This works every time

[simonsays7]

Am certain there is going to be flames, but maybe this will help other Bee's trying to make a first reaction work.


After many many many attempts at making the goods using matchbook rp with mixed results, swis aquired some phosphorus acid.  With dozens of attempts swis has settled for this series of steps to have fail safe goods every time.

Everything is clean..do a 10 gram reaction.  Use 10 gram white freebase,   12.5 grams black,  4 grams phos acid,  3 grams water.   Use a condenser or at the very least run a hose from the top of the reaction vessel into and out of the freezer.  You need the reaction liquid condensing back into the reaction vessel.  Bring to a boil very slowly like an hour.
When it boils to a amber color or an hour of boiling or 2 hours at least then take off the heat and cool for 30 minutes.

Next take 6 grams of mbrp, and 12 grams of black,  and 2 grams of water and dump in individually.  Bring this to boil until it is clear, meaning all of the dark i2 is gone and your reaction vessel is clear of iodine color. This usally takes about 2 hours. You are done.  Process in the usual way.

This must seem like a waiste to some of you.  How much of a waiste is it to have a reaction fail of unreacted goods.  Swis just got tired and this is a full proof way to the end result.

[barkingburro]

a long time ago. you are wasting your i2, ut beyond that not wasting much. you can however get basically the same results if yoyu bump your phosphorus acid up to 12 instead of 3. and bring the temp of teh flask to 130. in essense what is occuring in your procedutre is that the h3po3 is making the initial HI and then becoming h3po4, the rp however when added acts as the recycling agent fist converting I to HI the rp to h3po3 and then under the continued heat the h3po3 additionally recycles becoming h3po4 and the i2 once again becomng HI.

[geezmeister]

Barkingburro's analysis works for SWIG. Adding more I2 to the reaction isn't needed, or for that matter helpful, if you added enough I2 to start with. More I2 usually means lower yields. SWIG cooks his phos acid reactions a little long on time, eight to twelve hours, stewing away quietly at 120C or thereabouts inside the flask. The reaction starts with H3PO3 which will degrade over the life of this reaction into mainly H3PO4 at the temperature used to react pseudo. If the reaction is doing nothing -- I mean, nothing. Its just sitting there being yellowish/ gold. Hmmm. Touch the fluid. See an iodine stain? Think about this... elemental iodine does that. If you have I2 in the flask it means its not being recycled into HI by the phosphorous. Why not? Most likely because the H3PO3 is already oxidized into H3PO4 and the latter won't recycle iodine. 

If you have that sense of the reaction-- that its not doing a thing but sitting there--- add some active phosphorous to the reaction. Add some H3PO2, add some more H3PO3. orr add some red phosphorous. All of them will work. You will have activity in the flask for a short time, then it will die back again.

Add some phosphorous compound. Skip the extra I2.

[Scottydog]

1 pt E/ 1.25 pts I2/ 1.5 pts phos acid

Multiply the amount of phosacid that you use times .6 to get the proper water ratio (tap or distiled) doesn't matter!

Weigh out phos, place in a glass jar with plastic lid, dump in water, put lid back on and swirl until all phos is dissolved. Put this solution in the fridge.

While this solution is chilling, prepare flask in oilbath with all of the E and I2. Put on the condenser and turn up heat to 150F. When thermometer reads as 150F, crank up the electric fryer all of the way.

Take the phos solution from the fridge and pour it down the condenser and secure your 16" punch balloon with electrical tape. Within 30 minutes the oilbath should reach 130C.

When it does reach 130C, turn down the fryer to stabilize the temp at 130C and let it go for 4-6hrs. It generally finishes right around 4 hrs and 20 minutes.  

If contents are still orange to red, more of some 50% phosacid or hypo solution can bee added and refluxed for an additional hour or two at 135C, this is rarely necessary!

It really is short and simple Mr Simon!  

[relic2279]

Simon,
What kind of yeilds are you seeing with your method?

[simonsays7]

depending on how small and how careful the articulator is.

 Around these parts black is easy and plentiful to aquire the phosphorus is not.