H3PO3 "TO" Hell in a hand basket...

[greensleeves]

First let me say that none of what you read in this post is true. It's all made up to impress a bunch of people I never met. In fact someone I never met dreamed it all...

                     SWIGS told me he had a weird dream one night and this is how it went.
     He started with 10pkg's 48ct generic white 60's and used "a novel extraction technique by SWIVE" to get pure pseudo for  an H3PO3/I/E/DH20 rxn. SWIGS noticed when purchasing said pills that there was a new inactive on the list: (Hypromellose) he paid little attention to it...Rookie mistake...He extracted 21gms of a possible 28.8 Not too bad for a rookie BUT as most of you already know there was evil lurking in that sparkly clean pseudo. After he did his extraction he left his feedstock to dry for a couple days before he "tried" to react it.
     The big day finally came and SWIGS says his dream went on for about an hour before getting his presto oilbath meth maker set up and adjusted correctly. He dreamt of a 250ml rbf popped through a piece of 1/4" plexi-glass with appropriate holes drilled for zip-ties (to hold the flask) and candy therm. Then the whole mess was topped off with a 200mm WatEr cooled condenSer Then a punch-ball baloon.
     The dream took a strange turn when 18ml of DH20 was added to the flask at room temp. 23gms of H3PO3 was then added to the DH20 and stirred with a wooden stirring implement (a stick).  Then 24gms LGI2 was added...ooopsie! Forgot to crush that I2 SWIGS wonders will it matter? Probably not as much as the slight M.E.K. smell in the pseudo 21gms he just added.
     SWIGS then says that in this dream he stirred all the added chems till it resembled something hacked up by a 20 yr smoker. He then brought up the heat slowly but surely in about an hour to (oilbath temp) 100° C where he was under the impression that some type of quick violent rxn was supposed to take place, he was counting on this rxn to tell him when the inner flask temp hit 80° C so he would have an idea of what the temp was inside that flask. Since that said rxn NEVER happened SWIGS kept jacking up the temp thinking that the temp difference must bee the problem....WRONG-OH!  The temp went up and up and up to 170° C and even higher...ooops. Is that covert military tree-people I hear??? Oh I think it is...
     OOOOOOver the next hour the mist that came up from the rxn fluid condensed at about half way up the condenser and had an orangish clear color... strangely enough not thought of as significant at this point by GREENHORN The reflux began to move up the condenser to almost the top. SWIGS had a thought...UH-OH...Perhaps the heat is too high...but the rxn hasn't occurred...hmmm something must bee wrong. In fact something had been wrong for quite some time it just went unnoticed by SWIGS's newbee eyes. In the next hour the rxn fluid was observed as being red...blood red...the droplets falling from the end of the condenser appeared as cough syrupy looking schmegma. SWIGS thought "Dammitt! Something ain't kosher in Denmark!"
     SWIGS was right, there were some turnips on the meat fork. SWIGS dreamt that he turned the heat down and let the concoction ride for about 4 more hours at 140-150° C (Oil bath temp.)  When at last SWIGS gave up the ghost...the rxn fluid was observed as being blood red in color and rather thick and gelatinous. SWIGS turned on the good ol' Fuck-it switch and performed a holy shit, it's fucked anyway, so let's hurry through and find out if there's gonna at least bee a good high in it, friggin' redneck crack-ho EXTRACTION. The heat was turned off and the rxn allowed to cool to about 125° C.
     To the rxn was then added 3 volumes of DH20 equal to 60ml. The rxn fluid was observed as being murky-orange...barely translucent...It was then washed with 200ml of xylene for about 5 minutes then again...then again.  The xylene was observed as being yellow like too much vitamin piss yellow.
     The rxn fluid was then based with a 20% NAOH solution...and based and based and based, Some orange/amber colored globules were seen racing out of the solution toward the bottom...I'm not sure what the PH was at.   So here's when the rdneck crack-ho extraction kicked in...The rxn fluid wasn't all milky white it was about half-way milky white...fresh np was added in about an equal portion then blah blah blah water then blah blah blah 31%HCL then blah blah blah shake da fuck outta it then blah blah blah sep, evap acetone crash sm0okey sm0okey, snorty snorty Holy fucky is that C.M.T.P. AND voices in the other room blah blah blah....wheeeew!
     Three days later the rxn fluid was titrated again and 6 more gms of half reduced backache makin' tweek yer balls off white powdery shit was yielded.
                                       THE END
Thanx to everyone who didn't contribute to this dream that was dreamed by someone whom I never met, in a world far and long frome here in a universe that never existed.

?'s
1) What the hell caused this rxn to turn red?

2) Are the ratio's screwed up or just plain wrong?
Thanks SWIGeez

3) What the hell is hypromellose??? It seems to be anything they want it to be.

Thank-you all......CUL8RgsOUT

EDIT: SHORTY I'm positive the H3P03 was good...it was a fresh bottle and had been stored properly.

[SHORTY]

Sounds like alot of the h3po3 had decomposed.  It may bee the ratios but i have never used h3po3 so can't help on that.  I have had the same problem when using hypo that was too weak.  My guess is its the h3po3, either it's bad or you didn't use enough but i could be wrong.

[Scottydog]

"3) What the hell is hypromellose???"

It is my understanding that hypromellose is also known as, hydroxypropylmethylcellulose. Maybee they are trying to save money on ink? For bees, they should just start labelling it as HPMC.    It is one of the major gakk ingredients in what Ware calls the "dry matrix" formulation.

Swim has had both theoretical successes and failures with H3PO3 rxns.

Gakked or tainted pseudo will stop one dead in its tracks, especially PEG.

Sounds to Swim like it never even kicked off, so this could have been your problem.

