Author Topic: Hydriodic Acid--Step by Step Write-Up  (Read 17375 times)

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myles

  • Guest
thanks
« Reply #20 on: November 02, 2002, 09:25:00 PM »
Works well thank you for your help, from my friend of course.

The BEE game is why im here top score 300 points

mofessto

  • Guest
You Deserve a Medal!
« Reply #21 on: November 03, 2002, 05:06:00 PM »
Thank's alot Argox from a newbee information worth saving.

"For every second passing is yet another missed chance to turn it around"

Ph0enix

  • Guest
Where the F**K..
« Reply #22 on: November 04, 2002, 10:20:00 PM »
has this post been hiding?

Thank you Argox and I'm sorry to see this excellant post go so long before receiving the recognition it should have long ago (since February!?!)

Thanks again. :)

...though I know no one who employs such methodology it is quite obvious.
~PVnRT_NC8~

Rhodium

  • Guest
History of the thread
« Reply #23 on: November 05, 2002, 12:37:00 AM »
I moved it here from methods discourse recently, as I thought it really should be a sticky thread here instead.

It has also been present on MY PAGE for SEVERAL MONTHS - don't you people search there BEFORE asking things here?

shineon

  • Guest
could this help the bumping
« Reply #24 on: November 08, 2002, 07:48:00 PM »
by putting some broking glass or boilling stones in the reaction,

12345x

  • Guest
57% stabilized....
« Reply #25 on: November 21, 2002, 06:03:00 AM »
in the old days one would buy HI
at the store as 57% stabilized
the fine print would say stabilized with phosphorous acid

now if you heat 46 ml of water
then add some rp "say 20 gms or more"
then add 57 gms of iodine.
and boil for a few min's

and when its a clear color.
you filter out the remaining rp
your liquid is apx 108 gms of 57% HI in water
with apx 8 gms of phosphorous acid."thats what the rp thats used
gets turned into"


now dont you think this is how it was made
when they sold it at chem supply stores?

honeysmoker

  • Guest
IMPRESSIVE
« Reply #26 on: January 04, 2003, 02:49:00 AM »
A+++ Quick witted, knowledgeable, Mature. Would read a post from this man again.  Good communication.  A++++++++++
No bull shit could be detected.


(attempted Hive/E-bay rating)

HS

Rhodium

  • Guest
New ways for making HI
« Reply #27 on: January 17, 2003, 12:58:00 PM »
Hydriodic acid from Iodine, Water and Sodium Sulfite

Na2SO3 + H2O + I2 -> 2 HI + Na2SO4

Six parts crystalline sodium sulfite, one part water and three parts iodine (by weight)
is heated together in a flask, gaseous HI is formed together with solid sodium sulfate.

Ref: Philosophical Magazine [3] 35, 345; Jahresbericht ueber die Fortschritte der Chemie 253 (1849)

Hydriodic acid from Iodine, Water, Barium Oxide and Sulfur Dioxide

BaO2 + I2 -> BaI2 + O2
BaI2 + I2 + SO2 + 2 H2O -> BaSO4 + 4 HI

Ref: Comptes Rendus 142, 279; Chemisches Centralblatt I, 732 (1906)

The above preparation methods and many others can be found in

Gmelins Handbuch Der Anorganische Chemie (1909)

(https://www.thevespiary.org/rhodium/Rhodium/djvu/hydriodic.gmelin.djvu)
To view the DejaVu file, you need a browser plugin from

