Trying to cram a lot into one topic, but SWIM is going to share some findings which are intended to open a discussion to optimize extraction purity and yield...

Abstract:
In some side-by-side extractions using Heptane and Naphtha as solvents at elevated, yet different temperatures, several things were noticed about yield and purity from initial pulls. The reason for elevated temperatures is to increase the solubility of the solvent. The testing is not exhaustive and the intention of this it to open a forum for discussing in detail which solvents are best and what ratios and temperatures in which to perform an extraction. Ultimately, from this discussion, a refined method can come of this, or possibly scraping this method entirely and choosing something else. Also note: this is an on going test.

Based on previous extractions/results/experiences, Here are the inputs to the conducted tests. Only small test extractions were done.
-400ml distilled H2O
-67g LYE
-40g powdered MHRB
Allow mixture to sit at least 1.5 hours

Ex1: Heptane Pulls at elevated temperature: 145°F:
First Pull:
60ml Heptane added to solution at temperature of 145°F(Water Bath Temp appx 180°F - 200°F)
4 cycles of mixing. 1 cycle consists of 5 minutes gentle mixing/rolling of solution and solvent together, and then 5 minutes of rest in hot water bath.
On Last cycle, sitting time was extended to 10 minutes inside sep. funnel.
Throughout the 4 cycles, the average solution temperature was 140°F. Maximum noted temp was 151° and lowest was 130°. But Typical high was 145° and low was 135°.

Second Pull:
Same as first pull

Both Pulls FP'd

Results:
Total un-purified Yeild: 1022mg. Very Yellow-ish + some goop/oils. waxy. xtals.

Notes: Heptane became yellowish after first 15minutes of cycling.
FP was easy and relatively clean. Nothing floating in solution Heptane evaporates easily as well.


Ex2: Naphtha Pulls @ average water bath temperature of 130°F (Note:Test conducted at later time so some methodology changed)
4 Pulls total
1 Pull = 4 mixing Cycles with 30ml Naphtha
1 Cycle = 1 minute of gentle swirl/roll and 3 minutes in water bath
(like Noman's)

Combined 4 pulls in one container and covered tightly. FP'd.
Results:
620mg very slight yellow hue, NO goop. dry product.

Notes: Naphtha had taken very on little yellow tint...It stayed pretty clear throughout the pulling process.
FP much slower than Heptane, but FP crystals were slightly larger with Naphtha.


Ex3: Naphtha Pulls @ average water bath temperature of 200°F
4 Pulls total
1 Pull = 4 mixing Cycles with 20ml Naphtha
1 Cycle = 1 minute of gentle swirl/roll and 3 minutes in water bath
(like Noman's)

Using less Naphtha due to elevated and temperature and increased solubility.

Combined 4 pulls in one container and covered tightly. FP'd.
Results:


Notes: Naphtha had taken very on yellow tint, similar to Heptane experiment.
Again, FP much slower than Heptane.
Strained excess Naphtha and found less xtal growth, with a yellowish slurry below. Gritty. Naphtha is very slow at evaporating as compared to Heptane.

Results:
Coming soon!




Overall Notes:
Ex2 had cleanest results thus far. Naphtha is hard to evaporate..after working with Heptane and having seen it evaporate instantly it's frustrating.
Based on Ex1 and Ex3, higher temps increase to solubility, but they will dissolve in more unwanted crap(oils, whatever else) into solution and seem to hog up space so less of the desired solute is absorbed into the solvent.



Future tests:
Room Temp Naphtha and Room Temp Heptane


Please comment, critique, and make suggestions to any all aspects of this thread. If some information is left out or confusing, please let us know. More testing is to be done. Ex3 will be updated ASAP.

Regards,
HT

Heat drove oils and plant crud into your heptane on your first pulls, and that's why the naptha pulls came out cleaner.
Pulling with heptane and then naptha is a good way to get nice clean product at first and then a broader spectrum later, but if you want to compare the two, next time you should split the basified solution in half and pull each half with naptha and heptane - this will give you an apples to apples comparison.
I usually save heat until the end so that I'm getting clean product at first and making sure that I'm not leaving anything behind at the end.
Good work. Keep at it.

Thanks. Yea, heat seems to very touchy too hot and you get unwanted solute and too cold and there's trouble separating the solution from the solvent. On that note, another thing noticed was Naphtha seems to separate from the bassified solution a little quicker than the Heptane, but also noticed that room temp extractions have a slower separation time between base and solvent. But in this case, SWIM may have accidentally gotten a little aggressive with the rolling this time and is now in emulsion purgatory...Thinking centrifuge...

SWIM's Update in process:

"Room Temp"(herein "RT"
Ex4: Naphtha Pulls @ average water bath temperature of 120°F - 130°F Trying to Keep Solution around 100°F (Note:Updated Methodology)
5 Pulls total
1 Pull = 3 mixing Cycles with 25ml Naphtha <-Changed to 3 mixing cycles from 4.
1 Cycle = 1 minute of gentle swirl/roll and 3 minutes in water bath or air to keep solution around 100°F *
*Wait 10 minutes after 3rd mixing to allow NPS to separate from solution. Some cases 15 minutes wait.

Pull1: 25ml in ->appx 22ml out
Pull2: 25ml in ->22ml out
Pull3: 25ml in ->15ml out (low, but SWIM moved on)
Pull4: 30ml in ->20ml out

--4 pulls FP'd in separate sealed containers and wait overnight--

Pull5: 0ml in -> 20ml out (Let remaining 26ml to separate from solution overnight at room temp.) it seems that as gentle as the rolling it, some NPS still gets emulsified


Notes/Observations: Again Naphtha had taken light yellow tint.... pulls 1 and 2 appear to have nice yields from FP. Pull 3 is minimal, but clean and pull 4 seems to be about 1/4 of pulls 1 and 2. All white-ish xtals. minimal gunk/yellow.

Pulls 1-4 are evaporating/drying
Pull 5 FPing.


Results:
Pull1:233mg
Pull2:161mg
Pull3:31mg
Pull4: 47mg

total: 472mg from 40g bark-> 1.2% yield.
crystals have very little yellow and should clean up to nice and white after Heptane Re-X.


Pull5: ...still waiting....




Future tests:
Change to 2 cycles of 50ml "RT" Naphtha. 2 pulls. Wait overnight to pull remaining solvent from first 2 pulls. Thoughts?
Try same exact scenario with Heptane at NPS.


Keep your thoughts coming.

Regarding your emulsion problem, there is an easy way, to get the two layers properly separated.
Add a bit more lye, this always worked for me when I used heptane and naphta. I´ve heard that salt (NaCl) might also work to break the emulsion.

Now I´m using benzinum medizinale (Wundbenzin; mostly pentanes; no heat necessary) and I´m shaking!!! the hell out of my mix, because this softly rolling thing makes me bored.
My mix clears up in about 15 minutes. I give it 3 shakes per pull, and need only 3 pulls to yield about 2% out of mhrb.
Therefor I´m using the following ratios 1/1.5-2/15 MHRB/lye/water.

The bezinum medizinale seems to be very selective, because it only pulls tiny amounts of oils etc. The spice comes out nearly white.