Too much water will kill it as well and since H3PO3 is so hygroscopic, its difficult to tell how much water was already absorbed in your fertilizer. Scaling down the water ratio never hurts.

Like Shorty said, H3PO3 will decompose to H3PO4 (phosphoric acid) So scaling UP the fertilizer ratio, may also help.

Swim has had failed rxns because internal temps never got high enough to where H3PO3 would recycle the HI. So it would kick for a few hours until percentage of HI dropped below 57% and then would abruptly die out. This is most likely NOT your problem.

This rxn is VERY sensitive to certain factors. (gakk, water, temp, purity of phos acid and oxygen)

Maybee your salt is brand new?

Swim was once under the impression that the salt decomposes with contact from air. (the opening and closing of the jar) this would of course expose it to oxygen but with no heat being present, the decomposition is probably minimal.

I believe "fierceness" once said, H3PO3 + heat in the presence of oxygen will give H3PO4. So essentially, this could quite possibly bee happening, right in the flask? Maybee this is what is really causing the rxns to start and then stall/fail?  

By looking at a pile of PhosAcid salt on a scale, one might think, WOW! there is 20 grams here. Looks are deceiving and as time goes by even more so. By the time absorbed water and phosphoric acid is computed into the equation the 20 grams might actually bee 10 grams.

Then again the amount of water called for in the required ratios in addition to the water already present in the salt might bee enough to drown the rxn.  

Swim has yet to dream of a rxn after displacing the oxygen in the flask with helium but may have some merit. Has anyone tried this? It is mentioned in Rhodium's original write-up!

If all else fails, one can use a little RP to kick it off at the beginning.

At least that is what Swim says, when he refers to his insomnambulistic dreams. Some sleep walkers, stumble and bump into walls late at night while others... well, you never know what Swim is capable of doing.  

[barkingburro]

swibb has had experience's of these magnitudes.

firstly the pills that swibb suspects you are using also have a little recognized nactive called polypovirolidone, it is listed on the generic packaging that are tArGeTed from a certain distributor but NOT listd on the same type of pills from the same manufacturer in generic packaging from other stores. swibb cannot be sure but he is pretty sure that this is the underlying cause of the rid sticky goo that at a high eough temp rises to the top of the solution. it sticks to EVERYTHING and in some way prevents the reaction from getting going. the addition of psuedo wiht the i2 and h3po3 was another complication. getting the solution to 87deg C cooling and then adding the psuedo is a much safer and seemingly more effiecient path to generating the initial HI. the amount of water is also VERY important. it is vastly more important to have enough water than not enough. not enough water allows the HI to escape the solution readily and go into the condensor/baloon/never never land. too much water slows the reaction but less gas in the flask means the HI cannot contact and reduce the p/fed. overheated h3po3 in te presence of water but not in the pressence of iodine readily degrades to phosphoric ad phospinic acids. bth of which do you no good. tis occurs when the psuedo and pprd (polypovirolidone) become physical barriers between molecules.

and to answer your question heat does play a part. HI generates frpom i2 and h3po3 at 87 but does not readily recycle to 120 and above. remember if your oil bath is 170 your flask could be as low as 130 or if thick ghetttoed glass is used than even lower temps would be reported from within.

swibb's expereince with degraded h3po3 especially wet h3o3 is that it will appear to be doing it's job, producng the initial HI creation as normal but it's recycling properties become GREATLY impaired. h3po3 is VERY hygroscpoic. it may not look like it but the stuff hold VOLUMES AND VOLUMES of water. cacl2 seems to be the most effective dessicating agent, but the two will react quite violently if they make contact.

it seems that for long term storage h3po3 as a reagent is not a good choice. it ages rather quickly, degrades on a steady slide down hastened by moisture and heat ad also introduces h3po4 as a contaminant if it has degraded.

for someone loing to get bulk and keep for a long period of time RP is prolly a better choice, but something that is going to mae use of the h3po3 quickly the choice is a very good one.

[wareami]

"3) What the hell is hypromellose???"
Good Call Sdawg...

Post 480250 (missing)

(wareami: "Overkill???", Stimulants)

[geezmeister]

Hypromellose is the appellation approved by the FDA for listing HPMC, so the label would not be so long. Remember methocell? Another word for the same thing.

[greensleeves]

ici_rhi,Ware,Sd,Geez,SHORTY,barkingburro,RHODIUM & last but DEFIANTELY NOT LEAST mr_pyrex....SWIGS Thank you for the clarification...In short SWIGS believes that the problem was a combination of the ratio's and tainted or gakked pseudo. SWIGS next dream is going to be dreamt using the molar amount of each and reflux for a full twelve. SWIGS may be incorporating the slanted E-GULL for his next hypothetical extraction and hope beyond hope that he has the patience to recrystallize with success. CUL8RgsOUT

[ChemNewbie]

Holy fuck it's CN...He ain't dead after all.....

Some of yer problem is that you didn't really have enough water to begin with. When Swic first started using H3PO3, he made the same mistake. Even with not-so-clean feedstock, if he made sure to use the at least the same amount of H20 as psuedo (at least 21ml in your case) he rarely had such problems. Yes he is familiar with the murky brown rxn fluid, but if the fluid is still blood red, then it is not done, next time let it go longer. Also, after adding water to the post rxn fluid, if it is brought to a boil for a few minutes, a lot of the color (mostly extra I2) will fade and leave a somewhat translucent mixture. Xylene washes will then remove most of what color may be left.

Just as an aside....Swic usually did small rxn's and usually there wasn't really an initial violent reaction signaling the beginning of HI production.  One thing he did always see though - at least with successfull rxn's- was the golden BB ballet goin' on inside the flask, which is about the only way I can describe it. Those who use H3PO3 on a regular basis know what i'm talking about.

Anyway.....