Reaction unit and push/pull tanks by Hematite

Separatory Funnel
Add a separatory funnel
Separatory funnels are often made from a plastic two liter soft drink bottle, the top of a liquid dish soap dispenser is the stop valve, or simply a small hole in the cap operated with your finger. You must either squeeze the bottle lightly or provide a tube or hole to equalize the pressure.

At this point, you may begin dreaming in the alpha state of mind , not unconscious sleep
but an aware state of peaceful relaxation,, If you choose to come out of the alpha state simply flex your arms and you will awaken, alert , feeling well rested and happy

Part 1 Extracting ephedrine
Part 2 Iodine And Phosphorous
Part 3 The Reaction

Flask
Stopper and hose
Push/ Pull
Ratios
More preparation
Adding Chemicals
Reaction Signs
Construction
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Flask
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Revised 11/23/99

The Reaction

This reaction is exciting, and rapid. You must really focus your attention at this point it is of primary importance, that you have your wits about you. It is common to have a tired assistant sleep through most of the procedure, only to wake up to watch the reaction fire off.

Injuries occurring, during the reaction can be avoided
1) never place the flask on a hard or cold surface, rest the flask on a towel or something soft.
2) there is no reason at all to place the flask directly on the burner, hold it above or set it on the soft towel,
3) wear some heavy heat protective gloves
4) wear clothes to protect you from spills, especially wear shoes and eye protection.
Nothing like full body armor, just don't let your stuff be hanging out bare

5) keep the injector hole and flask sealed when a burner is on,
gas from the flask will explode in air with a flame or spark.

The entire ephedrine cleaning procedure is here: Extraction of Ephedrine
The cleanup of the ephedrine has become very important. Use toluene or toluol
when using ephedrine with naphtha heat up the Naphtha, and you will get a good yield of E . The heat allows the Charcoal lighter fluid to hold much more E.
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Starting the dream reaction - Starting the reaction

Ratios

Iodine weight

Iodine = 1.2 x E (by weight)
. you can go as low as 1(E) : 1(I2)
or as high as 1(E) : 1.5(I2)

Phosphorous weight

RP can be 1/3 of the weight of E under a Ounce of E use 1/2 the weight of E Lowest amount I know of is 20% of the weight of E Highest I have used is 100% the weight of E

Water

I have a syringe in the hose so water may be added after the flask is sealed. If not using a syringe you will need to add water to the reaction. It is suggested to put a capfull of water or peride in the flask in with each oz. of E.

Hydrogen Peroxide

If using recycled phosphorus use peroxide in place of water

Preparation

1) - Weigh out the Ephed , RP and I2, in a ratio of 1(E) : 0.5(RP) : 1.2(I2)
2) - Mix the E and Iodine together well, in the reaction vessel and place in the freezer for 5-10 minutes
r3) - prepare a pan of water with ice to cool the flask, if it needs it
4) - Prepare a pan of hot boiling water to heat up the flask, if needed
5) - Cut your 8-10 strips of tape 6" long and have them ready
6) - prepare a small cup of water and another with hydrogen peroxide these will be injected into the flask through the hose generally by a needle inserted into the hose
7) - insert the needle into hose and check to see it works
8) - Have something to drink for yourself within reach
9) - get the thick gloves ready

Addition

This will begin the reaction and it usually lasts 30 minutes to 1-1/2 hours

There are many ways to mix this stuff togrther here is one way:
1) Remove the reactants from the freezer put the RP in the flask with the E and I2,
some prefer to add the RP during the reaction as needed
2) While dry and cold Mix it all very well, it should begin to begome more fluid like a stiff mud
3) Add capful of peroxide 1-capful / oz of E
4) Put on stopper and strap it to the flask tightly with tape, mix in the peroxide
5) If no reaction then put in warm water bath, look for bubbling to occur
6) You will notice the contents begin to rise, let it rise
if it begins to over flow then shake the mixture a little until it goes down
If you get very very thick yellow or red fumes, shake it down hard then add a ml of water

7) Keep the rection going with a little hot water bath if needed if this fails to keep the reaction bubbling use one ml or two mls water or peroxide
Try to add very little water

8) If reaction seems dead, and watered down prepare a 1/4 the original amount of RP and I2 , Carefully open flask (it may have pressure from the P/P, add the fresh reactants swirl and heat up in water bath till it bubbles
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You will need every observation skill you possess. he reason is you must make some decisions during this process concerning the state of the reaction and what to do next, thjis is the hardest part because it varies so much.
Generally it fires off, you see most of the signs and are satisfied that it is complete.
The problem arises when something is not right.
This is difficult to determine if you do not know what is normal.
Listed are numerous signs to look for,
If you really doubt that you had a reaction for a long enough time period 10-15 minutes, then open it up and add 1/4 th3e original I2 and RP to fire it off

