Here is an example from none other than the good man Rhodium at the best place on earth:

quote:

(From The Hive)

Rhodium

(Chief Bee)

08-10-02 08:22

No 344011

Recycling of HI + new RP substitute

(Rated as: excellent) Bookmark Reply

Here is a document which goes into detail on how to sustain a HI reduction of alcohols with continous recycling of formed I2 back to HI, using aqueous phosphorous acid (H3PO3) as recycling agent instead of the watched Red Phosphorus/Hypophosphorus Acid.

I have never heard of anyone using phosphorous acid for this purpose before, have I missed something or is this a completely novel idea? H3PO3 costs only around $40/kg, but it does not readily regenerate HI from I2 at room temperature (but easily at the boiling point of an aqueous solution), and I believe that is the reason they have forgotten to schedule it, its functionality is not directly obvious to non-chemist meth cooks, and therefore its popularity has been as low as not alerting the DEA, and they most likely didn't think of it either.

Partial reactions

Ephedrine + 2 HI -> I2 + H2O + Meth

H3PO3 + H2O + I2 -> 2 HI + H3PO4

Overall reaction

Ephedrine + H3PO3 --I2--> H3PO4 + Meth

The overall reaction is simply phosphorous acid being oxidized to phosphoric acid and Ephedrine reduced to Meth, while any added HI or I2 is just recycled in the reaction.

Their preferred molar ratio between ephedrine/HI/H3PO3 is 6:9:5, and with their molar weights being 165.24:127.9:82.0 (ephedrine considered freebase and HI a 57% solution), the mass ratios are the following:

9.9g Ephedrine freebase

20.2g 57% HI(aq)

4.1g H3PO3

If you want to use I2 instead of 57% HI, use the amounts below:

9.9g Ephedrine freebase

10ml Water

11.4g Lab Grade I2

11.5g H3PO3



Experimental suggestion:

In a 250ml Round-bottomed flask with a 24/40 ground glass neck, carefully add the phosphorous acid with good stirring to the water (exothermic!), then the finely powdered lab grade I2 is added, followed by the ephedrine freebase. The flask is fitted with two sequential Friedrich condensers with ice water running through them to compensate for the vigour of the following reaction.

With good stirring, the reaction mixture is placed in an oil bath (or heating mantle) and slowly heated to reflux temperature with vigorous magnetic stirring. At about 100°C a powerful exothermic reaction sets in and frothing commences, and after a while you will attain the reflux temperature of ~118°C. The reaction mixture was refluxed overnight, cooled and worked up as usual.



Phosphorous Oxyacids

Reference:

Org. Proc. Res. Dev., Vol 3, No 5, 352-356 (1999) (http://www.rhodium.ws/pdf/hydriodic.recovery.pdf)



There is a ton of info on H3PO3 as recyclant/HI producer at The Hive. Good luck. SWIM might give this a whirl himself.

Mad where the Hell have you been Bro?!

Good luck buying some.



Jam.

Jam.





[This message has been edited by Jamiroquai (edited 11-30-2003).]

white flakes fertilizer

or phosphoric +ki

are one way but there are many less obvious routes as well--so I hear



[This message has been edited by dan46 (edited 12-19-2003).]

i have a quick question on this method... in essence, it is the same as the rp/i method, but with h3po3 "replacing" rp? this method sounds like it may be worth looking in to.

Yes. It replicates the action of red phosphorus. If you can find it and it is indeed out there, it(phosphorus acid flakes) is going for around $60-90 per 500 grams.

Imagine the free time surplused from not having to catch:"match-scra tch-fever"!!!



Jam.

thanks for clearing that up... looks like the "plan" needs to be reformulated now, and we can get the project up and running by christmas... oops, did i say we?

Hop on board Diasaster!!

The trains bout to leave and I wouldn't count on another coming this way again!!

He who hesitates........masterbates!!!



Jam.

