Pictures. Saturated saline solution for Nomans tek.

[Kerberos]

After reading the salty threads and receiving some pointers from ChemisTryptaMan and cyb i am having a go at this.

i am following my normal extraction method except i am starting with a saturated saline solution and also i will be cooking the mixture for 24 hours.
Step 1
I have a 2ltr kilner jar which is filled with 1900ml of de-ionised water. This is placed in a 1.5ltr crock pot (£10 from a store that sounds like bilko)which i am using as a water bath. To this i have added initially one tub of rock salt 362g. I have used rock salt as all the other salt contained anti caking agents. Pic attached.

i Heated this in my water bath up to the same temperature as the mixture will be cooking at. I then kept adding salt until no more would dissolve, this was a total of 450g. I then on ChemisTryptaMan advice let this cool down to room temperature and remove any salt left in the bottom of the jar, approx 5g.

Step 2
i added lye at the rate of 1g per 15ml of water as per Nomans tek a total of 127g. the solution turned milky white and stayed this way. i have taken a small sample to see if it clears over time. I have taken a ph reading from this sample and it is 14. (Pic attached as "ph reading") As of writing it still is milky white several hours later. UPDATE there appears to be a denser layer separating out on the bottom of the sample. i initially thought it was salt crashing out but it is liquid. i will post pic when i get new batteries for the camera.

Step 3a
Added 40g of powdered bark, this was produced with a dry spice grinder. All the fibers where removed and kept with all the other fibers from previous grindings. It is my intention to do an extraction just with these fibers to see what the percentage of DMT is contained in them.

Step 3b
As i added the bark, which i always do slowly, the mixture turned a very strange (scary)dark green colour. I didn't take a pic because my hands where full at the time. The mixture ended up a dark chocolate colour and looks thin if that makes any sense.

Inner coating
The jar looks like it is coated with oil on the inside and makes the jar look smoaky. pic attached.

The mixture is now in my newly acquired water bath and will be cooking until this time tomorrow. It will be allowed to cool to room temperature before being pulled with hot solvent as per the advice of ChemisTryptaMan.
I will be doing three pulls initially as this is the way i normal extract, 40ml, 30ml and 30ml before freeze precipitating. I will then take suggestions on how to proceed after we see if this has worked or not!

All observations gratefully received.

Speak to you tomorrow.
Kerberos
Edit. just had a smell of this and it does not smell of the usual lye/caustic smell. I smells more like a hit of DMT tastes if you know what i mean.:shock:

 

[benzyme]

Meetings with the chemistry team were downright hostile at times when there was a disagreement, which I never really understood.

that's called politics. it exists in any place of business, and is the product of egos and incompetence.

I look forward to your contributions to the community, you are well on your way to earning the flask.

 

[ChemisTryptaMan]

Kerberos, where's the pics and how is your extraction going, your leaving us hangin here. Just kidding brother, get us this info as soon as you can. I've been anxiously waiting to hear more from you on this thread.

 

[Kerberos]

Kerberos, where's the pics and how is your extraction going, your leaving us hangin here. Just kidding brother, get us this info as soon as you can. I've been anxiously waiting to hear more from you on this thread.

Sorry CTM been working.

 

[Kerberos]

Mixture was allowed to cool down to room temperature after 24 hours in water bath. No layers present but the mixture looks more like normal i.e. black. I have now identified the smell i kept going on about and it is the smell of my used solvent. i am assuming that this is due to the plant fats/oils been pushed out by the salt. I didn't recognise it at first because i never smelt it hot before.

I put in 40ml of hot solvent and did my normal mixing for 2 minuets. When i stopped, the solvent layer started forming in 15 seconds and appeared to be fully separated at 46 seconds. Excuse the picture quality as its not my camera, i am sure it has a macro feature (I'll be glad when i find it.).

 

[ChemisTryptaMan]

No layer is a dissapointment, as this would have eliminated some of the oils we dont want in the NPS, but oh well, I guess we will have to deal with this later(or maybe not, the re-x at the end should take care of it). Please let us know about your yields whenever you finish your first evap/freeze precip.

edit: there may actually be some sort of dark layer either on the edges of the jar or at the bottom that is mixing with the plant material, but more likely on the walls as it wouldnt be dense enough to sink in water(most likely)

 

[ChemisTryptaMan]

Just checking here, but you do agitate the mixture more than once right. This should be done several times to allow the NPS to grab as much spice as possible.

