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SilverFox1983
#1 Posted : 8/7/2022 5:31:38 PM

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Welcome to all

Let me start by saying all the hard work goes out to the respected users who`s teks these are as I am just following in their footsteps and making a few changes as I go to see what works for me and with what is available and I will link there threads respectfully as all credits are due to them.

So I will be doing a standard Kash A/B with a mix of Phlux with a twist and a hint of Fable Tek.

I took 4,218g of fresh cut off pieces

and made them about 15cm in length and placed them in a bucket with a lid and put that in the freezer for two days, I then let it thaw for for 24 hours and was very soft to work with and slimy Big grin

I then took off the skins, thorns and bad parts but leaving the core as it was soft and broke apart with the strips as I was cutting the ribs.


and was left with 3,207g


excluding the juice's and bit of water that I was rinsing my hands off when I needed to do other things in-between cleaning it


This was all added to a large pot with 6 liters of distilled water and 10ml of AR grade Glacial Acetic Acid


This was boiled on high until boiling point and then placed on simmer for 2 hours with a timer and strained and squeezed out while still hot

I was warned about snot or over boil but never had any of these or worried about it with such a large pot Very happy

I then done another 2 hour boil followed by the 3rd boil at 4 hours, each time adding 6 liters water and 10ml of glacial, after the 3rd boil the water had very little color and my mate also recommended to bite and taste the spent material for any salty or bitter taste and had no taste but a little vinegar and water.

I was then told to add all aqueous solution to a 20 liter bucket rather than reduce, now here is where I sort of went wrong as I add the last of my boils to the previous it was at boiling point, now my mate who told me try do this said upon freezing there should be a pocket of frozen goodies separate from the water thus saving boiling down 18 liters, so I did this waited 48 hours and took the bucket out the freezer

So as you can see there is a pocket of super juice but also no clear separation but I will be testing this on my next try will let the bucket completely cool then place in the freezer, another test will be to see how long and how much gas is used in reducing and see time versus cost versus work and what is best for my situation.

I then poured out the super juice from the block of ice and proceeded to work with this, it was around 2 and a half liters and was told to reduce this.


I reduced it down to about 600ml, I let the ice block thaw over the next few days covered and will come back to this later.


I then measured out 50g AR NaOH and added that to 100ml as per Kash`s tek, and mixed while in a bucket of tap water to keep it cool, this was added to the 600ml juice I reduced and mixed well over 4 hours.


While doing this I setup my separatory funnel and please don`t moan about how it is setup I know it`s not those most ideal but while I was waiting for my stand I made due with what I have Embarrased


I added the based solution and 200ml AR Toluene, now another newbie mistake on my part I shook it rather than swirled it and landed up with an emulsions to have nightmares about Twisted Evil


Next morning it was halfway gone but I could not wait so I separated the solution and kept the solvent/emulsion in a jar, I then proceeded to add the next 200ml of Toluene and this time swirled it rather than shaking it, here is the 4th pull and 5th and final.


These were all done over a few days to let settle, but I will try warm bathing next time as well, I then added all the solvent pulls to the same jar, then placed back into the sep funnel to try get rid of that emulation I pulled on my first go


The now separated solvent was then poured out the top of the sep funnel and placed aside, I left some solvent left over in the base rather then have contamination for the salting step and this will go towards the next pull anyways.


I then added the solvent to another sep funnel and added 100ml distilled water to this and swirled but with more vigor this time, I did so for 10 minutes letting settle and did this 2 times, I then added 0.5ml of AR hydroiodic acid and mixed 10 minutes 2x then checked the ph was 4, this was then drained to an evaporation dish, I then placed the solvent back into the sep funnel and repeated the procedure again, adding the second 100ml to the first.


I then boiled water and put it in another dish and used the steam to evap my dish above, I did this a few times throwing water out and boiling filling more, I then needed to go out so I placed a fan blowing over the dish, 24 hours later I came back and not much had evaporated, now on day 3 and eager to know if I even had anything I contacted my mate and he advised with double bathing to heat and change water every 10 minutes or so, so I whipped out a pot and was re-boiling the water and keeping the glassware warm, I then saw this in the dish and was excited as the day my child was born


I then changed the water 2 more times and this is what I got and was so happy as this was my first ever extraction of mesc.


I scrapped it up and weighed it, it is a lot lighter in color and more translucent than the camera captures, it also as my mate described it has an opal effect Love


I then went back to my based aqueous solution and added to the sep funnel and instead of doing 5x 200ml Toluene pulls I done 4x 250ml pulls, then salted 2x 100ml adding 0.4 acid that was 6 drops and evaporated, I also picked this skillet fry pan, at a thrift store to help aid me on evaporation.


