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Dijii
#1 Posted : 9/7/2009 5:43:22 PM
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I havent posted before, but read plenty on these forums, so first off... Hello everyone! And respect to all the people who have helped merge experience and knowledge from & for the community, you have made the Nexus what it is right now; a rich haven of collaborated information and a kind helpful community Smile

If I get full membership I would like to repost this in the STB section to make it more accessible to people, and once the plan is straight, tried and tested I would love to add photos in as a step-by-step guide! I also wish to take part in other topics, as I have a wide interest in psychedelics, particularly mushrooms and salvia at the moment.

SWIM believes to have all the items necessary for SWIM's first ever MHRB extraction through an STB (Nomans Tek) and would like to just run though the plan to get a little input from some experienced extractors. Hopefully any flaws in this can be picked out beforehand to save wasting anything, and any tips will be much appreciated by SWIM. Also SWIM is UK based and hopes this may serve to advise other UK extractors in finding and using materials needed.



SWIM has gathered the following things to perform extraction:

125g MHRB (eBay seller)
500g Lye (Obtained from Wilkinson's, back of packaging claims 100% pure Sodium Hydroxide)
125ml Zippo Fluid (SWIM has evaporated a shot glass full to confirm nothing remains in glass)
A slightly under 2L Jar for mixing (randomly scavenged from FOAF, sorry! Looks like a large pickle jar though, check fish and chip shops!)
A jam jar for collection (found 'Bonne Maman - Strawberry Conserve' in supermarket, it has no shoulder on the jar aka Widemouth jar)
Turkey Baster (eBay)
pipettes (for more careful smaller quantities)
N95 respirator mask (probably overkill as masks go but SWIM already has them)

Has yet to buy:

coffee filters (supermarkets)
appropriate safety gloves (any materials a good/bad choice for working with solvents+lye? disposable latex are a cheap option, any use?)
appropriate safety goggles (would swimming goggles suffice?)



The extraction plan is:

1. Pour 1875ml Water into large mixing jar.
2. Add 125mg Lye to jar and shake up with lid on.
3. Blend MHRB. (although mostly powder there is lots of long stringy/fiber in there)
4. Add MHRB, shake jar thoroughly and leave for 2 hours.
5. Carefully pour in 125ml Zippo Fluid and seal the jar.
6. Turn the jar upside down slowly making sure emulsion does not form, then swirl the mixture around by moving it in circle motion for a minute.
7. Wait until liquids separate and repeat step 6. a few more times.
8. Use baster and pipettes to move Zippo Fluid into collection jar
9. Seal jar, place in freezer for 24 hours (or for longer?)
10. Pour all contents through a coffee filter above a glass, catching crystals in filter and Zippo Fluid in glass.
11. Bathe the glass of Zippo Fluid in a bowl of boiling water to raise temperature without flame. (any better ideas? Also what temp is ideal?)
12. Pour warm Zippo fluid into mixing jar and repeat steps 6-12 another four times, each time heating the solvent and using a new coffee filter. Final pull will be left in freezer for 48 hours, and after filtering, will evap the remaining fluid from the jar and scrape jar clean.



SWIM's main concern is does it matter how long the MHRB, water, lye solution is left to soak? Because as SWIM only has one, possibly two collection jars, this extraction could take ~5 days.

Should the DMT crystals be stored in particular way? SWIM plans to empty all into same dry glass/plastic vial and store in freezer. Will leaving them in open air help evaporate any leftover residue, or will that damage quality/deteriorate crystals?

As long as pipette extraction is careful to not pick up MHRB/lye solution could sodium carbonate cleaning be safely skipped? SWIM has trouble locating sodium carbonate at current time... well... reasonably priced anyway. How much of a danger could remaining lye pose? mild distaste/irritant or 'dissolve your throat' kind of threat?


Respect love and thanks to all, I hope your trips bring you much enlightenment,
Dijii
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
corridors of my cells
#2 Posted : 9/7/2009 6:33:07 PM

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....and nice to meet u too. Razz i saw u straight into the subject, probably won't get many answers tho, coz its not a very correct place to post that iguess Smile. try here instead http://www.dmt-nexus.me/forum/default.aspx?g=topics&f=45
 
d*l*b
#3 Posted : 9/7/2009 8:49:31 PM

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Quote:
appropriate safety gloves (any materials a good/bad choice for working with solvents+lye? disposable latex are a cheap option, any use?)


