First time nano hypo-cook

[drjuiceflow]

SWIM never did a cook before. SWIM has been observing and learning from the hive bees.

SWIM acquired most chemicals/equipment for a hypo cook. SWIM will follow the method posted on the Rhodium website, but he will attempt to reduce 1gr of ephedrine hcl, instead of 7g of ephedrine hcl(SWIM lives in a country where ephedrine hcl is OTC). SWIM feels that the smaller the initial transaction the better, just in case there are fumes created that will attract attention.

SWIM would like to hear opinions/advice from hive bees on this. Would only reducing 1gr of ephedrine easier for a newbee ?

SWIM will be using the following ratio:

1 gram of pure ephedrine hcl

1.6ml lab grade 30% hypo ? (Should use more? SWIM could only acquire 30% from chem supplier, is this concentration enough? )

2g I2 iodine crystals


SWIM wants to know where to acquire a VPU (Vapor containment Unit), for setting up the reflux. What exactly is the purpose of the VPU? Will it contain the fumes created while reflux ? Could SWIM use a fume hood ? SWIM has a fire extinguisher ? Is it wise for SWIM to purchase a chemical face mask so SWIM doesn't inhale any fumes ?

In regards to yields SWIM hopes to get at least 300mg of chili, from 1gr of ephedrine to begin with.

SWIM read that higher concentration hypo will yield better results. But is it also more difficult to work with? Heat up faster/fumes/risk of explosion? SWIM doesn't mind using low conc. hypo 30% to begin with, as long as SWIM gets some final product.

Also when chili is dissolved in a small amount of dry alcohol, in recrystallization, what is a SAFETY FAN and why would SWIM need it?

[SHORTY]

In my opinion your ratios are a bit high.  I would use 1:1:1.5 e/hypo/i.  In that small of a rxn you only need a balloon for containing the fumes.

[kris_1108]

Hi how are ya
It seems you have your head around the concept of reducing ephedrine/pseudo-ephedrine to methamphetamine, thats a great start. Some people here will try a reaction (with almost no understanding), fail a few times, and then learn how to do it properly!

1gm is possible; someones first few cooks may only yield 20% or 30%, and as experience and practice is gained, yields may increase to 60 70 (even 80%). So if you work with a larger amount of epehdrine (maybe 3gms or 5gms) you may have more success.
Its kinda like when you learn to butter a piece of toast, if the toast is 1" x 1" square then it will be difficult to paractice on.  But yeah if its bigger then it will be easier to work with.

If you want to use 30% hypo then you probably will need to reflux for a long time (like 12 or even 24hrs). Geezmeister and others would be the guys to help you with this one.

Vapour Containment Unit -  Its just to stop the smell. I think a balloon on top of the condenser should be ok for this... anyone else pull me up if this is not good (I know its ok with RP but I'm not sure if there's a difference with a hypo rxn). You wont need a face mask.

Recrystalisation is not neccessary, and on such a small amount you may find out you are left with almost nothing. After adding the HCl to the sep funnel and shaking, let a bit of the water out into a plactic cap or something, so you can test the pH. If it is still higher than 7, pour it back in to the sep, add a bit more acid, and shake again. REMEMBER - 1 drop of acid may change pH13 to ph12, but the same amount can change pH7.5 to something like pH4.5. The closer you get, the more sensitive it gets. If you're at pH8 or something you may want to add diluted acid; half acid and half water, so you dont over do it. When its ph7, drain the water/meth out on to your pyrex dish, and slowly evaporate the water to leave your meth behind, dont let the water boil.

A safety fan is just a fan that is aimed down on the evaporation dish to blow the fumes out of the way. When you are evaporating in alcohol, the fumes can be ignited by the flame heat source. The fan will just blow the fumes away so they dont linger and catch on fire. However, at the end of your cook, you will be evaporating in water so this wont be nedded.

[biotechdude]

"...Would only reducing 1gr of ephedrine easier for a newbee?..."

If you've got OTC ephedrine, i'd bump the reaction up to 5g+ (or 7).  This way, the visual indicators that happen in a hypo cook will actually bee noticable, and your work up will be much easier (as not trying to separtate 2 x 1mL layers or the like).

"...VPU..."

Vapour Containment Unit = Things that keep the smell local and out off the neighbours noses.  With larger quantities, this may mean working under a fume hood or using air purifiers or absorbing smells in kitty litter or coffee beans.  Or working in the middle of no-where... 

