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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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 #1 
Old 2003-08-18, 22:44
MÆE MÆE is offline
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Default Can Some One Read This And Verify If Info Is Correct

THANKS FOR READING

Can some one read this and confirm if the information is valid/correct.

any one with tips on it/corrections ect.

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Introduction

1. Equipment

2. Ingredients

3. Method

4. Acid/Base Extraction

5. Gassing

Equipment

* Various jars, glass vessels, beakers etc

* PH paper, or electronic PH tester

* Filter paper or coffeee filters

* A strainer that will fit your filters nicely, so that you get better surface area then a funnel

* Hair dryer, or heat lamps

* Hot plate, no open flames only heat elements

* Separatory funnel, or similar, or tube to siphon

Ingredients

* Pills containing psuedo-ephedrine Hcl or ephedrine Hcl

* NaOH/Sodium Hydroxide/caustic soda/strong base/lye

* Epsom salts that have been baked in oven (200°C) for an hour to dry!

* Methanol

* Acetone

* Toluene

* Distilled water

Method

If pills have red coating put in jar with acetone shake until red coating is dissolved and then continue as below!

Step 1: Ok first, put your pills in a jar. Add methanol about double the volume of the pills. Cap the jar and shake till they break apart. Leave to sit for a few hours shaking every 1/2 hour. Let settle into 2 nice layers then siphon or decant off top layer. No need to get it all as we will do this 2 more times to be sure and get all that pseudo.

Step 2: Once you have done it 3 times and have the 3 lots of methanol from the top put them together and put in freezer You want to get it real cold, near freezing and then filter it thru a very fine filter, this may take some time if you don't have a vacuum filtration setup but thats ok, we aint in a hurry! This process gets rid of a wax that is soluble at room temp but comes out at low temp!

Step 3: Note: This step is not necessary and only speeds things up! Ok after the chilled filter, we will reduce the volume of methanol/pseudo solution! So, with good ventilation and a fan blowing over pot, just reduce the volume of methanol, but not till you see crystals or anything just reduce it to a manageable amount, we just want a saturated solution, you'll notice it thicken a bit! Stop take it off!

Step 4: Now you want to pour a thin film of this methanol/psuedo solution out on a mirror or glass table for fast evaporation or you could just leave it laying around a couple of days and let nature take its course, and it does make perty crystals! Scrape all your crystals up when they are dry and put into another clean pyrex vessel!

Step 5: Now pour Toluene, about double your psuedo volume (dry/anhydrous, use your epsom salt) over your powdered psuedo, and heat till just before boiling with your fan blowing over it! Boil for 5 mins and then filter. Repeat this with fresh toluene until when you boil toluene it stays clear! To be sure of toluene doing its job, after filtering, add water to toluene before discarding and you'll see the shit come out!

Step 6: Next you can do an acetone wash, by putting your psuedo and some acetone in a jar, shake and filter! Dry pseudo and you should have fuckin clean pseudo Hcl...

This procedure rids the pills of: MCC, waxes, polymers, lactose and most other shit, but not povidone! more on that later!

You may choose to react your psuedo now! Or do an A/B (acid/base) extraction, basicly turn it into a freebase, or oil! Keep in mind... If you do an A/B now you may lose some psuedo to the povidone!

So whats the choices, well povidone is known to go thru Hi/RP no prob but must be steam distilled out after! Which is a good thing coz you got no seperations or emulsions and the cleanest meth around! Povidone is bad because povidone is known to absorb and hold amines! It depends on what reaction your doing!

Acid/Base extraction

Ok, get your nice dry white powder and add about equal part water. Now make up a 20% NaOH solution (or 4 parts DH2O:1 part NaOH) Add Toluene to water/pseudo solution about equal to water volume! Yes toluene first, it gives the pseudo somewhere to go instead of being burned by the base which can break it up and turn it into aziridines (toxic)! Add NaOH solution to water/pseudo/toluene solution till PH 13, and remember to test PH of water not toluene! Now shake the jar up very well and let settle into layers. Seperate toluene layer. Repeat this process 3 times and combine all your toluene! You can wash the toluene/pseudo freebase with water now if you like and seperate again! Now you can either, evaporate toluene now for freebase crystals! Or you need to turn the freebase into a Hcl salt again!

