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topper
#1 Posted : 11/13/2013 3:25:25 AM
Just starting out and I've read joshisom's a/b tek originally posted on 5/8/13. How long does this method take from the acid boil to the final product? If I followed the time frame correctly it added up to about 5 days....? Is this accurate or have I misread
Thanks!
"Never look back unless you plan on going that way."
HDT
 
shanedudddy2
#2 Posted : 11/14/2013 1:24:38 AM
Are you using MHRB or Acacia? I would suggest an STB for your first extraction.
It's considerably easier, and cleaner (less mess as there's no filtering of bark from the liquid).
The result is less pure, but that can be resolving by recrystalisation.

I personally use big 4L HDP jugs.
Before starting, you`ll want to get the lid off another 4L HDP jug (buy 2 or more of the same jugs) and use scissors to make a circular hole in the top of the plastic lid. You want to make the hole small enough to push in plastic tubing, and not leak.
When using the scissors to make the hole, which ever direction you are pushing outwards, feed the tube through this direction.
Push the tube through until only a centimeter or 2 is inside of the cap, (the bottle side).
You now have a cap + tube device that can easily be used to separate polar (basic solution) and non-polar (naptha) liquids.

I then add 250g of NaOH, 250g of Bark, then water...leaving some room for shaking.
Then, add a small amount of Naptha, I use ~100mls or so.
Give a good solid shake sessions every so often (using the untouched cap).
Let this sit on your final shake until the next day.
The next day, switch the cap to the modified cap + tube device.
When this cap is firmly in place, squeeze bottom ever so gently, and the solutions will rise, with minimal disturbance.
Place the other end of the tubing into a dish, and squeeze out the saturated naptha.
[This is best done with 2 people, one squeezing, the other holding the other end of the tubing.]
This can then be evaporated down and freeze-precipitated.
I normally do further shakes and then another pull the next day as well... I use Toluene, so 2 pulls is all I really need.
Have any questions, let me know.

I may make a more concise tek (with pictures and added descriptions) some time.
 
topper
#3 Posted : 11/14/2013 1:48:22 AM
Thanks for the info. I will explore the STB techs a little more before making a final choice.
"Never look back unless you plan on going that way."
HDT
 
dooby
#4 Posted : 11/14/2013 3:08:03 AM
Hello,

I would suggest you look into Cybs hybrid salt tek, it can be followed to the absolute T, but there is also plenty of room to adjust the time frame to your own wishes or needs without too much of a detrimental effect (if any) to your yield (if done correctly)...

Also, try not to use any plastic, aluminium or rubber for anything that will or may come into contact with your basic solution and/or naphtha - glass and stainless steel (oven-safe glassware is often made of borosilicate glass which is the same as what labs use) can be found easily and cheaply at a decent kitchen/cookware/cutlery store (sorry wouldn't know what to call such a place in Enlish)... You may choose not to care about this, it's your life...

Goggles, nitrile gloves and adequate ventilation are also things you will only regret not having paid attention to when it's already to late - better not sorry than unsafe Pleased

PLUR

My avatar was taken from google images and is actually a work of art by NEIL GIBSON, credit where credit is due!


Bodies don't have souls - souls have bodies


Old enough to know better, young enough to try again
 
topper
#5 Posted : 11/14/2013 6:57:30 AM
Excellent! thanks for the help. I am using ARB. I have 100g blended up and in the freezer. I purchased a glass syphon, several Pyrex dishes and a 600ml wide mouth test tube. I already have goggles, gloves and a canister style face mask(I work with epoxy in my spare time) which may be overkill but better to be safe I figure. I hope to start next week as my weekend is already full. I will post my progress. Thanks again for sharing your experience and knowledge.

T
"Never look back unless you plan on going that way."
HDT
 
topper
#6 Posted : 11/14/2013 7:30:36 AM
I just read Cybs hybrid salt tek and you are right, it sounds super easy and fairly quick. I am still wondering how to store the water/lye solution while I am freezing the naphtha from the first pull. I have read that it is best to reuse the naphtha for the 2nd and 3rd pull because it is saturated with product and will increase yield. Any thoughts? Should I just cap it tightly and place it in a cool, dark area for 12-18 hrs while I wait for the freeze precip or just use fresh naphtha for the subsequent pulls?
"Never look back unless you plan on going that way."
HDT
 
dooby
#7 Posted : 11/14/2013 11:07:54 AM
Both are possible, much depends on how much time, naphtha, freezer space etc. you have...

Besides, if you'll be doing 4-5 pulls and leave your solvent in the freezer for 12-18 hours in between them, your extraction might take a long time...

Also, less saturated pulls tend to have a need to be pre-evaporated before being put in the freezer or there won't be that much precipitating...

There are alternative options however... You could do a pull, salt it with vinegar, let separate, decant naphtha for next pull, save vinegar (now containing your product)... This step will take one hour at the most... At the end of your process, re-base the vinegar and pull again with naphtha... Not only can this save you from having to pre-evap some of your naphtha, it is also a purification step, as some of the impurities in the naphtha will not form acetates and will not be soluble in water (main component of vinegar)...

One thing you may also consider is not doing the heat baths that are mentioned in Cybs tek... The saturation of your pulls will increase as the temperature differential between solution and solvent gets bigger... Hot solvent in room-temperature solution... The trick is then to have it separated and pulled before the temperature between the two liquids is equalized...

Edit - Also, try not to discard of anything until you have your final yield - this way you'll be able to correct most if not all of the mistakes you may have made...

Hope this helps Pleased

PLUR

PS May your yield be pure and plentiful Pleased
My avatar was taken from google images and is actually a work of art by NEIL GIBSON, credit where credit is due!


Bodies don't have souls - souls have bodies


Old enough to know better, young enough to try again
 
topper
#8 Posted : 11/14/2013 5:21:50 PM
So awesome!!! Thanks again and again. Hoping to one day be very proficient at this and have all the answers Pleased
"Never look back unless you plan on going that way."
HDT
 
 
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