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HCl Salting Options
 
CAPTAIN HYPERSPACE
#1 Posted : 12/5/2011 1:05:09 AM

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SWIM has a FOAF who performed and STB on 200g of dried san pedro but would like a second opinion on the salting phase. 3 pulls have been performed using 1L Xylene @ approximately 330ml per pull, leaving a the Xylene a brownish green. Based on 1L of Xylene, what would be the best ratio's to mix the HCl with D-H20, and would SWIM basically be looking to achieve a pH of 6-7 after being mixed with the Xylene? SWIM realises there are many posts regarding this, but feels it is always better to be SAFE than sorry when it comes to chems. Thanks Smile
i am a compulsive liar with psycotic tendencies and nothing i say should be believed
 

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futura
#2 Posted : 12/5/2011 7:48:56 AM

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Best way to do this is titration....

add 20 drops 10% HCL to 1200 ML Distilled Water...

Add to 1 Liter Xylene and mix thouroughly...

Let settle for a few minutes and use Pipette or Turkey Baster or Straw to draw off some of the Salting Water only(Make sure no xylene gets in the straw or baster)

Test drawn off salting water with Digital PH Meter...

Ideal PH is 6.6-7.0 for the cleanest Mesc Only alkaloids...

keep adding a drop or two at a time of the 10% HCL till after mixing and left sitting the PH stays at 6.6-7.0...

Then let sit overnight for total mesc migration...

seperate salting water from xylene and fan evaporate with no heat...

Clean with freezing cold Anhydrous Acetone 3 times and freezing cold anhydrous IPA twice...

 
CAPTAIN HYPERSPACE
#3 Posted : 12/5/2011 7:52:18 AM

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So many conflicting reports on salting???!!! SWIM has added approximately 5 drops of HCl (from Diggers 30% HCl bottle), to 50ml of d-h20, then added to Xylene (approx 350-400ml), swirled and shaken, before freezing so the Xylene can be poured off and HCl/water solution saved to later evaporate. SWIM plans on repeating this process 5 times. Still worried that the above HCl solution will be TOO STRONG, as some teks say 5 to 6 drops in a 1 and a half cups of water. Any help much appreciated. Thanks
i am a compulsive liar with psycotic tendencies and nothing i say should be believed
 
CAPTAIN HYPERSPACE
#4 Posted : 12/5/2011 8:00:39 AM

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Thanks futura. Very helpful, although SWIM still has 2 queries as he is new to Salting, and usually works with Freebase DMT, and never bothers to turn it into a salt. First question is: if the bottle is 30% HCl, how would SWIM go about making a 10% solution?
And secondly, has no access to Anhydrous Acetone, and not 100% on how to make normal Acetone anhydrous.
Also, based on what SWIM reported in his last post, will this solution be to strong? Should his current acidic solution be discarded?
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Poekus
#5 Posted : 12/5/2011 8:14:38 AM
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5 drops of 33% to 50ml is a little too much. It doesn't matter that much if you clean it or want a full spectrum alkaloid extract. It's very hard to determine how much acid you should add without a Ph meter. It depends a lot on the alkaloid content in your solvent.

Excess Hcl evaporates off so don't worry about it too much.
You can clean with 99.x IPA. I get it at electronics store in a small spray bottle. It's got 99.7 purity from a brand called Kontakt. Don't know for sure if they sell it in australia. This will clean it to near white mescaline.
 
CAPTAIN HYPERSPACE
#6 Posted : 12/5/2011 8:49:33 AM

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Thanks Poekus. 99% IPA is available, as is acetone-(but not in anhydrous form). SWIM also has a digital pH meter, but is obviously missing something here...If using 30-33% HCl from the bottle, what would be the correct amount of d-h20 to mix with it, or what pH reading should SWIM try to acheive before mixing with the Xylene extract?
i am a compulsive liar with psycotic tendencies and nothing i say should be believed
 
CAPTAIN HYPERSPACE
#7 Posted : 12/5/2011 8:56:46 AM

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Futura suggested adding 20 drops of 10% HCL to 1200ml of water...Would this therefore equate to mixing a third of the amount of drops at 33% (say 6 or 7 drops to 1200ml) to acheive the same result?
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Poekus
#8 Posted : 12/5/2011 9:22:31 AM
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Aim for Ph 5.7-6 before adding it to the solvent. When it's stirred with the solvent the Ph can be measured again. If there was enough alkaloids in the mix your Ph will come to neutral levels.
You could salt your first two pulls with about Ph 5.7-6 and your last ones at 5 or lower to pull out all remaining alkaloids. Evaporate the saltings seperately. You'll have to clean the latter more but at least you got all the alks out.
Getting near pure mescaline in the salting is very hard to do. You'll probably even have to clean up a little of the first saltings if pure white is your goal.
If the water is cloudy when salted, the ph was too low.
 
