Cheelin
Rising Star
Finally ready to start the Solvent Repeated Reuse trial.
2/3: I have 5 jars of previously sodium carbonate-water washed solvents in the freezer (washing treatment B): Solvent S (S-S) - used standard solvent; S-B - used solvent from boiled-water paste; S-M - used solvent from microwaved paste; S-C - used solvent from chilled paste; and S-MC - used solvent from microwaved & chilled paste.
Once the ice puck and shards are removed from each jar, the first of three additional serial washing-freezing-extraction cycles will be run with these solvents versus a fresh EA run. The first extractions will be run using the standard tek scaled for 45g cactus powder runs using passive crystallization. The two subsequent sets of runs will be run the same way, but each will use 15g less cactus powder than the preceding sets of runs, to ensure that sufficient amounts of each solvent are available to complete the series.
2/6: Got delayed a couple days, didn’t have any observable effect vs 24-hr freeze. Decanted solutions through wire strainer-paper coffee filter-funnel into collection jars, separating ice shards from solution; frozen sodium carbonate pucks remained in original jars. All jars have a haze, so will let them settle a day or two, and decide whether I take the time & effort to do a dry sodium carbonate addition, before proceeding to the extraction runs. Once ready, I’ll post pH’s and a pic of solvnts.
2/10: Several layers of haze have settled, but jars still remain slightly hazy, I said screw it (with an F), and took the day off to run six 45g standard, scaled cactus powder runs, with the five once-used, washed solvents listed above and a fresh jar of EA. They all started at the same pH=5, nothing unusual to report through salting. Pics of the solvents and combined pulls are attached. Yields and any significant observations will be reported after 72hrs of passive crystallization.
2/13: All runs filtered after 72hrs passive crystallization, jars rinsed 2x w 5ml fresh EA and dumped through filter, filter rinsed 1x w 10 mL fresh EA, filtrated rinsed 1x w 10mL fresh EA. Pic, after filters appeared dry, attached. Jars washed 2x w 5mL hot distilled water, evaporated, scraped. All runs produced same appearance, fluffy white needles; which at these quantities is quite a beautiful sight. Total yield for each run rounded to 1.7%: fresh EA 0.754g, reused standard solvent 0.779g, reused solvent from paste made with boiled water 0.765g, reused solvent from microwaved paste 0.775g, reused solvent from paste made with chilled solvent 0.760g, reused solvent from microwaved paste made with chilled solvent 0.762g. Imo, quantities larger than fresh EA run are the result of slight calcium citrate precipitate from washed solvent.
Solvents will be washed with sodium carbonate-water method (steps 2 - 5 described here: https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1133316#post1133316 ), and after settling clear will be frozen for 24-hrs, decanted off of ice, then run in 2nd reuse.
2/20: After cloudiness settled, but all jars still had a haze, jars were put in fridge for 3 hours, appearing clear they were removed and allowed to come to ambient temp, a slight haze remained, but were placed in freezer.
2/21: after 24 hrs in freezer, jars were each decanted through a previously chilled seive-coffee filter-funnel to remove ice shards. Filtered solvents all had a heavy haze (not cloudy), and placed in fridge for 3 hours to settle haze, then stored at room temp.
Approximately 320 mL recovered of each de-iced washed solvent. Ice, defrosted puck water, and some amount of solvent trapped with ice shards were collected in a waste jar for further settling/separation.
2/23: Started 2nd Re-Use Trial, using six 30g cactus powder samples with scaled ingredients in: fresh Ethyl Acetate, and the five used solvents tested earlier. Each paste wss prepared in the standard way, then pulled 6 times (1 min stir, 2 min rest prr pull). This is the 3rd use (2nd re-use) of the five used solvents, Prior to salting each jar with 1.5g of citric acid, each jar was settled for at least one hour. No water was observed in the solvents, however all jars except the fresh EA jar had significant haziness. The hars will be passively crystallized for 72 hours.
2/26: Jars filtered after 72 hrs, jar washes evaporated; pic of drying filtrate below. The fresh solvent yielded 0.4683g, 1.6%, the yields of solvents’ 3rd use were: solvent that originally pulled standard paste 0,5745g, 1.9%; solvent that originally pulled boiled water paste 0.6072g, 2.0%; solvent that originally pulled microwaved paste 0.5863g, 2.0%; solvent that originally was chilled and pulled chilled paste 0.5873g, 2.0%; solvent that was originally chilled and pulled microwaved & chilled paste 0.6845g, 2.3%. Product from each run appeared and tasted similar, and had consistent appearance and taste as earlier runs.
I doubt the higher yields from the reused solvent runs vs the fresh solvent had anything to do with higher M levels, the cactus powder was the same for all runs and I doubt that any M from earlier runs remained in the reused solvents after the sodium carbonate-water washes and freezing. Rather, the higher yields are likely due to precipitation of calcium citrate.
In the next few days I’ll wash the solvents again, settle, and then freeze them. After removing the ice and letting them clear, I’ll do the 3rd reuse (4th run). I will be focusing on doing this next set of runs with crystal clear solvents (unlike the run that just finished), to see if this approach can reduce the suspected calcium citrate precipitation. It may take some extra time to get the solvents to settle clearly.