http://www.lizardtech.com/download/


ahgreich

  • Guest
Riddle me this...
« Reply #28 on: March 17, 2003, 08:26:00 PM »
Following Rhodium's last post as a very general guideline, SWIM put around 1/2 cm sodium sulfite in a test tube. Immediately topping it with around 1 gm of dirty pfed fb. a squirt of dh20, and, topped the cake with a slug of I2, approximating the ratios from the previous post.
Taped a punch baloon condensor on the end just in case.
manually placed end of test tube over hot plate on high, jiggling it gently to coax the reagents to mingle.
As soon as the I2 made it through the pfed layer, BANG! instant purple gooness that SWIM assumes is iodopseudo gunked the sides as in a small rp/i type event. Excitement.
Kept heating and gently jiggling the tube, iodo slime was quickly replaced with pale yellow sun goldenness, no I2 visible.
plug of sodium sulfite at the hind end of the tube made a  workup attempt seem unfair and not worth SWIM's time. Removal of said condensor and proximal nasal inspection was most unpleasantly harsh, though no visible smoke the duration of the reaction or post reaction.

Does anyone want to venture an explanation?
Could this have been The Stuff?!?

fierceness

  • Guest
Rhodium, could one use this as a RP substitute
« Reply #29 on: March 17, 2003, 08:41:00 PM »
Rhodium, could one use this as a RP substitute almost by performing an in situ production of HI?

Sodium Sulfite is very OTC here.. perhaps a suggested experimental for this in situ synth is the following (please correct any errors):

6g freebase pseudo + 8mL H2O + 12g Sodium Sulfite + 6g I2 combined in a small flask and refluxed for 6-12hrs... workup as per usual

Anyone see anything wrong with this before SWIF attempts it?

Rhodium

  • Guest
Old refs
« Reply #30 on: March 18, 2003, 03:39:00 PM »
One problem would be that you wouldn't get a solution with so much reagents in so little water, but rather a paste...

Also note that the above references are 100-150 years old, so you might have to research the topic a little bit further before actually using it in a synthesis, unless you have analytic equipment.

fierceness

  • Guest
hmm
« Reply #31 on: March 18, 2003, 04:57:00 PM »
ahh, true.. and adding more water would decrease the concentration of HI too low to actually reduce the pseudo.. what about substituting acetic acid for water, or using a 50/50 mix of water and acetic acid, since using acetic acid is supposed to increase the concentration of HI...

is there any way this could work?  swif is certainly willing to test this out with his reagents

I think he will just add the ingredients all dry and add enough water to give it the ability to actually reflux

Scottydog

  • Guest
Highly Intriguing
« Reply #32 on: March 18, 2003, 05:41:00 PM »
Highly intriguing info Rhodium! The ideas never cease.

Considering that what is being produced here is anhydrous sodium sulfate and HI. According to chemfinder, Na2SO4 has a melting point of an astronomical 884 degrees C. This HI could be essentially driven into a 2nd flask of h20 until a 57% solution is obtained and then this 57% HI solution used in excess (molar ratio of 4HI: 1 pseudo) and refluxed for a day to get golden gear?

Considering that Na2SO4 can withstand the outrageous 884 deg C, high temp does not seem to bee an issue.

So basically this Na2SO3/I2/h20 mixture is heated until all signs of moisture is gone. When the h20 is gone all HI has been formed? This combo can be constantly replenished until the 57% strength is reached?

With sodium sulfite available at approx $60 for 2.5kg and the same amount of KI for under $300, theoretically, HI has never been cheaper?  ;)

Thanks much...
___________
Refuse/Resist

fierceness

  • Guest
ahh! thanks scotty.. i was looking for the...
« Reply #33 on: March 18, 2003, 05:47:00 PM »
ahh! thanks scotty.. i was looking for the ratio needed for HI to reduce pseudo w/out red phos.. better yet, you could distill out the HI as you say, and reflux with pseudo and some more sodium sulfite.. the sodium sulfite should recycle the iodine as red phos does, right? then you wouldn't need quite as much HI..

swif is still going to attempt it was a straight RP substitute.. he's going to wet it enough to get a reflux going and reflux it for 6 hrs and see if it worked...

I'm still curious about the acetic acid thing.. i wonder if it would improve anything?

fierceness

  • Guest
another idea... crystallization
« Reply #34 on: March 18, 2003, 05:55:00 PM »
here's another idea.. i dont fully understand the theory of crystallization, so this idea may be stupid, but I thought i'd throw it out there anyway...

