Shake & Bake Recipe (TEXT ONLY)

Osmosis Vanderwaal

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This is 500% better than the first one. Could this work? It has a little background information and some actual measurements. Unfortunately many of them are wrong.I wonder how he screwed the simplest part up so badly? It doesn't exactly instill confidence in his methodology.
MgSO⁴ (anhydrous) mol.wt=120.x g
MgSO⁴(heptahydrate,)mol.wt=246.x g
Ie magnesium sulfate holds just over its own weigh in water, which of course weighs 1g/1ml.
1/4 of a 946ml (quart) mason jar is 236ml.
236ml of MgSO⁴ weighs 654.36 grams!
The solubility of water in hexane is 0.01%, as such 1 gram of magnesium sulfate would be more than enough to ensure it is anhydrous and stays that way.
Ok, so he added over a lb too much drying agent to the hexane. The solubility of water in ethyl ether is 1.5% @20c, ie 1.5ml/100ml. A quart of ethyl ether can hold 15ml of water. 30g of MgSO⁴ would be a large excess. He added a lb too much drying agent.
The thing about magnesium sulfate as a drying agent is, it doesn't just hold water, it'll absorb your solvent too, so adding 300 times too much is going to cost you an assload of money. All around he screwed this part up. Did you know if you pull it out of the oven at 15 minutes and shake it and again at 30 minutes, it won't clump up. Trying to smash it with a hammer is a stupid idea. It's literally as hard as concrete if you don't mix it up.
The ratio of ammonium nitrate to ammonium sulfate is 80/132 (this is the mol.wt. Of each. Each molecule has an amino functional group and another moiety. The ammonia is the same in both, so the weight difference is the difference a nitrate and a sulfate.the ratio to get the same number of ammonia sustituents is 1/1.6, 160% the weight of the nitrate to get the same amount of ammonia from the sulfate. 60 grams of ammonium nitrate or 96 grams of ammonium sulphate. Hes using twice as much ammonia with the sulfate,, which 8 feel is the more likely correct number, 120g of nitrate or192 grams of sulfate. I bet the amount of lye to ammonium is wrong too. Yea. 90 grams of lye is 3 moles I think, which corresponds to 80x3 240 grams of ammoniumnitratevir 132x3, 396g of sulfate. This guy doesn't know how to balance an equation. If someone scrutinized it heavily, the corrections would be longer than the method. Your big brother isn't going to let you find a good and complete method on dns. He'll make you work your ass off to fail, and laugh at you while slapping the cuffs on your wrists.
 

zaners

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You can't use Coleman's fuel?
 
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Osmosis Vanderwaal

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Because it might be blue. It's not a problem. Sometimes nitromethane is blue. Sometimes it's red. They dye it. You work up the Epsom salt by drying and crushing it, add it until it no longer clumps together, filtered or decant the magnesium sulfate out and use the stuff as soon as possible.
 

Osmosis Vanderwaal

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Coleman fuel IS NOT a replacement for diethyl ether or hexane. Not at all. Coleman fuel is a crude mixture of hydrocarbons and diethyl ether and hexane are far more refined and not similar in properties
 

SoldadoDeDrogas

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Coleman's fuel or naphtha can be used on its own and it will work. In fact, diethyl ether, hexane or basically any NPS hydrocarbon will work on their own. Some will have different effects on this reaction than others. It is recommend to use a blend of these for the best results. Check out the pdf file that flatline posted, he goes on to explain the "how and why" of this whole process very well. For best results, this entire reaction needs to be as dry as possible.
 

Osmosis Vanderwaal

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Ammonium sulfate ammonium chloride any acid salt of ammonia can be made to work. They are simply an ammonia attached to an acid component. They are Lewis acids. Simply adding a base to them will deprotonate them back to ammonia and sulfate nitrate or chloride ions. That is all we are doing in this particular reaction. If you know a farmer that has a tank of anhydrous ammonia, that would be ideal but it's dangerous and stealing it is even more dangerous. If you can get a tank of ammonia gas, get that but you can't. If you find any cold packs with ammonium nitrate in them buy every one. They haven't made them in 10 years. They use urea or calcium ammonium nitrate now just for this reason
 

SoldadoDeDrogas

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We can't get 'calcium ammonium nitrate' to work though, eh? Hmm.. is there anything we can do to CAN to get a workable salt?
I strolled into a CVS one day and just happened to find a box of AN instant cold packs, I took one pack out of the box to do a test run with. That was for my successful SNB run. I haven't found those cold packs since - they are all urea or CAN as you say. Perhaps one can go to the hospital or a health clinic and ask for cold packs and see what you get as a last resort.

I am kind of confused as to why liquid ammonia can't be used on its own with freebase suzy and Li, do you know why it has to be evolved into gas from a salt and condensed in this reaction? Thank you.
 
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Osmosis Vanderwaal

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Ammonia just is a gas under atmospheric pressure and temperatures. Liquid Ammonia is highly compressed and extremely cold you need 7.5 bar of pressure at 20°C or -30°C at atmospheric pressure to liquefy it. Both can be done but neither is easy. That's 104psi or dry ice. You could squeak by with calcium chloride/ice and a little pressure, maybe 15-30 psi. I'm 100% sure ammonium sulfate or chloride and lye will make ammonia. Try it, It makes ammonia for me
 

SoldadoDeDrogas

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Thank you for the information, my friend. You always seem to have some good hints for me.
May I ask what do you use as your source for ammonium sulfate or chloride?
During protonation, ammonia gas is evolved as well as the corresponding salt - nitrate into nitrogen, chloride into chlorine etc. Creating the inert atmosphere inside the RV such as with nitrogen is a good part of safety for this particular process I am sure. How can we figure out which ammonium salts will safely dissolve the lithium, - safely - , without creating a side reaction.. or bomb.. or which ones should be avoided?

Another question, if I may, how do you know what temperature/pressure is needed to evaporate or condense, for ammonia for example, or anything else. How do you figure that out?

As you can see, this is part of where my chemistry is lacking. I don't know how to figure some things out for myself. I missed out on the formal training. I'm not looking for easy answers, but if you could, show me how to fish, so to speak. Thank you again.
 

hirozaru

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I tested my Ammonium doing a water solvability test. I found a table with the amount that is dissolvable.
Ammonium Nitrate can dissolve more than twice Ammonium Sulfate or Chloride in water. So that was my hint to test my cold packs, making sure my ingredients are OK.

you can also put a little bit of your AN with NaOH only, those two things in a small petri dish, or any container, they should react together.
 

Osmosis Vanderwaal

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You don't want water in your Birch reaction anyway. 10 ml if you must but lithium burns when it touches water. Water solubility isn't relevant
 
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