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CaCl2 in HIELO

It seems to be used for drying in the TEK. Looks at this post. It's mentioned in the point number 6.
Ah yes thank you! I was looking at the wiki page instead: HIELO - DMT-Nexus Wiki
I wonder if the drying step is missing from the wiki by mistake or because it was ultimately decided to not be worth it.
 
Indeed. It seems to be an alternative to the fridge.
 
Ah yes thank you! I was looking at the wiki page instead: HIELO - DMT-Nexus Wiki
I wonder if the drying step is missing from the wiki by mistake or because it was ultimately decided to not be worth it.
It's an extra material, an extra separation step, and could lead to over-drying if too much is used. I think that's why it got omitted from the wiki. These factors add up to it being somewhat superfluous.
 
Ah, I didn't know that was possible. So the ethyl acetate does need to have some water in it then?

I bought some calcium chloride already, but it's cheap and even if I don't use it for HIELO it'll still be useful as a desiccant for mushrooms.
Citric acid may be less soluble in more thoroughly dried EA. An issue with CIELO was that over-dried EA pulls weren't yielding crystals because the mescaline citrate requires a bit of hydration to crystallise properly. DMT citrate honey is clearly a different beast so my observation is quite possibly irrelevant. Now that I've had a chance to read the thread title again 😂
 
@Transform , HIELO says to preferably use a french press to separate the ethyl acetate. I have one but it's made of plastic. I've seen that ethyl acetate seems to degrade plastic (I'm unsure about lime, from what I've read it seems that maybe it's not an issue). Do you think this will be a problem in practice, and so I should not use it?
 
@Transform , HIELO says to preferably use a french press to separate the ethyl acetate. I have one but it's made of plastic. I've seen that ethyl acetate seems to degrade plastic (I'm unsure about lime, from what I've read it seems that maybe it's not an issue). Do you think this will be a problem in practice, and so I should not use it?
No, do NOT use plastic. EA will turn most kinds into a mess surprisingly quickly. The exceptions are if the only plastic parts are polypropylene (PP, 5) or HDPE, but if you can't identify any individual part of your press as such it's best not to do so. Plasticisers will be leached quite rapidly by EA too.

I would only use a device with an all metal plunger, no matter if some of them have polypropylene or HDPE frames. Plastic lids or handles can be kept away from the solvent to a certain extent, but even so, a mishap can get messy or even mildly catastrophic. Hence, I'd stick with metal or glass appartus/utensils only.
 
It seems to be working well. The honey that is forming looks more transparent than that in the pictures. It flows easily, more like hot honey than normal temperature honey. Could it have too much water? Or is this how it should be? I added 5ml water with the citric acid, as the tek says.
 
I got the end result. It seems a little too fluid, I'm wondering if maybe it has too much water. @Transform , would it be a bad idea to add some CaCl2 to the honey directly and strain it? Is there any potential harm or loss in trying that?
 
I got the end result. It seems a little too fluid, I'm wondering if maybe it has too much water. @Transform , would it be a bad idea to add some CaCl2 to the honey directly and strain it? Is there any potential harm or loss in trying that?
CaCl₂ will potentially react with the honey citrate, forming insoluble calcium citrate and hygroscopic DMT hydrochloride, so I wouldn't do that. I was thinking solvent drying with something like 95+% ethanol, or maybe acetone or 99% IPA, would pull water out of the honey, but you'd then need to evaporate the solvent afterwards to recover potential losses.

Really dry EA would also pull out some water, so that may be your best bet since you already have EA and a drying agent. Repeat as necessary to achieve the desired consistency if mashing the honey under one batch doesn't suffice.
 
Really dry EA would also pull out some water, so that may be your best bet since you already have EA and a drying agent
I will do that, then. Thank you for this info.

Related to this, I was running the tek a second time with a smaller amount of MHRB to try drying with CaCl2 instead of the fridge method, just to see the difference. After drying the extract with CaCl2, it has become cloudy. As last time a similar apparent cloudiness disappeared after filtering, I filtered it several times, but no luck. Could the calcium chloride have reacted with the DMT? I just added 25g CaCl2, gave it a swirl, and let it rest for 3 hours.
 
I will do that, then. Thank you for this info.

Related to this, I was running the tek a second time with a smaller amount of MHRB to try drying with CaCl2 instead of the fridge method, just to see the difference. After drying the extract with CaCl2, it has become cloudy. As last time a similar apparent cloudiness disappeared after filtering, I filtered it several times, but no luck. Could the calcium chloride have reacted with the DMT? I just added 25g CaCl2, gave it a swirl, and let it rest for 3 hours.
What kind of CaCl₂ do you have? If you're using the domestic dehumidifier crystals, bear in mind that they generally contain powdery, insoluble impurities from their manufacture.

You could try drying with anhydrous sodium carbonate instead, since it's easily produced at home.
 