Ratio of 6:2:3 sodium sulfite:water:iodine

I double the amount of water so that we get an approximate 50% of HI in solution.. now, can one drop the temperature of the solution just above freezing to try to crystallize out the sodium sulfate and then filter it leaving HI?

Maybe swif should just try these ideas out instead of asking all the time.. he just doesn't want to inadvertantly create an explosion or some kind of toxic gas (other than HI, of course)

fierceness

  • Guest
TFSE findings
« Reply #35 on: March 18, 2003, 07:20:00 PM »
Scotty, there is a chance that your 1:4 ratio is flawed...
Check out

Post 386152 (missing)

(Rhodium: "57% HI", Stimulants)
  the whole thread.. specifically that one and this one

Post 392251 (missing)

(WizardX: "The problem is the HI dissociation.", Stimulants)


will a 4:1 ratio of HI with no recycling agent (RP) be enough to reduce pseudo to meth in a 12hr reflux?

fierceness

  • Guest
Little experiment
« Reply #36 on: March 18, 2003, 08:40:00 PM »
swif did a little experiment to see what the rxn contents woudl look like at a 6:3:2:2 ratio (Na Sulfite: I2: H20: pseudo)

The reaction contents looked somewhat like the old days of the 'dry' push/pull reactions.. there was a definite liquid portion, and also an insoluble portion (the I2, i assume).. it *Definitely* made HI with little or no heat at all...

swif did not want to continue any furthre, though without some comments here.. there is no way that H2S will be produced by this is there?  swif would rather not have hydrogen sulfide poisoning..

Anyway, my point is that even though the 'paste' is not completely a solution, it is possible that this method will work, as he has seen it work in the 'dry' runs.. swif will try this again, as soon as someone convinces me that H2S will not be a problem..

At least HI was definitely made with ease! just double the water and use stirring or swirling if possible... however, scotty's suggestion of piping the HI(g) to a flask of water may not be a bad idea either..

I feel bad for seemingly cluttering this thread -- If you guys feel i should start another one for this, please let me know :)

ahgreich

  • Guest
assumptions about HI concentration...
« Reply #37 on: March 18, 2003, 11:01:00 PM »
In Swim's unschooled mind, he was thinking that keeping the dH20 volume very low (just enough to moisten the sodium sulfite), that the HI would a) be a free gas in the tube and 2) as heat was applied, the vapors formed would be very highly concentrated HI aq???
Also, he was thinking that since Pfed FB was used, no HCL to remove, instant iodopseudo, shortening reaction time?
total time for the entire experiment was less than 5 minutes, from raw pfed fb - > iodo - > ?? (pale yellow something on sides of tube). No I2 visible at finish.

fierceness

  • Guest
the pale yellow was probably HI(aq)..
« Reply #38 on: March 19, 2003, 01:36:00 PM »
the pale yellow was probably HI(aq).. however, HI as a gas does NOT reduce pseudo.. you need the 57% solution at reflux to efficiently reduce pseudo... see the stimulants FAQ posts by Osmium to confirm this..

The fact that you saw a lot of gas means that you weren't really reducing much.. the little bit of water that you added dissolved as much HI as it could (hence the yellow color)..

amalgum

  • Guest
HI
« Reply #39 on: March 21, 2003, 09:35:00 AM »
Well hell yeah!  Could this make rp obsolete?  SWIM was finishing up a good ol' rp/I2 reaction when SWIM read this, so after hitting a tester of the finished product, SWIM went and searched through an old box of chemicals that was laying around.  Low and behold, SWIM came across a big bottle of sodium sulfite.

