01-07-04 21:48
No 481074
Hello bees,
Swim is trying to find a way to safely react the maximum amount of material in the smallest possible reaction vessel using the phos. acid synth.
Some of you may remember this part of a post from Osmium:
"Lowjack: NO!
We do not want the whole shebang to react exothermically and spew gas in our direction!
1) add pfed to flask
2) add rP to flask
3) add water to flask (enough water to produce 55~60% aqueous HI.
Doing it in this order is not critical, adding rP after the water but before the pfed will produce the same results
But the last step, number 4, MUST be done after all else is in the flask!
4) Add I2. Gradually. Take your time. Wait until the temp goes down again before adding more. attach reflux condenser for smell control inbetween additions. You can even try to add the I2 through the condenser! Wow!
Usually adding the I2 in 4 or 5 portions will work. Use a mag stirrer or gently swirl the flask in between I2 additions, we do not want a big unreacted blob of I2 at the bottom of the flask which will then, suddenly, without warning decide to react violently."
What swim is wondering is if this approach can bee used for phosphorous acid synths? So basically you:
1. Add phos acid + iodine + water to vessel
2. Heat to ~80 degrees to facilitate HI production
3. Add small portion of sudo to flask (through condenser), wait for reduction in activity, then add another small portion. Continue until all sudo is used up.
4. Reflux for desired time at desired temp.
Swim has found posts where bees suggest adding phos acid and iodine, heating to make HI, allow to cool, add all sudo, and reheat. But he has not found one which suggests the above approach, and is wondering why it could not bee used successfully in these reactions. It seems it would save time (no waiting for solution to cool), while allowing minimal gas production. Or what about the following, for the biggest reactions in small vessels with small condensers:
1. Add phos acid + iodine + water to flask
2. Heat to 80 degrees to allow HI production
3. Allow to cool
4. Add small portion of sudo through condenser
5. Heat to 100 degrees
6. Allow to cool
7. Add another portion of sudo
8. Heat to 100 degrees
9. repeat steps 6,7,8 until all sudo added
10. Reflux at desired temperature.
What do you think?
BTW, Is there any problem (other than being a waste of acid and iodine) with using alot of excess (say 2x) phos acid and Iodine in these reactions to ensure a complete reaction?
BTW2, Some may say that swis should stop asking so many questions and start actually cooking, but swim thinks it is better to be annoying and ask lots of questions, learning from your experiences and mistakes, rather than make his own, wasting time, money, and possibly lives.
(Hive Addict)
01-07-04 23:40
No 481093
Why do you want to add the pseudo in portions?
How will this improve the rxn?
It wasn't Me!
(Hive Bee)
01-08-04 00:09
No 481097
Swix uses pre-made 57% HI, so is unable to comment on order of reagent additions. He assumes the pseudo is added in portions to 'quench' the fast production of HI and keep it in a 57% solution.
Regarding other aspects, Geez and has commented that the best product results from a reflux temp of 120`C (when he has an operable thermometer, that is =P
"...BTW, Is there any problem (other than being a waste of acid and iodine) with using alot of excess (say 2x) phos acid and Iodine in these reactions to ensure a complete reaction?..."
Adding a slight excess is ok, but a large excess (2x) runs closer to the risk of competing side reactions; 'killing' the pseudo and final yields. Also, Bees have had problems with a 'trademark' taste from Phos Acid rxns. This was overcome by using rtios closer to the theoretical recommendations (from Rhodium); and finishing with a recrystalisation.
Lastly, your knowledge seems enough to start a little observational trial run and test your luck...
(Newbee)
01-08-04 04:04
No 481153
Shorty,
Swim was not proposing to add the sudo in portions to improve the reaction, he was just hoping that it would reduce gas generation and make the reaction easier to contain and prevent gas loss from an inadequate condenser.
(Stranger)
01-08-04 05:54
No 481163
Suss, You can do a reaction the way you have described. However, the method you have suggested is not the best approach and your yields will suffer.
SWID has had many successful rxn's with H3PO3 and it is sweet! There is no comparison to the RP/I2 rxn, H3PO3 beats it hands down every time.