Buy the thickest ones you can from somewhere like Homebase / B&Q etc. Get a few pairs.

Quote:
appropriate safety goggles (would swimming goggles suffice?)


Go to shops as listed above, get some for painting / decorating / DIY work. Swimming goggles will probably get a bit sweaty after a long session.


D × V × F > R
 
transitory
#4 Posted : 9/8/2009 11:27:57 AM

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Dijii


Great detailed first post.

I first extracted using Nomans and will add my thoughts below;



Wilkinson's Lye: have used with great success (NB: don't use the yellow or black bottled drain liquid they sell)

Zippo Fluid: Again great success- the Ronsonol (yellow tin) also works.

Pickle Jar: ensure a tight fitting lid (if not wrap WELL with cling film.

Bonne Maman Jam Jar: Mushroom flavour?Laughing (see above)

Turkey Baster: I have used plastic ones from Wilkos without problem

Pipettes: I used eye droppers (79p from chemists- very controllable)

N95 respirator mask: Definitely overkill but looks the part & scares the wife! Laughing



Your extraction plan:

You have obviously done some serious research for which I commend you!Very happy Very happy Very happy Your method looks sound but I will offer my thoughts:
You may wish to consider using up to 3 jam jars so that you may decant from one to another. This will help to separate out any plant fats/oils/lye and is also useful for recrystalisation.


Quote:
Seal jar, place in freezer for 24 hours (or for longer?)


You may wish to evap. your solvent by 75% before freeze precip. I know this will cost more in Zippo but it's the baby you're interested in- not the bathwater. Evap. at room temp. no fan (minimised oxidation). Cover with single sheet of kitchen towel secured by rubber band. Be patient- evap can take some days with Mr Zippo. (longer it's in the freezer the better). Don't worry if you cant afford to evap 75% though (time/money)I still got good results without.


Quote:
Pour all contents through a coffee filter...


If you're lucky (and careful), you may not need to filter- the crystals should cling to the sides/base of you jar. I would avoid filtering if at all possible- just be very slow and steady pouring off the solvent (using the filter only as a safety net). NB: When your crystals remain in the jar PUT THE LID BACK ON, TURN UPSIDE DOWN AND PUT BACK IN THE FREEZER to drain off the solvent at low temp. This will help prevent your crystals re-dissolving.



Quote:
Bathe the glass of Zippo Fluid in a bowl of boiling water to raise temperature without flame. (any better ideas? Also what temp is ideal?)


Bathe the whole pickle jar instead in a pan of water (stood on a 'trivet' available at Tesco)- temperature should be just too hot to be able to put your hand in but NOT boiling! For turning your jar you will want to wrap in a tea towel. Turning a nice warm pickle jar for 10 min. is quite therapeutic - DONT loose concentration and drop it!)Sad


Quote:
SWIM's main concern is does it matter how long the MHRB, water, lye solution is left to soak? Because as SWIM only has one, possibly two collection jars, this extraction could take ~5 days.


Relax- you're well with the time frame- the longer/warmer the soak the more alks/oils/fats you can pull. Subsequent re-crystallisation will clean up your product nicely.


Quote:
Should the DMT crystals be stored in particular way? SWIM plans to empty all into same dry glass/plastic vial and store in freezer. Will leaving them in open air help evaporate any leftover residue, or will that damage quality/deteriorate crystals?


Leaving crystals in open air for a few days and occasionally agitating will help to evap. any residual solvent. I have noticed only minimal oxidation here. For longer term storage airtight is better. If freezing airtight is essential- condensation due to temp changes otherwise.


Quote:
As long as pipette extraction is careful to not pick up MHRB/lye solution could sodium carbonate cleaning be safely skipped? SWIM has trouble locating sodium carbonate at current time... well... reasonably priced anyway. How much of a danger could remaining lye pose? mild distaste/irritant or 'dissolve your throat' kind of threat?


I would always perform a warm sodium carbonate wash although some yield will be lost. I have sourced this labelled as dp brand Soda Crystals/ Washing Soda (look up soda-crystals.co.uk) available for £1 ebay / 79p Wilkos.


Hope this helps, good look.



Love


"Give enough that it feels good but not so much it hurts"
Life is not a task. There is absolutely nothing to attain except the realisation that there is absolutely nothing to attain.
What is sought remains hidden from the seeker by already being everything.

