The Colour Purple.

[8ball]

Swi8 has just completed 1st stage of cook using 16ml of H3p03 ,20g of I and 16g of E in this order. Reaction was fine with H and I, then added E and heat. An excessive amount of HI seemed to be still produced so i decided to add some dh20 to try and trap HI. as i squirted dh20 down through top of condenser white blobs of snot was forming on the end of the syringe and up the sides of condenser falling into the solution and dissolving. Once either the gasses from either the HI or I subsided i noticed that the solution was a fairly dark purple?
Does anybody have any ideas on this?
Once my fatty acids form i will try to bring it over and see what happens.
                    cheers 8ball.

[geezmeister]

You did not start with water? Are you trying to react the ingredients dry? Why?

You need water with the phosphorous acid and E and iodine. Is there some problem with the method that Rhodium suggested in his lead thread on the phosphorous acid thread?
Is there some problem with the molar amount of water he said to use?

In my experience, the method he described worked well. You should do the synth the way it is written, with clean freebase pseudoephedrine. Might make a big difference in the results obtained.

I have no idea why you got a purple color. If I knew where your "E" came from, and how it was extracted, I might have a better idea.  Maybe not enough water? Are you subliming your iodine now? And having purple gas?

I'm guessing because there is not very much information in your post, and you force the rest of us to guess what the problem might be.

[8ball]

Water has already been added to acid to dilute to 50% plus approx. 10ml at start of reaction to try and trap HI. E was extracted from 60mg sudafed sinus and nasal by adding pill to methylated spirit soak overnight shaking occasionally then filtered through 1 then 2 then 3 coffee filters until spirit is crystal clear then evaporated over low heat until crystalized. i have been using this method religously for the the last 2 1/2 years with not a problem, until now. Maybe it is not a problem, but it is certainly not normal.
                          8ball.

[8ball]

I have just had a look in flask and my fat content is forming to a nice beige yellow colour but the remaining fluid underneath is a dark purple, other than that it looks fine, only time will tell.
                                    8ball.

[geezmeister]

That sounds a little dry to me, and the fluid is pretty viscuous even with more water. You have two different layers of fluid? One purple, on yellow?

Stir, man. The heat it up to at least 120C, somewhere along the way you will get that sudden surge of action when the I2 and phos acid react to make the rest of the HI. I wonder with the small amount of water you had and heating it you oxidized you phosphorous acid to phosphoric and have nothing to recycle the I2. Got a little red phos? Toss some in and stir. Might surprise you what happens. If the reaction gets active and goes yellow, you can bet you did not have the phos acid in the right molar amount to sustain recycling during the reaction.

How are you going to get a reaction to complete if your ingredients are not homogeneous?

[SHORTY]

I have never used it but if he started with a 50/50 solution of h3po3 and then added an additional 10ml to the 16ml of 50% then he would have 26ml of 30% h3po3 to 16g of E and 20g of I.  Could he possible have too much water for the h3po3 and iodine to react?  The oxidation of h3po3 to h3po4 is a slow process although heat does speed it up but i would guess that not that much has oxidized.  This is based on my experience with hypo so it may bee different. 

8ball,
I suggest you try to bring it to a gently boil with the condenser off and frequent stirring to evap some of the water off. 
Or you could add more h3po3 or even better add some rp like geez's suggested and see if your iodine reacts.  If so, then you should probably add a little more iodine to make sure you have a strong enough HI to complete the reduction.

[halfkast]

Geez, shorty is right he used plenty of water, he said from the start it was a h3po3 solution?
8ball it sounds like you used way too much water.
Do you mean to say you added 6ml of a 50% solution plus another 10ml of straight water?
Or 16ml of 50% and another 10ml of H2O?

They are both fucked so UTFSE! you need a lot more H3PO3 and a lot less water.

edit: irritating rant deleted.

[8ball]

I started to bring it over 1/2 hour ago and just got the flow of little diamonds running at the moment, so every thing seems ok at present i,ll get back to it and let you know my yield once i'm finished.
                                    8ball.
p.s. I probably should has said h3p02 instead of 3 sorry my mistake, i was a bit vague last night.