CAPTAIN HYPERSPACE
#9 Posted : 12/5/2011 10:28:08 AM

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SWIM has removed his jar from the freezer, and added another 100ml approx, although assumes the damage is already done?
He has now separated the acidic solution from the Xylene (which is now very much orange). This was done before reading the previous post regarding pH, but tested the 2 different solutions and found that the Xylene by itself is pH 7, and the acidic solution is pH 3.3 Some parts of the acidic solution are indeed cloudy. SWIM will evap off the cleanest part of the acidic solution in one dish and the cloudy junk in another. He believes that the cloudier shit also has a small amount of Xylene left in it. Is he correct in thinking that this will evaporate off anyway? Maybe SWIM will just have to write this extraction off as a 'learner', and start from scratch again. One thing SWIM has noticed is that the acidic solution has a very 'fishy' smell to it, which he has smelt before after drying out a shitload of phylodes from Acacia Acuminata. He believes this smell to be a quality of phenethylamine? Thanks again Poekus, your last post without a doubt, made things 100% clearer in the way you explained it.
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Poekus
#10 Posted : 12/5/2011 11:47:42 AM
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Do a evaporation test with 10ml ofyour clean pure Xylene on a glass dish. See if any residue is left. If there is no residue your extracted product is safe to consume.
The cloudiness are mostly the cactus oils. When you clean the extract with IPA and evaporate the dark leftover IPA you'll have a very smelly (very unique herbal smell I actually like it) dark purple oily crush. Also Xylene dissolves in IPA so any small leftovers are removed with a IPA wash.
Watch out when evapping your HCl water. I fucked up my 'rust-free' oven with it once. Best to do it outside.
 
cruisinalltheway
#11 Posted : 12/6/2011 6:08:05 AM

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anhydrous acetone: use epsom salt; bake it in the oven for 30 min-1hr? to remove any moisture and then after it has cooled, add it to a safe container with acetone, shake it up a bit and if i remember correctly you now have 99%+ anhydrous acetone, perhaps someome can comment with actual weight or proportions, its been a long time for me Rolling eyes
 
futura
#12 Posted : 12/6/2011 7:06:15 AM

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Yes your PH(3.3) is way too low...That means you got a lot of Non Mesc alkaloids as well.

also when you evap crystals will be crunchy and reddish brown form acid oxidation...

All is not lost however...

Do the three freezing cold anhydrous Acetone Washes and two freezing cold anhydrous IPA washes and you will remove most non mesc alkaloids and have nice off whit to tan Mesc Crystals...Make sure you use like a mortar and pestle and crush crystals completly while washing in the acetone and IPA!!!

My advice after doing the 5 total washes is to pour very hot(not boiling)water into glass used to hold washed crystals and then evap that to remove all traces of Acetone and IPA...

To get 10% HCL from a 30% solution simply add 33 ml 30% HCL to 67 ml water and you should have an appox. 10% solution...

I find it easier to titrate with a weaker solution like 10%... you dont overdo it with a drop or two like can happen with 30% or higher!!!
 
futura
#13 Posted : 12/6/2011 7:09:12 AM

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cruisinalltheway wrote:
anhydrous acetone: use epsom salt; bake it in the oven for 30 min-1hr? to remove any moisture and then after it has cooled, add it to a safe container with acetone, shake it up a bit and if i remember correctly you now have 99%+ anhydrous acetone, perhaps someome can comment with actual weight or proportions, its been a long time for me Rolling eyes


This works for IPA as well...add about 30 Grams after the epsom salts cools down(leave it in the oven with the door closed while cooling down so it does not draw the moisture back in) to a mason jar containing 1 can Acetone or 1 bottle 91% IPA shake well put inn freezer shaking every few hours then just let sit for a day and siphon off what you need from the top trying not to stir up epsom salts...

NOTE: Put foil Under mason jar lid as the acetone or IPA will dissolve the rubber seal if you dont!!!!

I would spread the epsom salts in a thin layer on aluminum foil and bake for 2-3 hours at 400 Deg F to totaly dry it...
 
CAPTAIN HYPERSPACE
#14 Posted : 12/6/2011 10:51:46 AM

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Thanks a lot again guys. Very helpful. After evaporating off, SWIM was indeed left with a slightly crusty red to brown product. Will attempt to clean it and see what we come up with. SWIM is now a lot more confident with the titration process so hopefully next extraction will be more successful. Can anyone find any problem in these quantities used in the extraction?

