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CIELO attempt troubleshooting Options
 
desertdweller
#1 Posted : 7/14/2022 10:46:51 PM

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So, last year I tried out the CIELO tek, and at the time, the wiki page was definitely not as exhaustive, and I had to check the main topic on the forum to be more assured about some of the details.
However, it might not have been the best time in my life to do that anyway, as I was pretty stressed out, and to get my mind off of it I wanted the tek to work so hard that it might, in part, explain some of my mistakes.

To cut a long story short (I can give you more details later), I thought I had failed, since I was not really sure any precipitate had formed after the addition of citric acid - in retrospect, I guess it might only have been a couple of citric acid crystals that later dissolved, confusing me all the more.
I rinsed the last vessel with water, believing it would dissolve the precipitate that was supposedly there, left it to evaporate, and left home for a couple of weeks and when I got back, I could not see any true crystal, only oily/waxy residue, and - this was the most depressing - I could see some molds had had their way with the last drops of liquid.
I concluded I did a heavy mistake somewhere, and that either some insignificant amount of precipitate had to be recovered from the moldy plate, or even none at all.
I stored all my material away and decided to look it up later, with close to no real consistent hope, so that's why that phase lasted a while.

That changed a couple of days ago, when I stumbled across one of the pieces of glassware I had used : a separatory funnel.
(now you may ask why since it's not used in the tek : well actually this was because of my french press : I tried to squeeze up the EA, but at some point the plunger would not budge any lower, and as I was convinced it clearly still could, I used to much force, resulting in spilling the EA and sludge, subsequently, I had some residue in my EA that needed separation)
Well I discovered the separatory funnel has a nice layer of neat crystals inside (quite small, but they definitely look like the real mccoy) !
So now I know I did not fail the tek as much as I initially thought, but some questions remain.

Firstly, why did crystallization happen in the funnel when it was only supposed to happen afterwards, with addition of citric acid ?
Obviously, either I added acid disregarding the tek's steps - but I don't remember that happening - or : the funnel had acid in it unbeknownst to me.
So how could that have happened considering I was using it for the very first time ?
(well I had ordered it on ebay from china, having sought the lowest price, since I'm not that wealthy - yeah sorry I know what it sounds like)
I believe :
1 - either I tried to wash it because I think I remember noticing a smell upon receiving my package - if that's the case, I'd probably have used vinegar, and just did not realize I rinsed it with insufficient water
2 - or I did not even clean the funnel thinking it had to be clean since it was sold to me (I mean, what kind of people sell unwashed glasses without warning the buyer !? - as you probably guessed, in this scenario, I forgot about the smell at some point, which may simply have been because this extra step was not supposed to happen in the first place) and the acid was from its previous user

So my first question will be the following : can I regard this precipitate as safe to ingest ?
Would it be wiser to recrystallize (B/A) and/or charcoal wash it ?
(I mean if [2] is true, is there any chance the precipitate has held on to potentially toxic, unwanted materials ? or maybe there's even such things as acids that, even in the minute quantity the precipitate holds, are harmful to humans ?)

[I realize there's a lot of uncertainty here, for which I apologize but rest assured I've learned two lessons : always check glassware cleanliness, and also, take notes asap when there's a problem so as not to forget any details !!!]

My second question is way simpler : I'm going for a second round of this experiment, and a portion of the material I want to add is more acidic than it should.
That's because I rinsed the mixer I used with vinegar and water to collect the very last bits of cactus tissue. I can't remember how much vinegar I used so I fear I might not have enough lime left to attain desired alkalinity.
My question is : can I use other bases without adverse effects on the following steps of the tek ?
I have NaOH and NaHCO3 at hand, can I use those or are they going to make things harder and I should only do it with lime ?

There you go, thanks in advance for your kind replies !
(also, sorry I'm not that good at keeping it short)
 

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Homo Trypens
#2 Posted : 7/15/2022 7:40:34 AM

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You can add some NaOH if you want - i've done it once and the process still worked.

However, i doubt that you could use *only* NaOH, as it turns the moist cactus powder more liquid/slimey. The lime seems essential for attaining the fluffy/crumbly consistency that ensures good contact between the material and the ethyl acetate.
 
desertdweller
#3 Posted : 7/15/2022 2:01:17 PM

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Ok, so I guess the consistency is really the main factor, here.
I mean I can buy more lime, but I'm not too sure where to find it in smaller quantities where I live (bought it from the internet last time, which I can do again, but the delivery will take time).

Thanks for you reply Homo Trypens !
 
Loveall
#4 Posted : 7/15/2022 2:53:21 PM

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Yes, definitely use lime. Do not modify any steps of the TEK. Use a small cactus powder sample (~5g) and scale the ingredients. Once you verify you can get it to work use the full 100g. Follow the recommendation for new commers: settle the extract in the fridge for 24h or until clear, decant/filter leaving any water dropletts behind. Only then add the citric acid.

I don't know what happened in your separatory funnel, sorry.


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