Syrup Disasters

[kris_1108]

Hi
Swil attempted an extraction on TEN bottles of syrup recently. The yield was unbelievely low (probably less than .5gm of theoretical 6gms). Actualy I had about the same yield doing TWO bottles a while ago.

I have never seen a 2L coke bottle DEFORM and have a solution BOILING in it, all by itself.
I dont want to bore any one, lets make it quick.

*Added the bottles of syrup to a 2L coke bottle (1L total syrup).
*Added 120mLs of xylene
*Quiclky added a still-warmish 50% NaOH solution. After 300mLs of NaoH soln the color went orange-piss color. pH meter batts were flat so no check was made  
*Swirled and waited 15mins, meanwhile the syrup goes dark.
*Removed the NP, added 100mLs NP, swirled, waited 10, added to first pull.
*The blue seal in the lid of the bottle half melted and fell in the the BS/NP. Great.
*Ready to wash the 220mLs of CLOUDY NP. All washes were 50mLs. 25% hot NaOH wash, hot dh20 wash, cold dh20 wash. Each wash ended up WHITE(!), so Swik decided to do more washes on the STILL cloudy NP. Done two more dh20 washes, then a hot dh20 wash, then another cold one. The NP was STILL cloudy and the washes STILL white. After the seven washes, Swik thought 'ok, this will not end. The NP must bee fine to titrate from now."
*Mean while, the coke bottle SHRUNK at the top, went SUPER hot, and STARTED BUBBLING!!! LIKE IT WAS GOING TO BOIL OVER!!!!! Swik quiclky moved this to the bath tub where it boiled over. It was literally steaming it was that hot. WTF happened?
*Titrated with 10drops acid in 50mLs water. Then with 5drops in a fresh 50mLs. Evapped and flashed to yield about 400mg of pfed. Another 10drops pull showed a tiny bit more pfed.

Swik does not like syrup anymore.
He think the pseudo was still in the BS that went down the bath or maybe in the collection of the seven white washwaters.

Ideally,
-I would have a 2L sep funnel
-Syrup would be clear, and would go white and cloudy when pH 14+
-pH meters would not turn themselves on and go flat for you
-The NP would either be clear, or clear up after three washes

This is not really a cry for help, a suggestion not to f*ck with syrup or maybe just some do's and dont's learned.

However, does anyone know,
Why did the NO go cloudy upon basing, and
Why didnt it clear up after SEVEN 1/4vol washes?

[embezzler]

xylene first?

sounds like it started to dissolve above room temp.

[kris_1108]

Yeah, I've done the same xtraction on two bottles and had no such problems.

[auntyjack]

maybe the blue seal sets things off?

[SHORTY]

I told you so!

Anyway, did you dilute the syrup at all? Why didn't you wash with xylene before basing?
You should make sure your naoh solution is thouroghly mixed and allowed to cool before using.
How do know that you added sufficient amount of acid?

[kris_1108]

Every time I say 'I' or 'me' in this post, I am actually referring to someone who is not me

First of all, let me say....  I told you so!
Yep, but you didnt tell me that I'd completely screw it up!  

Anyway, did you dilute the syrup at all?
I didnt dilute the syrup. I posted about such an extraction a while ago and concluded to let the naoh solution base the syrup. See here

Post 493480

(kris_1108: "Help with Pseudo Extraction from Syrup", Stimulants). Next time I attempt such an extraction, I will dilute the syrup, probably 50/50.


Why didn't you wash with xylene before basing?
I didnt do a xylene wash before basing bacause I think it is un-necessary. I may be wrong. (Well Im probably AM wrong). If I got as far as to produce a 'reduceable' amount of pseudo I could modify the extraction procedure according to the qulaity of the product. (i.e if the meth was shit I would wahs the syryp with xylene next time)

You should make sure your naoh solution is thouroghly mixed and allowed to cool before using.
The NaOH had fully dissolved before I added it. Regarding the temperature, I was worried about this a while ago, and checked with an elderbee, and he said its ok if its still slightly warm. I am not, by any means, saying that any one is 'wrong.' I just went by what I was told... I can wait for it to cool, though, no problem! If that will give me more chance of success

How do know that you added sufficient amount of acid?
I don't. My time was 'limited', if you know what I mean. I had the shits, I had only produced a small amount of pfed, and also thought that there would be some pseudo in the wash waters and in the boiling BS that went down the drain. Everything seemed to be going against me. The ph meter had batt flatteries. I, regretfully, thought 'bugger it' and packed up. Sure, I may (or may not) have lost pfed down the bath, but I should have pulled again from the NP and and also the washwaters.

I would like to thank you (Shorty) and Biotechdude and Geez (and others too) for all their help and guidance with not only this subject (pfed from syrup) but for everything. I have learnt so much over the last 6 or so months although I havent really done any ACTUAL exractions/reactions/recrystalizations/getinghighations, I find this stimulating    and educational. They didn't teach me this stuff in science at high school.
'Good Morning Mr Simpson, boys, and girls. My experiment is how to.....' haha wouldn't that go down well