3/4: Light stirred 42mL of washing solution into each jar containing approx 280mL of solvent; after layers appeared, stirred 5 full revolutions (5 seconds; enough to fully mix layers); washing solution made according to previously mentioned post. Initial pH ~3.0, post mix pH 4.0; got to get back to pH of 5-ish, after an hour stirred 5 more revolutions (5 secs), in hopes of neutralizing with minimum haze after settling.
3/5: Light stirring has helped improve settling speed, solvent layer about 1/4 clear in 24 hrs; However, initial stir-in plus 2 light stirs only partially neutralized pH. Did one additional 5 revolution stir today, pH rose to comparable (5-ish) level of fresh EA. Will let solvents settle, then freeze & decant.
Due to large excess yields in previous run (more than this cactus powder yields), I want to try to rule out the possibility that dissolved M is remaining in the solvents after the washing process. So, after this washing cycle, I’ll re-salt the solvents with citric acid to see if any crystallization occurs; if M crystals do not form, I think it will be safe to assume that the excess yield is due to calcium citrate precipitation. After re-salting, I’l re-nuetralize, wait until solvents become crystal clear w no haze at all, then do another decant to minimize calcium citrate (could be a long time waiting for gravity to do this), and then begin 4th-use run.
3/9: Decided yesterday, in an attempt to reduce haziness after freezing, to syringe decant the cleared solvent (~80%) to clean jars, and then further decanted 90% of the hazy remainder to testtubes. I’ll decant the clear portion in the tubes & recombine the cleared portions after a few more days of settling. The cloudy/hazy residuals were decanted off the sodium carbonate and water, combined to settle, for future reuse.
Hoping to freeze, filter off ice, proceed to salting w citrate (to determine whether any M remains in solution after washing) this weekend. Then do final neutralization, and re-use.
3/12: Syringe decanted (using 100ml glass, gasketless syringe) the haze-free portion of solvents out of testtubes into the previously cleared solvents, put them all in for 24 hr freeze. Will cold filter-decant off of ice tomorrow, and then proceed to re-salting with citrate.
3/13: Cold filtered the solvents, all had significant and roughly equal amounts of ice shards. Dropped one of the jars, no further “boiled” solvent, insert expletives here! After warming to ambient, all jars remained clear; added 0.9g citric acid to each jar and stirred a couple revs. They all clouded, but seem to be precipitating what looks like a slight amount of calcium citrate powder. Will settle until clear, decant, then neutralize.
2/3: I have 5 jars of previously sodium carbonate-water washed solvents in the freezer (washing treatment B): Solvent S (S-S) - used standard solvent; S-B - used solvent from boiled-water paste; S-M - used solvent from microwaved paste; S-C - used solvent from chilled paste; and S-MC - used solvent from microwaved & chilled paste.
Once the ice puck and shards are removed from each jar, the first of three additional serial washing-freezing-extraction cycles will be run with these solvents versus a fresh EA run. The first extractions will be run using the standard tek scaled for 45g cactus powder runs using passive crystallization. The two subsequent sets of runs will be run the same way, but each will use 15g less cactus powder than the preceding sets of runs, to ensure that sufficient amounts of each solvent are available to complete the series.
2/6: Got delayed a couple days, didn’t have any observable effect vs 24-hr freeze. Decanted solutions through wire strainer-paper coffee filter-funnel into collection jars, separating ice shards from solution; frozen sodium carbonate pucks remained in original jars. All jars have a haze, so will let them settle a day or two, and decide whether I take the time & effort to do a dry sodium carbonate addition, before proceeding to the extraction runs. Once ready, I’ll post pH’s and a pic of solvnts.
2/10: Several layers of haze have settled, but jars still remain slightly hazy, I said screw it (with an F), and took the day off to run six 45g standard, scaled cactus powder runs, with the five once-used, washed solvents listed above and a fresh jar of EA. They all started at the same pH=5, nothing unusual to report through salting. Pics of the solvents and combined pulls are attached. Yields and any significant observations will be reported after 72hrs of passive crystallization.
2/13: All runs filtered after 72hrs passive crystallization, jars rinsed 2x w 5ml fresh EA and dumped through filter, filter rinsed 1x w 10 mL fresh EA, filtrated rinsed 1x w 10mL fresh EA. Pic, after filters appeared dry, attached. Jars washed 2x w 5mL hot distilled water, evaporated, scraped. All runs produced same appearance, fluffy white needles; which at these quantities is quite a beautiful sight. Total yield for each run rounded to 1.7%: fresh EA 0.754g, reused standard solvent 0.779g, reused solvent from paste made with boiled water 0.765g, reused solvent from microwaved paste 0.775g, reused solvent from paste made with chilled solvent 0.760g, reused solvent from microwaved paste made with chilled solvent 0.762g. Imo, quantities larger than fresh EA run are the result of slight calcium citrate precipitate from washed solvent.
