02-16-04 22:53
No 489135
1. What is the attachment called that connects the reaction vessel to the reflux condenser, for a meth hypo cook ?
2. SWIM plans to connect tubing at the top of the condenser to a vapor containment unit( I will probably use a 1000ml flat bottom beaker). Should I use electrical tape to seal the connections?.
3. Also is there an agent/chemical SWIM can add inside the vapor containment unit to absorb and/or eliminate the fumesfumes? Is electrical tape SWIM's best bet to avoid fume leakage?
4. Also during recrystallization of the final product should SWIM use filter paper and a regular funnel, or buchi funnel? Which one is better.
(Hive Bee)
02-16-04 23:01
No 489140
Sorry guys, one more very newbie questions. Please don't flame me. I am just trying to learn the process.
5. I have a hotplate/stirrer, should I use make an oilbath(using a big round Pyrex dish), or just place the 250ml round bottom beaker directly on the hotplate/stirrer. Also should I turn the stirrer, and how fast should I turn it? I am planning to reduce about 5g of ephedrine hcl(not pseudo, I have actual pure ephedrine, as well as hypo 30%).
(Hive Addict)
02-16-04 23:40
No 489148
Post 451057 (SHORTY: "Many improvements….", Stimulants)
Post 411130 (SHORTY: "Success with Sodium Hypophosphite", Stimulants)
Also....where is SWIK...SWIM...The neighbors pet
???
a little less conversation, a little more reaction
(Hive Bee)
02-17-04 00:12
No 489156
1. What is the attachment called that connects the reaction vessel to the reflux condenser, for a meth hypo cook ?
Depending on whats avail to you at the time either a distillation bend, i prefer to use an angled splash head, some use clear plastic pipe.
2. SWIM plans to connect tubing at the top of the condenser to a vapor containment unit( I will probably use a 1000ml flat bottom beaker). Should I use electrical tape to seal the connections?.
A bucket would do with a wet towel over the end of hose, just make sure theres no liquid able to be siphoned back up thru hose to flask.
3. Also is there an agent/chemical SWIM can add inside the vapor containment unit to absorb and/or eliminate the fumesfumes? Is electrical tape SWIM's best bet to avoid fume leakage?
A few inches of water in bucket, sit hose on a brick or something. A wet towel will seal it pretty good. It could come in handy as well in case of fire, you can smother with wet towel.
4. Also during recrystallization of the final product should SWIM use filter paper and a regular funnel, or buchi funnel? Which one is better.
I dont like using paper after recrystallisation, it's to easy to put tiny paper fibres back in gear, it defeats the purpose of recrystallising, but thats my opinion, more so if using coffee filters. I have a piece of silk the size of a hanky, just takes a little longer for solvent to pass thru.
I'm not racist,I hate everyone.
(Hive Bee)
02-17-04 00:42
No 489164
A sand bath would probably be better than oil, cleaner.
I would'nt personally put a rb flask directly on hotplate in case you get a bit of movement if contents start bumping, i've sat erlynmier flasks directly on plate before. (Flat bottom conical flask= erlynmier)
I would'nt bother stirring, no need.
Your hypo is a little on the weak side, i would probably double the amount you were thinking of putting in. Hypo 10-12ml : I 8-10g assuming its lab grade and your 5g of E.
That's me though, if you manage to get hold of shortie get some advice from him if possible. IMHO he would be the hypo guru, but hit the UTFSE.I would prob put balloon on condenser as well since you've got 30% hypo, i normally use gas tape/thread tape to keep together under pressure but no matter what have a wet towel handy, i feel you might need it, i hope not.
good luck.
I'm not racist,I hate everyone.
(Hive Addict)
02-17-04 02:37
No 489190
The same as i would except for i would prefer a oil bath rather than sand. If your 30% hypo is labgrade then i would not increase the amount it will work fine. If anything you should increase the amount of I because even with 30% you will still have an excess of Hypo for the rxn. Use a balloon for vapor containment although i doubt you will need it. I have also found that taping the balloon is not necessary. I have had a balloon inflate to the size of a basketball without leaking and no tape was used. Your balloon shouldn't get much larger than a grapefruit. If your balloons are thin put one inside another.