SWIM has seen other people put the flakes in water and injecting the solution into the flask. SWIM has heard of people just putting the flakes in the flask (no water) and proceeding as usual. So now SWIM's question is should one add water or not to flakes?

quote:Originally posted by Uncle Bill:

SWIM has seen other people put the flakes in water and injecting the solution into the flask. SWIM has heard of people just putting the flakes in the flask (no water) and proceeding as usual. So now SWIM's question is should one add water or not to flakes?

Att. Jam... SWIM second's that question??? Thank's "Peace-out!"

Jam:

Been busy lately so not much time has been spent online. As soon as SWIM gets to get settled in at the new site, expect that PM.

Also, over a pound of rp substitute for under $100 bucks makes SWIM a helluva lot more interested in HI reductions again. However, if it's a place where it has to be mail ordered from, SWIM might not like it too much. SWIM is really leary about mail ordering anything related to this. However interest is still there. Now a better pseudo source/synthesis would be icing on the cake!

UncleBill and dragonman:

SWIM is a little confused by the way you worded that question, so SWIM will try as best as he understands to answer.

If a solution of 57%HI and pseudo is added to H3PO3, then no additional H2O is needed.

If I2 is used for insitu HI production, as long as H3PO3 is being used (not H3PO2, SWIM is unsure of that mechanism nor wants to take the time to speculate about it, just know that hypo or H3PO2 and H3PO3 are different acids), H2O is needed.

One cannot proceed by adding H3PO3, I2, and pseudo to a flask. No reaction will occur (if reagents were totally anhydrous, I2 esp. homemade can carry a lot of H2O with it). The H3PO3 needs H2O to make HI from I2.

1H20 + 1H3PO3 + 1I2------>1H3PO4 + 2HI

H3PO3 steals the oxygen from the H2O and becomes H3PO4, the left over hydrogen reacts with iodine, producing the HI.

Depending on availability and suspiciousness of buying H3PO3, as said in other thread a fungacidal phosphite foliar spray should be very easy to find at appropriate location. These are solutions of K2HPO3 and KH2PO3. Reaction with HCl acid and evaporation gives mix of KCl and H3PO3. Extract H3PO3 from KCl crushing result and mixing with boiling methanol. Cool to rt, filter out KCl. Evaporate yeilding the acid.

phosphorus and hypophosphorus are both WATCHED -in most cases

However, if I am not mistaken, there is phosphorus flakes in many ferts that can be bought and modded for not much cas



[This message has been edited by dan46 (edited 12-07-2003).]

[This message has been edited by dan46 (edited 12-19-2003).]

[This message has been edited by Jamiroquai (edited 12-04-2003).]

There are an infinate amount of ways to produce HI

Many are very ,very otc

[This message has been edited by dan46 (edited 12-19-2003).]

Delivery Status Notification (Failure)Delivery to the following recipients failed. 46

foursix

method@dan46 Jam --you should pm me or let me know when chemhead is up





Jam

hushmail.com?

water keyboard shorting out cant type no keyboard having to copy and paste words

so I can communicate at least until tommorrow



Jam

jam

my email is available as I have nothing to hide

I only cook a good meatloaf but aspire to become a culinary pro

[This message has been edited by dan46 (edited 12-07-2003).]

[This message has been edited by dan46 (edited 12-19-2003).]

I remember, Jam, a few months ago when you wrote up the post about the new way to go and I thank you so much for that info. I have always paid attention to your threads from along time ago when you wrote up the a/b

exractions for everyone. Excellent to say the least. As soon as your post about the flakes was typed, I quickly put this info in the Bible of Knowledge, and I'm glad I did because later on you removed it from flak from somebody. You were right about everything from money orders to asking no questions, and all would turn out fine. It did!!! Thanks Jam, I hated cleaning those damn matches anyway! Peace and Merry Christmas

Merry Christmas

quote:Originally posted by dan46:

jam

you can reach me -NOW- but keep trying as the darned ziplip keeps filling-up with hundreds of ms/ microsoft spam

otherwise, you should have no problem as I clean it out as often as possible

[This message has been edited by dan46 (edited 12-07-2003).]



I keep trying but Delivery Status Notification (Failure)keeps automatically generated

Jam