strip (a brand I kinda consider polluted these days), but if not, it was Ass Hardware's.

A few months down the road, after quite a bit of product had been fictionally "circulated", I was told by my ex-girlfriend (a scientist with a master's working on her PhD... sigh) that she had just been told by a scientist colleague of hers who had run my stuff up on GC/MS that its purity was amazing. She said that he told her it had a perfect spike where it should have at MDMA, and no other tics at any other place. I was stunned, and then a few minutes later, very proud. I would have expected to see at least a blip at around the ketone's range, or safrole's, or like you say maybe a hint of a solvent impurity or two. Did NOT want to see anything about Hg or Al, obviously!

I don't argue that because of that experience, I shouldn't have the ethic you expressed. I do. (more distillation... sigh) But it shows that things can still come out very clean using hardware store solvents.
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Shake

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Re: new additive in OTC acetone, others
« Reply #7 on: April 21, 2011, 09:45:05 PM »
i say use otc, yes there may be lower yields but just run it more times to compensate!

I have a question regarding this. recently when working with mdma freebase in toluene freshly pulled from my post al hg sludge, i ran out of dh20 for the washes.. i did the washes with tap water instead.. also i used tap water in my 02 wacker which is right next to me stirring

any direct experience with el tappo water ruining anything?

i know with lsd it destroys it but mdma seems like you get yields even when its run dirty
« Last Edit: April 21, 2011, 09:48:17 PM by Shake »

pyramid

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Re: new additive in OTC acetone, others
« Reply #8 on: April 21, 2011, 09:48:29 PM »
This is about acetone, run what more times?
Washing toluene with tap water?? What you talking about?
I see you have a 'good enough attitude', no problem but at least I know not to eat your stuff

Shake

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Re: new additive in OTC acetone, others
« Reply #9 on: April 21, 2011, 09:53:14 PM »
the topic is about additives/contaminants right?

did you read methylmans last post??

im asking (without starting a whole thread) how does using tap water effect things as opposed to dh20

Using otc solvents as he describes affects yields but obviously not the purity based on what methylman said.

how does what im talking about not make sense?
« Last Edit: April 21, 2011, 09:57:30 PM by Shake »

pyramid

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Re: new additive in OTC acetone, others
« Reply #10 on: April 21, 2011, 09:56:40 PM »
This is about the additives in acetone, and there is no need to get all uppity about this. I do not appreciate people who think about things with a good enough perspective, especially when producing products for consumption.
Also, please do not call me a dick or a fag ( yes I saw that you called me that in another thread then removed it)
I think you may want to read more carefully what Methyl Man wrote, it was regarding acetone.

Using tap water should be no problem, by the way
« Last Edit: April 21, 2011, 10:10:18 PM by pyramid »

Shake

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Re: new additive in OTC acetone, others
« Reply #11 on: April 21, 2011, 10:20:24 PM »
ok well regarding the acetone from the store, i dont know what was in it but it would not leave my crystals, it stayed in them and puffed them up, as opposed to MEK which was really good at cleaning the crystals..

at the end of the day pyramid its only .1g dose its not like you are having a big bowl of the stuff so a few impuritys are not going to harm anything, imagine how much mdma youd have to take before the impurities from the acetone got to you?

psychexplorer

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Re: new additive in OTC acetone, others
« Reply #12 on: April 21, 2011, 10:28:54 PM »
i say use otc, yes there may be lower yields but just run it more times to compensate!

I have a question regarding this. recently when working with mdma freebase in toluene freshly pulled from my post al hg sludge, i ran out of dh20 for the washes.. i did the washes with tap water instead.. also i used tap water in my 02 wacker which is right next to me stirring

any direct experience with el tappo water ruining anything?

i know with lsd it destroys it but mdma seems like you get yields even when its run dirty

No, blanket OTC is not okay. The attitude of throwing more reactant at a problem to get more product reeks of cookery and is a disservice to anyone who takes the product. If you care about the science behind the product, it also lowers your stature as someone genuinely interested in the chemistry as well as the product.

I have to take exception with simply running it more times and wasting more reactants. Aside from my general dislike of waste, why would you spend the time on a second batch or a larger batch if you could instead take the time to do it right?

As for tap water, it should always be considered unacceptable. Sometimes it hurts, other times not so much. The dissolved Ca and Mg salts are the least of your worries. Tap water has a variable pH and is full of unknown concentrations of unknown nasties, particularly chlorine and chlorinated compounds.

