downwardsfromzero
Boundary condition
Somehow this list of options makes me think of a flow chart format as being potentially helpful - although it might be a daunting behemoth of a flow chart.Cheelin said:
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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
Cheelin
Rising Star
All ideas welcomed, lazy-but-effective is a key concept in this tek.
But a detailed flowchart might be more in line with ISO methodology.
All of this is in the tek now (to some extent), but consciously addressing these items will help pay attention to them during processing, and provide key info for identifying problems afterwards.
For example: goo production before filtering may be a moisture or pH issue, after filtering is likely a washing issue. If a moisture issue, it should have been evident when viewing the combine pulls; if pH issue, likely had something to do with citric addition.
But a detailed flowchart might be more in line with ISO methodology.
All of this is in the tek now (to some extent), but consciously addressing these items will help pay attention to them during processing, and provide key info for identifying problems afterwards.
For example: goo production before filtering may be a moisture or pH issue, after filtering is likely a washing issue. If a moisture issue, it should have been evident when viewing the combine pulls; if pH issue, likely had something to do with citric addition.
Cheelin said:
In my first attempt in July, there was a greenish-amber goo under the EA, and no crystals. I was able to separate it by carefully pouring off the EA, but destroyed it in various attempts to convert it to freebase and back to different salts. I did however grow some nice needles in subsequent runs. Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus
This run looks nice
powder of course, because i did the quick precipitation. Hard to judge purity of a powder by eye, but i don't see why it wouldn't be in the same ballpark as before.
Cheelin
Rising Star
Your previous product may have been a more potent form of M citrate, related to low citric addition, sounds similar to one of Loveall’s runs.
Rerunning goo in a 5g Cielo run, as described a few posts ago, is a great recovery method (maybe Loveall’s suggestion to do this came from your earlier work). I am still optimizing it, but recovered about 2/3s of relatively pure input needles in my latest run, in addition to what was expected from the cactus powder.
As for current run, my washing work shows that “purity” of reused solvent runs depends on how well the used solvent was “cleaned” with washing technique, and could be substantial (1/3ish?) non-M.
Impurities are believed to be calcium citrate.
Hard to tell from your pic, since the material was from a powder run and subsequently squeezed, but imo, upper right flat parts of pic could be an example of calcium powder precipitate layer.
Calcium will have no flavor, it precipitates with citrate, which has an acid flavor; the M citrate has no acid flavor and moderate bitterness.
Rerunning goo in a 5g Cielo run, as described a few posts ago, is a great recovery method (maybe Loveall’s suggestion to do this came from your earlier work). I am still optimizing it, but recovered about 2/3s of relatively pure input needles in my latest run, in addition to what was expected from the cactus powder.
As for current run, my washing work shows that “purity” of reused solvent runs depends on how well the used solvent was “cleaned” with washing technique, and could be substantial (1/3ish?) non-M.
Impurities are believed to be calcium citrate.
Hard to tell from your pic, since the material was from a powder run and subsequently squeezed, but imo, upper right flat parts of pic could be an example of calcium powder precipitate layer.
Calcium will have no flavor, it precipitates with citrate, which has an acid flavor; the M citrate has no acid flavor and moderate bitterness.
oetzi13
Rising Star
Loveall, yes the EA did not move through the filter fast enough and some dirty solvent/goo got stuck. Washing didn’t help. Oh well. It was just the first round.
Cheelin, I crystallized by dropping in 15 g of citric acid on a magnetic stirrer. It all looked just fine until I filtered.
Some product came through the filter, and some formed in the jar afterwards. I just collected everything cause I didn’t know what’s what anymore.
I will attempt the recovery method you posted.
How do you guys get baking powder consistency ? I only have a coffee grinder. It did not make fine powder!?
Cheelin, I crystallized by dropping in 15 g of citric acid on a magnetic stirrer. It all looked just fine until I filtered.
Some product came through the filter, and some formed in the jar afterwards. I just collected everything cause I didn’t know what’s what anymore.
I will attempt the recovery method you posted.
How do you guys get baking powder consistency ? I only have a coffee grinder. It did not make fine powder!?
As long as the solvent is washed with sodium carb and the excess citric neutralized I've never seen calcium citrate form. Only time I encountered it was when re-using unwhased solvent as a test.
