Shake & Bake Recipe (TEXT ONLY)

Douda

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Recommended Materials/Tools:

• 1 box 24-hour Sudafed (2.4g Psuedoeffedrine)
• 90 grams Lye (Sodium Hydroxide –NaOH)
• 60 grams Ammonium Nitrate Crystals (NH4NO3– AN) or 180 grams Ammonium Sulphate.
• About 100ml of Diethyl Ether (starter fluid)
• About 200ml of Hexane (CRC QD Electronics Cleaner)
• 1 "AA" Energizer Advanced Lithium battery
• 2 Pairs of Plyers
• 1 Medicine syringe/ eye dropper
• 1 Bag of Ice
• Pail/Container
• Box of Ziploc Baggies
• 1 500ml SodaStream Bottle
• 1 Roll of Gorilla Duct Tape
• Can of Acetone
• Blowdryer
• Small Pipe Cutter for Batteries
• 4 Coffee Filters
• Paper towels
• A Mason Jar
• A Pill Crusher\Coffee grinder.
• Small glass jar with lid
•Plastic Funnel
• An Evaporation Plate
• Some Dry Epsom
• A Bottle of isopropyl alcohol

If you want to water titrate you will need:
• Muriatic Acid mixed... [4 Parts Water : 1 Part muriatic acid] after being purchased
• About 4 litres of Distilled Water.

If you would like to gas you will need:
•Some table salt (NaCl)
• A bottle of Sulfuric acid (H2SO4)


Notes about ingredients:

• PSE - Pseudoephedrine HCl should be the only active ingredient whenever possible. Also,
the red 30mg tablets are desirable, because they have less gak to remove.

•NH4NO3 - Obtained from instant cold packs. Beware of urea containing packs, they will not
work. If unsure what you have, open the box. Ingredients are printed on each pack. Generics
tend to work the best. Get them from pharmacies or sport/sporting injury areas of big
stores.

• Lithium - Obtained from lithium batteries. Each AA battery contains approximately .94g of Li
metal. Reacts negatively with hydrogen. Sparks on contact with other metals. Can ignite
spontaneously if not properly handled. Should be kept out of open air and away from any
moisture.

• H2SO4 - Obtained from a big chain home improvement store. Marketed as drain cleaner.
The bottle will say "concentrated sulfuric acid" somewhere on it, and should be inside a
sealed bag on the shelf. If you can't find it in the cleaning section, check the plumbing
section.

• Toluene - Flammable. Harmful vapors. Skin and eye irritant. Obtained from a big chain home improvement store. It will be in the paint thinner section.

• NaOH or lye, caustic soda.
Use solid only. Highly corrosive.
Obtained at a big chain home improvement store. Marketed as drain cleaner. also sold in some supermarkets as caustic soda drain cleaner says on the container “perfect for making soap”

•Acetone - Flammable. Obtained from a big chain home improvement store. It will be in the
paint thinner section.

• Methanol or denatured alcohol - flammable. Obtained from a big chain home improvement store. It will be in the paint thinner section.

• MgSO4 - Regular unscented Epsom salt. Obtained from pharmacies or any big store. It will be in the health and beauty section or the pharmacy area.


Notes about gases produced:

•NaOH and NH4NO3 react to produce ammonia (NH3) gas and H2O. Ammonia gas is
corrosive and damaging to soft tissues. The H2O produced is nominal and does not pose a
safety threat.
• NaCl and H2SO4 react to produce hydrogen chloride (HCl) gas. HCl bonds with water in the
atmosphere, producing smoke-like vapors of hydrochloric acid which is corrosive and an
irritant to soft tissues.

Pre-RXN:

Place your dH2O into the refrigerator.

Preparing anhydrous MgSO4 (dry Epsom):
Spoiler

MgSO4 is a desiccant, meaning it absorbs water. It is used to make solvents anhydrous (without water) as well as gases.