SWID would recommend that you dissolve your H3 in an equal amount of warm DH2O and then add the I2 and produce HI. I know it takes a little longer but your yields should improve. When the temp reaches 87C HI will form and the color will change from a dark color to a light amber/yellow. When this happens your HI is ready! It's just that simple. At this point turn the heat off and let the flask stay on the heat source and cool gradually. You want any of the HI that is in a gaseous state to return to the H2O. Takes about 30 minutes, you'll know when its ready because the balloon will collapse. Probably not completely but it will collapse.
Once the HI has cooled dump your entire E into the flaks and stir it up good, reattach your balloon and cook it! SWID likes to run his rxn between the temps of 110-120C. He would not recommend any higher temps because the quality of your product will start to suffer. What SWID means by that is there will start to be unwanted side effects to the product.
SWID started out cooking with H3 for 5 hours, then he decided to take the advice of the more experienced Bees and let his rxn run for 23 hours. Let me tell you, the difference between quality of that product and the product that was spawned from the 5-hour rxn is as different as night and day! ALSO, SWID noticed a slight improvement in his yield when he let the rxn go to full completion.
You can certainly run your rxn anyway you see fit but SWID would strongly urge you to make your HI first. Trust me, you will not be sorry. When you add all the ingredients together at once, E/I2/H3 and start your cook you will notice some smoke in the flask when HI starts to form. This smoke is your produce “going up in smoke”. In others words this is product that you will not get the benefit of. I know you can watch the rxn VERY CLOSLY and stop a lot of the smoking but why? Why would you want to have to baby the rxn that way? Hell, it’s much simpler to just make the HI first, you don’t have to baby it or coddle it AND when the HI is formed your can see it immediately and you know its ready for the E. This isn’t true when you dump all the ingredients together at once, the only color change you see is when the E/I2/H3 change to a light amber/yellow about 2 hours into the rxn. If you make HI first you will get 2 color changes, first when HI is formed, and second, when the E/I2/H3 turn colors.
On yes, and there are different opinions on this, but when the E/I2/H3 changes colors it is NOT finished! It’s just getting started, so let it cook for several hours after that happens. Geeze says to let it cook for another 8 hours after the color change but SWID likes to let it go even longer to ensure complete conversion of the E
One other thing, an H3PO3 rxn is very tame! No violent bubbling or trying to get out of the flask as with an RP/I2 rxn. This being said, you can do larger rxn's in smaller flasks. SWID has done a 40g cook in a 500-mil flask and the flask looked empty during the rxn. SWID is preparing for a larger cook, perhaps 60g, and plans to use the 500ml flask for this also.
Good luck with you RXN and keep us informed as to the progress.
Peace
(Hive Bee)
01-08-04 06:05
No 481167
DarkSky is right on the tee. Make your HI first, then cook away. You bake the bread first and then add your filling....The end result is a mighty tasty sandwich.
<<"meth sandwich for table 5!">>
(Of Counsel)
01-08-04 07:37
No 481173
As to whether I'd do the synth the way you propose: Probably not. I see no benefit to adding the pseudo in portions. You have to cool down, open the reaction up, add, heat, then cool down, etc. again. Why? You already have HI. Each time you open the reaction you lose some.
You could add half of the phosphorous acid at the outset and the other half with the pseudo, but beyond that, there is no reason to add anything in portions.
As to adding extra iodine or phosphorous acid: it is unnecessary. The ratios in the lead post in the RP Substitute thread work just fine. You need enough phosphorous acid, but all an excess seems to do is affect taste. Adding more iodine than called for seems to result in lower yields. I've done some of these reactions making more HI than needed, some with additional I2 , some with a spike of phos acid after the first few hours. Be sure to keep the temperature in the 120C range and be sure there is phosphorous acid available to recycle the I2.
mostly harmless
(Newbee)
01-08-04 07:47
No 481174
Darksky,
An excellent post with very usable info! Swim thinks you slightly misinterpreted him though, as he was advocating making the HI first as you described (hence the heating to 80 degrees after mixing I and Phos). Swim just got the temp wrong (should have said 87 degrees, but memory is a bit messed up these days) :) In any case swim was agreeing that the HI should be made first, but was proposing the gradual addition of sudo. You have made it clear that this is not necessary, and that the reaction is quite tame. Thanks alot. Your post was most useful, especially regarding reaction times and colours. Swim has found the same info previously, but it was segregated between many posts, and conflicting views were making it difficult to completely predict the reaction nature. It is nice to find all the info in one post!