It wasn't Me!
(Chief Bee)
02-17-04 20:49
No 489370
(Flat bottom conical flask= erlynmier)
For future reference, it's spelled Erlenmeyer.
Emil Erlenmeyer was a German chemist (1825-1909)
The Hive - Clandestine Chemists Without Borders
(Hive Bee)
02-18-04 21:19
No 489581
SWIM thanks both of you. Your input was very valuable for SWIM.
SWIM wants to add that:
1. Iodine, and Hypo 30% are both lab grade purchased from Canadian chem supplier. The ephedrine SWIM purchased from Canadian fitness/bodybuilding product supplier, but it is also 100% pure Ephedrine HCL(no additional additives.
2. SWIM would like to inform 8-ball that he has neither a distillation bend, or angled splash head available at the moment, but SWIM will purchase an angled splash head to connect the flask to the reflux condenser(SWIM has the condenser which looks like a spiral coil, SWIM forget's what it is called.)
3. In regards to Vapor Containment Unit, SWIM is still debating whether to connect a hose on top of the condenser, that will lead to the bucket which will be sealed with a wet towel as suggested by 8-ball, or just use 2 balloons(one inside the other) on top of the condenser as suggested by Shorty. SWIM will try using the balloon method as a VPU first, since it will work great(according to UTSFE info) for only 5g of Ephedrine.
4. SWIM would like to ask Shorty and/or 8-ball, if turning on the stirrer on the hotplate/stirrer combo, would hurt the reaction? SWIM is aware that it is not needed, but what would be the effect of the stirrer being on?
5. SWIM collected more info from UTFSE. Shorty and/or 8-ball your input on the following?
- SWIM will use a big round pyrex dish(the one that covers the whole surface area of the hotplate). He will fill it halfway with oil(oilbath).
- SWIM will invest in a 2 necked Round Bottom Flask(In order to monitor the temp as well with a thermometer). UTFSE suggested it is better than a flat bottom flask. Shorty/8-ball, what size 2-necked RBF would be appropriate for a 5g of E reduction?
- SWIM will not let the 2-necked RBF touch the oilbath, will secure it with a clamp about 1cm above the oilbath.
-Shorty/8-ball will cold tap water suffice, or does swim have to circulate ice water through the condenser?
(Hive Bee)
02-18-04 23:29
No 489606
1. Iodine, and Hypo 30% are both lab grade purchased from Canadian chem supplier. The ephedrine SWIM purchased from Canadian fitness/bodybuilding product supplier, but it is also 100% pure Ephedrine HCL(no additional additives.
I only dream of ingredients of that quality. I'd be real careful, your leaving one hell of a paper trail, i'm sure you realise this.
4. SWIM would like to ask Shorty and/or 8-ball, if turning on the stirrer on the hotplate/stirrer combo, would hurt the reaction? SWIM is aware that it is not needed, but what would be the effect of the stirrer being on?
I can't imagine it would hurt, but i can't see the point in it, no doubt somebee has done beefore, if so, it was never adopted as common practice.
- SWIM will invest in a 2 necked Round Bottom Flask(In order to monitor the temp as well with a thermometer). UTFSE suggested it is better than a flat bottom flask. Shorty/8-ball, what size 2-necked RBF would be appropriate for a 5g of E reduction?
You could probably get away with a 250ml rbf easily, though i have not seen one that small, and i am sure your reactions won't stay at 5gms either so i would step up to a 500ml rbf twin neck, one a B14 thermometer slot and the other a 19/26. This also depends on the size of your coil(from memory, sounds like a graham). If i'm wrong Rhodium will no doubt correct me. hehe
-Shorty/8-ball will cold tap water suffice, or does swim have to circulate ice water through the condenser?
I guess that depends where you are, the cold water out of my tap would be 24c-26c at the peak of the day, so i run iced water out of my esky(thats always full of beer)through a fish pond pump.