Reaction Signs

During the reaction you may note these positive signs of a reaction.
1) bubbling of the mixture with a rise in the level of the solution
2) fuming thick yellow-red cloud not good, shake then add 1 ml of d-water chill if see this
3) White cloud not very thick is OK
4 ) The hue of the liquid changes from reddish purple to a drab purple
as the reaction approaches completion

Finishing Signs

1)The big whoosh( may or may not happen), the liquid mix suddenly begins boiling hard and pushing serious amounts of gas
2) When swirling the flask the thick mud no longer sticks to the sides
the burgundy mud on the sides turns into a bland drab purple
3) the push pull tank is no longer pushing
4) cessation of all bubbling

Observation of ANY these signs means you PROBABLY have have successfully reacted a the I2 and have a product,

NOTES

Be prepared, the RP hitting the I2 will often start the reaction.
If it does begin to go off, - Do Not Panic - put the stopper on and tape it into place , watch the inside of the flask
It may be full of vapors, and impossible to see inside the flask at all, shake it down hard , and keep shaking it hard until you can determine what is going on looking for a nice easy bubbling
if the mixture starts to rise up too high, shake it a little.

HAZARDS

EMERGENCY???? then - Quench the reaction with lots of water water The worst thing to do is to run away, leaving it out of control, probably will result in a fire , injuries, and your arrest.
if you can not get the stopper on , place your wet towel over it , Quench it with water
Then get you and the flask to a safe area, away from all flammable, get it sealed or water it down , the smoke and shit will stop with excess water.
The smoke will bring the heat on you, The phosphorus is hell to put out and smokes like crazy You want to avoid the contents that may be tossed out of the top of flask that is the real danger, since you are not using heat the risk of fire is reduced but not gone,
If the Phosphorus begins burning and spewing you have the most dangerous situation the amount of smoke is unfathomable , get the hose immediately. The gasses are not healthy, but a little will not kill you
The fumes are not a deadly toxin, but it is vaporous HI acid, and a little phosphine(not phosgene). Avoid breathing the fumes
Keep the wet towel handy, always, and use it, if you have trouble,
That towel will turn potential serious disaster, into a laughable "won't do that shit, again" story
. I used to cook wearing basically zero clothing, After considering what would happen if burning phosphorus were to land on skin and the effect of broken glass on bare feet, I now wear full body armor, with helmet
. Your chances of serious injury, depend upon you
. If your a fucked up type high, stoned, thick headed, or a goof trooper you will get injured,
. If your on top of the situation you will probably have no injuries perhaps a minor cut or burn now and then.
.

The RP and I2 concentrations determine the reaction rate, and completeness of the reaction
The RP determines how quick the I2 will react, (assuming there is enough I2)
More RP and the reaction will have a stronger initial surge
More I2 the reaction will go to completion but can discolor the stash
Less RP the reaction is slow or may not fire at all
Less I2 the reaction will be slower , incomplete turnover of the E , and possibly will fail to react at all.
The thick yellow fumes is a part of the reaction you don't want or only want to see for a short period of time.
Too much of this fume is bad because it indicated the destruction of ephedrine.
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Filtering and Purifying the Product- Time to get Serious

Dirty glassware, poor reagents, sloppy technique was all swept under the rug until now.
From this point on any screw ups affects your product in a big way. So clean everything double good
Dilute the reaction mix with an amount of water to facilitate filtration
Prepare the standard cotton balls and 4 coffee filters, wet them down with d-water
Filter.
if solution is still red or orange or yellow re-filter through the same RP and filters again, continue re-filtering until it has no added clearing effect.
This filtering should remove most of the cloudyness and red color.
It may require re-filtering 3 or 4 times.
You end up with a clear yellow or colorless solution that can have many different odors.
Since this is the final product waft some of the odor toward your nose.
If you smell the ephedrine bummer,
but the smell of meth and HI it is distinctive, thats great

Add a non polar solvent (Coleman, Charcoal lighter fluid, toluene, naphtha, ether, hexane ..etc) This protects your meth from degradation due to high pH levels
Not a lot is needed, because it adds more contaminants and is a pain to deal with let us say at least 100 ml then 50 ml for evey ounce

* IMPORTANT*

All pH measurements are made only on the water layer (lower layer)polar solvent.
To take a pH reading on the non-polar upper-oil. solvent is useless.