BTW, you suggest 1:1 phos acid and water. What ratios of iodine and sudo do you suggest? (I have utfse, but good to get another opinion)
Cheers
(Hive Bee)
01-08-04 10:33
No 481194
and the remaining 35% at the time swim adds the p/fed. this satisfys the molar ratios for the production of HI and the molar ration of 6:9:5 for further reduction. adding in incriments is uneeded as the main problem with gas not being absorbed fast enough is solved by not adding the p/fed until after HI production. if using i2 from tincture swim uses the following ratios: 9.9g p/fed fb (12g p/fed hcl) to 14.82g i2 to 13.8g h3po3 (9g into mix at start of rxn for HI production, the remainder at time of p/fed addition) and 13ml of d/h20. also swim uses boiling stones (glass marbles ground to provide vaporization spots). geez is very right about the temp and it can become a real bitch to maintain an even temperature throughout the flask without the stones.... someone mentioned flask size earlier and swim has run a 75g rxn in a 250 round bottom succesfully. bouncing the temp also seems to be of some assitance. swim's theory is that when the temperature drops and the resulting drop in pressure re-introduces any HI that might have seeped into our friendly ballon. rememebr that the rxn creates h20 so there is a place for that gas to go and stay as the rxn progresses. by the end of a 6 hour reflux swim's baloon is limp and has no HI within.
one last note, swim has noticed a side effect of excess phos. the dope has a pinkish color. the more excess of phos the pinker it is. this washes out quite readily after the evap faze of extraction with acetone, and it gives the dope a somewhat sweet almost syrupy taste. swim's been speculating on why this occurs but has nothing conclusive yet
(Stranger)
01-08-04 12:21
No 481214
Thank you Suss, I'm glad I was able to help.
As far as H3PO3 ingredients I can tell you what SWID uses;
E/I2/H3 : 1/1.25/1 with 1mil of DH2O for every gram of H3. Make sure your I2 is completely dry, if not scale back on the DH2O you add to the reaction.
All the apparatus that SWID uses is completely ghetto. He has a small 500mil milk bottle that he purchased at W**-M*** which he uses for his reactions. The top of the bottle is just large enough so he can get a 1 ½” Braided Hose slipped over the end of it. His hose is 18” long and in the end of that he has a PVC reducer so he can reduce the hose size down to ¼”, attach a 18" long 1/4" hose to this and attach a balloon to the free end of this hose. Everything is held in place by Hose Clamps.
SWID changes his hoses and reducer for every reaction. Your only talking $3.00 worth of material. It would a shame to ruin a reaction that took weeks to prepare for all because of dirty hoses contaminating the fluids. The length of the 1 ½” hose coupled with the reduction to a ¼” hose helps keep the HI fluids contained in the reaction vessel and larger hose. No condensation migrates into the ¼” hose, it is all contained in the 1 ½” hose and bottle.
In order to heat his reaction he uses a 2-quart pot with approx 3” of sand in it. To this he adds vegetable oil so he has about ¾” of oil covering the sand. All this is placed on the kitchen stove to heat. SWID buries the flask in the sand so that the top of the fluid level in the bottle is the same level as the oil, reason being that when you do this there is approximately 40-45C difference in the temperature of the oil and the temperature of the bottle. If you burry the bottle too deep in the sand the temperature in the bottle will climb, deeper you bury the bottle, the higher the temp goes. SWID learned this, and many other things, from Geez.