For reference, here is a photo of a swimming pool recently filled with tap water containing the nasty chloramine:

h**p://upload.wikimedia.org/wikipedia/en/9/9c/Rkinch_chloramine_pool.jpg

Do you want that in your lab?

dH2O is so cheap and readily accessible that it doesn't make sense to waste the time and energy thinking about when it might be okay to substitute unknown tap water with maybe a dollars worth of dH2O, or to worry about whether it is contaminating product or impacting yield. Most tap water should not be considered fit for human consumption, so why use it in preparative work?

Using dH2O guarantees that you are working only with H2O.

As the saying goes, garbage in, garbage out (GIGO). Attention to detail is a good habit to build.
« Last Edit: April 21, 2011, 10:30:45 PM by psychexplorer »

Wizard X

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Re: new additive in OTC acetone, others
« Reply #13 on: April 22, 2011, 12:20:49 AM »
Do you want that in your lab?

dH2O is so cheap and readily accessible that it doesn't make sense to waste the time and energy thinking about when it might be okay to substitute unknown tap water with maybe a dollars worth of dH2O, or to worry about whether it is contaminating product or impacting yield. Most tap water should not be considered fit for human consumption, so why use it in preparative work?

Using dH2O guarantees that you are working only with H2O.

As the saying goes, garbage in, garbage out (GIGO). Attention to detail is a good habit to build.

Excellent advice psychexplorer!!!
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

Methyl Man

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Re: new additive in OTC acetone, others
« Reply #14 on: April 22, 2011, 12:30:34 AM »
As it turns out, that biodiesel place's solvents, all of them, have a COA that is posted right there (if you click on the item in question) so it looks like they have stuff that is at least lab grade and has a COA to back up its 99.5%. The reason this is cool of course is that purchases from a biodiesel supply place are all pretty chill since everyone is using it to make biodiesel. Could be different two years from now, but right now that looks like the good place to get quite a few things.
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psychexplorer

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Re: new additive in OTC acetone, others
« Reply #15 on: April 22, 2011, 12:52:44 AM »
I feel a bit uncomfortable talking about a specific, easy-to-find source's products in an open thread. Even though this isn't an open board, that vendor can be found with about 10 seconds of Google work, so it's just like posting a hyperlink.

There is a lot of quality acetone out there....no need to stampede one specific vendor which appears to be rather soft and ripe for abuse.

Methyl Man

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Re: new additive in OTC acetone, others
« Reply #16 on: April 22, 2011, 01:01:14 AM »
Sorry, that's probably true. Should I edit my posts a bit?
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psychexplorer

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Re: new additive in OTC acetone, others
« Reply #17 on: April 22, 2011, 01:19:54 AM »
Ultimately it's Vesp's call, but I don't see much to be gained from hinting at a specific place's 99.5% acetone. We can speak in generalities about lots of 99.5% acetone sold as pure acetone (as opposed to a product sold as generic solvent which happens to contain acetone).

In general, though, you're likely to find a better quality of acetone from a single ingredient product, sold as the chemical itself (not as a purpose), with a COA to back it up, as compared to whatever is on the shelf at the hardware store. That isn't to say that everything at the hardware store is junk - you'd be surprised at some of the purities - but I would trust the analyzed chemical over the OTC purposed formulation.

Shake

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Re: new additive in OTC acetone, others
« Reply #18 on: April 22, 2011, 08:13:01 PM »
psychexplorer seriously you need to lighten up. i dont run my al hg amalgums in broad daylight, more likely at night and at night mid way through the washes i ran out of dh20, all the stores were shut and i had 1 or 2 washes to go so i used tap. the last wacker i used 14mills of tap water, woopey.

i know its cheap, here it is 5 dollars for a 4L bottle so it aint that cheap.

as for attacking an acetone vendor seriously these boards have approximately 20 people from all over the world online a day i think the vendors reputation wont be too tarnished.  ::)

And finally
Quote
why would you spend the time on a second batch or a larger batch if you could instead take the time to do it right?

because, genius, these drugs are category 1. doing it right by taking a few extra hours to distill your toluene or whatever as opposed to just using it straight, serious man you are living in fantasy land where you think you have all the time and freedom to make your stuff ever so clean and perfect when it does not make alot of difference. and if we were to go and purchase all lab grade chems how much more does it cost.. ALOT more. you need a business name to get lab grade chems where i am from.

Most of us have full time jobs and have this as a side hobby, make do, get the yields you can get and if you want more run it again or clean up your lab technique

« Last Edit: April 22, 2011, 08:22:55 PM by Shake »

psychexplorer

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Re: new additive in OTC acetone, others
« Reply #19 on: April 23, 2011, 03:34:16 AM »
One of the reasons we're here is to learn from each other. If we didn't, we'd be plagued by bad habits, poor yields, and injury.

