DUAL SOLOVENT CRYSTALIZATION AND SIMPLE TITRATION
BY DG
begin extraction ala Foaf
(i will add some thoughts here: more base is better! also, recommend extreme blending with water and base (paint mixer on high ) about 24hrs before any np is added. this frees up the goodies, but minimizes emulsions.
image one:
this is for the average guy, no special equipment needed, see pic
besides any appropriate safety gear, gloves goggles etc
jars w' lids
coffee filters
cotton balls
acetone
water
pipette or baster or tubing
ph down sulfuric acid- pet store
crock-pot or pan and spark less hotplate combo is nice here
basic wide range ph papers
funnel
a freezer helps
lots of possible work arounds, or other improvements to gear, suction and better filtration, pipettes, lab glass etc, etc
image two:
1.pull CLEAN np from vessel, if cloudy or milky, add it back to the vessel with the polar, and wait until it clears up! or let set in jar over night and decant clear np before proceeding
2. add 1/2 cup water and
3. 20-40 drops of acid to the np.
shake well
image three:
it will look like this
image four:
3. with baster, suck up some of the water/emulsion layer, and let water pour over ph papers as it goes back into the salting vessel
4. continues adding drops of acid, shaking, and ph testing until ph 6-7 is reached
image five:
now its time to rid ourselves of the emulsion, i find heat to be the most effective fool proof method to do this. BE SAFE, SPARK-LESS, VENTILATION ETC!!!!
heat until the solution is clear, both the np, and salted layer
see image six
image six:
decant clear layer, a baster is fine.
image seven:
stuff a cotton ball tightly into the funnel, pre wet/ test the cotton ball, it shouls slowly filter thru, too fast is bad..
if its tight enough, the traces of np that might come along will float and the water only will come thru
image eight:
combine all saltings before proceeding,
add water to glass or stainless steel pan, fast boil it down.
notes: you want to remove as much water as possible w/o scorching product, i like medium heat on an average gas range.
as the concentration of the solution increases the sound the boiling makes changes, and it sounds syrupy. you may also notice the solution get cloudy(a sure sign you have gone far enough.
if you dont boil off enough, thats ok! but you will need to add more acetone see image nine to get it looking like image ten...
image nine:
let the solution cool a bit, and add acetone20-50% of solution, depending on concentrations.... it may boil rapidly, use caution
image ten:
when enough acetone has been added, the solution will get cloudy-the start of xtal formation
toss it in the freezer, crystals form overnight
image eleven:
in the morning it looks like this
image twelve:
while still freezing cold, filter thru funnel and coffee filter
image thirteen:
let filter dry for a day or so
image fourteen:
enjoy
additional notes,
re-use all solvents!!
dg attached the following image(s):
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