So you can add fresh dH2O (about 2mL for each gram of pseudo) to your toluene and drop HCl acid slowly with shaking each time into the toluene. Check pH all the time and stop just before neutral! Shake again, and recheck, this is very tricky and takes patience! Now seperate the water from the toluene. Now you can evaporate your water to get your pure pseudo Hcl. You can repeat this another 1 or 2 times and get a little more!

Gassing

Gassing makes things easier coz you just gas it, filter and theres your crystals, but it is tricky to get the hang of and Hydrogen Chloride is dangerous! It will burn your fuckin lungs instantly! You need to pipe HCl gas into your jar full of toluene and pseudo freebase, but the gas and your toluene must be dry/no water, or everytime the gas forms crystals it will be reabsorbed by the miniscule amounts of water! If you don't know how to extract, you shouldn't play with gas yet! If you know how to gas then read on... So, you need to dry your tol/pfed solution with pre-baked epsom salts to absorb the water, and then filter them out! Then gas your solution and you will see a snow storm before your very eyes! Then just filter and dry crystals! But still may contain povidone!

THANKS FOR READIND & THOUGHTS
 #2 
Old 2003-08-18, 23:05
kirby kirby is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

wheres the part on how to do the reduction ??
 #3 
Old 2003-08-18, 23:31
MÆE MÆE is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

What the phuck i had it in there pasted.

_______________________________________________

When ephedrine or pseudoephedrine is heated with hydriodic acid, with red phosphorus or without, initially the hydroxyl is replaced with iodine. From this point the rearrangement chemistry of trace impurities starts. The halo compound is subject to reduction in the hydriodic acid medium leading to the target compound, methamphetamine. Hydrogen iodide dissociates at higher temperatures to iodine and hydrogen. The reaction is reversible. Its equilibrium is shifted in favor of the decomposition by the reaction of hydrogen with organic compounds (iodoephedrine in this case) in the reduction, but it can also be affected by removal of iodine. This can be accomplished by allowing iodine to react with phosphorus to form phosphorus triiodide which decomposes in the presence of water to phosphorous acid and hydrogen iodide (a cyclic oxidation of the iodide anion to iodine and reduction of iodine back to the anion by the red phosphorus, the latter being converted to phosphorous or phosphoric acids). In this way, by adding phosphorus to the reaction mixture, hydrogen iodide is recycled and the reducing efficiency of hydriodic acid is enhanced.

_____________________________________________

I dont know the measurments off hand but we will try this just for the post.

1000 ml flask/150 gms iodine crystals

to 150 gms of red phos/ in 300 ml water ?
 #4 
Old 2003-08-18, 23:52
kirby kirby is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

my forte is birching--but the cleaning procedures look fine and the red/phos iodine reduction looks spot on--wait for some of the other lads to wake up and give there opinion but it looks right to go
 #5 
Old 2003-08-19, 08:25
MÆE MÆE is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

does any one have any one have comments on the birching they can add.
 #6 
Old 2003-08-19, 12:03
kirby kirby is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

yeah ive got a chook yard full of comments on birching, but they have got bugger all to do with the phos/iodine reduction
 #7 
Old 2003-08-19, 13:36
daveydavey11 daveydavey11 is offline
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Default Re: Can Some One Read This And Verify If Info Is Correct

Good method

This is what swim is doing, however......

In the gassing process......

Would you add double the psuedo volume with water and match the volume of water to toulene and make basic ph12....then gas??? Or, jsut add double psuedo with toulene then make basic ph12....then gas??? which one???

DD
 
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