200g of dried, de-spined, de-skinned San Pedro...this was added to:
4L of d-h20 basified with approx 400g of NaOH to a pH of 11...
3 pulls over a 24hr period with 400ml of Xylene per pull...
Approximately 20 drops of 10% HCL added to 1200ml of d-h20 to acheive a pH of 5.7 to 6, then:
Acidic solution added to the 1L(approx) of Xylene, shaken for 3-5 minutes, then left until layers have separated.
A small amount of the bottom HCL solution tested for a pH of 7, and if correct:
Left to sit overnight for the mescaline to migrate fully (with repeated shaking over this time)?
The bottom layer drawn off and (either) placed on low heat hotplate to reduce amount of water, or left under a fan till evaporated, followed by the anhydrous acetone/IPA washes.


*** SWIM wonders, if the amount of basified d-h20 can be reduced to say 2L instead of 4L, with whatever amount of NaOH required to get the pH to between 12-14, instead of pH 11 as in last extraction, or is 11 fine?

***SWIM wonders, when using approx 20 drops 10% HCL solution added to 1200ml of d-h20, is this only added once to the Xylene, pulled and evapped, or is this amount split and 3 x 400ml pulls performed before combining and evapping?

Also, if the amount of basified d-h20 used IS reduced to say 2L instead of 4L, would the 1200ml of acidified solution also be halved...Again, SWIM has seen so many variations on quantities used, it makes his brain hurt lol. One tek, using 200g of dried cactus called for 200g of NaOH in 300ml of water...to SWIM this seemed ridiculous???

So, a huge thanks again to everyone, and if anyone wishes to add their comments to the quantities used in the above tek, and what they consider to CORRECT quantities, it would be much appreciated...thanks...


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dg
#15 Posted : 12/6/2011 2:25:44 PM
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cruisinalltheway wrote:
anhydrous acetone:

or, just use a salt form that isn't very soluble in cold water
 
Poekus
#16 Posted : 12/6/2011 6:55:12 PM
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dg wrote:

or, just use a salt form that isn't very soluble in cold water


Do you have an example of a salt which you can use, which has its possible excess volume evaporated or cleaned up with cold water instead of Acetone, IPA or MEK without dissolving the mesc? I'm very interested to experiment with this.
 
futura
#17 Posted : 12/8/2011 5:21:44 AM

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CAPTAIN HYPERSPACE wrote:
Approximately 20 drops of 10% HCL added to 1200ml of d-h20 to acheive a pH of 5.7 to 6, then:
Acidic solution added to the 1L(approx) of Xylene, shaken for 3-5 minutes, then left until layers have separated.

I use a Braun electric stirrer I got at a garage sale for 6 bucks... Put your xylene and salting water in a large glass pitcher and stir it up for five minutes...Then check PH and keep at it till ph stabilizes at 6.6-7.0..(Remember ONLY check PH of Salting Water...any Xylene or D-Limo or other NP solvents will mess up PH reading!!!)

[quote=CAPTAIN HYPERSPACE]A small amount of the bottom HCL solution tested for a pH of 7, and if correct:
Left to sit overnight for the mescaline to migrate fully (with repeated shaking over this time)?

No just let it sit and do not shake or stir so emulsions seperate and alkaloids fully migrate...You can then after that check PH again and carefully bring it back down to PH of 6.6-7.0 if there were so much alkaloids present the PH rose over that after letting it sit for 24 hours...be carefull though...at this point a single drop of even 10% HCL can push the PH way too low again!!!

[quote=CAPTAIN HYPERSPACE]The bottom layer drawn off and (either) placed on low heat hotplate to reduce amount of water, or left under a fan till evaporated, followed by the anhydrous acetone/IPA washes.

I suggest being patient and using no heat while evaporating...you will get bigger cryatals which will have less plant oils in them and be easier to clean...


[quote=CAPTAIN HYPERSPACE]*** SWIM wonders, if the amount of basified d-h20 can be reduced to say 2L instead of 4L, with whatever amount of NaOH required to get the pH to between 12-14, instead of pH 11 as in last extraction, or is 11 fine?

Get PH to 12.0 at least(It will produuce less of an emulsion layer at 12.0 to 12.5) and yes you can reduce liquid by simmering at 150 Deg Farenheit...Watch temp and be carefull as you can easily burn alkaloids and lose potency...

[quote=CAPTAIN HYPERSPACE]***SWIM wonders, when using approx 20 drops 10% HCL solution added to 1200ml of d-h20, is this only added once to the Xylene, pulled and evapped, or is this amount split and 3 x 400ml pulls performed before combining and evapping?