Heat your oven to 400F (204C).
• Line your baking dish with aluminum foil. It gets sticky for a while.
• Pour the whole bag of Epsom salt into the dish. Spread evenly and put in oven.
• Bake for approximately 1.5-2 hours, stirring occasionally, until you are left with a very hard, very dry, chalky, white solid.
• Allow to cool, place in a Ziploc bag, place a towel or something over the bag, and crush the MgSO4 with a hammer. Not too large, but not powder.
• Transfer to a new bag without holes and seal.


Preparing anhydrous Diethyl Ether:

• Fill a mason jar 1/4 full with anhydrous MgSO4
• Fill the rest of the way with diethyl ether
• Put on the lid and place in freezer.

Preparing anhydrous hexane:

• Fill a mason jar 1/4 full with anhydrous MgSO4
• Fill the rest of the way with hexane.
• Put on the lid and place in freezer.

Preparing anhydrous acetone:
Spoiler

• Fill a mason jar 1/4 full with anhydrous MgSO4
• Fill the rest of the way with acetone.
• Put on the lid and place in freezer.

Preparing anhydrous methanol:
• Place 5g of anhydrous MgSO4 in a baby food jar.
• Fill the rest of the way with methanol.
• Put on the lid and set aside in a warm place.
(Once the solvent has been dried using MgSO4, it will naturally try to reabsorb the lost moisture by taking it from the atmosphere. Acetone does this rather quickly. Be sure to keep dry solvents in airtight containers.)


Preparing the HCl gas generator:(only if gassing.)

• Rinse and dry the soda bottle and lid.
• Using a drill or utility knife, make a hole in the center of the lid large enough that the
aquarium tubing will fit snugly.
•Cut off around 18in (45cm) of the tubing and attach it to the lid through the hole you made.
(It should be very snug or HCl gas will leak out, and that stuff is pretty nasty.)
• Add 64g NaCl to the bottle and put the lid on.
(I have heard of :bee using damprid instead of salt but I cannot confirm for myself… Water titrating is my thing)
• Set aside for later

RXN Procedure:


1. Heat the Bottom of the Soda Stream bottle with a blowdryer until the glue holding the bottom part to the bottle heats up and you are able to twist the bottom part off of the bottle.

2. Gorilla Tape The Bottom of the Bottle, an about an inch up the side of the bottle, and the seams going down the bottle.

3. Add about 100 ml of Ether and around 200 ml of hexane to a baggie.

4. Water Wash this Fuel Mix twice, and the transfer the fuel to the Soda Stream Bottle.

5. Fill the Pail/Container with Ice about 1/2 way and add a about 100mm of water.
• The colder the better. Some bees use an ice shaver to shave the ice into snow like powder.
• Now put the crushed ice into a pitcher about 3/4 full... then add a couple of inches of water to make a ice bath.

6. Put the SS Bottle with the Fuel into the ice-water bath, and leave it to allow fuel to get cold.
(A good rule of thumb to follow is to put SS Bottle with Fuel in the Freezer about an hour or so before performing the rxn.)

7. When fuel is nice an cold, remove bottle from ice water, but keep it accessible.

8. Crush and Powder the PSE Pills and put the powder in a container or baggie for later.

9. Remove guts from battery and leave them submerged in some fuel.

10. Add 60 grams Ammonium Nitrate or 180 grams of Ammonium Sulphate to the SS Bottle.

11. Add 90 grams naoh (lye) to the SS Bottle.

12. Tear the Li Strip in "stamp" size flat pieces or smaller and add them to Bottle.

13. Add about 5ml distilled water to SS Bottle, quickly screw the cap on, and swirl the bottle to "re-coat" the Li with fuel.
• Cold = Ammonia Gas Condenses to Ammonia Liquid at lower pressures. AN + LYE still react even in the cold temp because of the addition of water.
Therefore, easy to create Ammonia Liquid and start the bronzing quickly.
(This is not needed but is recommended)

14. While the reaction is "Rolling" violently for the first 5-10 minutes, let the pressure in the bottle build until you cannot depress with the "thumb test", but perform small vents as needed.
(Thumb tests are simple.
A: Before starting find the easiest spot to push in with both thumbs remember this spot for later.
B: this is where we will test pressure by pushing with both thumbs.
C: If you are unable to push with both thumbs it's time to release pressure)

15. Depending on the strength of the reaction... you could see initial lithium bronzing within the first 2-3 minutes.

16. When the reaction Starts to slow, let pressure build to your "Thumb Pressure Test" capacity, and then submerge the bottle in the Ice Water Bath and Leave it for about 10-15 minutes or so.
• Keep an eye of the pressure to be safe.
•If your ice bath is not cold enough to quickly slow the reaction, be sure to vent bottle as needed to prevent bottle failure.