Cheelin
Rising Star
Loveall said:
Here are 2 pics of the same run, one with flash off, one with flash on, both shitty photos, but best i could take with my phone. This is a 30g run of material that should yield somewhere between 1.4 to 1.8%, using sodium carbonate washed solvent and passive crystallization. The product was filtered yesterday and was clearly a combination of needles and powder, the powdered component was bland, without bitterness, but acidic. Total yield was 0.662, 2.2%.
The quality of the wash makes a difference, this was from one that was problematic, causing me to change my approach, to one that hopefully will be much better.
Attachments
CatPharm
Rising Star
Finally finished the thread, what an awesome read!! Thank you nexus for what y'all do!
Finished a few runs also and originally believed we were only getting goo. After filtering to new jars so we could collect our goo, we had some beautiful snow globes within hours!!
Finished a few runs also and originally believed we were only getting goo. After filtering to new jars so we could collect our goo, we had some beautiful snow globes within hours!!
Attachments
Looks great, congrats CatPharm.
igorcarajo
Rising Star
Ugh, followed the tek, everything went as expected, the consistency of the paste seemed perfect, did the “fast crystallization” option…no crystals. Assuming that I got the alkaloids out of the powder and into the ethyl acetate, now that I acidified it with citric acid, is there any kind of fix?
igorcarajo
Rising Star
350 ml of ethyl acetate and 5 g of citric acid.Cheelin said:
Cheelin
Rising Star
1ml EA is 0.9g, so you have 350 x 0.9 = 315g EA
You have used 5g of citric acid, so you are currently at 5/315 = 0.016 g citric/g EA, so 16mg citric acid/g EA.
Have you reviewed this, from the tek:
Q: After adding citric acid, I saw clouds but didn't get crystals to precipitate, what gives?
A: First make sure the TEK instructions were followed, in particular: well mixed paste, short pull times, clean extract free of debris (including water droplets), citric acid is in range, etc. Before adding citric acid, allow the extract to rest. Issues that are suspected to cause goo are water droplets 1 or debris in the extract. To help ensure these are not an issue, allow the extract to rest for even more time in the fridge (24+ hours) before salting. If excess water is an issue, drops will form on the jar walls and/or bottom that need to be decanted carefully. If no goo is present and instead nothing is precipitating, bring up the citric acid concentration up to 20mg/g or more (stay below 40mg/g due to solubility concerns) and wait a few days. Check the jar walls, a transparent product may have precipitated there (e.g. this has been reported for whole bridgessi[17]). If all else fails, pulling the extract with water, evaporating, and washing with fresh ethyl acetate should leave behind a potent residue (dose will be less accurate and can be made proportional to starting cactus amount).
You have used 5g of citric acid, so you are currently at 5/315 = 0.016 g citric/g EA, so 16mg citric acid/g EA.
Have you reviewed this, from the tek:
Q: After adding citric acid, I saw clouds but didn't get crystals to precipitate, what gives?
A: First make sure the TEK instructions were followed, in particular: well mixed paste, short pull times, clean extract free of debris (including water droplets), citric acid is in range, etc. Before adding citric acid, allow the extract to rest. Issues that are suspected to cause goo are water droplets 1 or debris in the extract. To help ensure these are not an issue, allow the extract to rest for even more time in the fridge (24+ hours) before salting. If excess water is an issue, drops will form on the jar walls and/or bottom that need to be decanted carefully. If no goo is present and instead nothing is precipitating, bring up the citric acid concentration up to 20mg/g or more (stay below 40mg/g due to solubility concerns) and wait a few days. Check the jar walls, a transparent product may have precipitated there (e.g. this has been reported for whole bridgessi[17]). If all else fails, pulling the extract with water, evaporating, and washing with fresh ethyl acetate should leave behind a potent residue (dose will be less accurate and can be made proportional to starting cactus amount).
Cheelin
Rising Star
Loveall said:
How much sodium carbonate do you use in the “drying” addition?
