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Rhodium
(Chief Bee)
08-10-02 05:22
No 344011
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Recycling
of HI + new RP substitute
(Rated as: excellent)
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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 phosphoric 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.
Reference:
Org.
Proc. Res. Dev., Vol 3, No 5, 352-356 (1999)
(http://www.rhodium.ws/pdf/hydriodic.recovery.pdf)
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foxy2
(Distinctive Doe)
08-10-02 05:34
No 344014
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They
didn't schedule it cause nobody knew.
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I have
never heard of anyone using phosphorous acid for this purpose before, have I
missed something or is this a completely novel idea?
Yes its novel. I don't know of anyone who has used it.
But I do know someone who has seen various references analogous to the one
you posted. They were going to try it sometime. 
Rhodium
You just opened the floodgates!!!
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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lugh
(Moderator)
08-10-02 05:43
No 344017
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Differences
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Note that the researchers used two Freidrichs condensers to control the very
exothermic reaction, and that a nitrogen atmosphere was used 
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foxy2
(Distinctive Doe)
08-10-02 06:01
No 344019
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hehehe
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Now that I ask him, my friend had that ref. and this patent.
They are pretty much the same.
Patent US5516960
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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wareami
(Hive Addict)
08-10-02 06:14
No 344023
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LughLughLugh!
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Lugh:Always bursting my balloon with exothermic atmospheric considerations!
Rhodium:Thanx for checking into this route. Ibee had run into some facts
while researching a post by aquagirl in AquisitionForum regarding List
Schedules of HypoPhos!
It was unclear as to whether aqueous phosphorous acid had the properties
necessary for a reduction.
He's tried researching the chemistry books available at the time and only
came up with info related to the differences between Phosphorus and
Phosphrous.
I also believe Scottydog had inquired through PM about phosphorous acid a
while back, but in Ibee's mind...Geez, Mnkyboy, and WizardX were the experts
concerning the phosphoric routes!
Foxy2:Yes! I believe SWIF2 might be right about the Floodgates!
Peace of
the reaction
Have FUN-Bee SAFE
Everything
Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt
ô¿ôWareami
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morpheus
(Hive Bee)
08-10-02 13:51
No 344119
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recycling
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Five stars Rhodium!
Guess it shows why your chief bee
My nomination for my newly created 2002
Avagadro award goes to you.
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Psalty
(Stranger)
08-10-02 15:09
No 344153
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This
would be significantly more OTC than rp or ...
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This would be significantly more OTC than rp or hypo. A quick search of
phosphorous acid sources reveils that its potassium salts are used in
fertilizers as an alternative to phosphates in NPK formulations. Having
one less oxygen molecule than phosphate, phosphite has a much higher degree
of solubility and mobility in the membranes of plant foliage and roots,
making it more readily absorbed by plants. Hmm... Looks like yet
another fertilizer may be stigmatized by its clandenstine uses.
The
true danger is when liberty is nibbled away, for expedients. (Edmund
Burke)
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Rhodium
(Chief Bee)
08-10-02 16:40
No 344180
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The
meth bunny
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That sounds really good. As no iodine is ever consumed in this reaction (only
converted into iodide), it can be recycled indefinitely by the aid of
hydrogen peroxide oxidation of the aqueous mother liquors gotten after
extracting your product.
If Phosphorous acid salts are as abundant as you say, this invention can
really become a perpetuum mobile of meth synths.
More Phosphorous acid info: http://www.biagro.com/chemdiff/
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BenWiFFen
(Line Monitor)
08-10-02 17:00
No 344185
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Close
but no...
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BenWiFFen: ""EVERYMAN's" HI"
(Newbee Forum) Close but no doobee.
Sign
here____________________
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Scottydog
(Hive Bee)
08-10-02 18:59
No 344221
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Swis
may be wrong as usual but in other words, ...
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Swis may be wrong as usual but in other words, the lower voltage electrolysis
application that hypo was discussing at the end of Lugh's thread lugh: "Hypophosphoric Acid Synthesis" (Acquisition
Forum) might have functionality as a starting point to obtain the
necessary phosphorous acid?
In this thread Swis asked if HCL could be used as an electrolyte and Hypo
said it would result in phosphoric acid. Will phosphoric work as well as the phosphorous
acid? Are they one and the same and if not can someone please explain the
difference? It would be so beautiful to start from scratch. (Electrolysis)
For fun and education sake.
Considering this acid is not regulated, Swis understands that this caveman
electrolysis is not totally necessary.
Using the low voltage electrolysis and a dilute solution of H2SO4 as the
electrolyte, Hypo says that the end result would also contain hypophosphorous
acid. Would the small amount of hypo acid interfere with using H3PO3 as the
recyclant in this newly revealed process or would it further help in the
reduction?
Swis likes to turn a molehill into a mountain. So much info to ingest
that Swis' brain is about to explode.
It is obviously easier to just buy the H3PO3. On another note Swis notices
this method calls for the addition of water. H3PO3 comes available in
solution in concentrations listed at 85%/15% water. Can this theoretically be
used "as is" without actually adding h2O to the mix? Is Swis on
track or is he still confused
by the ic/ous endings? God its getting deep around here.
Forever learning! Thanks Rhodium...
___________
Refuse/Resist
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PrimoPyro
(Hive Prodigy)
08-10-02 19:09
No 344224
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Buy
It
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Just buy the acid while its available. It isnt expensive.
You might get confused on the ic/ous endings because lots of people fuck them
up and state them wrong. There are no such things as hypo_______ic acids or
per______ous acids.