17. After 15 minutes, you will probably have at least 1/2 of the Lithium “Bronzed” (Dark Bronze Flakes at this point), and the bottle will be depressurized considerably, and little to no reaction will be happening.

18. Shake the bottle
• If you AN/NAOH Reactants have become big hard clumps at the bottom... Shake the bottle until you break them up.
• Worst comes to worst the reactants will "de-clump" later when we heat and shake...

19. Begin heating the bottle with blowdryer and shaking it, to re-initiate reaction.

20. Perform small vents as needed while raising temperature to get the reaction rolling again.
(As the fuel gets hot, you should see the Li Bronze flakes convert to Gold BB's and/or a Gold puddle.)

21. Once Fuel is Hot and reaction is rolling strong again... Build pressure to limit and submerge into Ice bath one more time for another 10-15 minutes.
(After removing from Ice Bath again, You should have 80%-100% Li Dissolved.)

22. Remove Bottle Cap, add PSE, and Add some recharge Reactants if you like.
• I always add about half of the original amount of AN and NAOH with the PSE.

23. Shake the bottle and you should have black fuel instantly.
(you may know this as “chocolate milk” from my previous posts)

24. Begin heating the Fuel and shaking the bottle.
(At this point it's best to keep the fuel as hot as possible and maintain pressure as high as possible.)

25. Continue Heating and Shaking (small vents as needed) until the fuel goes completely clear within about 15-20 seconds after shaking it, or until you have absolutely no Lithium left at all (Meaning that your lithium losses were too great and you did not have enough to reduce all of the suzy)

• DO NOT get in a hurry. Sometimes this reduction phase can take upto 40 minutes.
(As the saying goes “Great things come to those who wait.”)

Filtering:
( WARNING: This is the most dangerous step in the entire process. You will be exposing molten Li to open air for an extended period of time. Be quick and efficient. Puddle Lithium will ignite if left in open air. Do your best to keep as much of it in the bottle as you can. Some will inevitably make it through. Don't worry. As long as you keep it wet with the solution it won't ignite.)
(This is just a quick, rough filter to separate the solution from the solid ingredients and reduce the risk of fire. A more thorough filter will be performed once the reaction vessel is secured.)

1.. Take a ziploc bag and seal it shut with air trapped inside.

2. Now press firmly with both hands on the front and back of the bag and listen for leaks.

3. Open the bag and line your pitcher with it.
Check another bag for leaks and add a small amount of hexane to it.
(Your filtered crap will go in this bag.)

4. VERY slowly vent all of the pressure from the SS bottle.

5. Using a funnel, filter the solution into the bag inside the pitcher.

6. As soon as all the solution has been retrieved, cap the bottle and place in the freezer.
• This will stop the RXN
(The lid can be used as a makeshift screen to help trap unwanted Lithium and such from getting to the filter. This filter will contain molten Lithium. Be careful! Liquid lithium tends to be more volatile than strips!)

• As soon as used filters are not needed, put them in the bag with the small amount of Hexane.
(Storing/coating the lithium in hexane will keep it from igniting.)

•Make sure to put all the filter papers and anything with stuff on it from inside the bottle into the bag with the hexane and seal it.

•Put it in the freezer as well.


Filtering (after securing lithium).

