Finnaly my friend did finnish his LWR.
It stood for about 48 hrs with the following ratio
11g E.HCl
13.2g I2
5.5g rP
8.8 dh20
Placed in oilbath @ 120 <-> 130C (oilbath temp) for about 48 hrs.
NP Solvent of choice: Toulene
Took of condenser and boiled off remaining iodine for 15 min.
Added 30 ml h20 to rxn fluid. Water turned milky orange just as some bee said.
rP fell to bottom like bricks after swirling. He then prewetted filter with dh20
and filtered the rxn fluid.
Then he added 20 ml to rxnbottle, swirled, and filtered this into the 30 ml he already had.
Time for NP washes.
2 x 50ml and one 100ml. NP looked pissyellow.
But he knew it was iodine as he has been there before and panicked...
Read ph, was between 0 and 1.
Added NaOH sullotion and checked Ph; around 5.
He based some more until no more colorchange cold be seen.
Checked PH again 15.
Seemed like meth oil floated on top, cause he saw a yellowish layer on top.
It could also be poorly decanted np with i2 in, but he didnt think so.
Layer was about 3ml in a 250ml beeker.
Aqua-layer started to semi-solidify, added some hot dh20.
Worked like a charm.
Started np-extraction.
Added 200 ml np.
Sepfunnel only 100ml, so he had to use a bottle to shake and carefuly decant.
He shook like hell, let sit for 15 min and decanted.
Repeated this three times.
Now he was left with 600ml np solvent.
Read geez's wonderful post, and tried to extract with 3x125 ml dh20.
Lost his dammed pipette so he measured HCl by ml.
He added 5 ml hcl on the first extract.
Shook, let sit 15 min, decanted and checked PH.
Ph was around 7.
Added 2 ml hcl on next 125ml dh20 extract. Ph was now way down to about 3.
Shook, let sit 15 min, decanted.
On the last extract he only had a few drops of HCl.
Finnaly he was to evap. the h20.
This took quite some time, and when he looked for crystals to form, there only
came a yellow sludge that never wanted to crystlize.
After some time he decided to try to flood with acetone.
This worked somewhat and removed the yellow acid remains.
He filtered the tone, and was left with some white powder.
Yeilds however where devastationly low.
He wondered if he used the right volumes for extractions.
Like for instance; should he really use 3x200 ml of NP to extract amines?
If you bees have any tips on increasing yeilds he would be forever grateful!
Thanks to geez, wareami and all you others that helped him out this far.
He is forever indebted to you all!