Did the first synth
(edited with e.hcl amount)
As swim preparing for a LWR he tried one ala curbshot yesterday, but with proper glassware and LabGrade reactants.
But things didnt turn out exactly as planned, so he have some questions the TFSE couldnt answer.
(or at least he couldnt find the answers)
Equipment
1 50ml rb flask
1 three-necked adapter
1 rubberstopper
1 thermometer
1 liebigcondenser (w/ waterbath and pump)
1 heating mantle
Chems
3g LabGrade I2
2g LabGrade RP
1.5g e.hcl
4 drops of dH20
4 Drops HCl
20ml + 20ml dh20
50 ml Toulene
Placed RB in Freezer for 5 min.
Greased all glassware joints.
Mixed chems in following order I,E,RP, h20.
Fitted in condenser and therm (plus cork for the unused opening in the three-neck adapter).
No sponstanious reaction occured.
Added some heat to the mantle.
(The mantle has only three settings, swim put it on setting two. As the themp rose swim switched it to setting one).
The ballon began to inflate, good sign. But it woulndt inflate fully so some gas leeked out of the system
(not too much though).
Swim couldnt see exactly where the leak occured, but checked all joints and all seemed good.
Swim have a supicion though, and that is that the balloon was to "hard" to inflate (as some new balloons are).
1. Are swim's assumtion correct or is there some kind of sealing the glassware swim is unaware of?
The reaction seemed to go ok, but swim read that the gas should be yellow.
My gas was totally transparent, until it came in contact with the outside air.
Then it seemed gray-like
2. Should it be yellow or transparent?
Swim kept on cooking, but as the flask was submerged in the heating mantle it was very difficult
to observe what was going on.
Also the temperature was _very_ difficult to maintain at a certian level.
My glass therm only goes to about 110 c, and swim was afraid to blow up the thermometer.
so swim kept adjusting the mantle, but it is slow to respond, as it already was very hot.
So the temp swung from 70 to +110C. Kept it from 90 to +110C the most of the time though...
Swim knows that he probably should use an oilbath, but as the term dosent go higher than 110C,
its difficult to do this as the internal temp of the flask is much lower then the oilbath itself.
And when the reaction is supposed to go @ 100-120 its difficult with my therm...
Also how the **** kan i keep the temp stable with the oilbath?
If the hotplate has setting of 1 the temp still rises, although slowly...
3. How can he keep a stable temp?
Swim read that many use a "candythermometer", but what the hell is that and where might one aquire such an item.
Again swim dosent live in the US, so he was just wondering what kind of store sells this....
As swim plan to do a LWR a stable temp over a long period of time is cruicial.
Swim read in TFSE that people use deep fatfriers, but he cant find one here (swim dosent live in US),
and also coffemachines to keep the temp @ 90C.
4.Isnt 90C too low for this rxn?
Swim stirred a little with my therm, but as stated above he couldnt see the entire flask.
Well, upun inspection after 1 hour he saw that the sollution had done pretty dry.
Too dry he guess, he saw some of the reaction amost had burnt/fastened itself to the surface of the flask.
Swim was told by VE to nix the peroxie and use dh20, but the writeup suggests "With a dropper add 4 drops"
5. His rxn ran dry, should he add more water, and if this is the case , how much?
He tried to recover it anyway and filtered it trough a coffefilter.
He got a yellowish sollution (yeeei) and it turned milky when he based it.
So everything seemed ok (swim is aware that yeilds would suffer greatly in his first rxn,
but was just hoping for _some_ product)...
Did the AB, added som NaCl as he read that it whould help.
Some sort of powder/product already formed in between the layers..
4. What could that bee?
So, final stage. Evaporated h20, got 0.5 grams. 2 guys biotested 0.1 g each. No special effect. Just some heat rushes.
Swim thinks all product was unreacted e.hcl. Swim lives in a place noone has seen meth before (just regular amphetamines),
so nooen can verify smell, effect of apperance.
5. Does meth.hcl look/smell/taste the same as e.hcl or it there a distinct difference?
Finnally about the eventual oilbath. He tested to make one but he had a lot of "bumping", or bubbles comming up from the
oil, sometimes a little violent. Swim even used many boiling chips. (from a broken cuffecup) Swim placed it in a coffejar on a hotplate.
6. Does he have to use a special oil or does he have to use a different setup?
Swim realizes that perhaps questions are redundant or downright silly, but he has tried to use TFSE, but with no handson experince with meth, its difficult to verify the endproduct.
He thanks you for your time, and hoping for some advice...
Thanks again!