I2/RP reaction

[Curtains]

SWIM is in the mist of his first cookout
heis doing a
11g psuedo
11g lab grade idione
6g matchbook red phosphorus
2.5ml water
In a 25watt lavalamp with balloon on top

SWIM's reaction has been going on for 14hours now and looks like....a large clump of material on the bottom looks like idione/blackish color surrounded by a yellowiish/red liquid....
my question is this a normal look?
and is it possible to over cook a reaction

[Ascension]

Since your using MBRP you should of used a bit more id day, bout 8 grams.

And your doing a LWR and only added 2.5 mls when you had 11 grams of pseudo, big mistake mate.

Should of been at least bout 7 mls of water, and there should of been more I2, maybe about 14Gs.

Also what heat does the bulb bring the inside of the flask to? This is a huge factor that you will need to find out if you dont know.

When you first added everything did it just fire off in one big heap then slow down pretty quick? If it did that would of been because of the low amounts of water, and this is bad IMHO.

[wareami]

First off...as ascension says...the ratio's are a bit lopsided and the HI may not be sufficient to completely reduce.
Before proceeding....take off the heat and let cool.
Uncap the rxn and stir the contents with stirrer/bamboo skewer. SWIC might find that the contents are rather thick...like chewed bubblegum.
If not don't worry...it will be by the end if you follow the advice here.
Ibee would add two more grams of I₂ and one and a half grams MBRP along with 2ml extra dh20.
Recap after thoroughly mixing and Cook another 24-36hr.
That's the bare minimum Ibee could suggest to finish.
Next time...SWIC should base the rxn on suggested ratio's.

The rxn cannot be overcooked so go for the 48hr mark if patience isn't a big deal, just make sure the rxn doesn't dry out. 10hr Checkpoint stirrings if need bee.

[Ascension]

Do what ware says and you'll be fine

But before you start the rxn again make sure you get another rxn flask, chuck a bit of oil, a thermometer and put it back onto the lava lamp, let it sit for bout an hour and then read the temp.

If its too low, say <90C then this isnt good, but i really doubt its too low.

Lavalamp bulbs a quite fuckin hot, the surface of the blub reaches 200C+ quite easily.

Im more worried about the bulb heating the rxn too much. It could easily bring the stuff up +150C which can be quite bad.

[lutesium]

2.5ml water!!! Things that you describe are normal bro  

I am not talkin about reducing suedo or whatever but the amount of water must be abjusted according to the I2(see an old post of mine in this form called "calculartions") And calculations show that you are at danger levels! You must at least be using 13-15 grams!!

[geezmeister]

If that mbrp is first use and you did a good job of cleaning it from the good matches... the mbrp will not be a problem. If the temp of the bulb doesn't raise the contents of the flask too quickly and you haven't gotten the contents too hot, you don't have a problem. If you added some water to start with, and I would have started with almost nine (9) ml of water, you would have been fine if you brought the temp up to about 100C for the first twelve to twenty four hours, then up another 20-40C for the next twelve to twenty four hours.

Everyone has a recommendation, and none of us agree on what it should be. I recommend letting the flask cool, adding 6.3 ml of water, stirring well, adding another gram or so of I2 (since you left yourself with no alternative but to open the reaction up and tinker with something that would be fine if you added enough water at the start and just left it alone) and then using a device called a thermometer to see just how hot you actually get the inside of the flask on that light bulb. If its 105C or higher, fine, let it sit for at least thirty six after it starts bubbling good. If not, find a heat source capable of the heat needed to drive the reaction. 

Water is an essential ingredient in this reaction. You either know how to use very clean ingredients carefully with a little bit of water, keeping your eye on the flask damn near all the time until its done, or you don't. Sounds like you don't. I suggest, for those among us with little tolerance for multiple failures on a long learning curve, that you use more water, reflux for longer times, and enjoy success much earlier in your range of experience.