Bring the pH of the water soluble layer
up to 12 with NaOH shaking and testing the pH.
if your Digital pH meter sticks at a level around 11.0 and additions of lye do not raise the pH your done adding lye it has enough, and your pH is probably near 13+
Adding table salt(saturate) several tablespoons full causes the water to drop the meth and increases your yield

Dump the Lye

To remove any excess I2(Iodine) still present, Absolute recommends using a few drops of Sodium Thiosulfate
This will separate I2 into 2I- by adding a pair of electrons, The thiosulfate is a photographic fixer, available cheap at a photography supply store.
If you have double filtered the reaction mixture through the Red phosphorus coated filter paper, most of the I2 is gone already, more will be lost to the lye as it is flushed.
Shake it well
Allow the mixture to layer, then separate, discarding the lower water/lye layer.
save the lye in case it containds the meth , just in case

Wash the freebase and fuel solvent with about 1/3 the amount of water as there is solvent with hot d-water becareful of pressure from hot d-water

Add d-water recently opened and heated , add about 1/3 of the volume of the fuel layer
Shake, Twist, swirl the separatory funnel then and remove waste water
.....repeat 2-3-4 times untill the little water droplets that settle to the bottom look clear,
there is a grey film that sits between the oil and water and coats the last little bits of water droplets, it sticks to the walls of the separatory funnel
that is the last of the gakk and is hard to spot sometimes, look for it , you want it gone for sure .
It ruins the taste for meth smokers.

Move meth to D-water

Add d-water a smaller amount than the fuel, it is easier to evaporate the less water you use
then add HCl drop wise with shaking until the water layer tests to be pH 8.0 or less
This is about 6 drops of HCl per gram of expected product.
Check the pH after shaking until you get two of the same pH readings and are sure the pH is stabile
Best is pH 7.2-7.5

Too much acid

If it goes below pH 7.0 do NOT add a NaOH basic solution to raise it up.
This will produce huge amounts of troublesome salt
Instead remove about 1/4 of the water/ acid /meth ,
add fuel ,
add lye solution to pH 12 +
, Shake well,
let it layer, separate,
flush lye
Wash again with hot water
add this back in the over pHed solution
and pH it again
evaporate the water layer, appearing will be crystal meth

Second pulls

Add more water to the fuel, add HCl drop wise, testing and shaking layer , separate , evaporate for the second pull

Addendum If you get a solid, wax, or gloppy junk in the oil or water layers that follows the meth around
Run the layer through a filter to remove it before doing you final hot water washes Filter once, very easy, no cotton ball just single coffee filter, toss out the 1-2 ml of fluid that stays in the filter paper

Filter the toluene-freebase.
After removing the lye/water solution and after washing with d-water when washing the toluene-freebase. Whenever the non-polar solvent appears cloudy it needs to be filtered this will clear it up immediately. I'm not real certain if the cloudiness is just the non-polar holding water bubbles or what the deal is.

Premix lye water solution, 20 grams lye to 100 ml of water
it is important to make fresh batches or store it sealed.
It will absorb crap in the air quickly.

Realize that we use good reagents, but none of the hardware stuff is really clean.
So everything us cavemen and cavebabes use is in need of purification.
The distalled water ids the purest thing we can use
and the consumer always deserves the very best(in this case the cleanest) we can produce.

Purity is the difference between OK the great shit.
We are fortunate, what others call super good, we will honestly label as just OK,
because we know the difference.
It is those last hotwater washes that will tell how clean it is

Lastly be aware of airborne contaminants especially when evaporating.
Aerosols, air fresheners, dust, smoke, I swear highly filtered humidified air would be sweet.
Use a hair dryer along with the stove to evaporate.
The hair dryer has improved yield greatly, if keep the airborne shit to a minimum.
The hot air of the hair dryer actually will cool the solution by evaporation.
When hot enough to boil water you are loosing ephedrine and M
Those vapors rising from the surface of water have quite a bit of ephedrine and meth in them
The alcohols boil low enough to not be a problem but the alcohols increased evaporation rate is phenomenal with a hair dryer.
When the solvent has almost totally evaporated away, the hair dryer is hot enough to melt the shit.

For the glass like shards and crystals there are many ways,
mostly dry it slowly at the end, this can take a day or more in water
99% isopropyl dryed slowly works there are some chilling and filtering methods that work good too.
I evaporate hot until it is thick and skins then spread it around the inside of the bowl ,
This usually dries to nice enough looking quick glass shards when scraped off with a razor blade
any excess pour into another bowl, warm that up till dry then add a little isopropyl
let it evaporate under a fan, for the rest of the crystal shards.

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Flask size

Absolute minimum