ETOH and AL/hg

[blaztoff]

SWIM was wondering if some denatured he found would work for the Al/hg. The bottle says contains 96% denatured and 4% methanol. Denatured is basically Ethanol mixed with Methanol or where Swim lives Acetone MEK and a couple of other things. Shouldnt this be labeled ethanol with methanol or is there any other substance in this mix to make it labeled as denatured. SWIM was wondering if this would cause a problem for the Al/HG MeNO2. Swim was going to run this with a mix of 99% IPA.

[PrimoPyro]

Any ketones ppresent may condense with the methylamine and be reduced to amines.

Hey, it finally worked!  

                                                 PrimoPyro
Vivent Longtemps la Ruche!

[blaztoff]

Swim just found out that it also contains 1% MEK. I think somewhere in a previous thread Rhod stated that the MEK would have to be removed first or it could riun the formation or sonething like that trying to find the post. But not really sure. Will MEK do anything to the rxn? Would this have to be distilled first?

[PrimoPyro]

MEK's bp is very close to that of ethanol. Have fun distilling that out. Yes I think it needs to be removed. As I've stated repeatedly to bees, it is my preference that ketones be removed by simple bisulfite crystallization with sodium bisulfite, or if you have it, sodium iodide. UTFSE here for exact details on these procedures for interesting ketones, and look at Rhodium's page as well.

It's either that or fractionally distilling the mixture with a long ass condenser for decent fraction seperation.

Or find another source.  

                                                   PrimoPyro
Vivent Longtemps la Ruche!

[blaztoff]

This was to be used in a Al/Hg MeNO2. SWIM has no avenue for MeOH on the weekends. The only place that sells it around SWIMS area is closed and SWIM has never run the AL/HG with only IPA just MIxtures of IPA and MeOH. SWIM was wondering about distilling some vodka for some pure ETOH and use a 50/50 mix IPA but dont know how if that will work. Swim has used Diffenrent solvent combos but always with MEoH as one of the solvents.
Damn fraction of a BP apart. How the hell does it work for OS variation if the MEK will fuck up this but wont fuck up it with MeAM?

[PrimoPyro]

Doesn't Osmium have a writeup with methylamine that uses only IPA? I seem to recall this being one of the first procedures I ever read as a Newbee.

                                                   PrimoPyro
Vivent Longtemps la Ruche!

[Chromic]

You're thinking of Bright Star's writeup which is based on Osmium's method.

[PrimoPyro]

Yes that is what I meant, you nitpicker.  
Vivent Longtemps la Ruche!

[blaztoff]

But how will a Al/HG MeNO2 via MM work with straight 99% IPA solvent instead of MeOH. Or what would be a good mix if no MeOH available.

[Osmium]

Doesn't matter what alcohol you use, they will all work. You can even use wet ether for the Al/Hg.
I'm not fat just horizontally disproportionate.

[blaztoff]

One thing SWIM noticed when running straight IPA as the solvent that the aluminium does not really get broken down that well. Swim in the past added a touch of NOAH to mixes that contained a lot of IPA. But this is first time straight IPA and the aluminium at the end of the rxn was not all broken down and after basifing was still little bits of aluminium that turned brown and settled on top. STunk sort of wierd not quite like a MeoH run at all. Also the rxn never really refluxed at all. It did get hot a little but rather a calm rxn. The color of the mix was perfect exactlly like the Meoh rxns but  there was a bit of al that refuses to break down and its got a brownish tinge to the solvent.
Any ideas to the different apperance of IPA Rxn to the MeoH. Swim takes it the rxn does not take anything from the solvent . Will denatured work if it has the MEK in it?

[terbium]

Any ideas to the different apperance of IPA Rxn to the MeoH.
Methanol is a lot stronger proton donor than IPA so its side reaction with the amalgamated aluminum would proceed more rapidly. The main reaction(s), the reduction of the imine (and nitromethane), also requires a proton donor but people's experience seems to be that IPA is sufficient.

[blaztoff]

Thank you for confirming that. Swim suspected that the pure IPA reaction would proceed a lot slower. That would mean the addition of ketone mix would not be the same as Meoh correct. The Al would break it down slower so youre addition would be slower. Swim noticed that when IPA mix the reaction would proceed a lot smoother no real volcano.
How would this effect yield. What guidelines would you go for the addition. Would flashing work better even though no Meam made for the rxn?

[baalchemist]

When Baal has used just IPA-99% without MeOH, a longer time waiting on foil amalgamation to kick in was spent. When it was nice and bubbly, the addition was started. Under a Freidrichs condenser, the addition rate was actually same/faster than that with MeOH. Keeping that post-addition reflux at about a medium rate is important in breaking down that foil,(thats what makes the reaction progress)leftover foil usually indicates an incomplete reaction w/ the Al/Hg/Nitro route. In my 'Kickin up the yield" posts, Baal switched to the IPA/MeOH mix in order to give the reaction some new parameters that would help keep the exothermic expansion rate down, while allowing it to progress at the faster reaction rate accompanied with MeOH based reactions. Using flashing would be pointless unless youre reducing large-scale quantities. 
GODISNOWHERE

[blaztoff]

Thanks Baal. Went along with what I had observed. I dont know if adding NoAH hurts the reaction but Swim noticed that after waiting for the first champagne bubbles that When Swim added a 25ml 25% Noah it really got the amalgation going. Instant bubbling and aluminuim starts really breaking down and the whole apperance turns cloudy.
What swim became worried about was the rate of addition of the ketone mix versus the breakdown of aluminuim. All posts and from trial and error state that the faster the addition better yield. But with the 99% IPA the rxn never realy takes off. So it would appear that instead of addittion in 15-30 minutes it might take 1 hour or more with intervals between addition to make sure it keeps pace with the brweakdown of Al.
After the addition the mix would look like it wa supposed-nice bluish color but after lettimg it cool wait layers start to seperate a tiny amonut of base added instant fizzing steam whoah. Swim has experienced this before so backs off and now two layers form. seperate the top layer and proceed to basify the bottom layer. Add base and swim be damn A fucking shit load of heat steam gass . Good thing it was slowly.  Now a handfull of aluminium pieces float around and after alowing to cool add some tol to extract. now tol becomes a brownish color unlike the yellow you recieve from unreacted ketone. Still have lots of al around. Probally aroungd 1/10 original volume. More aquesous layer forming from sludge so swim says fuck it throws all together and seprates the aqueaous layer. Later will try to vap it down see if any oil is there.
Baal with the IPA/Meoh mix did you grind youre foil up or did you leave it in squares. Seams unreacted Al looks like about 1/4 original balls. Would think that the squares mith help it sped up easier for amalgation but slow enough with the IPA to not run out.

[Dr_Sister]

i think the reason IPA takes longer to amalgamate is the reduced solubility of salts that results as the size of the alcohol increases, apply some heat heat during amalgamation. or if you want simply amalgamate in H2O, decant, add your IPA and rock n roll dude.
7.10.01