[SHORTY]

In that case 30% will work fine with your ratios but if you had added 10ml to 16ml of 50% hypo then you would have 26ml of 30% hypo and this is why your rxn didnt take off and also the reason for the purple.  I would have increased the i to match the hypo by adding another 6 grams of i.  Or if you don't have anymore i then just let it cook alot longer than usual and it should be ok.

[8ball]

Well i'm done everything seemed to go alright but i had to dump a bit more caustic in than i had expected to get a yeild of 7.5g once ph and drying was done.Time to test, well i was a bit weary because of the purple colour earlier so i had half a point and this is when lift off started to occur, i dont think the twin towers shook this much on 9.11,so a little bit of cut and i dare say the punters will be very happy.
Heres a thought, if my E had been sitting around for a couple of months could this have an effect on the colour?
          8ball.

[LoW_JacK]

but, doesnt hypo run a higher risk of explosion or flask fire or some odd shit somewhere in the RXN process?

And dont hit me with a UTFSE cuzz I aint gunna. This here topic is about this 8ball person using hypo to cook him some dope, so I'm asking this on this thread. Actually my Q was directed at Geez.

[geezmeister]

My experience, and understanding, is that if you concentrate the hypo, and/or if you heat the reaction too much, you can expect to generate phosphine gas and have "fun" watching the resulting fire that occurs when oxygen reacts with the phosphine gas.

Sudden excitement. Orange film in the flask. Hope you had good ventilation and did not inhale all that white smoke.

I understand that refluxing the 57% solution at a reasonable temp solves the problem and works very well. Shorty has the experience and expertise to give complete answer on the usual concentration  and the reflux.

[SHORTY]

I have been using hypo for quite a while and have completed well over a 100 rxns without ever having a fire.  According to literature by a producer of hypo and its salts, the acid is safe in concentrations up to 50%.  They claim that concentrations higher than 50% are unstable.  However, in my opinion if care is used when handling it and the heat is carefully monitored then even higher concentrations can bee used. However, in my opinion higher than 50% is not necessary anyway.  Considering that rp releases hypo and phosphorous acids at a very slow rate and in very small amounts into water then obviously a 50% solution of Hypo is going to react much faster than any amount of rp will.  I know a bee who uses 30% following the same synth as mine with excellent results. So even a lower concentration could probably bee used if one wanted to do a long reflux.

I did have a hypo fire not to long ago but not during a synth.  I was evapping the water off after filtering out the hypophophite and made the stupid mistake of leaving the room to check my email.  I returned about 10 minutes later to find that the thermostat on the hotplate was stuck and the shit was boiling very rapidly and some was splashing out in droplets which ignited when they hit the hotplate burner.  Then before i could do anything the whole beaker ignited and then came the smoke. Luckily the fans were already on and the smoke was carried straight out the window.  I grabbed the wet bath towel kept in a 5 gallon bucket of water and threw it over the beaker and hotplate and pulled the plug on the hotplate.  I then took the beaker still covered with the towel, outside and sprayed with a hose.  After it seemed to bee cooled down i carefully pulled the towel off and within 5 seconds the beaker reignited so i sprayed it with water until it was cleaned out of the beaker. 
I later took the hotplate apart and found that the contacts on the thermostat had in fact stuck together probably from arcing over time as it has been used alot. 

The smoke generated from a hypo fire is unbeleivable and i was lucky i have a very strong ventilation setup cause it was very thick.  I watched as a huge cloud of it moved up from the window and couldn't beleive how long it took to finally disperse.  Since then i never leave this particular procedure unattended.  I was lucky to get through this unharmed and won't take that lesson for granted.

[8ball]

No dramas with fires yet. Touch wood. I actually have a Labmaster Isopad so there are no naked flames present whilst my illegal endeavour is in process, which i thank my lucky stars for because last night i cracked my flask towards the end of the cook and all that happened was the circuit breaker tripped out.