For your quantities, just make sure your doors are sealed and squeeze a balloon on the top of your flask/condenser so the HI gas doesn't escape and smell up the joint.  Then, make sure you keep your solvents lids on, and spray some toilet spray at the end.  For nano-scale; a mask isn't necessary IMHO (i'd bee more toxic walking in the city)...

"...SWIM read that higher concentration hypo will yield better results..."

IMvHO; concentrating the hypo just 'turbo-charges' its activity in HI production and I recycling.  This increases the rate of reaction (faster cook times).  This can bee good, however concentrated hypo can be very vigorous and not leave much room for error with a newbee.  Lastly, the 30% lg will work just the same; but longer cook times will bee necessary (but still faster than 90% of the other methods). 

To sumarise your remaining concerns Re concentrating/heating/fans - BASICALLY, flammable chems explode when they have an ignition source or they get to crowded (that they ignite themself!).  SO, if you were to concentrate hypo / heat alcohol...logic would suggest that an electric hotplate (non-sparking) and (safety) fan blowing across your work area would solve those two killer conundrums.

LATE EDIT - Sorry Kris; wasn't meaning to repeat u, after i posted your post showed up!

[livid]

Good info, but I feel you need more info to get this dream right. It would bee inappropriate for me to give hypo advice at this time.

[drjuiceflow]

Thanks for everyone's input.

SWIM will go for longer reflux(SWIM will try 24hr or maybe 36hr reflux). SWIM will use the 30% lab grade hypo. SWIM doesn't mind the longer cook times with 30% hypo, since as SWIM has been advised it will still do the job, but just take longer.

SWIM will use a balloon for vapor containment. SWIM will use regular balloon sold at department stores, unless any bee can suggest a better vapor containment unit that can be purchased from dept/chem supply store?

SWIM will stick to attempting to reduce 1gr of ephedrine to start with since it is safer. SWIM will not recrystallize as advised by kris_1108. SWIM will drain the solution to a Pyrex evaporation dish and place on a hotplate for evaporation.

[SHORTY]

I would not reflux more than 12 hours and keep the temp no higher than 120C with 110C being the target.

What makes hypo so much faster than rp is that rp will release hypophosphorous acid and phosphorous, phosphoric acids at a very slow rate in small amounts.  When using hypophosphorous acid you simply cut out the middle man.

I hope you are going to do an a/b before you evaporate.

[drjuiceflow]

1. How do you run ice water through the reflux condenser? I can run cold tap water from the tap by connecting the tubing from the condenser to the tap, but how would I make it ice water? I checked the multimedia reflux videos from Rhodium but none of them use ice water. Just cold tap water.

2. For the ice bath what is the difference between a:

a. ice cube+ water  icebath
b. ice cube+ acetone icebath? What is the ratio of acetone to ice? Do I also add water to this bath?

3. I want to get a digital PH meter. Will the ones that you can purchase for  use in swimming pools work fine for, or do I need one specifically for chemistry?


4. Will any adhesive tape suffice to secure the balloon(vapor containment) to the condenser? Can I double or triplewrap the balloons for extra strength, and to avoid any problems caused by a hole/rupture of one of the balloons ?


5. Also regarding shorty's comment, why is 110C the ideal temperature for this reflux?

6. What does the term a/b stand for ?

[kris_1108]

Hi
In answer to some of your q's;

1. If you want you can run ice water through a condenser with a fish tank water pump, and a bucket of cold water with ice in it. The pump will plug into your wall outlet, and hoses running from the bucket > pump > condenser > back to the bucket will recycle that water through the condenser.

2. Sorry dunno that one  

3. As long as the meter will read pH then you should be ok. I bought one for $AUD100, its not specifically for pools or chemistry but it works fine.

4. I think you could use electrical tape to secure the baloon to the condenser. I dont know much about holes or ruptures...

5. Dunno that one either...

6. A/B stands for Acid/Base. It is a method of extracting goods out of a solution by using a Base (sodium hydroxide) and an Acid (e.g. Hydrochloric/Muriatic acid). Read here

https://www.thevespiary.org/rhodium/Rhodium/chemistry/equipment/rextal.a-b.basics.html

[SHORTY]

Tap water will work fine as long as its not hot. 

If your balloons are thin then you can put 2 or 3 (inside each other)to make them thicker  and electrical tape works good to hold the balloon on.