 

[Kerberos]

I mixed for a further two times at 2 minutes each before letting the mixture settle. I then use my funnel to help me extract the solvent. I do this by inverting the funnel and lowering it in to the Kilner jar. This forces the thin layer into the small spout of the funnel. The solvent obviously protrudes above the level of the liquid allowing me to see when any black stuff starts to come through when i draw off the solvent with a pipette. I do this a few times allowing the solvent layer to settle in between extractions before pushing the funnel back into the mixture.

i am sure someone can do the math of the volume of liquid in a circle with the radius of r and a depth of h. Then work out the height of cylinder (the spout) with the volume from the previous equation. Bottom line is i can extract, cleanly, 80% of my solvent in about 30 seconds.

 

[Kerberos]

Please excuse the multiple posts as i am trying to keep some order with the pics. i am also missing your post CTM as i am compiling the information i have!

 

[Kerberos]

This is what the extracted solvent looks like. It is as expected a lot darker than usual and even darker than my other solvent which i have used multiple times.

 

[Kerberos]

I did 3 pulls initially at 40ml, 30ml and 30ml before placing in freezer. as previously stated the solvent i am using does not evap quickly by any stretch of the imagination.

I took the glasses out this morning and filtered the contents. I do this by scraping edges and mixing all precipitation in to the solution. The glass you may notice have aluminum foil sandwiched in between two layers of cling film/saran wrap. This cuts the smell right down so you don't contaminate your freezer. (this is a very important step with a wife like mine:roll: )

 

[Kerberos]

This is the filtered first pull from my 37g of bark. When i have filtered the crystals i fold the paper in half and blot it between some absorbent kitchen roll. I then transfer this to another filter paper and break up to aid drying. The weight of the first pull is 229mg.

 

[Kerberos]

All the pulls were done right after each other. The second pull only yielded 87mg and the 3rd pull only 43mg. However i was doing the pulls the way i normally do my pulls.
I have another 30ml in which i will leave for 24 hours before pulling to see if this makes a difference. I will post these results when i have them.

UPDATE: the weight stands at 302mgs as of now after drying all day.

 

[ChemisTryptaMan]

So your yielding under 1% it seems at full saturation. I suggest diluting the contents of your jar and trying some more pulls on them when your done to see if you can get more out of the mix, but now we know that over-salinating is a hindrance. At least we have the upper limit tested now. Thanks for experimenting.

 

[Kerberos]

Actually CTM the last pull i put in the freezer, after the first three, is clouding quite nicely. I left this over night as i am thinking that the oils and fats are inhibiting the speed of the take up of DMT.I have also put another 30ml of used solvent in but i am also heating this in a water bath and agitating frequently and vigorously. I will put this in the freezer tomorrow. I will keep you posted on the out come.

One thing i have noticed is that the DMT looks like it is twice the amount of my last extraction but is only half the weight!? I was going to re x all my extractions from this experiment but to be honest i think i will bio assay it first:want:

I am expecting some more bark so i will redo this saturation test but using cybs tek. I am really enjoying this and i hope i can contribute to yours and cybs findings.

(I tried PMing you but i am not a full member. Just to wish you all the best with your health)

 

[Kerberos]

Actually CTM the last pull i put in the freezer, after the first three, is clouding quite nicely. I left this over night as i am thinking that the oils and fats are inhibiting the speed of the take up of DMT.I have also put another 30ml of used solvent in but i am also heating this in a water bath and agitating frequently and vigorously. I will put this in the freezer tomorrow. I will keep you posted on the out come.

One thing i have noticed is that the DMT looks like it is twice the amount of my last extraction but is only half the weight!? I was going to re x all my extractions from this experiment but to be honest i think i will bio assay it first:want:
Also saturation may only be a hindrance in this method, I am expecting some more bark so i will redo this saturation test but using cybs tek. I am really enjoying this and i hope i can contribute to yours and cybs findings.

(I tried PMing you but i am not a full member. Just to wish you all the best with your health)

 

[ChemisTryptaMan]

I tried PMing you but i am not a full member. Just to wish you all the best with your health

Thank you, I truly appreciate your kindness.

 

[Kerberos]

Hi to christian, thanks for the PM. i cant Pm you back as not full member yet. I really will have to get the Intro essay written!
i have another pull in as we speak which as been in the mixture for over 24 hours. I have also put another pull in which i have in the heat bath just to see.
I regularly get over 1% with a normal STB nomans tek so i know you are right about the amount in there.

I use that amount of solvent because i am guaranteed it will crash out, also using the upturned funnel i can get it out of the mixture quickly and cleanly.