The points raised here are important, at least if you want to become a better chemist rather than just a cook.


psychexplorer seriously you need to lighten up. i dont run my al hg amalgums in broad daylight, more likely at night and at night mid way through the washes i ran out of dh20, all the stores were shut and i had 1 or 2 washes to go so i used tap. the last wacker i used 14mills of tap water, woopey.

i know its cheap, here it is 5 dollars for a 4L bottle so it aint that cheap.

If you are suprised by running out of dH2O midway through a procedure, then what other unpleasant surprises might be in store? Lack of clean glassware? Reagent shortage? Equipment problems? A good chemist will make sure everything is in order before beginning a series of steps. Running out of dH2O is almost as bad as not paying the power bill and watching your stirplate shut down halfway through.

Assuming the ridiculous price of $5/4L is in fact the best you can do, don't you have a distillation apparatus? dH2O can be prepared by distilling H2O.

One of the first points taught in any into lab course is that when a chemist says water, he means dH2O.

Strike felt it important enough to write this in TSII:

Quote from: Strike, TSII
Since we're on the subject of lean water, this is as good a time as any to discuss what kind of water is used in all this chemistry. By clean water Strike means distilled water (dH2O). All reactions are to use distilled water (dH2O) only. All solutions and dilutions are to be made with dH2O as well. Distilled water sells for about $1 a gallon down at the supermaket. Tap water is an absolute no-no in chemistry except for cleaning the glassware.

Every introductory textbook will echo this same point. Since people often ignore the textbooks, maybe the book on MDMA might mean a bit more.

Take another look at that pool full of tap water.

If you think "clean enough" means "clean" when it comes to water, then I'd hate to see your definition of "dry enough" when it comes to your ether in a Grignard. Attention to detail matters. Sloppy is no good. We need our water distilled and our ether dry.


as for attacking an acetone vendor seriously these boards have approximately 20 people from all over the world online a day i think the vendors reputation wont be too tarnished.  ::)

I never attacked any vendor. What I took exception with was a clear reference to a specific source. The source rule is one of necessity. We don't post sources in the open because that ends up burning good sources, whether it be from a stampede of spoon-fed kidiots, or (on an open board) the vendor finding the link and having to tighten up the order policy because he is no longer naive nor could he claim ignorance.


And finally
Quote
why would you spend the time on a second batch or a larger batch if you could instead take the time to do it right?

because, genius, these drugs are category 1. doing it right by taking a few extra hours to distill your toluene or whatever as opposed to just using it straight, serious man you are living in fantasy land where you think you have all the time and freedom to make your stuff ever so clean and perfect when it does not make alot of difference. and if we were to go and purchase all lab grade chems how much more does it cost.. ALOT more. you need a business name to get lab grade chems where i am from.

Possession of toluene isn't illegal. Distilling toluene isn't illegal. This goes back to the lack of foresight to have enough dH2O on hand. Solvent evaluation and cleanup should be done well in advance, as there is plenty of time for it. Why leave dirty toluene sitting around when you can clean it up when you get it and keep it for later? If you don't assess and purify your OTC solvents well in advance, what will you do if you're short of time and dealing with a mixture which is harder than usual to purify?

If you have to fit this all in a very short few hour window, that makes me wonder if you're cooking in a motel room, a camper, an apartment, a place with roommates, a familial residence, or something like that.

There's a reason why they round up thousands (maybe tens of thousands) of SnB'ers for every guy like Pickard. When you have the proper mindset, the proper location, and follow the rules, then you have the time to do it right.

If a few hours is the difference between a bust and not, then you shouldn't be doing it in the first place. If you can't take as much time as you need, but not more, then your security needs improvement, or it shouldn't be run at all.

What it is means very little when it's behind the right veil of privacy.

Now suppose that toluene is a reactant, not a solvent. Would you nitrate dirty toluene in a makeshift lab on a very tight schedule? Now suppose during that nitration you ran out of ice because you forgot to buy enough beforehand. See where I'm going with this?

Sassy is simply unavailable where I live. That has been much more of a hinderance than the lack of common ACS grade reagents sold to anyone who is buying. Not having the standard stuff from a lab supply company sucks, but with good technique, you can prepare much of it yourself. The synthesis of safrole from only readily available chems is much more difficult than the synthesis of MDMA from readily available safrole sources. That $1.25/L dH2O isn't looking so bad after all.


I think your attitude towards quality says it all:

it does not make alot of difference

Which is why I only eat my own. The thought of a cook getting sloppy near the end and impatiently rushing to completion when he should be washing out the Hg is not pleasant at all.