1. Stuff 2 cotton balls into the neck of your funnel.

2. Place 2 filters into the funnel above the cotton and add 64g of MgSO4.

3. Place 2 more filters on top of the MgSO4.

4. Line your pitcher with another bag and filter the solution into it using the prepared funnel.

5. Repeat 1,2,and 3.

6. Check the pH and be sure it is 13+. If it is below 12.4, base it again by adding NaOH.
• Once the pH is at 13+ re-filter.
• Seal the bag. Discard filter crap.
(It is VERY important that the solution be as basic as possible when the water is added. If the pH is too low (high), the meth freebase will slide back into the water layer and you will throw it out without ever knowing it.)

The solution should be crystal clear, like water. If it is cloudy or you see crud floating in it,
filter it until you don't.


Water washing the solution:
dH2O (distilled water) is used to wash the solution of sulfur impurities.
•These impurities are what give shooters that massive head rush.
(If smoking DON'T skip this or you WILL have at least some brown residue in you're flute)

1. Add ice cold dH2O equal to half the volume of the solution and seal the bag.

2. Shake vigorously for 30 seconds.

3. Allow to separate.
(The top layer will be the freebase solution, bottom is the waste water.)

4. Decant (pour off) the water layer and discard.
• Easy way to do this is simply cut the corner of the bag off and allow the water to drain out, then pinch it shut when it gets to the solution, and then pour solution into a fresh bag.
(Adding water causes the pH to slowly head toward neutral, so best to check that pH again.)

5. Re-base if needed (shouldn't need to).
Repeat 1-5. Another 4 or 5 times
•VERY IMPORTANT: Water wash the fuel a good rule of thumb is to do 4 or 5 very good washes of the fuel or until the fuel barely clouds the water anymore. (This makes a world of difference.)


If you want to water titrate:

1. Save about 25ml of fuel in a separate container to use as "Bring-Back" fuel while titrating.
(You can thank Werner Karl “Heisenberg” for the bring back fuel idea)

2. Add about 15ml of distilled water to the clean fuel.

3. Add Muriatic/water mix SLOWLY (1-3 drops at a time) and shake until you see the fuel go cloudy and the layers have difficulty separating (this indicates the solution has become acidic).

4. Add the "Bring-Back" fuel to raise the PH back to neutral or slightly above.

5. Separate, drain & Collect Water, and Evaporate.
(When water/Meth mix thickens, Pour a splash of dry Acetone on the plate and continue evaporate to crash out the crystals.)

If you want to gas:

1.Add 3 capfuls of H2SO4 to the soda bottle with the NaCl (salt).

2. Quickly screw on the lid tightly. Pinch the hose to prevent gas from escaping.

3. Open just the corner of the bag with the freebase solution and gently squeeze the soda bottle to force the gas into the bag.
(Once there is a good amount in the bag, seal it.)

4. Agitate the solution inside the bag to maximize exposure. The solution will start to become cloudy at first, like milk.
(This is the gas raising the pH of the solution and starting to drop the meth HCl in solid form.)

5. Hit it with the gas again, seal and shake the bag.
(It should start to look like a snow globe in there)

6. Hit it with the gas seal and shake the bag again, allow to separate.
(If solution is still cloudy, continue gassing until it is crystal clear when it separates)
Hint: If the gas starts to sputter out, it can be refreshed by simply adding more NaCl and H2SO4.

7. Stuff 2 cotton balls into the neck of your funnel.

8. Place 2 filters into the funnel above the cotton and add 1/2c (64g) of MgSO4.

9. Place 2 more filters on top of the MgSO4.
Line your pitcher with another bag and filter the solution into it using the prepared funnel.

(The stuff in the filter, that's what all this is for.)

10. Squeeze as much of the solution out of the filter (that's full of good stuff) as you can without ripping it.

11. Twist the top of the filter closed so nothing escapes, grab a towel and fold it lengthwise until it is about the size of your wet dope filter.

12. Roll the filter tightly in the towel and step on it.
(Put all the weight of your heel on the towel to force out remaining solution.)

13. Retrieve the dope from the towel and open the filter. Set it down and allow it to dry.
Scrape off the filter onto something.


Conclusion or not?

This product is completely usable at this point or you can recrystallize to further purify the little crystals and form it into bigger crystals/shards.


