foafs stb questions

[highRvibratoryfreq]

Hi im just starting out with this tek for the first time and have a few questions..

im doing a small test batch with

100 grams dried p.torch chips
100 grams lye
1.5 litres of water

ive blended the mix heavily and left to sit for nearly 24 hours. now im curious as to the texture i should be looking for, it is still a little bit snotty, nowhere near as bad as when i first added the base but still not completely runny.
is it ok to add the xylene too now?
i dont want to end up with a horrible emulsion i cant break.
i will keep the whole thing heated when i add the nps
i just want to be sure that its broken down enough and minimal snottiness is acceptable!

thanks

 

[dg]

it should be runny. add another 50g lye then
go ahead w/your pull(add nps)

no need to mix the heck out of it. but when the ph is at 14 you should be able to mix it thoroughly and still have it separate quickly. the heat will help

feel free to pm me if you have troubles

 

[highRvibratoryfreq]

i checked ph was at 13 so ive added another 50 grams of lye, and remixed will do the pulls later..

do you use the paint mixer to mix the nps aswell? im using an electric hand whisk as this batch obviously doesnt need a big mixer ill try to mix at a low speed for say 5 mins then leave it sit for an hour or 2 between each pull, ill keep it in a bucket of hot water the whole time aswell

ill post the results

 

[highRvibratoryfreq]

oh one more question..

i have 96% sulphuric acid should i make a weaker solution to add dropwise onto the nps if so what percentage should i aim for?

 

[cyb]

13 is fine...don't overdo the lye..it may make the solvent very dark....

 

[highRvibratoryfreq]

ok so i added the xylene and mixed and it seems to have got lost in the soup which is what i was worried about im leaving it in hot water. any ideas on how to free it up or should i just add more xylene and mix a bit more gently the second time,id say about 50 ml out of 200 has re-surfaced and its been sitting half an hour.

 

[Phlux-]

salt often works well for breaking up emulsions

 

[dg]

13 is fine...don't overdo the lye..it may make the solvent very dark....

??
nothing wrong w/dark solvent- wont effect saltings

as for the emulsion- base- heat- time
(dont mix so much next time )

yes- dilute the acid considerably!
its very easy to overshoot your titration

 

[highRvibratoryfreq]

well the 200ml i lost initially has never made it back out i definitely overmixed, also im thinking the mixture is too thick its dense and still slightly slimy so maybe more water was needed.

ive done 4 pulls around 600 mls total. i did the extraction in a large glass mason jar, and tried just rolling the solution and occasionaly stirring as the cactus didnt eat the nps this way, left it for atleast an hour or 2 between each one.

the colour of the nps certainly isnt dark its piss yellow.

i will make a ph 3 sulphuric acid solution with distilled water
then add 5 mls plain distilled water
then add dilute acid drip by drip into the bottle around 25 mls shake and test the ph.
then keep adding more dilute acid and rechecking until ph reaches 6-7
then repeat 2 more times
pool the 3 saltings filter reduce
then add the 60 percent acetone
and freeze!

hope thats right still a little confused on the titration

 

[highRvibratoryfreq]

2 drops of 96% sulphuric acid were dissolved in around 220mls of distilled water to reach a ph of about 2.9

first salting came out at 6.6

second @ 10.5

third salting @10.4

why second and third so high?? too much acid added?

ive combined the second and third and kept the first seperate.

first salt i just evap'd i figured if theres hardly any thing there no point recrystalizing in acetone just yet. after evap no more than 20-30mg white crystalline sulphates were recovered

and after evap of the second and third salting no more than 60mg recovered this was darker coloured and clearly not as clean most likely due to high ph pulling more crap?

so no more than 100 mg total yield which surely means i havent mixed the nps well enough in the cactus slurry.

so ive re added half the xylene placed in a hot water bath and blended for about a minute. will wait for emulsion to seperate and do another pull and hopefully see if it get more this time around.

i still believe the mixture is too thick would it be worth adding more water at this point to thin it out maybe the xylene will be able to grab all the alks easier?

 

[Bezerker]

dg said:

as for the emulsion- base- heat- time

Your first post was 1-17-13

You posted results on 1-18-13

Your supposed to wait at least 48hrs after mixing your slurry/np before you pull your np.

I think dg waits 24 hrs after mixing his slurry before adding the np.

Emulsions take time...be patient.

op said:

why second and third so high?? too much acid added?

High ph is basic....you need to get your ph around 6-7 during your salting. Too much acid will lower your ph not increase it.