From lowest oxidation state to highest, the possibilities are:
Hypo______ous acid
______ous acid
______ic acid
Per______ic acid
So for chlorine oxyacids, you have hypochlorous acid, HOCl, chlorous acid,
HOClO (or HClO2), chloric acid, HOClO2 (or HClO3) and perchloric acid, HOClO3
(or HClO4)
Just about always (I cant think of a single exception, but Im covering my ass
anyway) the number of hydrogens stays the same for all oxyacids of the same
central species, only the number of oxygens vary. Ah, one exception would be
hyponitrous acid, there.
PrimoPyro
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blondie
(Hive Bee)
08-10-02 19:49
No 344236
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phosphorous
acid
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if the salt was available how would you go to the acid?
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foxy2
(Distinctive Doe)
08-10-02 20:20
No 344255
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Coming
Soon
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Hold tight blondie.
It will either bee here soon or really early in the morning tomorrow.
The salt is WIDELY available right now. Pick up a 55gallon barrel while
you can.
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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wareami
(Hive Addict)
08-10-02 20:36
No 344263
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ESEE
description!
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Scotty: The easiest description in the difference between the spelling
suffixes...-us and the -ous is:
The element ends in -us and the +3 compounds end in -ous.
Chemical Principals and
Properties Second Edition
Peaceof
the reaction
Have FUN-Bee SAFE
Everything
Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt
ô¿ôWareami
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Psalty
(Stranger)
08-10-02 20:36
No 344264
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Titrate
your salt with a strong acid, such as ...
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Titrate your salt with a strong acid, such as HCl, to convert back to the
acid.
KH2PO3 + HCl --->
KCl + H3PO3
pKa =
-7
pKa = 1.5
Separating the KCl from the H3PO3 wouldn't be to difficult. H3PO3 is
very soluble in EtOH but KCl is considered insoluble in EtOH. So, one
could boil of the water after the titration, add EtOH to the solid mass, stir
vigorously, and then decant the supernatant leaving the KCl behind.
Alternatively, one could perhaps exploit the great differences in the melting
points of KCl and H3PO3. KCl melts at >700C while H3PO3 melts at
around 74.7C. You could heat the solid until the H3PO3 melts and then
remove the liquid H3PO3 somehow. Someone please correct me if I'm
wrong, or if these procedures have some inherent danger that I omitted.
The
true danger is when liberty is nibbled away, for expedients. (Edmund
Burke)
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foxy2
(Distinctive Doe)
08-10-02 22:27
No 344275
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Salty
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Your a bright cookie. And a smart chemist to.
The only possible problem might bee the inerts which are bound to bee in
fertilizer grade KH2PO3. I wonder what those inerts would typically
bee?
o-Phosphorous Acid - MSDS DATA (100%)
B.P. Text: 392F,200C
M.P/F.P Text: 165F,74C
Spec Gravity: 1.7
Solubility in Water: 30%
Appearance and Odor: WHITE OR YELLOWISH HYGROSCOPIC CRYSTALLINE MASS.
Stability Condition To Avoid: FLAMMABLE, POISONOUS GASES MAY ACCUMULATE IN
TANKS AND HOPPER CARS.
Materials To Avoid: VIOLENT RXN W/BASES &/OR OXIDIZERS. REACTS
EXOTHERMICALLY W/WATER. CONT W/ACETIC ACID RELS FLAMM PHOSPHINE. (ING 2)
Hazardous Decomposition Products: THERMAL DECOMP PROD INCLUDE HIGHLY TOXIC
OXIDES OF PHOSHOROUS, FLAMM HYDROGEN AND PHOSPHINE GASES.
Handling and Storage Precautions: MAY BURN BUT DOES NOT IGNITE READILY.
FLAMMABLE, POISONOUS GASES MAY ACCUMULATE IN TANKS AND HOPPER CARS.
Other Precautions: MAY IGNITE COMBUSTIBLES (WOOD, PAPER, OIL, ETC).
http://www.setonresourcecenter.com/HMIS_Msds/096/BNBGF.HTM
Someone want to get this Journal Article, I don't have access to this
one. Its a review of the preparation and reactions of H3PO3 and H3PO2.
Tervalent phosphorus acids.
Dahl, O.
Organophosphorus Chem. (1991), 22 87-113. ISSN:0306-0713.
Abstract
A review contg. 97 refs.
Those
who give up essential liberties for temporary safety deserve neither liberty
nor safety
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PrimoPyro
(Hive Prodigy)
08-10-02 22:40
No 344277
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Man.....
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I find myself recommending chemical suppliers more and more and more lately
to people struggling with scraping chemicals from OTC sources and wondering
wtf is in them.
This chemical is not illegal, not watched, and is relatively inexpensive. On
top of that, you know some good reasons it's used for in case someone were
nosy enough to ask. What is holding you back from just calling up a chemi
company and ordering a 1kg "sample" followed by a 10kg order for
your crops?
If they want you to set up some sort of account, do it, its almost always
free. Fuck, its so easy I cant stress how easy it is with words. And once you
have an account set up, the only question you'll ever get when you make an
order is, "Do you have an account with us, Sir?" And you just say
yes, it is under ____ ____.
Whatever accounts you set up will be for NONSUSPICIOUS chemicals, though. You
buy your suspicious chems with a Fake ID and an Anonymous Credit Card, a la
MaDMAx. (UTSE)
Trust me, its easy as pie, and you'll get so much better results.
PrimoPyro
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