And in 5 hours rather than 3 days and many boils I got this from my 2nd pull, I thought it was close to my 1st pull but cause it was spread out I was wrong upon scraping and weighing this is what I got, so nearly 1/3 of what my first pull got.


I then restarted the whole processes over again but this time doing 2x 500ml Toluene on the based solution, I then received this, and upon scraping up it weighed.


Now comes the Dash of Fable tek, but before this, I took the bucket that had the ice block in and reduced it and added it to the based mix and ph was check in at 14, I then added 100g of salt to the based aqueous solution and mixed a few times over the next 2 hours, I then done 2x 500ml Toluene pulls and repeated the 2x 100ml salting and was blessed with this,


I also on the last pull pipetted out as much solvent as I could from the based solution and added that to a 100ml sep funnel to work with, I also did the same with the last run of salting.


Now beaming with joy I looked at what was the solubility of salt in 1 liter of water, found out to be 357g so I then added another 50g of salt to my based mix and repeated the steps again, upon evap I was left with this, I never added this to my previous extracts and will come back to this later.


I then put 30ml of AR Ethyl Acetate in the freezer for 2 hours in a small sealed jar and that in a small plastic cup as I was unsure if the glass would crack and it mess on my food.


I then took the first pull that I kept in one jar, and the other 2,3 and 4th pulls that were in another jar and wanted to try clean them up, the little jars had a strong alkaloid smell, I put the first in a working jar and crushed it up, I then added the other collections


I tried to work as quick as possible mixing and not letting the Ethyl get warm from my fingers, I rinsed each small jar into the next and then into the main work jar as there were small leftovers in each, I then after 2 minutes poured off the solvent, I then repeated this step again with the remaining Ethyl, it got a lot lighter as the solvent did it`s magic and the crystals had a pink hue, and all the hair and dust still in there gross Sick , after pouring off the solvent I will be storing it until I have enough to distill off and then evap for a bunch of mesc mixed alkaloids but more on that later.


I then saw that there was quiet a lot of the solvent trapped in the crystals so I warm bathed it while I was peppering my filter step that did not go so well, I was advised to put some cotton wool in a funnel and cut a piece of coffee filter to clean out my mesc from debris, I never had any cotton wool so I use gauze and lightly stuffed it in the funnel and the cut a piece of coffee filter and used a rubber band to hold it in place, I then drop 1ml of distilled water through it to pre wet it.


so after water bathing off the Ethyl and there was no remaining solvent smell, I added 10ml of water to my now dry crystals.


Sorry I don`t have any images of the events that followed as I was stressing and also was unable to touch my phone until my hands were clean from mesc, but what happened was I poured the now watery mesc into the funnel and it was so congealed it was only dropping a drop every 3 to 5 minutes, so with that I tried to pour more water on top of the funnel and it did not help at all, so now with a full funnel and stressing I thought best to take a whole coffee filter and pre wet it with distilled water and pour all of that through the filter and rinse all the stuff I had just used, so now resulting in about 150ml of water run through the filter I started evaporating that, an hour went be and this is what I saw


egger to know now what will it look like and what was lost during the attempted clean up, so another hour passes and this is what I see


I then set my alarm for 30 minutes as I am getting close to done, apon returning I find this, when holding up to the light I thought it was contamination in the center,


But then I put my phones flash on and WOW what I saw was breath taking, well for me it was hahahaThumbs up that opal shine is so beautiful, and yes I can still see small amounts of non mesc alkaloids present, upon scraping this up I was happy, but when gathering my scraping to weigh it my scale went off, normally I zero it with the paper then blow on it while gathering so it don`t switch off, but it happened this time as I need new batteries, so I weighed it with the paper then the paper alone.


So now if you still here and following I have 2.555mg of almost white crystals and has almost zero smell, when opening the jar I can get a faint hint of something unknown but when trying sniff it out I can`t place it, my mate suggested trying it as is then doing a Phlux's Quick Mescaline Hcl Recrystallization tek on the remainder and seeing a difference on the two.



So this is where I am at folks, I know it`s mess and I have lots to learn but that is why I am here to share what I have done and try better myself each time, and if someone else can learn something that is great too, I wanted to test some out last night but unfortunately the set and settings were not right and I`ll wait for next weekend, thanks for stopping by all comments and tips are welcome.