20g per quart, per later post
I’m about to do the next step on my washed solvent. Initial sodium carbonate-water washing, to “nuetralize” pH and remove sediment/precipitate, was done on 1/15 using steps 1 through 5 in this post: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus
Step 2 treatments, to dry solution and finish clarifying solvent:
A. Decant and dry with sodium carbonate.
B. Freeze, remove puck and ice shards
C. Decant and dry with sodium carbonate, freeze, remove ice shards
D. Freeze, remove puck and ice shards, dry with sodium carbonate
1/26 update:
On 1/24 I began a 2nd washing step of the used solvent, using two 1-quart jars of approx 650mL used solvent that was previously mixed with sodium carbonate & water solution, that settled for approximately 9 days. On 1/24 the initial cloudiness of the solution had settled, to the point where the solution looked clear, but had the slightest haziness when a flashlight beam was shined through each of the jars.
One of the jars was syringe decanted off the by then solid settled layer, and split into two 1-pint jars, both jars were dosed with 10g each of Arm & Hammer Super Washing Soda (A&HSWS) and stirred for about 30 seconds; on 1/26, the solvent was cloudy, with the top 1/4-1/2 inch clearing.
The other jar was placed in a freezer, within 24hrs forming a frozen puck of settled material in the bottom, a large liquid layer in the middle, and a mixed liquid-ice shard layer at the top. Not much appeared to change by 48hrs, when the jar was decanted off of the frozen puck through a stainless steel strainer into a coffee filter & funnel placed on a collection jar. The ice shards mostly collected in the strainer, amounting to approximately 19g; a small amount (probably 2-3g) made it into the filter. The decanted and filtered liquid looks crystal clear without apparent haze.
After the jars that were re-salted with A&HSWS clear, one of them will be frozen to check for ice shards and clarity.
One of the previously frozen jars was, today, dosed with 10g A&HSWS and settled, to see if any additional change is observable.
1/27:
One of the previously unfrozen jars that was re-salted, was placed in a freezer; the previously frozen jar that was re-salted has settled, clearing to same level as the other previously frozen but un-re-salted jar.
1/28: Three jars had their final decant today: the unfrozen one that had dry A&HSWS added (A above), and the frozen one that then had dry A&HSWS added (D above) were both syringe decanted; the unfrozen one that had A&HSWS added and then was frozen (C above) was just poured off the puck ( the puck was hard but did not appear “frozen” and there were no ice shards visible). The fourth jar that was initially washed (like all the others) with water & sodium carbonate, but then frozen (B above), has not been treated in any way since it was strained & filtered after removing from the freezer.
Solvent recovery: treatments 1 and 2 approx 320mL (97%), treatment 3 approx 280mL (85%), treatment 4 approx 300 mL (91%).
Clarity-wise, as of today, both freezer-treated jars are visibly clearer than the jars that did not go into the freezer. The difference, however is at a level of haziness, not cloudiness.
Attached are pics of pH strips and solvent, 48 hrs after final decant. pHs appear the same as fresh EA, approx pH 5; no change to clarity as described directly above.
I’ll start the test extraction runs for yield and filtrate quality today. Those results will be posted separately, and linked back to the post linked above.
Attachments
Cheelin said:
About 20g per quart of EA (~900g).
Logic is that used EA can be ~3.4% water (or maybe a little more because of plant stuff changing the EA). Coming off saturated wash, it should be ~2% water (a guess based on the NaCl published data). My sodium carb is the monohydrate (arm and hammer super washing soda). The monohydrate (124 g/mol) is stable in room conditions, and can absorb 9 molecules of water (162g/mol).
So in 900g of EA,
~20g could be water
-20g of my washing soda wash can absorb 20*(162/124) ~ 26g of water
Therefore, the 26g washing soda should absorb most/all the water (~20g) in the washed EA.
You can also see clumps of washing soda forming. The clumps should be the decahydrate. People say in lab notes that you want clumps and a little bit of excess powdery drying agent to know the solvent is dry.
igorcarajo said:
To verify, you got clouds and no xtals? Cheelin gave you good advice. Keep us posted.
igorcarajo
Rising Star
I don’t think there were any clouds.Loveall said:
igorcarajo said:
There should be clouds, it is not a good sign to not have them: I think no clouds indicate no product was pulled. Are you sure you used Ca(OH)2 (and enough of it) and ethyl acetate? How sure are you the cactus is active?