Recrystallization:

1.Crush meth into a fine powder.

2. Put it into a little glass jar.

3. Measure out 240ml of your dry methanol and put it in the microwave.

4. Microwave it 10 seconds.

5. Microwave it 10 more seconds.
(Watch for boil over.)

6. Once it is just hot enough to start boiling, remove it from the microwave and add to the jar containing the dope with your medicine syringe/ eye dropper until the dope dissolves.

7. Add hot methanol dropwise until the solution turns clear.

8. Filter out any solids. These are impurities.
Place the lid loosely on the jar to prevent foreign objects and put somewhere warm.

As the solution slowly cools, the meth becomes more and more concentrated in the methanol, making it over saturated.

Crystals then form and grow until all the meth is used, leaving any remaining impurities at surface level or in the remaining methanol.

Don't disturb the solution while the crystals are forming.
(Disturbing the solution breaks the forming crystals apart, forcing them to start over.)
• Disturbed solution = smaller crystals.

•Freezer cooling = small crystals and clean
•Fridge cooling = medium crystals and cleaner
•Room temp cooling = big crystals and even cleaner.
(The slower you cool down the solution the bigger the crystals and cleaner the meth because the when the meth is reconnecting with its mates in there if this happens to quickly impurity can get stuck or ruin the structure of the crystal.)

9. Allow to cool/evap for around 4-6 hours.
Chisel off the crystals and swish the whole thing around to make sure you get everything.

10. Filter out the crystals. Place remaining fluid onto an evaporation tray and evaporate to catch any remaining product that didn't crystallize.

11. Rinse with dry, cold acetone.

12.Allow to dry.

That's all folks
P.s
 

Burke

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Source?
 

Douda

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I got the recipe from IDOC
 

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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Who said that? I never said that Coleman feel is just mixed hydrocarbons, basically naptha
 

hirozaru

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I have a similar question. Maybe he meant to ask, can we use Coleman's fuel instead of diethyl ether+hexane ?
Do we still need to mix the coleman fuel with Epson Salt to get an anhydrous solution ?
 

hirozaru

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Any reason why Coleman fuel might be blue? Is this a problem?
 

hirozaru

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I would also like to know about Epsom salt. When to add, isn't clear
 

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.
 

Douda

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Naphtha is also labelled "BENZINE" in other 3rd world countries
 

hirozaru

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I don't understand what it means when you write
> if you want to gas
or
> If you want to water titrate:

what does that mean ?

at what point is the product is safe or oral consumption ?
 

SoldadoDeDrogas

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After you HCl gas and precipitate - "snowglobe". You filter and collect. At this point, the product can be used, however, it is HIGHLY recommended one should wash the product with cold, dry acetone and let dry before use. After the acetone wash one can further crystallize.
 
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hirozaru

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Thanks. This is my first time. I don't know what is "Snowglobe"
I just got a first reaction that appear successful. I see golden pieces on the top of the solution. Is this what I should collect and wash ?
 

hirozaru

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Ok, I get it now. How long should the gasing take?
 

SoldadoDeDrogas

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Gassing takes about 5-10 minutes of active bubbling in my experience. After a few minutes nothing will be happening and you will think it's bullshit. Then all of a sudden it will look like sand is coming out from your bubbling hose. It takes a short moment to finish and you will know it's done when no more solids are being formed.

Ammonium sulphate is mentioned in this recipe as a substitute for ammonium nitrate at a 3-1 proportion, but who knows what the stoichiometric amounts are. Ammonium sulphate can be made easily enough according to wikipedia, using liquid ammonia and sulfuric acid. Seems like it may be a good alternative to ammonium nitrate, unless somebody has a better idea... ?
 

tankikan

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Hi,

Does it similiar to this?

Perhaps your's was more details.

Video
 

SoldadoDeDrogas

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Where can one obtain Ammonium Sulfate? Or is it easy enough to make?
 

hirozaru

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I don't think sulfate works. You need ammonium nitrate from cold packs

Not easy to make as far as I know
 

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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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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