(Tony Parsons)
 
Dijii
#5 Posted : 9/9/2009 4:01:54 PM
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corridors of my cells wrote:
....and nice to meet u too. Razz i saw u straight into the subject, probably won't get many answers tho, coz its not a very correct place to post that iguess Smile. try here instead http://www.dmt-nexus.me/forum/default.aspx?g=topics&f=45


Thanks, for some reason I thought that this was the only thread I could post in until full membership Razz I don't know if I should repost this now or not? maybe I'll wait and do a revised version.
 
Dijii
#6 Posted : 9/9/2009 4:09:15 PM
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Quote:
Buy the thickest ones you can from somewhere like Homebase / B&Q etc. Get a few pairs.

Go to shops as listed above, get some for painting / decorating / DIY work. Swimming goggles will probably get a bit sweaty after a long session.




Good point on the goggles! I was thinking of just wearing them during grinding the root bark down more but I'm going to go get a pair that I don't mind wearing for long amounts of time.

For the gloves though, are you talking about plastic type of gloves? like would marigolds do? or material (like gardening gloves)? Just the reason I thought of using those disposable latex ones is that I can still feel/grip things carefully and not struggle with fiddly things like pipettes etc. Also if anything gets spilled on them I can just take them off in a second.
 
corridors of my cells
#7 Posted : 9/9/2009 4:25:07 PM

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here u go a few tips. Always put your mask, gloves and googles during working with lye or solvent. I was like the same thinking what harm can this shit do to me, at last its some solvent and some base Razz then had some blurred vision on my left eye, not so noticable but i suspect its coz i didnt use googles.

Another tip is that, i mostly use jars in my STB extractions and after i shake it makes pressure, becareful when opening the lid, you try to force it on a table not while holding it on your hand and near you body. As an advice i can tell after adding the solvent and shaking open the lid a minute after that and close it so there will be less pressure for later and you wont think its just stuck

Zippo fluid is good however i dont recommend using Ronson fluid. And if you dont have a pH meter you can buy from ebay which is more accurate than any pH papers (coz pH papers i bought from ebay wasnt working so well for high values after 10pH), So for your basified water you need pH around 12.5-13.5... less NaOH will give less but cleaner yield, more NaOH will give you more yield but also more impurities.

If you face any emulsions; http://www.erowid.org/chemicals/dmt/extraction_guide1/dmt_extraction_guide1.shtml try looking for "STEP 9" from this link

Gud luck in your extraction Smile
 
Dijii
#8 Posted : 9/9/2009 5:39:10 PM
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Cheers for the info on Ronsonol I think I'll use that, better than paying ~£3.50 per 125ml of Zippo! Definitely no residue on evap?

I've tested the jar and turned it around full of water, no leakage but I'll remember that cling film trick for future Smile

Hehe, not yet but in a month or two they may be mushroom flavour Very happy They were bought with that in mind anyway. Only downside is it would mean piercing the lids. When you say 'see above', do you mean cling film for that problem as well?

Quote:

You may wish to consider using up to 3 jam jars so that you may decant from one to another. This will help to separate out any plant fats/oils/lye and is also useful for recrystalisation.


Do the fats/oil/lye separate from the solvent? Just trying to get an idea of why to decant... Well I've got another couple of jars open right now but it looks like another 2-3 more weeks of jam on toast every morning until they empty! Laughing

Quote:
You may wish to evap. your solvent by 75% before freeze precip. I know this will cost more in Zippo but it's the baby you're interested in- not the bathwater. Evap. at room temp. no fan (minimised oxidation). Cover with single sheet of kitchen towel secured by rubber band. Be patient- evap can take some days with Mr Zippo. (longer it's in the freezer the better). Don't worry if you cant afford to evap 75% though (time/money)I still got good results without.


Hmm I think I read somewhere before about that, although I cant remember why/how it helps? Why the kitchen towel? If I use Ronsonol then I don't mind the cost, its actually easier not to though because I don't have a measuring jug accurate enough for quantities (I think the lowest point is 200ml), so its ideal that lighter fluid comes packaged as the exact amount I need. Does it work as much of a yield booster?

Quote:
When your crystals remain in the jar PUT THE LID BACK ON, TURN UPSIDE DOWN AND PUT BACK IN THE FREEZER to drain off the solvent at low temp. This will help prevent your crystals re-dissolving.


