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Pictures. Saturated saline solution for Nomans tek. Options
 
benzyme
#21 Posted : 2/8/2013 6:08:19 PM

analytical chemist

Moderator | Skills: Analytical equipment, Chemical master expertExtreme Chemical expert | Skills: Analytical equipment, Chemical master expertChemical expert | Skills: Analytical equipment, Chemical master expertSenior Member | Skills: Analytical equipment, Chemical master expert

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ChemisTryptaMan wrote:
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.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 

Live plants. Sustainable, ethically sourced, native American owned.
 
ChemisTryptaMan
#22 Posted : 2/10/2013 1:52:44 PM

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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
#23 Posted : 2/10/2013 5:01:54 PM

Michael


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ChemisTryptaMan wrote:
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 attached the following image(s):
Extraction time.jpg (699kb) downloaded 143 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#24 Posted : 2/10/2013 5:06:52 PM

Michael


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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.).
Kerberos attached the following image(s):
S7301208.jpg (1,774kb) downloaded 142 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
ChemisTryptaMan
#25 Posted : 2/10/2013 5:14:39 PM

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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
#26 Posted : 2/10/2013 5:16:43 PM

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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
#27 Posted : 2/10/2013 5:20:51 PM

Michael


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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 attached the following image(s):
Using the funnel.jpg (572kb) downloaded 136 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#28 Posted : 2/10/2013 5:23:11 PM

Michael


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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!
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#29 Posted : 2/10/2013 5:24:32 PM

Michael


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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 attached the following image(s):
Colour of solvent.jpg (544kb) downloaded 133 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#30 Posted : 2/10/2013 5:32:14 PM

Michael


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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 mineRolling eyes )
Kerberos attached the following image(s):
S7301215.jpg (832kb) downloaded 131 time(s).
S7301216.JPG (1,677kb) downloaded 128 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#31 Posted : 2/10/2013 5:50:05 PM

Michael


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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 attached the following image(s):
S7301217.jpg (228kb) downloaded 126 time(s).
S7301218.jpg (367kb) downloaded 126 time(s).
S7301219.jpg (525kb) downloaded 126 time(s).
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#32 Posted : 2/10/2013 5:58:41 PM

Michael


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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.
and when the world stops
you will find me there
waiting to embrace you
 
ChemisTryptaMan
#33 Posted : 2/10/2013 10:05:55 PM

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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
#34 Posted : 2/10/2013 10:27:55 PM

Michael


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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 firstDrool

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)
and when the world stops
you will find me there
waiting to embrace you
 
Kerberos
#35 Posted : 2/10/2013 10:30:05 PM

Michael


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Kerberos wrote:
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 firstDrool
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)

and when the world stops
you will find me there
waiting to embrace you
 
ChemisTryptaMan
#36 Posted : 2/11/2013 4:15:56 AM

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Kerberos wrote:
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
#37 Posted : 2/11/2013 10:14:46 AM

Michael


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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
and when the world stops
you will find me there
waiting to embrace you
 
Infundibulum
#38 Posted : 2/11/2013 11:12:01 AM

Kalt und Heiß, Schwarz und Rot, Kürper und Geist, Liebe und Chaos

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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,
ChemisTryptaMan wrote:
... 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.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
ChemisTryptaMan
#39 Posted : 2/11/2013 12:43:03 PM

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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
#40 Posted : 2/11/2013 12:54:59 PM

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