[ampdup]

I have noticed that, geez.  It is consistant throughout this site.  Is there a formula that is "set in stone" on the amounts of RP/I/E/DH20 that should be used?  The only constistancy in the formula is that at some point in time, they all are put in a flask.

I started a thread yesterday with this question, but deleted it and tried to UTFSE some more, But, it is sort of like trying to find out what SWIM means.  SWIM is such a common word, you could look at posts all day long and never find the one which has the definition of the word See What I Mean? <--(SWIM thought that was what it was for a long time...a trendy catch-phrase or something...been a good many years since I have been "hip", if I ever was.)

Anyways...is there a guideline to the quantities that ya'll use? Some sort of rule of thumb?  Cause what SWIM uses ain't even close to any of these.  Swim uses 80g I, 40g E, and no less than 20g RP with as much as 70gRP at times, depending on whats left from last time.  But I always add 15g fresh, cause SWIM fears failure.

[kewlcanuk]

If you press the links button in the top right hand corner and then goto the abv. page you will find all the answers you seek.

[ampdup]

I wasnt asking what SWIM meant..I know what it means, I was just using it as an example. Obviously, not a very effective one, but an example, never the less.

[ChemoSabe]

Here's the old standard now living over at Rhodium's.

https://www.thevespiary.org/rhodium/Rhodium/worlock/rxn1.html#rati

[Ascension]

Warlocks info is very good, but the truth is those fast hot rxns are old, out of date.

That page is almost like reading a history book, of how things use to be done.
IMHO its misleading to newbees as they think this is how it should be done now.

Today water is a major part in the rxn, and 24 hours while being held at reflux is almost the norm.

[ampdup]

Although dated, it was exactly what it was looking for to fill in a few blanks that SWIM had been struggling with.  SWIM's apprenticeship was cut short when the teacher made a few bad choices and is now a guest of the state.  Even though it reads like "history", SWIM thinks newbees would benefit greatly for reading it.  It outlines the basic procedure clearly and is very easy to comprehend.  As long as NooBees understand these "simple" steps and can perform them with some successful consistancy, They should have no problem (or maybe just less of a problem) incorperating the more complex and modern techniques that are being tossed around presently.  Understanding the steps and knowing when to perform each task can be harder than the actual task itself, IMHO.  Great link BTW.

[Ascension]

ampdup the info is good, but please dont get confused.
You dont want to follow the ratios set out on that site, unless you want to set up a push pull, which is unnecessary.

Theres is nothing complicated at all about todays ratios once you understand.

1 pseudo
1.2 I2 (MIN), can bump up to 1.5 if felt necessary
.4 RP (MIN if using Lab Grade) around .6 min for MBRP super clean, people use much more sometimes aswell.
.5 water, people have used up to 1 ml water per gram of pseudo

The water really depends on how long you want to cook i believe, if your going to be cooking for 48 hours you should have the water up above .8

As geez said these ratios are in the envelope for success, and you can move these ratios around as long as you stay inside the envelope.

[geezmeister]

Is there a formula that is "set in stone" on the amounts of RP/I/E/DH20 that should be used?  The only constistancy in the formula is that at some point in time, they all are put in a flask.

Nothing engraved in stone. There are any variety of ratios that will fit within the envelope of success. I have mentioned these ratios and discussed their relationships to each other in a few posts:

Post 449625 (missing)

(geezmeister: "reaction parameters", Stimulants)

Post 478526

(geezmeister: "the envelope of success", Stimulants)

Post 467035

(geezmeister: "crystals in the condenser", Stimulants)

Post 487707

(geezmeister: "suggested parameters for first LWR", Stimulants) 

I will say this much about the ratios you use: You are using far too much iodine. You are losing yield using that much. At the size reaction you are doing 1:1 ratios of I:E will be sufficient; you never need to exceed a 1.2:1.0 ratio of I:E except maybe in nano reactions.