Great advice, thanks Smile

I was thinking of boiling the water, turning off the hob then putting the glass in, so hopefully water isn't quite boiling temp and will just raise the heat of the glass afterwards. I'll instead put the mixing jar in there, and heat the water with it in, probably separating the base of the pan and glass jar with a tea towel or something if I can't find the trivet.

Quote:
Leaving crystals in open air for a few days and occasionally agitating will help to evap. any residual solvent. I have noticed only minimal oxidation here. For longer term storage airtight is better. If freezing airtight is essential- condensation due to temp changes otherwise.


a ziplock baggy or airtight vial at room temp is fine for storing for quite a while?

Quote:
I would always perform a warm sodium carbonate wash although some yield will be lost. I have sourced this labelled as dp brand Soda Crystals/ Washing Soda http://www.soda-crystals.co.uk available for £1 ebay but also some High St shops.


I actually have a bag of those exact soda crystals already! I got put off when I checked it though because the back of the packet says:

sodium carbonate decahydrate
greater than 30%


I wasnt sure about what decahydrate means, if that makes it unsuitable. (Although now that I think about it, it sounds related to water, or lack of water and not a different but similar substance) Also the greater than 30% is a little vague, is it saying 70% is something other than sodium carbonate decahydrate? It was a turn off to see that percentage anyway because I thought it made it sound rather impure. But if thats fine then I've no problem finding that and adding a little purification to the end of the process!
 
Dijii
#9 Posted : 9/9/2009 5:48:25 PM
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Thanks for the safety advice corridors of my cells, I hope your eye has recovered.

Mmm I figured at least while heating the jar that I should take the lid off in case of pressure. You say 'shaking' but the impression I get from what people have written is that anything rough will make it form an emulsion, so I was planning on moving it very slowly to be sure. Would you need to shake it very hard to form an emulsion? Thanks for the link incase that does happen, it may be very useful!

Any reason why you dont recommend Ronson lighter fluid?

I hadnt planned on checking the pH, I figured if I used equal amounts lye-root bark then it should roughly have the same pH as everyone else. I'll have a look for pH meters anyway, many other things I can use it for Smile
 
corridors of my cells
#10 Posted : 9/9/2009 6:02:19 PM

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Dijii wrote:
Thanks for the safety advice corridors of my cells, I hope your eye has recovered.

Mmm I figured at least while heating the jar that I should take the lid off in case of pressure. You say 'shaking' but the impression I get from what people have written is that anything rough will make it form an emulsion, so I was planning on moving it very slowly to be sure. Would you need to shake it very hard to form an emulsion? Thanks for the link incase that does happen, it may be very useful!

Any reason why you dont recommend Ronson lighter fluid?

I hadnt planned on checking the pH, I figured if I used equal amounts lye-root bark then it should roughly have the same pH as everyone else. I'll have a look for pH meters anyway, many other things I can use it for Smile


I never had emulsions to be honest. and im always shaking it gud Razz and tried ronson but after evaporation i saw it leaves much dirtier product than zippo did. but yea i dont know may be what you get there is not what we get here anyways. We have fake brands for everything Razz so...

and yea what you say about the pH is correct actually.. i mostly measure tho , personal curiosity i guess Smile eheh

EDIT: btw just came accross with this while just surfing and thought it may help

http://forums.mycotopia.net/dmt-spice/33197-entropymancers-dmt-extraction-overview.html

it says:
Quote:
The internet community has really stepped up in terms of providing step-by-step walkthroughs to guide the layman through the process of extracting DMT crystals. A quick search for DMT extraction teks turns up dozens of procedures; but how’s a body to know which tek to choose? I've seen a lot of posts by people having problems with purity due to trying to follow a tek too closely (especially ones that don't give the reader a target pH).


you will also find some brief info about purifications. gud luck!
 
acolon_5
#11 Posted : 9/9/2009 9:21:20 PM

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If it hasn't been mentioned already if you are grinding up MHRB yourself you should wear a mask. A fine purple/pink powder will get everywhere and it will royally screw up your sinuses for a few days.
The Spice extends life
The Spice expands consciousness
The Spice is vital for space travel
___________________________________________________________________________________________________
Never underestimate the power of STUFF!


I am certifiably insane, as such all posts written by me should be regarded as utter nonsense or attempts to get attention.