Solvents will be washed with sodium carbonate-water method (steps 2 - 5 described here: https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1133316#post1133316 ), and after settling clear will be frozen for 24-hrs, decanted off of ice, then run in 2nd reuse.
2/20: After cloudiness settled, but all jars still had a haze, jars were put in fridge for 3 hours, appearing clear they were removed and allowed to come to ambient temp, a slight haze remained, but were placed in freezer.
2/21: after 24 hrs in freezer, jars were each decanted through a previously chilled seive-coffee filter-funnel to remove ice shards. Filtered solvents all had a heavy haze (not cloudy), and placed in fridge for 3 hours to settle haze, then stored at room temp.
Approximately 320 mL recovered of each de-iced washed solvent. Ice, defrosted puck water, and some amount of solvent trapped with ice shards were collected in a waste jar for further settling/separation.
2/23: Started 2nd Re-Use Trial, using six 30g cactus powder samples with scaled ingredients in: fresh Ethyl Acetate, and the five used solvents tested earlier. Each paste wss prepared in the standard way, then pulled 6 times (1 min stir, 2 min rest prr pull). This is the 3rd use (2nd re-use) of the five used solvents, Prior to salting each jar with 1.5g of citric acid, each jar was settled for at least one hour. No water was observed in the solvents, however all jars except the fresh EA jar had significant haziness. The hars will be passively crystallized for 72 hours.
2/26: Jars filtered after 72 hrs, jar washes evaporated; pic of drying filtrate below. The fresh solvent yielded 0.4683g, 1.6%, the yields of solvents’ 3rd use were: solvent that originally pulled standard paste 0,5745g, 1.9%; solvent that originally pulled boiled water paste 0.6072g, 2.0%; solvent that originally pulled microwaved paste 0.5863g, 2.0%; solvent that originally was chilled and pulled chilled paste 0.5873g, 2.0%; solvent that was originally chilled and pulled microwaved & chilled paste 0.6845g, 2.3%. Product from each run appeared and tasted similar, and had consistent appearance and taste as earlier runs.
I doubt the higher yields from the reused solvent runs vs the fresh solvent had anything to do with higher M levels, the cactus powder was the same for all runs and I doubt that any M from earlier runs remained in the reused solvents after the sodium carbonate-water washes and freezing. Rather, the higher yields are likely due to precipitation of calcium citrate.
In the next few days I’ll wash the solvents again, settle, and then freeze them. After removing the ice and letting them clear, I’ll do the 3rd reuse (4th run). I will be focusing on doing this next set of runs with crystal clear solvents (unlike the run that just finished), to see if this approach can reduce the suspected calcium citrate precipitation. It may take some extra time to get the solvents to settle clearly.
3/4: Light stirred 42mL of washing solution into each jar containing approx 280mL of solvent; after layers appeared, stirred 5 full revolutions (5 seconds; enough to fully mix layers); washing solution made according to previously mentioned post. Initial pH ~3.0, post mix pH 4.0; got to get back to pH of 5-ish, after an hour stirred 5 more revolutions (5 secs), in hopes of neutralizing with minimum haze after settling.
3/5: Light stirring has helped improve settling speed, solvent layer about 1/4 clear in 24 hrs; However, initial stir-in plus 2 light stirs only partially neutralized pH. Did one additional 5 revolution stir today, pH rose to comparable (5-ish) level of fresh EA. Will let solvents settle, then freeze & decant.
Due to large excess yields in previous run (more than this cactus powder yields), I want to try to rule out the possibility that dissolved M is remaining in the solvents after the washing process. So, after this washing cycle, I’ll re-salt the solvents with citric acid to see if any crystallization occurs; if M crystals do not form, I think it will be safe to assume that the excess yield is due to calcium citrate precipitation. After re-salting, I’l re-nuetralize, wait until solvents become crystal clear w no haze at all, then do another decant to minimize calcium citrate (could be a long time waiting for gravity to do this), and then begin 4th-use run.
3/9: Decided yesterday, in an attempt to reduce haziness after freezing, to syringe decant the cleared solvent (~80%) to clean jars, and then further decanted 90% of the hazy remainder to testtubes. I’ll decant the clear portion in the tubes & recombine the cleared portions after a few more days of settling. The cloudy/hazy residuals were decanted off the sodium carbonate and water, combined to settle, for future reuse.
Hoping to freeze, filter off ice, proceed to salting w citrate (to determine whether any M remains in solution after washing) this weekend. Then do final neutralization, and re-use.
3/12: Syringe decanted (using 100ml glass, gasketless syringe) the haze-free portion of solvents out of testtubes into the previously cleared solvents, put them all in for 24 hr freeze. Will cold filter-decant off of ice tomorrow, and then proceed to re-salting with citrate.
3/13: Cold filtered the solvents, all had significant and roughly equal amounts of ice shards. Dropped one of the jars, no further “boiled” solvent, insert expletives here! After warming to ambient, all jars remained clear; added 0.9g citric acid to each jar and stirred a couple revs. They all clouded, but seem to be precipitating what looks like a slight amount of calcium citrate powder. Will settle until clear, decant, then neutralize.