Thanks for the message mate. i will be posting in a couple of days on the extra stuff i have got out (he says!)

Kerberos

 

[Infundibulum]

ChemisTryptaMan, have you done any controlled experiments on the salination thing (e.g. salinated vs not)? Would be interesting to see.

Also, it would be interesting to suggest that other people are doing control runs, such as salination vs not salination because this is what's going to give power to the results obtained. For the moment you really want good, controlled reproducibility of the salination tek.

Finally,

... but now we know that over-salinating is a hindrance. At least we have the upper limit tested now. Thanks for experimenting.

Isn't it a bit quick to reach to such a conclusion? To claim that over-salination poses a hindrance is against the mechanism you propose and might require an explanation on its own.

Most importantly, without controls run from Kerberos you cannot assert that there was a hindrance. It could very well be that in Kerberos' plant material there was just that much to begin with and you got it all out.

Please try to be less assertive (amidst the lack of controls) in the future.

 

[ChemisTryptaMan]

I understand, there is actually a few people working on various perspectives of this. This forum is currently growing a large body of collaborators on this. It seems many people have seen what cyb's tek is producing and are now far more interested, as several people are working with me right now to perfect this.
It is a bit hasty, It's just that at very high ionic strengths(especially at pH extremes), very weird things can happen. I have only done what I posted in my thread "Salt", sorry for not prividing a link, but's it's been a very active thread with a lot of good experimentation on it. It was shown for instance that salting and dry-teks are a bad combo.
I plan to resume my own experimentation with the return of my money from uncle sam in the coming weeks. I would like to continue working with MHRB and confusa simultaneously, but I only have about fifty grams of the powder I used for my mass extraction at that time. But I also have a few hundred grams of some shredded mimosa that a friend had trouble getting product from. I'm hoping I have better luck with it. I'm just waiting for the right time to begin my experiments, but right now I am spending a lot of time preparing for them. I'm taking this very seriously, I'm unemployed at the moment, so I have the time, I want to make as much of a contribution to the availability of spice for those who desire to work with it.
Me and cyb are currently collaborating on writing a new tek that can be applied to various source materials and hopefully provide yields as high as we can go. Using Acacia deadhoor5 just yielded 2.85% and was sure he could have contiued pulling. Ancotar has done a side by side comparison of salted verus unsalted teks and shown a drastic difference. There are more but I think the point has been made that exactly what you suggest is already happening. I would be honored to hear your input on all of this stuff and perhaps here some of the "theories" you have on them so that we can make some "fact" out of them on here.
These projects all mean so much to me, I have found so much beauty and love on this forum and think it is a very special place. I agree that at times I can be a bit hasty to draw conclusions, but always with the intent on testing the idea further to make sure. Over time We are all going to make the spice availability issue a non-issue if we all put our minds and resources together and make the teks we use fully explainable to those who are using them, so that through knowledge they may gain spice. If this is going to happen this forum is the place that will make it happen and I am working my hardest to make this a reality, along with others who are so generously providing time and supplies to run these experiments.

I have much respect for you infin, your posts helped me when I was first getting started. So I express sincere apologies for my eagerness to understand these situations and hope we can get you working with us on this to whatever extent you can.

Much love and respect brother,

CTM

Back to the thread:
I have a theory on how this was caused, or at least effected. I'm thinking that once the lye was added a common ion effect with the sodium caused some to be suspended in the mixture with both lye and salt. This could have caused some disturbance to allowing access to the spice when agitating, perhaps micellar formations from the fatty acids trapped some of the spice. I would guess that having such hih ionic strength would force those fatty acids to form micelles. We could try to lower the salination lightly by changing the way we prepare the saline solution. I would suggest trying something like heating some filtered water and supersaturating it like before, but to then store the solution in the refirigerator overnight, then the freeze, but only long enough to get i a bit colder, not long enough to freeze. This would cause a greater amount of NACL to precip, and then when the solution is as cold as possible and as much salt suspended in the solution has settled, one could decant the required amount and allow it to warm back up. The solution would then be less than saturated enough(hopefully) to allow addition of the lye and for complete solvation it. I would try this if I could but a few weeks from now and if nobody else has given it a shot will try it myself. If anyone out there has everything needed to run cyb's tek using this method please do and please let us all know.

Always with the utmost love and respect,

CTM

 

[ChemisTryptaMan]

Also, if micelles are the problem a defat under acidic conditions would solve that easily.