I don't know SWIM and personally don't trust him at all. If SWIM is posting, most likely I will not respond...as I said, I don't trust the guy. YOU I trust, but never SWIM.
 
d*l*b
#12 Posted : 9/10/2009 3:21:03 PM

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Dijii wrote:
Any reason why you dont recommend Ronson lighter fluid?


I've heard scattered bad reports from the US. According to the MSDS it's just VM&P naptha in Blighty at least. Nowt wrong with it that I've found.
D × V × F > R
 
transitory
#13 Posted : 9/10/2009 7:52:36 PM

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Dijii


Quote:
Cheers for the info on Ronsonol I think I'll use that, better than paying ~£3.50 per 125ml of Zippo! Definitely no residue on evap?


There was no residue on my evap tests for either Zippo or Ronsonol but Swan left an unmistakable oily film. Perhaps an evap test should always be performed as this stuff may vary from batch to batch.


Quote:
I've tested the jar and turned it around full of water, no leakage but I'll remember that cling film trick for future


Still take care- warm naphta seems to achieve leakage where water doesn't!


Quote:
Do the fats/oil/lye separate from the solvent? Just trying to get an idea of why to decant...



Sorry, I was a little tired when I refered to decanting- I was recalling my attempts at recrystallisation where decanting is most usefull. Shouldn't be necessary at all before freeze precip. unless you can see some lye-water in there. This will fall to the bottom of the jar and can be left behind with carefull decanting of the solvent into a second jar. As for partial solvent evaporation before freeze precip I believe the reason is to bring the solvent nearer to its room temperature DMT saturation point. This leads to the DMT crashing out of solution more readily at -20deg since the solvent can no longer hold it. Some report the solvent beginning to appear milky at room temperature as the total volume decreases- the milkiness being the beginnings of DMT precipitation. Don't worry if this doesn't happen though- I've gained significant yield from solvent that appeared 'empty'Very happy The reason I suggested covering with Kitchen towel is just to keep airborne particles out of your solvent whilst evaporating. It's surprising just how much crap can appear as if from nowhere! Sorry I can't comment on comparative yields for alternative solvents - I just don't have enough extractions under my belt yetSad


Quote:
a ziplock baggy or airtight vial at room temp is fine for storing for quite a while?



Certainly. I however found a more aesthetically pleasing women's cosmetic 'powder compact' for mine. My spice soon took on an unexpectedly precious significance. Plastic baggy just didn't sit right somehow.Wink



As for the safety of the "sodium carbonate decahydrate . . . greater than 30%" I am hoping that someone more chemically accomplished than myself will chime in here- I decided myself after some research that it was OK to use(I had had exactly the same points of concern as yourself)- but I can't for the life of me recall my reasoning!Embarrased

The main thing is to take your time, Be safe and enjoy the process! The extraction and purification of the spice was almost a ritual to me. Rites of passage, ceremony stuff. There is a wonderful feeling that you have somehow earned your sacrament. I'm glad that you began this thread Dijii. The lack of explicitly UK relevant extraction topics is frustrating. Certainly some pointers will be left here for future UK psychonautsCool


Please do update us all as to your progress and good luck.



Love
"Give enough that it feels good but not so much it hurts"
Life is not a task. There is absolutely nothing to attain except the realisation that there is absolutely nothing to attain.
What is sought remains hidden from the seeker by already being everything.

(Tony Parsons)
 
Dijii
#14 Posted : 9/10/2009 11:29:54 PM
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Quote:
There was no residue on my evap tests for either Zippo or Ronsonol but Swan left an unmistakable oily film. Perhaps an evap test should always be performed as this stuff may vary from batch to batch.


Thanks, Swan was another option I'd thought of testing but I'll steer clear. Hopefully once I get some money together before next time I'll be able to compare a few brands in an evap test and get the results up.

Quote:
Still take care- warm naphta seems to achieve leakage where water doesn't!


Noted!

Quote:
The reason I suggested covering with Kitchen towel is just to keep airborne particles out of your solvent whilst evaporating. It's surprising just how much crap can appear as if from nowhere! Sorry I can't comment on comparative yields for alternative solvents - I just don't have enough extractions under my belt yetSad


Useful advice. And don't worry, I'd think there wouldnt be a great deal of difference in the yield from different lighter fluids, although I expect other solvents like white spirit could make a difference in how much can be pulled each time. Saturation points I suppose.