I'm not racist,I hate everyone.
(Hive Addict)
02-19-04 05:44
No 489678
If i had those precursors and wanted to make 5g of meth i would use the following:
I would add 5ml of hypo to a 100ml rbf in an ice bath. I would then add 3 x 2g of I allowing each portion to dissolve before adding the next. I would then add 5g of E and attach 2 balloons to the top of the flask and remove from ice bath and allow to reach room temp. I would then place the flask in an oil bath and slowly increase the temp until the contents start to react and continue to increase the temp to keep the rxn going. I would not increase the temp of the oil bath any higher than 120C. The contents would most likely stop reacting within 2 hours and the solution would be nearly clear like water with a maybe a hint of yellow tint. I would then work it up.
It wasn't Me!
(Hive Bee)
02-19-04 12:33
No 489720
SWIM thanks both of you for your prompt replies.
Regarding the paper trail, in SWIM's country things are a little more relaxed than the USA. Also SWIM is a registered business owner, and hypo is used for legitimate purposes in SWIM's business. The only thing is that the business concept that SWIM set up is entirely fictitious...if you catch SWIM's drift..he set it up because some things are easier to acquire as a business, than as an individual.
SWIM will purchase a 500ml RBF twin-neck, with a B-14 thermometer slot and the other neck with a 19/26, (SWIM has no idea what the B-14 stands for, or the 19/26, but SWIM is sure the chem supply rep will know what they mean..thanks 8-ball, SWIM will also request the appropriate adapters/connectors from the same company.
Where SWIM lives tap water is COLD! Especially during the winter. SWIM is guessing here but it must be around 0-5C. When SWIM turns on the cold tap water and lets it run on his hands, his hands get freaking cold really fast(5-10 seconds).
SWIM will try cold tap water first, and if it fails, then I guess SWIM will go with the FISH POND PUMP/ICE WATER recycle route.
8-ball what the hell is an "esky"?
I guess SWIM has no more questions/inquiries for know, SWIM will collect the appropriate equipment, and start his "project" soon.
Shorty/8-ball do you guys ever sleep?...hehe..thanks for everything guys.
(Hive Bee)
02-19-04 12:35
No 489721
SWIM thanks both of you for your prompt replies.
Regarding the paper trail, in SWIM's country things are a little more relaxed than the USA. Also SWIM is a registered business owner, and hypo is used for legitimate purposes in SWIM's business. The only thing is that the business concept that SWIM set up is entirely fictitious...if you catch SWIM's drift..he set it up because some things are easier to acquire as a business, than as an individual.
SWIM will purchase a 500ml RBF twin-neck, with a B-14 thermometer slot and the other neck with a 19/26, (SWIM has no idea what the B-14 stands for, or the 19/26, but SWIM is sure the chem supply rep will know what they mean..thanks 8-ball, SWIM will also request the appropriate adapters/connectors from the same company.
Where SWIM lives tap water is COLD! Especially during the winter. SWIM is guessing here but it must be around 0-5C. When SWIM turns on the cold tap water and lets it run on his hands, his hands get freaking cold really fast(5-10 seconds).
SWIM will try cold tap water first, and if it fails, then I guess SWIM will go with the FISH POND PUMP/ICE WATER recycle route.
8-ball what the hell is an "esky"?
I guess SWIM has no more questions/inquiries for know, SWIM will collect the appropriate equipment, and start his "project" soon.
Shorty/8-ball do you guys ever sleep?...hehe..thanks for everything guys.
(Hive Bee)
02-19-04 13:31
No 489725
<<4. SWIM would like to ask Shorty and/or 8-ball, if turning on the stirrer on the hotplate/stirrer combo, would hurt the reaction? SWIM is aware that it is not needed, but what would be the effect of the stirrer being on?
