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
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