Links to threads used:
Kash's A/B Mescaline Extraction
Working with fresh cactus - a pictoral
The Mescaline Extraction Thread
Phlux's Quick Mescaline Hcl Recrystallization tek

Much love and respect, SilverFox
 

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doubledog
#2 Posted : 8/30/2022 11:23:47 AM

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I really like your post, silverfox, it looks like you had lot of fun working with cactus Smile

Freezing is probably not very effective in separation of actives from concentrated cactus tea.

Maybe one advice from my side:
drying and fine filtering your toluene before salting with acidic water could help with the purity of the product. Basic water and toluene are not miscible, but some water (together with some base) could be mixed/dispersed in toluene. When acid is added, this base forms a salt.
For drying, common method is to add some dehydrating solid salt as drying agent.
 
SilverFox1983
#3 Posted : 10/9/2022 8:49:16 AM

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Hiya doubledog

And sorry for the late reply life can keep one busy sometimes from relaxing and posting Smile

Many thanks for the kind words as it really means a lot for a novice like myself, and the advice is most welcome, and yes I have had just as much fun extracting as I have had consuming it and wish I could do extractions every day as I really enjoy it Big grin

I have done another run with reducing rather than freezing to save time, but at the cost of gas, so I will be trying the freeze method again but when I have time.

I was advice by my mate about drying my toluene with microwaved bicarb or was it Epsom salts, sorry a little stoned and distracted as I am busy boiling down my 3rd batch now and 3rd boil to add to the run, so lots going on today in the kitchen.

what I have been doing when separating to make sure no cross contamination is leave some toluene behind and then to pipet it off and work in a smaller separating funnel, I mainly am doing the filtering after I do the ethyl washes and drying as it gets all hair and dust out of my end product just before storing, but I will try filter my toluene in another batch so I can see if there is difference in purity.

Much love and respect, SilverFox
 
SilverFox1983
#4 Posted : 10/13/2022 12:11:03 PM

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Welcome to all

So I am back at it again and on this run I have only done one type of the cactus I have growing to see the yield, and I have had some complications along the way but will add them here Worts and all.

So here is a few images of the cactus I am working with on this batch, maybe a more experienced user can identify it for me as I got a few types in my garden that I have no clue, this piece was not used the pieces were sitting in the garage for about 3 months.
÷ñÒ22...Ö0õæ÷

So the pieces were frozen for 24 hours maybe more and then thawed


This was then sliced and cleaned up, some cores were hard and some soft


This was then boiled with 6 liters of distilled water for 2 hours with 10ml Acetic Acid Glacial ( Sorry this was not weighed ), strained and boiled again for 2 hours with 10ml, then a last boil for 4 hours with 10ml,( I have found with the extra time boiling I have had to add extra 1 or 2 liters of water, so that the plant material stays submerged in water ) this was all reduced to around 500ml and let cool for 2 hours, then 50g NaOH was added to 100ml of distilled water and mixed until all was dissolved while in a bucket of tap water to keep it cool, this was then added to the tea and mixed well every 10 minutes for 2 hours also sitting in the bucket while the reaction takes place and bubbles, this based tea was then added to the separatory funnel with 500ml of used toluene and swirled not shaken Rolling eyes


This was then separated leaving behind a little toluene so no cross contamination and poured out the top of the funnel and placed aside, then another 500ml of used toluene was added swirled and then separated and added to the other 500ml of toluene, this was then placed in another sep funnel and 100ml of distilled water added and mixed vigorously for 10 minutes, then 0.4ml of HCI was dropped in and mixed well for another 10 minutes, this was then let to settle for an hour or two and separated and placed in the evap dish, with a little water still under the toluene in the sep funnel then another 100ml of water and 0.7ml of Acid was added and mix again, then drained into the evap dish.

This was the result of the first run, it was way more than I expected


I then add 200g of NaCl to the based tea and mixed until most was dissolved, I think I added too much this run but when pouring into the cup that I then pour into the sep-funnel I made sure to leave behind the excess salt, then 500ml of used toluene was added and swirled over 2 hour every 30 minutes and then settle for 2 hours and separated and I found that after draining that I like to vigorously shake and swirl the bottle and let settle again for an hour and I find a little base tea left again to drain, once I have separated this again and let a small amount of toluene go through, I then pour the tolulene out the top of the sep-funnel, I then repeat this with the other 500ml of toluene and then combine the two.

I then add the toluene to another sep-funnel and add 100ml of water and shake vigorously for about an hour every 10 minutes, I then add 0.4ml of HCI and shake again for an hour and let settle, then drain into the evaporation dish and add another 100ml of water to the sep-funnel and then add 0.7ml of HCI mix again and separate and this to the evap dish, it normally take`s about 5 hour to evap 200ml of water on my frypan.