Use all 1200 ml at once if titrating with ph meter...smaller amounts are better for blind salting(Just guessing your PH and having no PH Meter)...

[quote=CAPTAIN HYPERSPACE]Also, if the amount of basified d-h20 used IS reduced to say 2L instead of 4L, would the 1200ml of acidified solution also be halved...

NO...1200 ML should get all the goods in one salting if titrating...but you can always save xylene and salt again to be sure...Remember though that the xylens will have a lot less alkaloids in the second salt so way less acid will probably be needed to not go under ph 6.6




 
LawnMan
#18 Posted : 12/8/2011 5:54:18 AM

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I know it too late but I've had the best resuls with 3-5 drops of 33 percent hcl per 100 ml. If u get the acid ratio right in the titration process (comes with experience) a wash isn't tototally necessary. U end up losing a fair amount of product
 
floatingwater
#19 Posted : 12/22/2011 5:19:51 AM
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Just realized that all of futura's very helpful salting dilutions are based on weight / weight calculations.

So let's say that you find muriatic acid at a hardware store. The bottle says 30% HCl. Now let's get more specific here; 30% of what measurement is HCl?

It turns out that the 30% is calculated from the weight of HCl gas divided by the total weight of the solution (which is HCl gas weight + water weight). For instance, 30g HCl / (30g HCl + 70g water) = 30% (weight/weight)

So when futura is talking about making a 10% HCl solution from the store bought HCl, which reads 30% on the label, futura is sticking with the weight/weight (or w/w) designation of percentage when he says mix 33 mL of 30% HCl with 67 mL of water. This is essentially a (1/3) dilution of the original 30%. 30% (w/w) multiplied by a dilution factor of (1/3) equals 10% (w/w).

Now you're thinking, yeah so?

Well, if you think you can just take a shortcut and buy 10% HCl that is fine but beware that it could actually be 10% HCl (volume/volume). In other words a 10% dilution of the original store bought 30% HCl solution by volume and not by weight.

This means that, for example, 10 mL of the 30% store bought HCl solution was added to 90 mL of water. Or in other words a (1/10) dilution factor using volume/volume as the meaning of percentage. ** This would actually be the equivalent of a 3% (weight/weight) HCl solution **

So, to get straight to the point it will change your calculations of how many drops of HCl to add per however many hundreds of mLs of water used depending on how the percentage of your HCl solution is measured; whether its (weight of HCl / weight of solution) OR (volume of original stock HCl / volume of solution).

Please, if this is totally wrong, let me know, but this is what I'm decyphering from reading through these threads

 
chemisch
#20 Posted : 2/17/2012 11:38:58 PM

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floatingwater wrote:
Just realized that all of futura's very helpful salting dilutions are based on weight / weight calculations.

So let's say that you find muriatic acid at a hardware store. The bottle says 30% HCl. Now let's get more specific here; 30% of what measurement is HCl?

It turns out that the 30% is calculated from the weight of HCl gas divided by the total weight of the solution (which is HCl gas weight + water weight). For instance, 30g HCl / (30g HCl + 70g water) = 30% (weight/weight)

So when futura is talking about making a 10% HCl solution from the store bought HCl, which reads 30% on the label, futura is sticking with the weight/weight (or w/w) designation of percentage when he says mix 33 mL of 30% HCl with 67 mL of water. This is essentially a (1/3) dilution of the original 30%. 30% (w/w) multiplied by a dilution factor of (1/3) equals 10% (w/w).

Now you're thinking, yeah so?

Well, if you think you can just take a shortcut and buy 10% HCl that is fine but beware that it could actually be 10% HCl (volume/volume). In other words a 10% dilution of the original store bought 30% HCl solution by volume and not by weight.

This means that, for example, 10 mL of the 30% store bought HCl solution was added to 90 mL of water. Or in other words a (1/10) dilution factor using volume/volume as the meaning of percentage. ** This would actually be the equivalent of a 3% (weight/weight) HCl solution **

So, to get straight to the point it will change your calculations of how many drops of HCl to add per however many hundreds of mLs of water used depending on how the percentage of your HCl solution is measured; whether its (weight of HCl / weight of solution) OR (volume of original stock HCl / volume of solution).

Please, if this is totally wrong, let me know, but this is what I'm decyphering from reading through these threads




well ph is measured in hydronium ions so hcl techinically is not an acid. 1 hcl to 1 h2o is an acid hence the reaction Hcl+h20= cl + h3o+
if you can bassify in ammononia and extract with dcm why not smoke it?
 
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