To test the theory, SWIM placed a little iodine in a beaker.  Then some of the anhydrous NaSO3 was thrown on top.  The two dry chemicals were mixed, with no apparent rxn.  SWIM then went to add the water required to facilitate the rxn, and accidently added what looked like probably too much.  SWIM swirled the beaker contents around a little, and it appeared that only about 1/8-1/4 of the total amount of NaSO3 dissolved making the solution yellow.  The rest stayed at the bottom, along with the iodine.  Nothing was happening.  Since SWIM only added a little bit of iodine and a lot of NaSO3, SWIM added more iodine.  Swirled the shit around, still nothing.  "Fuck it", SWIM thought, "maybe it just needs a little energy, one last try".  SO SWIM placed the beaker on the stove burner and turned it on to about 3/4 power.  There wasn't much in the beaker, so it only took about a minute to begin to boil.  When this happened SWIM took the beaker off the stove (it was soft glass, didn't want to crack it), and swirled it around.  This time, as soon as SWIM began to swirl, all of the iodine instantly dissolved, and it looked like about 90% of the NaSO3 dissolved.  Then a wonderfull thing happened.  Even though there was quite a bit of water, it began to smoke.  That white smoke looked awfully good and familiar, and upon a quick wafting of the vapour from the beaker to SWIM's nostril, the umistakable smell of HI was detected.  "Hey this smells like the damn rxn SWIM just ran with the rp", SWIM thought.

So, basically, as soon as SWIM's friends uncles dad gets some more pseudo, this rxn will be tested.  Let me get some things straight first.

Is the eqaution like this?:
1NaSO3 + 1H2O + 1I2----->2HI + 1NaSO4

If so, this is what SWIM came up with:
Since a double molar amount of HI is needed to reduce e fully to methamphetamine, SWIM calculated a test reaction ran with four grams e.  If the equation of the HI rxn is as above, then that means SWIM would technically need an equalmolar amount of NaSO3 to ephedrine (since double the molar amount of HI is produced).  For four grams e HCl, that would mean about 2.5g of NaSO3 is needed (which a slight excess, like 2.7-2.8g is actually used to try to make up for effeceincy losses, and recycle most of left over iodine). As far as iodine goes, again an equalmolar amount is needed.  That would mean about 5g of iodine is needed.  No excess of iodine is needed, in fact SWIM figures one might get away with using less than an equalmolar amount of iodine, because I2 is reformed when HI reacts with the iodometh (technically, you could get away with adding a little over half an equalmolar amount SWIM guesses, because the half would be enough to turn all e into iodometh, and the slight excess to make enough HI to start reducing the iodometh to I2 and meth, which the I2 is reused, but for a first time SWIM doesn't wanna take that chance). Now the reaction is gonna need some water to start.  Since SWIM figures that an equalmolar amount (to the e) of water is produced after it all gets turned into iodometh, only half of the H2O needed to produce the required HI will be added.  SWIM doesn't want to add less than that for fear that their might not be enough, because there would be enough to get it started, but not enough is produced to finish the rxn.  SWIM doesn't want to add more becuase of the nature of this type of rxn.  So basically, a half molar amount of water (again to the e) is used, which is about 400mg, or .4g, or about half a milliliter.  First E and I2 will be mixed dry in the rxn vessel, then the H2O will be added.  After it's mixed well, the NaSO3 will be added, and the rxn vessel closed up like in a typical rp/I2 rxn (unless of course your using an open vessel and condensor).  The four reagents will be mixed well, and then heated enough to start the rxn.  Rxn will pretty much be treated like a regular rp/I2 rxn, keeping a close eye on the rxn clues of course (so one could work out proper rxn times, etc).  When done, water will be added to the contents, and pour into a pestle and mortar.  All the NaSO4 that is present will be crushed under the water as fine as possible.  The rxn matrix will then be filtered, and the NaSO4 washed with a little extra water.  Then workup will proceed on the rxn matrix as normally done.  Washing the solution before basification of course to help get rid of extra iodine if so present.

SWIM knows it is a long post, but what do some of your guys think?  It's definitely worth a try!