With 100g starting material, you'll be lucky to get 1-1.5g of goodies. My guess is you'll yield less than 1g.

 

[highRvibratoryfreq]

i left the slurry to base for 24 hours

and ive noticed now that when i mix the nps and leave it in the hot bath it clears in about 3 hours. so the first runs i think i didnt mix enough and was too impatient/ worried it was emulsified and wouldnt come out.

48 hours seems like a long time between each pull in that case it would take 8 days to do 4 pulls! surely thats not right...

and as for the salting your right i should have been adding more acid to bring it down lower.

getting there slowly :thumb_up:

 

[Bezerker]

from foaf's STB cactus tek:

and let it settle at least 2 days undisturbed, 2 days is very important.

Maybe that has changed, but thats what I do. These cactus extractions take time.

 

[Phlux-]

check the extraction questions thread - you may find some info there
2 day long pulls ? totally not required

 

[highRvibratoryfreq]

ok im in the midst of my second attempt at titrations this time from a much darker better mixed nps..

now ive been adding mixing and ph testing with a digital ph pen and the ph just doesnt seem to want to go below 9. ive added atleast 200 mls of ph 3 solution and it keeps coming back out at 9. is this ok? should i just keep adding more and more ph 3 solution until the ph gets down to 6-7?

 

[highRvibratoryfreq]

i seperated the salting, and added another 10 mls of distilled water followed by approx 15 mls of ph 3 shook and ph came down to 6.8 so i seperated and repeated again this time ph came down slightly too much around 5.8.

i evap'd the first pull which didnt drop below 10 this yielded 0.4 grams of slightly green and waxy sulphate xtals, maybe i over shook from re adding ph3 solution and shaking/adding more about 5 or 6 times

the evap from the second and third salt crystallised into a beautiful sheet of needle xtals :want: and after drying and scraping they have a slight yellow and white tint very sparkly and fluffy not too waxy, this yielded 0.4 aswell.

so including yesterdays under mixed pull that brings the total to 0.9 grams

im going to do another round of pulls on the cactus soup just too see whats left

then i will redissolve everything ive pulled in a minimal amount of warm water and try adding the acetone and crashing out some lovely needles

now one last question!

is it a good idea to mix the slightly green waxy extract with the nice clean fluffy slightly yellow stuff when i do the re-x or will the impuritys still be recrystallised aswell?

would it be better to treat them seperately? im just worried that 400mg is a small amount to work with.

thanks for all the help everyone. im very happy with the results from my first cactus extraction :thumb_up:

 

[ipumaestro]

totally up to you, you could contrast the two or just combine and use it all anyway

 

[dg]

ok im in the midst of my second attempt at titrations this time from a much darker better mixed nps..

now ive been adding mixing and ph testing with a digital ph pen and the ph just doesnt seem to want to go below 9. ive added atleast 200 mls of ph 3 solution and it keeps coming back out at 9. is this ok? should i just keep adding more and more ph 3 solution until the ph gets down to 6-7?

1st. are you positive you didn't suck up some base with the nps?
if you are- then ph 9 is good. needing to add more acid means there is likely a fair mount of alkaloids present
yes keep adding acid until the ph is 6-7

 

[dg]

now one last question!

is it a good idea to mix the slightly green waxy extract with the nice clean fluffy slightly yellow stuff when i do the re-x or will the impuritys still be recrystallised aswell?

would it be better to treat them seperately? im just worried that 400mg is a small amount to work with.

thanks for all the help everyone. im very happy with the results from my first cactus extraction :thumb_up:

sounds like you've made some extra work for yourself.
next time take all the water from all the saltings and combine them before any reduction takes place.
less loss on surfaces and muck quicker.

yes add them together. you'll be surprised at how pure the crystals are when crashed from acetone and water. it leaves all the impurity out.

when you combine your material and add HOT water to dissolve- it is still good to reduce the amount of water over heat until the mix changes in consistency (when boiling it starts to spit like water/oil. or if not boiling starts to precip out around the edges)

 

[highRvibratoryfreq]

yes pretty sure.. the nps had been left for hours was well heated and clear when i siphoned it off

however after shaking i did get this layer of white precipitation between the nps and the acid water also even with heating and leaving for some time it seemed hard to totally break up the emulsion lots of milky looking bubbles that just didnt seem to want to free themselves, i ended up pouring off the clear stuff then after a while the remaining emulsion that wouldnt clear i poured through a cotton filter twice over which seemed to leave behind the nps and seperated out the last bit of clear solution.