I can't imagine it would hurt, but i can't see the point in it, no doubt somebee has done beefore, if so, it was never adopted as common practice.>>
It wont hurt as long as the stirring wasn't so vigorous that it retarded the ability to reflux or simmer. Swix puts his in with the stirrer up full blast so it just agitates (almost silently) and causes some nice bubbling off the stirrer rod. As the hypo rxn is 'strong', the stirring wont increase yields or effect a more complete reaction; as is the case with stirring weaker reactions.
Secondly, the use of stirrers is not common practise as most people dont have them and/or they aren't required. However some rxns (like large I/RP) can benefit from appropriate stirring.
<<If i had those precursors and wanted to make 5g of meth i would use the following:
I would add 5ml of hypo to a 100ml rbf in an ice bath. I would then add 3 x 2g of I allowing each portion to dissolve before adding the next. I would then add 5g of E and attach 2 balloons to the top of the flask >>
100% conversion SHORTY!! hehe, i'll forgive that cos your advise is spot on
LATE COMMENTS -
SWIM will purchase a 500ml RBF twin-neck, with a B-14 thermometer slot and the other neck with a 19/26, (SWIM has no idea what the B-14 stands for, or the 19/26, but SWIM is sure the chem supply rep will know what they mean..thanks 8-ball, SWIM will also request the appropriate adapters/connectors from the same company.
Dude, find out what they mean FIRST...they are socket sizes. The Rep will be suss if u are purchasing glassware and u dont even know socket sizes...
Where SWIM lives tap water is COLD! Especially during the winter. SWIM is guessing here but it must be around 0-5C
Be aware that water that cold will form condensation on the OUTSIDE of the condenser; which can drop into the HOT oil bath and sizzle and be a general unsettling pain. Maybe warm up the water to room temp and circulate that using a pond pump...esp for rxns of this size.
(Hive Addict)
02-19-04 21:42
No 489791
Damn biotechdude! I was going to edit that post but it doesn't matter now. No, i wouldn't expect a 100% yeild. My yeilds using hypo are 80% at best.
I agree with biotechdude, ice water is overkill and more trouble than its worth. Room temp or slightly lower works fine. Although i wouldn't even use a water cooled condenser on a 5g rxn. My 24 inch flourescent lightbulb tube air cooled condenser with plastic tubing collar that fits the flask and makes an airtight seal, works great for such rxns. My water cooled graham is used for the steam distillation of the meth.
It wasn't Me!
(Of Counsel)
02-19-04 22:56
No 489806
Shorty-- I don't think you are far from 100% reduction with the hypo synth. I used to get near-80% yields reaction after reaction with store-bought hypophosphorous acid, and hope to duplicate that soon with hypo from sodium hypophosphite. Ici_Rhi deduced the concentration was still a bit low, remedied that carefully, and the HI production occurred as swiftly and vigorously as the hypo reactions I recall from two and three years ago.
Yield figures will be available if those involved in production can resist the temptation to sample the goods before final weights can be determined, or (more likely) if the weight can be determined before I make it to lab.
My best guess is that yields may have to be estimated, despite the best of intentions.
Don't forget that if you are reducing pseudo HCl to meth the meth HCl molecule weighs about 82% of the weight of the pseudo HCl molecule. If you are gauging yield by weight, remember that a yield of meth HCl that is 82% of the weight of the pseudo HCl reacted is a near perfect yield. That is why the hypo synth's eighty percent yield figure always fascinated me. I have approached those yields only with rP long wet refluxes of 36-48 hours that were carefully extracted. An eighty percent yield by weight is very close to complete reduction and recovery. That high yield average is what made the hypo synth my favorite.
I loved your description in "If I had those precursors.." a couple of posts up. That is precisely what I observed before the heat was turned off. Here's hoping we are falling off the 80% log one more time! Thanks again, Shorty, for your notes on working with hypo from sodium hypophosphite. They are a great addition to the information available at the Hive.
mostly harmless
(Newbee)
02-20-04 05:31
No 489886
Actually Geez, for sake of accuracy, the F.W. methamphetamine HCl divided by F.W. pseudoephedrine HCl is 0.92 (92%).