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Magnesium Sulphate in an A/B salt tek, possible 3% yield (NEEDS TO BE CONFIRMED)

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anonenium

Rising Star
hello

ok was hoping to get some more input before talking about this but considering the silence here goes nothing.

a while ago there was a thread here


so after talking about it was attempted.

this was very rough.

THIS HAS NOT BEEN REPEATED YET AND THERE IS NO WAY AT THIS TIME TO ID THE PURITY, SO PLEASE CONSIDER THIS EXPERIMENTAL UNTIL RESULTS CAN BE SORTED OUT.


50g of MHRB soaked and boiled in vinegar and water was added to 800ml then was separated into two jars.

in jar one went 20g of sodium chloride (table salt).

in jar two went 20g of magnesium sulphate (dehydrated epsom salt).

both were then based.

added 50cc of naphtha to each, shook both like crazy and when it separated something interesting happened.

the magnesium jar's naphtha precipitated just by sucking the stuff up with the separator (pressure change possibly)

after seeing this (and opening the sodium jar and blowing on it to no precipitation) both jars were thrown together into one large jar, along with solvent, and another 20g of magnesium sulphate was added (into the already alkali solution) and everything was agitated.

the results after four pulls was just over 2.3g with more than 1g white after three recrystallizing (and oddly enough once the jar of yellow and red once put back in solvent, the red crystallized as room temperature on the bottom of the jar without anything other than the naphtha pulling it out (not sure if thats note worthy but the red fell out and solidify over a few minutes)).

now, the purity is not known, and although when tested it is active it may not be safe, and considering the variables (like the fact that two kinds of salt were used) there is still a bunch that needs to be figured out, so please dont presume anything.

so on that note, help is needed and appreciated, if anyone could tell what they would do as the next step from here then it would be appreciated, or can lend a hand then thank you.
 
thanks for the reply

it meant that when the naphtha was pulled up into the syringe it started precipitating while inside the syringe, like being forced through the small space knocked it out of suspension

never seen that occur before except after evaporating a jar which could cloud if you blew on it, kind of surprise it occurred directly out of the jar and since the sodium chloride (table salt) jar didnt do it, thats when everything was thrown together.

the cloudy syrine was put back in to the bog jar, probably should have decanted the saturated solvent since it was already at maximum but it didnt occur at the time, by the time the second attempt was made all of the solvent from both jars was fully saturated.

thank you sister.
 
a possible explanation for what happened is that the MgSO4 forced more of the dmt out of solution that the NaCl so that your naptha extration was actually saturated at that temperature, if everything else was equal. Due to its saturation any drop in temp (like coming in contact with a cooler syringe) would initiate precipitation.

So it sounds as though MgSO4 is better than NaCl for that purpose. Might be worth running a few more tests being absolutely certain that there are no other variables in your equation. If you results are repeatable then you may be onto something.

Thx for posting this
 
ok im going to try to do this again, instead focusing on just using magnesium sulphate.

here is what i need help with.

im no chemist beyond baking, i dont now how soluble x or y is, and beyond understanding that at higher temperatures more absorbtion occurs, i dont know how to calculate those numbers.

i need to figure out how much magnesium sulphate can be absorbed by water versus sodium chloride into 100ml of deionized water at room temperature (which is upwards of 25+c for me)

if that cant be determined then i need to know what would happen if i fully saturated dionized water with magnesium sulphate BEFORE i put the solution into the acid bath.

im trying to figure out how much magnesium sulphate should be added, using a fully saturated solution as the baseline, i dont know if this is a wise thing to do but this seems like the best first step to me.

just so everything is clear, im going to do a 25g test from two different source samples (one prepowdered, the other bark ill grind myself) using 300ml of deionized water and a fully saturated solution of magnesium sulphate, which will be acid boiled with acetic acid (dont know how many ml ill need), basified with lye (once again dont know how many ml needed) that will then be extracted.

hopefully the combination of two different samples will confirm repeatability, and fingers crossed the numbers will be around what came out before.

if im doing something wrong or if anyone has an opinion or warning, please let me know soon, because im planning to take a crack at this in the next week and i dont want to grow an eleventh finger or lose an eye if it is possible.

thank you.
 
