1st extraction fail :(

[spaceshuttle]

i tried my first extraction yesterday using nomans tek.

i got nothing but some tiny white specks in my glass dish

i think the part i went wrong was the amount of KN03 i used, potassium hydroxide (40% in water)
perhaps didn't use enough.

to get the PH up to around 13 i added 3ml of 40%/KNO3--60%/H20. (i used volume calculations because i dont have a PH tester)

i used "Shellite" (100% hydrocarbons)

i kept the temp of the whole solution between 40c-50c the whole time.

did 3 pulls, 18hrs in the freezer and then 1 hr evap outside.

other than that, every other step was the same as the tek.

 

[spaceshuttle]

can anyone shed some light on how much KN03 to add? the solution is 400g/l or 40%. should i add by weight the same amount as if it were lye?

 

[alive]

Hi
Sorry if I have misread but I understand that you "put the solvent in the freezer, then evaporate solvent". Did you pour off the solvent before the evaporation step? Were there visible crystals after freeze perciperation?
If you still have the solvent you used, try evaporating a bit of it until it turns milky and then freeze percip. It sounds like you have the rest of the tek down just fine.

KNO3 is potassium nitrate, also known as saltpeter (afaik). You're supposed to use drain cleaner, aka potassium hydroxide, aka lye. Could you double-check the label on your chemical and confirm whether you used KNO3 or NaOH?

 

[spaceshuttle]

i gave it another shot, i added 125ml of the solution to get 50g of KN03 for the 50g of MHRB i used.

straight away i noticed the solution was much darker once i added the MHRB. did 3 pulls. checked them after 30mins in the freezer and could see some magic starting to happen, will update in the morning. im planning on leaving it in the freezer overnight and then slowly evaporating it by covering the jars by about 70%.

i will post some pics tomorrow

 

[spaceshuttle]

thanks for the reply, yes its potassium nitrate KN03, . and second time round worked well, first pull was .5g

 

[tele]

If you keep failing, try another tek. With q21q21's white dmt tek it's hard to fail.

 

[spaceshuttle]

ps the best NaOH i can get in Australia is 55%, thats why iv used KN03

 

[gory dkalz]

Forgive me for my ignorance, but isn't mixing an oxidizing agent (potassium nitrate) with naphtha potentially dangerous?

And would the KNO3 even work in an extraction at all?

 

[ragabr]

What are you evaporating after the freeze precipitation? Are you pouring the solvent off and then evaporating the product, or are you precipitating and then allowing the solvent to get warm again?

 

[spaceshuttle]

ragabr- im poring it off and then evaporating the product in the fridge. should i be doing it differently.

gory dkalz - The KN03 worked well with the right amount, i read that it was safe to use, please correct me if im wrong

 

[gory dkalz]

Well if it works and gives you good clean spice, than I guess you are good. I wasn't 100% sure but I remember reading something on a naphtha bottle about keeping away from strong oxidizers. I guess KNO3 isn't a strong enough oxidizer to cause a problem.

 

[ragabr]

Hey spaceshuttle, that sounds right. Now that you've figured out your base, have you gone back and tried basing the original material that you boiled, like an STB on the leftovers, to see if there was anything left?

 

[spaceshuttle]

Hey spaceshuttle, that sounds right. Now that you've figured out your base, have you gone back and tried basing the original material that you boiled, like an STB on the leftovers, to see if there was anything left?

yep, its in the freezer now, will post results in 24hrs

 

[spaceshuttle]

Well if it works and gives you good clean spice, than I guess you are good. I wasn't 100% sure but I remember reading something on a naphtha bottle about keeping away from strong oxidizers. I guess KNO3 isn't a strong enough oxidizer to cause a problem.

as long as nothing is on fire then its not a problem.
in the event of a fire, an oxidizer will allow the naptha to burn more violently.
(any one correct me if im mistaken)

 

[geometric_wisdom]

No, not potassium nitrate, that is an oxidizing agent, not a base. you want to use sodium hydroxide "lye" "caustic soda" is all names it comes under. its used in drain cleaner, but i cant stress to you enough, it has to be 98% or more of sodium hydroxide or you are poisoning yourself. that will get ph to 14
and then mix with warm solvent and separate the solvent.
decant the solvent multiple times until its totally purely clean, put that in the freezer with an airtight lid or plastic wrap. then leave it for 24-48 hours and you will have xtals, to make scraping up easier, you can evap until not much solvent left and solvent is all cloudy. then do the freezer thing. better xtals

 

[geometric_wisdom]

ps the best NaOH i can get in Australia is 55%, thats why iv used KN03

go to woolworths go into the laundry section and get "caustic soda" from MECHANIX. its 98% pure, you can find the MSDS online