DreaMTripper wrote:700mg of actives from 54g is a good yield! Explain further when this 2mm emulsion happened..
Thanks for chiming in DreaMTripper, appreciated.
There was no complaints with the 700mg agreed, goo or crystals - it's all wonderful stuff.
Obtained a small clipping of the same A.Floribunda (confirmed) that previous actives were extracted from today, so another small 50gm extraction is on the cards when time permits.
Now to the emulsion. Greatly suspect it was a contamination of having not cleaned the glassware correctly. Usually glassware is rinsed for a while with tap water then run naptha or iso through and coat/swirl completely and let it evaporate. Seems to have worked in the past - any tips there are appreciated.
The emulsion formed after the cold base was added to the warm acidic solution and agitated. Previously mentioned the acid soak in a heat bath was at a pH of 2. 35gm NaCl and Deionized water combined and heated. Not all the NaCL would disolve so more deion H20 added until complete saturation then drew off the required amount of liquid and added it to the main vessel. 50gm of NaOH was added to the prescribed 200ml deionized water added to the mix then topped up with the extra 140ml. It wasn't quite dark enough and the pH was a little low around 10.6, so 10gm more was added which raised it to 12.4.
The vessel was agitated lightly and rolled end over end, swirled to prevent settling and a good mixing motion. The emulsion starts to present itself here. More like a spotty / patchy layer of something. The same type of something that if you were to pull some basified solution and place it on clean glasswear and allow to dry, that colour, texture and symmetry.
A tiny bit more NaOH was added again to try and remove the emulsion. Then tried to syphon it off. More kept forming with each agitation - maybe trace amounts of detergent. But always the same sized layer. After the second heat bath it was quite established - the emulsion that is. Heat baths were kept around 50-55 degrees monitored with a thermometer.
What do you think of both the pictures? Saturated enough?
It looked quite clean in the post precipitation picture but it is as if it is some type of crystalisation that disolves back to water/solvent. It has to be some extraction of matter, water doesn't freeze like that, and we know naptha and ethanols don't freeze.
The combined pull in the first picture has been in the freezer now for 24 hours, it will remain there for a further 24 hours in the interest of patience and its importance in the process.
A hairdryer (cold air) was used blowing freezing air from the freezer into the dish to evap off the naptha after having left it sit upside down on paper for an hour. Then it all turned back to liquid.
With a bit of luck this serves you enough information.