[drjuiceflow]

Thanks for the advice guys. SWIM will try running cold tap water through the condenser first as SHORTY suggested, since SWIM doesn't have a fish tank pump. SWIM will invest in one if necessary later on, but SWIM will try just using cold tap water first.

In regards to the balloons SWIM will secure 3 balloons (within each other) with electrical tape. Since SWIM never attempted a nano-hypo cook before, SWIM hopes that the balloons will contain most of the odour. SWIM doesn't want to get detected. After all SWIM lives in an apartment complex.

SWIM was reading up on fume hoods, especially the ductless carbon-filtered fume hoods. Any bees ever use these? They would supposedly eliminate the odour/smell of the fumes, but it will not do anything for their toxicity?

Also should SWIM use a stirbar during the reflux?

[drjuiceflow]

Could the reduction in this nano hypo cook, be done if SWIM only reflux to 40-60C? Assuming the ratio of e/hypo/i are the same as discussed:

1. How many days will it take to reduce the ephedrine to meth if I reflux at 40-60C? About 7-14 days?

2. SWIM assumes by reducing the reflux temp, the reaction would be less volatile, and less fumes/toxins will be produced? Please correct SWIM if he is wrong.

[SHORTY]

1. How many days will it take to reduce the ephedrine to meth if I reflux at 40-60C? About 7-14 days?

My guess would bee that it would not fully reduce the ephedrine no matter how long you waited at those temps.  But i could bee wrong cause i never tried it.  If you do try it let us know how it goes.  Never know it could work.


2. SWIM assumes by reducing the reflux temp, the reaction would be less volatile, and less fumes/toxins will be produced? Please correct SWIM if he is wrong.
  
For the reaction you are planning there will not bee that many fumes/toxins to worry about.  Especially if you are using balloons to catch them.  It also will not bee volatile with 30% hypo and such a small rxn.

[kris_1108]

Hi
Well its good to see your are getting everything together. Wont bee long 'fore your ready to bubble!
Just one thing about the fumes, I understand that you are concerned for your safety (and secrecy). But once you have done a reduction you will realise that the fumes arent really that bad. The first time I done a dodgy test tube rxn, I would take the balloon off occasionly to see how much activity was going on in there, letting out smellable amounts of HI gas   . Yep I got a few whiffs by accident, and coughed a little bit. And then I was ok. And im still able to type this po........
COUGH!!
AAAAARRRRGH!!!!
OOOOOOAAAAAAHHHHHHH
OOHHHH NOOOO HEEEEEEEEELLLLPPPP!!!

haha naa just kidding  
anyway yeah im still here. So im just saying its good that you are concerned but dont let it fully stress you out cos its not that bad and you want to focus on the rxn.
Cool have fun
Seeya
Kris

[Osmium]

> How many days will it take to reduce the ephedrine to meth if I reflux at 40-60C?

How will the stuff reflux at 40°C?
Let me ask another question:
will the cake be done when I put it in the oven for 2 weeks at 40°C? (yes, it will be very "ripe"  
Or do I have to bake it for 90 minutes at 180°C? Can't I shorten this to 15 minutes at 380°C?

[drjuiceflow]

Point taken. Good analogy.

[SHORTY]

Although i don't think that it would work, i wouldn't compare it to a cake.  The ingredients of the cake would of course spoil or at least some of them would.  However, if the contents of a rxn were sealed in a flask at 40C for 2 weeks after which the temp was raised to the necessary levels for the required time then the end product would most likely bee the same as any other rxn with the same precursors. 

I wouldn't want to turn up the temp on an oven holding a cake mix that was 2 weeks old.

[Osmium]

Ephedrine in strong acidic environment will spoil too, that's where the P2P and naphtalene impurities encountered in rP/I2/H2O reactions come from.

[SHORTY]

If one were to put all the contents in a flask and sealed for 2 weeks at and then proceeded to reflux as usual?

How can you tell if your ephedrine is spoiled? 

Would boiling it in a solution of hcl(no HI) for a couple hours cause this to happen or would it take longer than that?

[energizer]

If you're looking for a heat source that you can hide, use an electric heating pad set on low. Fold a towel in half to get two layers between the reaction vessel and pad. You can stick the whole thing in a laundry basket, closet, wherever.  It keeps it about 95-105 degrees. Adjusting the towel will adjust your temp.