Related to this, I was running the tek a second time with a smaller amount of MHRB to try drying with CaCl2 instead of the fridge method, just to see the difference. After drying the extract with CaCl2, it has become cloudy. As last time a similar apparent cloudiness disappeared after filtering, I filtered it several times, but no luck. Could the calcium chloride have reacted with the DMT? I just added 25g CaCl2, gave it a swirl, and let it rest for 3 hours.
Okay, (I think) I was able to guess what happened and successfully fix it.

I was using ethyl acetate that I had previously washed with a sodium carbonate solution. I hadn't dried after washing because, as I was going to dry it afterwards anyways, I figured out it wasn't necessary.

What probably has happened is that some water with sodium carbonate dissolved remained in the washed EA. Then, once it became completely dry due to the calcium chloride, it remained in suspension in the EA, becoming visible as there wasn't water to be dissolved in anymore. This is why towards the end of the drying process some fine white powder appeared around the calcium chloride when moving the jar (I thought it was just calcium chloride).

So I washed the extract with sodium carbonate solution and, after shaking well, it became clear again! Then I washed with water with some salt to remove more sodium carbonate from it. Now I'm following the normal fridge method.

Does this make sense? Should I worry about more sodium carbonate remaining inside the extract?

What kind of CaCl₂ do you have? If you're using the domestic dehumidifier crystals, bear in mind that they generally contain powdery, insoluble impurities from their manufacture.
I'm using food grade CaCl2, so I think it should be fine in that respect.
 
Okay, (I think) I was able to guess what happened and successfully fix it.

I was using ethyl acetate that I had previously washed with a sodium carbonate solution. I hadn't dried after washing because, as I was going to dry it afterwards anyways, I figured out it wasn't necessary.

What probably has happened is that some water with sodium carbonate dissolved remained in the washed EA. Then, once it became completely dry due to the calcium chloride, it remained in suspension in the EA, becoming visible as there wasn't water to be dissolved in anymore. This is why towards the end of the drying process some fine white powder appeared around the calcium chloride when moving the jar (I thought it was just calcium chloride).

So I washed the extract with sodium carbonate solution and, after shaking well, it became clear again! Then I washed with water with some salt to remove more sodium carbonate from it. Now I'm following the normal fridge method.

Does this make sense? Should I worry about more sodium carbonate remaining inside the extract?


I'm using food grade CaCl2, so I think it should be fine in that respect.
That all definitely sounds like progress, glad you appear to be sorting it out!
 
I'm thinking about putting it in the freezer to make sure I remove most of the water, in case it still has sodium carbonate. As I understand it, with ethyl acetate DMT won't precipitate in the freezer. Is that correct?

I'm also considering washing the EA with ammonia instead of sodium carbonate, to avoid this issue without needing to dry. And also because I have much easier access to ammonia.
 
I'm thinking about putting it in the freezer to make sure I remove most of the water, in case it still has sodium carbonate. As I understand it, with ethyl acetate DMT won't precipitate in the freezer. Is that correct?
I'm pretty sure the solubility of DMT in EA is high enough for this to be the case, and you can always freeze just to check. DMT would redissolve on warming anyhow.
I'm also considering washing the EA with ammonia instead of sodium carbonate, to avoid this issue without needing to dry. And also because I have much easier access to ammonia.
Ammonia should remove the excess citric acid, but you'd get some dissolving the EA. There's a risk of that reacting to form acetamide with ethanol as a byproduct. The strongly basic ammonia also risks hydrolysing EA to ammonium acetate and, again, ethanol.

All-in-all, a bit… risky.
 
Really dry EA would also pull out some water, so that may be your best bet since you already have EA and a drying agent. Repeat as necessary to achieve the desired consistency if mashing the honey under one batch doesn't suffice.
I did this, and it worked really well. Also, with a smaller amount, I experimented heating it up in a bain marie and it also seemed to work very well for drying. They ended up with very thick honey texture. Initially some parts were white, as described in the tek when it gets very dry.

And actually that turned out to be a problem. In the tek, you're supposed to mix it with PG in the same vessel you obtain the honey. But for certain reasons I have to wait to mix it and carry it in a different jar until I get access to my PG. And the honey texture made it almost impossible to move from one jar to another without leaving a lot stuck to the walls.

So in the end I dissolved it in water and did a mini A/B with heptane, I have it now in the freezer. Kind of pointless in my case to do HIELO if I was going to end up fumigating the house with heptane anyways, but I learned a lot doing it. In the coming weeks I plan to do again HIELO, this time mixing directly with PG.

Is there any reason evaporating the residual EA from the honey in a bain marie should be avoided?

Also, the second small scale attempt (the one that turned cloudy at one point) went well, with honey-like texture. But as I was doing the mini A/B, I added that honey to it as well.
 
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