1. I plan on using the meth I produce solely for self, no selling. I want to end up with ~7 grams of clean, methamphetamine hydrochloride. Is a two-neck, 500 ml 14/20 flat bottom flask adequate for the job? I plan on using one neck for a condenser and the other neck for a submerged lab thermometer. Is a 500 ml flask large enough? Is a flat bottom flask okay to use (as opposed to a round bottom flask--I plan on using a deep fat fryer for heating). What about 14/20 glassware for this size reaction, is it adequate? Do I need to move to 19/22 or 24/40?
500ml flask is fine. 14/20, 19/22, and 24/40 will all work fine.
2. Given that I plan on using a deep fat fryer/oil bath, how high should the oil be in relationship to the flask? Half way? What about the relationship of the flask to the deep fryer, is it okay/recommended to allow the flask bottom to touch the bottom of the deep fat fryer?
Halfway is good. It is NOT recommended to allow the flask bottom to touch the bottom of the deep fat fryer, because that could cause overheating. Jack's experience with flat-bottomed flasks are that they are unreliable when they are heated directly on a heat source. Keep it about half an inch to an inch above the bottom.
3. Assuming 14/20 is okay to use for this size reaction, what kind of condenser do I want? West? Friedrich? Liebig? Also, the 14/20 condensers apparently come in two sizes, 110 mm and 200 mm. I would like to be able to circulate room-temperature water and not have to use ice water, especially since I plan on refluxing for 48 hours. Can room temperature water be used? What type and size condenser to purchase?
The condensers you mentioned will all work fine for the size of the reaction you want to perform. Room-temp water can't be used as that defeats the entire purpose of using a condenser. Ice water MUST be used as it will condense the boiled water vapors and hydrogen iodide back to hydrodic acid. The acid will return to the flask where it can continue reducing the (pseudo)ephedrine to meth. Use the longer condenser if possible.
4. I've never quite understood what should attach *to the top* of the condenser. A drying tube? A balloon? Nothing? My guess is that nothing need be attached as long as the condenser is doing its job properly.
If you can tolerate the smell and are not in a populated area, you don't need to attach anything on the top. Otherwise, attach a 16" punchball balloon to the top. It will inflate partially and stay partially inflated a certain amount for the duration of the reaction. The inflation occurs in the beginning of the reaction where the proper concentration of hydriodic acid is being generated from the red phosphorus and iodine. You're right, a big enough condenser, with ice water, will keep all the vapors in the lab setup. Don't use a drying tube.
5. I think I remember reading something in one of Uncle Fester's books a long time ago about not using pool acid as a substitute for good HCL (aq). Is this true? Believe it or not, I'm having a harder time finding lab grade HCL than I did finding RP and I!
I wouldn't worry. Regular pool acid works just as good in Jack's experience, and it's easy to get.
6. Almost every post I've seen in terms of molar ratios/relative weights of precursors assumes matchbook- derived red phosphorus and tincture-derived iodine. My RP and I are reagent grade. Can someone please give me either molar ratios or, preferably, relative weights to use for this reaction for RP/I/E/H20?
Assuming lab-grade precursors: 0.4RP/1.3I/1E/1H20.
Assuming OTC precursors: 0.7RP/1.6I/1E/1H20.
7. Since I plan on doing a slow wet reflux, is making the HI in situ still frowned upon? Should I add the RP and I and water first, wait for them to react completely, and then throw in the E? Does it matter given a slow wet reflux? In what order should the precursors be added? Should the glassware or any of the precursors be chilled first in the refrigerator?
Making HI in situ is not frowned upon. It doesn't really decrease the yield any or reduce the potency. You worry too much man! It doesn't matter how the contents are added to the flask so long as the last item is either the red phosphorus or the iodine.
8. How important is grease for the ground joints? Any recommendations as to the type to use?
It's defenitely recommended for complete insulation so the smell and hydrogen iodide vapors don't escape. I doubt that will be a problem, but grease them with any diuretic silicone compound, like Dow Corning High Vacuum grease.
9. What about Keck clamps for the glassware? Are they needed?
Are you making meth or doing a Grignard? No, they're not needed, but they're defenitely recommended.
10. I've just finished using ahgreich's Tetra Trap method on some 12 hour 120s. The pseudo looks awesome--needle like shards, white as can be. 71% yield, if my math is correct. Can someone verify this for me? I started with 12 grams of GUPS. I've got 6.99 grams of pseudo freebase. 12 grams x 165.2322 (molar weight of pseudo freebase) / 201.6931 (molar weight of pseudo HCl) = 9.83 g pseudo freebase theoretical. 6.99 g (actual pseudo freebase) / 9.83 g (theoretical pseudo freebase) = ~71% yield. Correct?
So, do you want meth or do you want to become a professional scientist? Lol, just kidding. You got it right.
11. In terms of the pseudo freebase, is this okay to use in the reaction as-is? Do I need to convert it to the HCl salt first? I read where the reaction is even more exothermic if the freebase and not the salt is used. Is this a big deal? Will it require an ice bath initially? Does the use of the freebase vs. the salt have an impact on impurities?
Freebase is a little bit more reactive. Use 82% the amount as you would the hydrochloride. That is because the molar weight of (pseudo)ephedrine freebase - 165 or around that - is 82% the amount of the molar weight of (pseudo)ephedrine hydrochloride - 202g. One mole of either form can afford up to one mole of meth - 149g. So 165g freebase or 202g hydrochloride reduced in under the same circumstances would result in an identical weight in meth. And the maximum possible yield is 92%.
12. I've read that PEG may have gotton through the Tetra Trap. How can I tell if this is the case? How can I remove it from the freebase crystals? Will a simple recrystalization remove the PEG? Any suggestions/pointers here?
An effective recrystallization could, but it's difficult. Letting the reaction proceed for 48 hours will break it down into compounds that an acid/base extraction will remove from the meth base.
Good luck! With the details of the questions you asked, I doubt you'll need any luck, though.