Here is what I was blessed with on my second run


I know it looks really dark in the weighing pics but if I have the lights on, the scale screen does not show so nicely, so I then took the 3.577g of mixed alkaloids and added it to a work jar


Then washed with chilled 20ml of Ethyl Acetate and then poured off and washed again with another 20ml and then warm bathed to evap off any left over


So here is where I sort of stuffed up, I thought Ethyl Acetate could mix with water and I should of looked it up first but never did, and I was trying to do Phlux`s Acetone bomb method and it never worked so yeah had to clean that up but here is some pic`s and events

So I added 10ml of water and mixed


I then added 50ml of Ethyl Acetate, mixed well and let settle


I then left it for an hour when I cam back I found this


So I then only used Google and saw that Ethyl Acetate does not mix with water, so I poured off the top layer and used a pipet to get as much as I could off, this is the top layer evaporating


I then boiled the lower dark portion for a bit to get rid of any Ethyl Acetate and then added 100ml of water and evaporated that


So it now looks more dirty than when I started so I scrapped this all up and did another two Ethyl Acetate washes and done a warm water bath to dry it up


Sorry no pictures for this part I will try next run, I then add 100ml of water to my now cleaned powder and pre-wet two coffee filters one inside the other, I then pour my mesc/water solution through the filters, once finished filtering I add 50ml of water to the work jar and then pour into the filter, lastly I use a 5ml syringe and rinse the outside of the filters, this is all done over my evaporation dish, I then took one more pre-wet filter and place the two used filters inside of it and squeeze any excess water out and then rinse that with another 5ml of water, this was then all evapped


So yes there is still a little color and a mix of other alkaloids but I think its looking good enough to test


So when I was weighing and scooping up my scale switched off so I had to weigh it with the paper and the the paper alone


So now left with 3,475g and lost 0.102g on clean up after my stuff ups, I am now left with this sort of clean mescaline and almost zero smell again, here is a pic of this batch and what's left over from my first extract above



Thanks for stopping by friends and all advice is welcome.

Much love and respect, SilverFox
 
downwardsfromzero
#5 Posted : 10/13/2022 11:10:16 PM

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Nice report again. Just one thing makes me wonder - you have ethyl acetate (EA), have you heard of the CIELO tek? It uses lime - calcium hydroxide - as the base and crystals are precipitated directly from the EA using citric acid crystals to give a remarkably clean product. It would be very interesting to see if you could get some results using CIELO on fresh cactus (up til now people have dried their cactus first).
[It would probably be necessary to tweak the amounts of water used with fresh cactus.]




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donfoolio
#6 Posted : 10/15/2022 11:37:10 AM

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Nice project. Have you noted initial weight of your cactus?
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SilverFox1983
#7 Posted : 10/16/2022 8:43:04 AM

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Hiya downwardsfromzero

Thanks for the kind words

Yes I have heard and read about the CIELO tek and when I choosing which tek to follow the reason I never went with it was cause of dried starting material and not fresh, I would like to try this if you or someone could come up with a method that I can start with fresh chunks I`ll gladly give this tek a run.

I would have to still get three items for this tek and a few jars, I would need the calcium hydroxide, citric acid and washing soda as I don`t have these, but I will look for them soon and maybe by then you or someone would have come up with a plan for me Very happy

I would also have to look at getting food grade or AR grade, as my loved ones and I consume these medicines and I am sort of fussy with this regard.

Many thanks for the feed back, information and advice, I really do appreciate it Thumbs up



Hi there donfoolio

Thanks I am having lots of fun and learning so much, I did weigh the batch on my first post, but yes unfortunately I never did on the second batch, but it was about 4kg to 5kg max, as that is sort of what fits in the bucket that I use to freeze, I have made sure on my third batch to weigh it and will make sure moving forward I do weigh everything Embarrased



Much love and respect, SilverFox
 
Ice House
#8 Posted : 10/16/2022 4:15:37 PM

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doubledog wrote:


Freezing is probably not very effective in separation of actives from concentrated cactus tea.


In my own personal experience with brewing cactus, many out there freeze before brewing in order to expand the organic matter in the freezing process, this helps break open the plant material allowing or helping to get more trapped alkaloid out of plant material. There's actually quite a few of us out there who feeze fresh material or add water to and freeze dry material before brewing.

Very nice write up! I normally just brew it and drink it. This is a great post!
Thank You!

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