Haha that sounds just like something I'd do. If I store it in a tiny vial I expect I'll end up decorating it Razz


Well I managed to find the MSDS for that brand of Soda Crystals. But understanding what it means... Rolling eyes If someone who is familiar with MSDS's can take a look and help out that would be great.
All I've noticed is that it mentions an anti-caking agent, although it doesnt say anything more than that, I was hoping for a percentage, or something from it. If its worked for you and you havent suffered from it then I'll go ahead and use it anyway, I'm sure it clears more contaminants than it leaves! (if any)

Quote:
The lack of explicitly UK relevant extraction topics is frustrating. Certainly some pointers will be left here for future UK psychonautsCool


Tell me about it! I scoured the web and even on the nexus I found so much contradictory info on which solvents work and which don't. Once I can afford it, I'd like to do some evap tests on a wide range of solvents easily found in the UK.
I hope this will be useful to people. After SWIM's done the first extraction, there should be a new post with all this info I've found from around the place, compiled into a single guide for UK explorers. I'm sure a lot of others will help contribute, especially if they've got familiar with the meaning of trial and error!

I'll be sure to keep this updated Smile May be a few weeks though...
Thanks for all the help!
 
transitory
#15 Posted : 9/13/2009 9:05:04 AM

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Oops!

looks like I broke a rule about posting direct links to Suppliers.

Embarrased



In reference to a UK source of sodium carbonate, dp brand mentioned above produce sodium bi-carbonate also available at Wilkos for pennies. Ingredients listed as 100% sodium bi-carbonate. I have read here at the Nexus that sodium bi-carbonate can be used, but you can lose yield as it fails to raise the pH high enough. I have also read that it's perfectly OK with no additional loss of yield! Confused I haven't tested this myself.

In any case I think that this could be the most useful info:

"baking soda (sodium bi-carbonate) can be converted to to sodium carbonate by heating in an oven @ 400 deg F for 1 hour (put it on something that's glass, don't want to be forming any metal salts!)" Cool

(Info gained from Nexus post- sorry no source link)



Love

"Give enough that it feels good but not so much it hurts"
Life is not a task. There is absolutely nothing to attain except the realisation that there is absolutely nothing to attain.
What is sought remains hidden from the seeker by already being everything.

(Tony Parsons)
 
Mysterion
#16 Posted : 9/15/2009 10:21:59 AM

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Thank you for this amazingly detailed thread. I've been working on which tek is best for me and the above has answered many questions. Shall attempt my first extraction in the next few days.

Thanks all again for the wealth of information.

Much empathy emanating from this 'carbon unit'.

Smile
 
Dijii
#17 Posted : 9/23/2009 10:14:32 PM
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SWIM encountered a few problems....

First the water/lye reaction was far more extreme than expected. All 125g lye was added at once, stirred in and by the time it has been dissolved the water was boiling (or at least producing many air bubbles, while at high heat)
The water only filled the pan maybe 1/4 of the height, however the foam that was produced by just that water/lye reaction overflowed many times. It was like a comical chemistry experiment gone wrong.
Lesson learned... add lye slowly bit by bit and let the reaction finish before adding much more.

SWIM was forced to remove the foam and most of it ended up down the sink (more favourable than all over the kitchen)
Do you think this removed any lye?
SWIM is a little unsure but continued anyway. Just checking a bit of chem software it shows me a water lye reaction in the quantities that were used should product about 40 celcius heat and only evaporate some of the water.

The Mixing pot in the end was a pressure cooker as the largest jar found was still too small.
Any idea if the alkali/basic properties of the lye do harm to metal/ceramic/plastic/glass?
I know lye reacts with aluminium, although I'm fairly sure its not an aluminium pressure cooker Razz

SWIM just got hold of a cheap Ph meter and will check the mixture now. One pull has already been done and left in the freezer although SWIM hasnt personally checked it yet, SWIM hears there is a whiteish layer on the bottom of the jar.
Could crystals form on just the bottom of the jar?