The oil bath is slightly warm to cold when he places the bottle with the E back into it. You need to be careful here, if the oil is too hot you will shock your reaction and your quality and yield will suffer dearly. Anyway, SWID takes the next hour to gradually raise the temp of the oil to 165C, this should give him a fluid temp of 120C. He leaves the temp at this setting for the duration of the rxn. He swirls the bottle gently every hour for the first 4-5 hours to make sure he has washed all the E off the interior wall of the bottle, after that he might swirl the bottle every few hours.
His post reaction work up is similar to the one Geez has outlined in his the post-reaction workup thread although he does make a few minor changes to his work-up process. After the honey is made he dilutes it with 5 times its volume in warm DH20, then he makes sure its good and clean with several Toluene washes. If SWID is working with more than 250 ml of honey before he dilutes it he will break the fluid into smaller portions, treat these as separate projects and work each of these up individually . It's much easier to work with smaller portions AND if you have a screw-up and spill some of the honey or the cat knocks it over or you are unfortunate enough to have OG II contaminating your end product the smaller portions will act as an insurance policy to prevent total loss of all your hard work. Personally SWID thinks Toluene is the best NP to use for the A/B process. When you wash your honey with Toluene any peg that might be present will be drawn to the Toluene during the wash, leaving your E a little bit cleaner.
Now, here’s where SWID starts to deviate from Geezes Post Work-Up, after he is done with the NP washes he FILTER’s the honey as he separates it from the Toluene, this was a step missing in Geezes right up, I’m sure it was just a slip of the pen though. Now SWID has learned something very interesting when using Toluene as his NP, since SWID doesn’t have a separator funnel to use when separating the honey from the NP he will siphon off as much as he can without drawing off any of the NP and run this honey through a filter. Now, there’s always a small amount of Honey left on top of the NP so what SWID does to collect this is pour the top of this fluid off into THE WET FILTER that he was using for the honey. The moisture in the filter will allow the remaining honey to filter through but will trap the Toluene in the filter NOT LETTING THAT THROUGH. Caution here, you don’t want to get carried away and fill the filter up with NP when pouring off the top layer of honey, you just want to pour enough to collect all the remaining honey setting on top of the NP. Also, SWID has found that filtering at this stage not only traps the NP but it also traps any oils that might be deposited in the honey during the wash process, leaving them behind in the filter, and leaving SWID with a crystal clear, slightly gold honey…PERFECT!
SWID filters at every stage of the work-up when transferring the honey from one medium to another, it just makes sense to do this and insure that your product is a clean as you can get it.
The rest of the work-up is similar to Geezes write-up. SWID has found that Toluene is excellent for using to pull on the base fluid and will pull the majority of the freebase from the base fluid on the first pull, with the next 2 pulls resulting in lower amounts. SWID doesn’t stop there, he hates to allow even the smallest amount of freebase to escape him so after his first initial pulls he will do a 4th pull on the base. This pull he will allow to set for several hours. Also, to this pull, SWID will add a couple of small spoons of regular table salt to the Base fluid which helps the freebase on its way to the NP and then shake everything like his life depends on it…THIS IS THE ONLY TIME SWID will shake the fluids together, since he’s going to allow this to set for several hours he knows the emulsion will have time to clear.
SWID has also found that it is helpful to apply heat to the Base/NP solution for this pull. SWID will place the jar with the Base/NP into a small pot that is filled with water. Inside the bottom of the pot SWID will drop a hand full of toothpicks so when he sets the bottle in the pot it isn't in contact with any hot metal, don't want it to crack or burst. SWID will raise the temp of the water in the pan, there by raising the temp of the Base fluid and Toluene. This seems to hasten the migration of the freebase to the NP, perhaps because when you heat these fluids their moluces move further apart and allow a less restictive path for the freebase to travel, SWID dosen't really know, he only knows it works. SWID will apply heat this way for about 30 minutes. BE VERY CAREFUL WITH THIS HEATING OF THE BASE FLUID, you do not want to get it so hot that the NP will start to boil. Toluene has a much lower boiling point than the base fluid and if it starts to get very hot it will turn to a vapor, This will in turn increase the pressure inside vessel containing the base/NP solution. Too much heat will result in too much pressure, which could result in having your base/NP vessel bust and send little shards of glass and solution flying everywhere. BE CAREFUL NOT to let the NP stay in contact with the base fluid much longer than 24 to 34 hours. SWID has found that after this length of time the meth can migrating back into the Base fluid, it may not, but then again it may, bummer!
