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star's step 2 ...tragedy.. help !
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| Author | Topic: bright star's step 2 ...tragedy.. help ! |
| andrew.z Member |
posted 11-16-1999 12:47 PM
ok i have done it twice with same results i am doing something wrong to produce the meam... but what ? ok i have placed 120g paraformaldehyde and 108 ammonium chloride with 320 ml of distilled water in a flat bottom flask 500ml, on the fisher 's hotplate, i wrapped the flask with aluminium foil... oh i placed no boiling stones but my stir bar... ok ready i started... after 35 minutes between 60 and 80 degrees C the solution became clear like water and then the temp coninued to climb up but not upper than 104 while the stir bar was on 5 ( medium ). Drops of a water like liquid went into the receiving flask. After 3 Hours from the star i stopped everything as my receiving flask had collected almost 270ml of liquid, while the larger flask was containing a white/yellow not clear liquid about 230 ml . I have done it twice up to this point as something is going wrong as all that liquid is not supposed to come out that much and i ams upposed to have lots more liquid in my original flask. NOw the thing is inside the flask and it is resting waiting to be trashed or waiting for some more heating, filtering and then vacuum dist. So please tell me what i am doing wrong, i need a very good tutoring as i have followed Bs word by word letter by letter... |
| andrew.z Member |
posted 11-17-1999 06:47 PM
Ok so this is my third try: i have redone step2 but with boiling stones and a bowl of oil... heating was very slowly after 1.5 hours the oil temp was 100C while in the flask it was at 60 C ( later on i check when the oil was at 140 C the flask was at 100 C - temp taken from the termomether in the middle of the 3 way arm ). Ok so at 60c it was boiling and it was becaming clearer then it went up up to 100 C and i had it there for 3 HOurs. The water in the receiving flask was lesser than the other times but after 4.5 H ours from the start i put the flask to rest for 4 hours ( liquid collected was almost 180 ml ). Then i restarted until the flask was at 250 ml and i did the ice/water bath... after one minute i noticed like apowdery sandy thing... after 10 minutes i had a yellow liquid and a lot of sandy material white/yellow. I filtered everything with a buchnel filter with some paper ( no vacuum filtration... ) and then i placed less than 140ml of the liquid into his flask with new boiling stones and i waited for more liquid to come out... after 75 ml i turned on the vacuum aspirator and after a while i noticed that there was smoke inside the flask... i have waited for the chrystalization but invane... in the flask there are left almost 30 ml of yellow liquid now. For god sake what am i doing wrong ??? |
| lucky Member |
posted 11-17-1999 09:39 PM
andrew.z "the flask was at 100 C - temp taken from the termomether in the middle of the 3 way arm" The temp. should have been taken from the liquid in the flask. I recall BS saying this. You should check out Bright Stars initial post of his synth. Look for "Complete MDMA" in the general fourm if you haven't already. The temp. in the flask is probably really high. Your killing your wanted product if the temp. is anywhere near 220C. |
| Amanita Member |
posted 11-17-1999 11:46 PM
You want the solution to be at 104 c, not the air in the flask....you should submerse the thermometer tip into the liquid. Anything above 104 and you will just create di-and tri- and badness and distill over your liquid. good luck!! |
| andrew.z Member |
posted 11-18-1999 03:35 AM
Hey guys tell me this,if i just check the temp of the oil and maintain it at 104 C will the liquid then be at the same temp ? ' cos when i removed the termomether from the 3 way adapter then the fumes get out and i get intoxicated ( no kidding i had that lovely smell all over my face... ).. so what do you think ? just have the termomether collecting the oil's temp ? otherwise i will have to buy a new termomether and arubber tap and place it on the 3 way with the termomether that goes down to touch the liquid and stays there all the time... you tell me what's best. |
| r2d3 Member |
posted 11-18-1999 07:41 AM
What you can do is perform the reaction on a water bath. This would insure the temperature did not get too high. After the bubbling stops, apply vacuum and reduce the amount of liquid in the reaction flask. |
| artech Junior Member |
posted 11-18-1999 04:47 PM
Please correct me if wrong about the procedure. I'm redoing step 2 again: 1. Heat the solution for 4 Hours at 104C Thank for!!! |
| andrew.z Member |
posted 11-18-1999 06:03 PM
hey you are adding some steps... after the filtration you continue to distill no vacuum... and as soon as you have 1/4 of the original solution then you turn on the vacuum ... Bs doesn't say no more of 147C where did you get that temp ? |
| artech Junior Member |
posted 11-18-1999 06:21 PM
I ask BS this question before. I was not that clear from his reply. That why i post here again to see if my understanding of the procedure is correct. Could some fellow bee's comment on it. Thanks!!! |
| artech Junior Member |
posted 11-18-1999 06:24 PM
I was told by BS MeAM.HCI will sublimate at 147C. |
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