One final problem, only about half of the solvent that went in, came back out from the mixture. This is because even with pipettes it was impossible to grab the thin layer. SWIM has gained more.
Should more be added so that 125ml can be pulled back out of the mix pot next time?
 
transitory
#18 Posted : 9/24/2009 7:48:00 AM

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Hi Dijii


Great to see your friend taking the time to update this thread Very happy

His experience with the lye is a great warning to all of us- I have only added slowly in the past and did wonder what all the fuss with gloves & goggles was about. Shocked Did he have vinegar to hand for neutralising the lye? Vinegar would have ended its alkali action. Not sure whether the alkalinity of the water would have been reduced by the loss of foam but I've heard that adding more lye can do no harm.

Yes- I'm sure that I've had crystals form on just the base of the jar before. Adding a little more solvent may be an option, given that you may evaporate the final pull in order to recover anything that's possibly remaining in solution. I feel a better option could be to roughly decant the top layer (including some lye water) just to be sure he's got all the solvent. Then decant from one smaller container to another- thereby gradually separating all solvent from lye. My concern is that too much solvent will leave the solution unsaturated thereby making freeze precipitation ineffective. He may find all this to be less of a problem during larger extractions.


Sorry I couldn't help more but please ask your friend to keep this thread updated as to his progress.


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Dijii
#19 Posted : 9/25/2009 9:28:37 PM
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It seems that whitish layer was indeed crystals Smile First pull successful.

SWIMs cheap Ph meter wasn't appropriate, it wasn't an all purpose meter (its designed for garden use), so the range is too low to see if the water has the correct alkilidity, however it was pushing the needle to the end of the gauge pretty fast showing it was still very strong alkali.

After the first pull went through the coffee filter back into the mix pot, SWIM decided to put in another quantity of lighter fluid; approx half the amount used the first time, so that the next pull will be the amount that was originally put in (125ml). SWIM tells me he is checking the second pull later tonight, and promises to keep us updated.

transitory, I'm told the goggles and respirator were a godsend. When the fumes were coming from the pan during the reaction and even a short while after, they stung SWIM's eyes lightly from maybe a second or two looking down at the pot, but only on par with chopping onions. Although that was all the warning needed, so goggles stay on. Same with the mask, one or two occasions SWIM caught a whiff of the fumes, and then the mask stayed on. Gloves were not crucial but very useful nonetheless as there was some spillage and remember that mix dyes things purple pretty well.
Maybe we ought to write a basic safety guide on here, what certain substances like lye and particular solvents can do
Shamefully, no, vinegar was not to hand. For that reason gloves stayed on all the time lye was being handled.

Funny you say that transitory, SWIM had that idea too and ended up using the thinnest tallest glasses he could find, although would prefer to find something extremely thin and long, like plastic tubing, which should make decanting a lot easier by reducing surface area between layers.

Also I'd like to confirm Ronsonol as leaving no residue in a half full shot glass evap. So its much better than zippo for value.

At the moment, the plan ends at the point that several freeze precips have been done, all the crystals removed, dried and mixed together into one container...
Can someone please advise me on recrystallisation. What does it do? How does it work?
Same regarding cleaning with sodium carbonate.
Are either/both neccessary?
How would one know of lye contamination?
 
Dijii
#20 Posted : 9/27/2009 8:58:14 PM
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SWIM has had a catastrophe!

When SWIM checked the mix pot to perform another pull, he found it was bone dry. The solution in the mix pot (pressure cooker) has literally corroded through the metal making a small hole in the bottom of the pan. The pan has since been stored safely to dispose of later. He tells me he will probably scrape out the content and get rid of that, taking the pan to a tip/dump as its rather large and noticeable. What do you think?

Fortunately he was able to perform two successful freeze precipitations so it was not a complete failure. Those are not yet cleaned or weighed, they are wrapped up in the coffee filters still.

On the second pull (keep in mind this was in the same jar as the first, and the jar was not cleaned, just all the crystals scraped out) there was a different solid layer on the bottom of the jar under the crystals, incredibly thin and milk coloured. Could that be lye? If so, how could SWIM clean that out of the crystals? would anyone say a definite to recystallisation or sodium carbonate cleaning?

SWIM thanks you greatly for all the advice and tips I have been passing on.
I will make sure to post a new topic to inform everyone of all the problems SWIM has had with his first time so that they can learn from his mistakes.

EDIT: Ah... SWIM had a discussion with someone before beginning about the corrosive properties of lye on aluminium and came to the conclusion a pressure cooker couldnt be made from alu, it must be something else. Well apparently most pressure cookers are aluminium. So there...
 
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