Now when SWID siphons off the 4th pull of NP from the base fluid he will add just a little DH2O without any acid to the NP and do a PH test on this, if the PH is high SWID will continue with the Acid pull on this fluid, if the ph is low SWID doesn’t waste his time. Also, if the ph is high SWID will do another pull on the base, matter of fact SWID will pull on the base fluid until he gets a low PH reading from the NP/DH2O mixture. As long as your ph is high in the NP that’s removed from the base the pull is working. . Once SWID gets a ph reading back from the NP of 7 or less he will discontinue the pulls on the base. Waste not, what not!
After SWID finishes his 3 acid extractions of the freebase form the NP he will save all of the NP and combine this in a big jar until all the meth has been extracted, then SWID will do another extraction of the NP. He will add DH2O to the NP with NO ACID and check the ph level, if it is above 8 SWID will add acid drop wise to this until he gets his ph down to 7-6.5, but if its down to 7 or less SWID realizes he is finished and doesn’t waste anymore time on it.
One thing SWID has noticed, when you are doing an acid extraction if you screw up or get careless or if you don’t have any way to test the ph lever FOR THIS PHASE of the work-up and you happen to get the ph level below 6 not only will your yields suffer but your quality will suffer also. Now, SWID knows you can wash the meth with acetone to remove any excess acid but SWID has found that this is only a half cure. The product you are left with after driving the ph too low is substandard to the product you obtain when you extract at a ph level of 7-6.5. Even after several Acetone washes, dissolving the E you retrieve form the acetone in Denatured alcohol, filtering the alcohol to remove any HCl salts that might be lurking in the back ground and then evaporating to retrieve the meth, its just not as good of a product. To SWID this simple ph test is one of the most crucial things he does in the post A/B work-up. This small detail, or lack of, can have a terrible effect on your product. SWID never tests the ph level of the base fluid but he always tests the ph level of the acid extraction.
Oh yes, denatured alcohol will leave a residue on the meth so make sure you do an Acetone wash every time your meth comes in contact with denatured alcohol as a final cleaning process! Not only can you smell the sickening, sweet smell of the DA in the meth, but you can also taste it. Now, if you’re one of the individuals that prefer to take his meth via IV, as soon as you inject the meth you will immediately get that same sickening, sweet taste of the DA throughout your body, you will also get a giant rush as the DA works through your system. It only takes a few seconds for this process to work through your system but the sweet smell and taste will linger long after. SWID doesn’t think this can be very good for your healthy, so make sure that you wash your finished product with Acetone before you use it or distribute it to the public.
H3PO3 is clean, safe and fast as compared to the typical RP/I2 rxn, its also not listed as a Class I or II substance,,,,,YET, but SWID would not be surprised if that changes this year as our friendly, help full Government continues to attempt to control something that they can’t control! Regardless of the new laws they make, regardless of the chemicals they try to control, regardless of the punitive penalties they access to try and discourage the use, distribution or production of these products, there are those among us who will endeavor and continue to make advancements in the fine art of the cook….and I am firmly convinced that the conversion of E/P to a clean, high octane product is indeed an art and SWID takes his hat off to those among us who have pioneered this field.
(Hive Bee)
01-08-04 13:56
No 481238
"...one last note, swim has noticed a side effect of excess phos. the dope has a pinkish color. the more excess of phos the pinker it is. this washes out quite readily after the evap faze of extraction with acetone, and it gives the dope a somewhat sweet almost syrupy taste. swim's been speculating on why this occurs but has nothing conclusive yet..."
Man its good that PhosA synths are coming a little more common. Swix has dreamed PhosA gear that was pinkish just as you describe. He assumed it was from pHing technique or that the crystals absorbed colour from their surrounding environment.