foafs stb questions

[highRvibratoryfreq]

in the future i will do the acetone crash straight away. as this was my first time and i wasnt too sure if i was doing everything right i thought it best too see if i was actually getting everything out before i tried recrystallizing.

thanks again for all the help dg :thumb_up:

 

[dg]

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.

you done good w/the funnel
getting it really hot will break the emulsion for the most part

 

[highRvibratoryfreq]

another question for you dg

when you mix your nps in the 5gallon (20litre) bucket do you find the solvent is quite spread out and its difficult to siphon all of it off? or do you work on the fact that the majority of alkaloids move over into the bulk of the solvent over the course of all 4 pulls. id imagine that atleast a few hundred mls would be unretrievable unless you poured the mix into some sort of column to get the last of it out.

 

[dg]

yeah you never get it all

using a tall thin container to get the last lil bit should work

 

[Phlux-]

using a large plastic container with a large bore tap fitted to the bottom works to let all the basic solution out - leaving mostly xylene - then decanting the top layer including some base water into a narrow vessel is a good way to get it all. like i stated in the extraction questions thread - a large surface area between np and basic solution seems very efficient in minimizing the amount of pulls required.

 

[highRvibratoryfreq]

ok so the last pull i did instead of evaping i reduced and added my 0.9g of material got it down to a bubbling syrup approx 20-30 mls i then added approx 50 mls of fridge temperature acetone it went cloudy and i stuck in the freezer

just went to check and no crystals formed just a very thick syrupy mass with the odd crystal floating around no needles maybe i was impatient but i stuck another 40mls of acetone in there to loosen things up a bit and have put it back in the freezer.

from what ive read people were seeing crystals form in a few hours, id left mine easily 7 or 8 hours. hopefully in the morning there will be lots of goodies precipitated

 

[highRvibratoryfreq]

results are in

first 2 pictures are of evaporation of the cleanest salting and then scraped into a pile

next images are after dual solvent recrystallization final image is the contents of the acetone evap'd next to the clean sulphate crystals

the white shiny crystals weighed in at 0.7g and the brown crude remians at 0.3g

so 1gram total not bad eh?

one final question..

how come i didnt end up with pin needle crystals do i just need to let these dry more and break them apart? is it anything to do with overshooting a couple of my titrations a little? it still looks very very clean and i am more than happy with the results for my first cactus extraction, im sure they will only get better!!

:thumb_up: again to everybody who gave me good advice particularly dg very much appreciated kudos to you all!

 

[highRvibratoryfreq]

note images now in reverse order!

 

[Pup Tentacle]

using a large plastic container with a large bore tap fitted to the bottom works to let all the basic solution out - leaving mostly xylene

not concerned that the xylene may pull nasties from the plastic bucket?

 

[ipumaestro]

hdpe 2 i assume ^^

 

[Parshvik Chintan]

hdpe 2 i assume ^^

even still... i am fairly sure xylene leeches some of the plasticizers

 

[Pup Tentacle]

indeed - Snozz posted this in another thread - be careful friends

None of them.

Use glass

Phillips lists two major classes of chemicals that are not compatible with HDPE: aromatic hydrocarbons, and halogenated hydrocarbons. The basic aromatic hydrocarbon is benzene (a major component of gasoline); others are toluene (also called methylbenzene), and the three xylenes (o-, m-and p-xylene). Others include naphthalene (moth balls), and pdichlorobenzene (also moth balls). These aromatic hydrocarbons "permeate excessively and cause package deformation," says Phillips.

Source

 

[Phlux-]

heh i said plastic as i have seen it being used alot on the forum - personally, i always use borosilicate glass like pyrex for everything.