Solubility of MgSO4 in water
of the anhydrous salt
26.9 g/100 mL (0 °C)
25.5 g/100 mL (20 °C)

of the heptahydrate
71 g/100 mL (20 °C)

Solubility of NaCl
359 g L−1 = 35.9 g/100 mL

More solubility values are also given here for higher temps:
Solubility table - Wikipedia

Hope this helps! Values obtained from wikipedia. Did you still need help calculating the pH values? It sounded as though you were proceeding, are you using 300 mL + 100 mL MgSO4 solution for 400 mL in total or 300 mL in total?
 
300ml total split between two jars.

that way if nothing comes out i can combine both jars into one, pour in some good old table salt and salvage the results in one large jar while still leaving room for the solvent and air at the top to spare so it doesnt slosh everywhere.

thank you for the information cave painting, looks like ill do going for about 60-70g for each probably go for 70.

by the way, i dont know if it makes a difference, but i think it would be wise to dry out the magnesium sulphate in an oven before it is placed inside the jars, dont know why just some idea that if i put the stuff in and its already attach to water it wont attach to the molecules inside the goop.

dont know if that will change the numbers.

thank you.
 
ok odd side question

the first jar with the powdered bark is going, probably need to start taking pictures

the whole bark killed my grinder.

will putting the bark inside a jar of vinegar and freezing damage the end pull? i know doing it will make the bark much easier to break apart by hand put im trying to be as consistent as possible, if it will damage yields ill do the break apart by hand but im hoping to avoid it.

does anyone have any idea about what would happen to yields if i froze the whole rue back to make it easier to work with?
 
hello

sorry for the long wait.

ok the tek is going again and i just finished it up and im letting it cool but something interesting came up


oh by the way

2 sets of bark, one prepowder one whole bark ground. 25g each

50ml vinegar 5% each

added 250ml deionized water, allowed to boil for 30 minutes each

slowly added 70g of magnesium sulphate (140g total)

did them each in order both are sitting around to cool

now added 2 tablespoons of lye with 30ml of water solution to each

now hear is the interesting part, both soups thickened significantly after adding the base and the stuff is forming white veins in both, not salt white but whitish yellow in the thickened mass.

so the question is can magnesium sulphate drop out of suspension based upon ph? the amount of white doents look anywhere close to 70 g but it is very visibile and im wondering if i should make the solution even more alkali.

anyhow ill have my first results from these two pretty soon, ill let you guys know what happens.
 
Freezing roots before extracting is a common way of breaking down the cell structure in plant material. It will help yields, not diminish them.

And yes, oven drying MgSO4 is a good way to make it anhydrous. Anhydrous MgSO4 will bind more H20 than hydrated MgSO4.
 
hello

just posting an update, hit a little snag (i think im going to have to do this over)


the solvent came out as clean as could be imagined, turned out their is something in it (had to freeze it) but initially when i did this i thought nothing came out.

in other words their were no discolouring alkaloids, but what has come out of precipitation is as clean as could be.

ill have the results soon but im going to do this again anyway, i think the magnesium sulphate was added when the concoction was too hot and it might have ripped apart the alkaloids. (speculation yes, also i noticed that a small cube of it turned slightly green on the wood spoon when i pulled it out, if anyone has anyclues to what may have happened)

anyhow here is to round two, may their be a full spectrum this time around.
 
just posting a update

the last attempt was a partial failure (i know i can do better

anyhow the results

test 1 pre shredded 457mg from 25g of bark +/- 3mg

test 2 whole bark 472mg from 25g of bark +/- 3mg

so from 50g of bark thats about 930 mg of bark, comparable to standard sodium chloride results, but no trace or is coloured alkaloids showed up, which is interesting because that means with the trace artifacts this number should go much higher. what came out was absolutely crystal clear (if anyone has seen pictures of those "diamonds" thats what appeared)



i am reattempting this test again, same parameters

250mg deionized watch
50mg 5% acetic acid
25 g from two sources
acid boil for one hour each
70g magnesium sulphate (ONCE FULLY COOLED)
conversion to base (2 table spoons of lye, dissolved in the minimal ammount of water)
extract with naphtha


my mistake the first time where that i added the magnesium sulphate while the soup was still esentially at boiling temp (probably ripped apart the alkaloids, had a similar experience when i tried to add zinc to a different boil) and too much water was used (added too much trying to compensate for the boil off and did not check the total, this means that the saturation level could not be reached)

so here is to round two.
 
Here's the problem with magnesium sulfate:

Mg(SO4) + 2NaOH -> Mg(OH)2(ppt) + Na2SO4

reference:

Milk of Magnesia Demonstrations | Flinn Scientific

A very common misconception that students often possess is that solids are heavier than liquids. This demonstration will expose this misconception because two clear, colorless solutions will react instantly to form a white precipitate. If the total mass of the two solutions is determined, the...
www.flinnsci.com www.flinnsci.com

Magnesium products made by the magnesiu
m hydroxide decomposition process
will sometimes have a more gray and grai
ny or turbid appearance than material
made from the two-step magnesium oxide
process. It has been reported that
these products react with petroleum ether
(low molecular weight aliphatic
hydrocarbon solvent) to form hazy produc
t which indicates the presence of
carboxylate.
Click to expand...


I must recommend doing a solubility test of magnesium hydroxide in naptha before going any further.
 
hey motion

yeah i had a conversation about this last week, when i got near neutral ph it seemed to start to look very light brown and wispy, but once all the lye got in it turned black.

i going to do the same thing i talked to you about before, planning for good measure to buy a bottle of pure milk of magnesia tomorrow and test it just in case, but based off vaping what i have got so far it seems very clean.

but this is an experiment, im still a long way from any answers, even if their are any to find.

thank you inmotion.
 
ok i need some help here

i finally finished up checking the magnesium hydroxide concern (milk of magnesia) and something strange has happened.

first off it does not appear to be absorbed into the solvent, that so far is good.

the problem is that it forms a emulsion inside the naphtha and even after a few days does not fall out, you can see the difference clear as day, its heavier than the solvent, but it is not being absorb, but it is there. i then also added some epsom salts (hopign to break up the emulsion) without luck).

the end though was that the solvent i did pull out was as clean as day


the other thing is i saw nothing like this occur during the last two tests did (or any for that matter) so if someone can answer this question it would be of great asset.

magnesium sulphate is incredibly hydrophilic (hygroscopic), but would this property override the chemical reaction to produce magnesium hydroxide?

it appears that unless you have another chemical involved it doesnt happen, one obvious example is the production of copper sulphate, which will then when added to magnesium sulphate water and an electric current will produce magnesium hydroxide, copper sulphate and hydrogen.

now lye is a bit different here but the hygroscopic nature of epsom salts may override any chance for the lye to react.

im doing the test again, thus time intentionally NOT shaking it like crazy and hopefully ill have better luck, but so far with a jar of 8g of magnesium sulphate, 8g of magnesium hydroxide, 100ml of water and naphta to the top (didnt measure it probably about 30-40ml) other than the fact that the masgnesium sulphate got absorbed into the water and there were two white and two clear layers (milk on the bottom without bubbles, water with salt in it, milk with bubbles in it sitting inside the naphtha on top of the water and then naphtha.

it sounds more like im trying to make shots of alcohol.
 
Excellent thank you for running that test. I didn't think it was soluble but 3% yield is not a typical result. My only other concern was the initial one being the magnesium hydroxide precipitation. You weren't completely clear though, you did evaporate the solvent and there were no solid residues afterwards?

In your initial extraction are you sure that none of this milky emulsion was pulled alongside the alkaloid laden solvent? This would be an important thing to know. I assume you are tipping your experiment, if in a jar, end over end just like you would any other correct?

By removing hydroxide ions from the solution in the form of a precipitate this should lower the pH. To what extent I can't be certain but the majority of precipitation reactions tend to go towards completion. Also this means you are loosing ions and the supposed ionic effect is decreased. Which is why I don't know if MgSO4 is an ideal way to go about this.
 
hello again

ok the project is back on.

i got a brand new bottle of pure milk, added water and naphtha and turned it end over end instead of shaking it and having it emulsify.

nothing came up with the solvent clean as a whistle, so im going right back to before.

thank you inmotion.
 
anonenium, thanks for playign around with extractions!

Now....wouldn't that be sensible to do more side-by-side comparisons? In your first post you did a NaCl versus sodium chloride comparison but you didn't keep on doing that.. I think you should do a triple comparison, i.e.

1. no salt of any sort added
2. NaCl
3. magnesium sulfate (obviously added in the same amount as NaCl)

Without side-by-side comparisons you really can infer very little from your results.
 
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