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Author: Subject: ETN synthesis problem
Hennig Brand
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[*] posted on 25-3-2015 at 16:47


Quote: Originally posted by Deceitful_Frank  
Hey guys, just a quick question concerning the synthesis of ETN using erythritol, ammonium nitrate and sulphuric acid.

The ratios that I use are 1:4:12 but mass but towards the end of the erythritol addition to the mixed acids, everything becomes so thick that the whole deal is VERY difficult to stir with broken thermometers and partially nitrated shit being the result!

Does anybody know of an "inert" liquid that I could add to the reaction mix to thin it all down, make it easier to stir and promote homogenuity and give me a purer end product?

...sure I could just use more AN and acid but Ime not keen to waste my chemicals unnecessarily and dont want to lose any more ETN to dissolution in the acid bath.

Any help or ideas would be gratefully recieved,

Regards.



I know the question posted by the OP at the beginning of this thread was made many years ago, but I think I have a fairly decent solution that improves results in a number of ways. Using strong mechanical stirring, such as overhead stirring, general results in less unreacted erythritol and a thinner mix even after the nitration is complete and stirring is stopped. As stated by the OP, the nitration mixture normally becomes very thick and difficult to stir with manual stirring, increasingly so as more erythritol is added and the nitration mixture gets thicker and more difficult to mix effectively. When strong mechanical overhead stirring is used the nitration mixture never seems to "set up" and stays quite pourable. When I first witnessed this thinner mixture at the end of the nitration I figured that the yield would be low, but the yield was always at least as good or better as any nitration previously performed with manual stirring. It seems that the ETN formed is in smaller crystals when strong effective mixing is used and also that nitration products don't accumulate on un-nitrated particles of erythritol, or lower nitrates, nearly as much.

Just recently in the NG thread an erythritol nitration using a homemade overhead stirrer was briefly discussed. Here is a link to the discussion with pictures:

http://www.sciencemadness.org/talk/viewthread.php?tid=949&am...

I see that I already posted about an overhead stirrer from a cordless screwdriver in this thread, however, the overhead stirrer posted about in the NG thread is much better and more of the associated technical issues have been worked out as well.


[Edited on 26-3-2015 by Hennig Brand]




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[*] posted on 27-3-2015 at 12:21


Here is a reference of interest describing a mixed acid nitration of ETN and testing of ETN usefulness as a sensitizer for AN based compositions. This reference may have been already posted, but I am not certain so I am attaching it here.

Attachment: ETN as sensitizer for NH4NO3.pdf (201kB)
This file has been downloaded 645 times

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[*] posted on 30-5-2015 at 16:43


Check this video. The guy added water to the mix before filtering because ETN is insoluble in water. URL: https://youtu.be/HYmCxP2PVVs?t=67
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[*] posted on 31-5-2015 at 04:49


...yeah? That's what you do. Dump the mix into water, how is this noteworthy?
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[*] posted on 25-11-2015 at 12:54


Can low temperatures affect the yields of ETN nitrations? I have attempted the (seemingly) simple nitration of erythritol several times, but cannot get decent yields. Here is my method-
20 grams KNO3 are slowly added to 33 ml H2SO4, keeping the temperature under 25 degrees C (obviously). I stir the solution until the temperature doesn't rise anymore, and a precipitate of presumably potassium sulfate is visible, which I ignore. This is where it gets strange. As I start to add 5g of erythritol, no rise of temperature is observed at all. It only takes about 2 minutes to add the erythritol, only pausing to stir it into the mixed acids. It stays at about 8 degrees C, and the mixture only starts thickening after all the erythritol is added, near the end of the nitration period(the 15 minutes after the final addition of erythritol).
I have performed this synthesis twice, and have gotten similar results both times. My yield is supposed to be about 7 grams, but am only getting about 2 grams. I'm using a single coffee filter to collect the precipitate, as I forgot to order proper filters. No precipitate is noticed in the filtrate, however.
My guesses are that either-
1. The nitration temperature is too low. I considered removing the beaker from the ice bath to increase the temperature during the second reaction, but it was freezing outside anyways and I didn't think it would help.
2. The nitration period is too short. This would probably tie in with the above guess, as usually colder reactions take longer. I did notice that the slurry got much thicker near the end of the nitration.

[Edited on 25-11-2015 by TheAlchemistPirate]




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[*] posted on 25-11-2015 at 19:22


Just like with nitrating Phenol, a lot of the time the home chemist didn't fully nitrate the Organic molecule. With Phenol (or aspirin) this probably happens a solid quarter of the time, and with Erythritol slightly less. Its generally a good idea to do a second nitration if the product isn't up to par.
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[*] posted on 25-11-2015 at 21:12


Quote: Originally posted by Hawkguy  
Just like with nitrating Phenol, a lot of the time the home chemist didn't fully nitrate the Organic molecule. With Phenol (or aspirin) this probably happens a solid quarter of the time, and with Erythritol slightly less. Its generally a good idea to do a second nitration if the product isn't up to par.


That's one nice thing about ETN, the mono, di and trinitrate are water soluble so it's impossible to end up with any significant amount of lower nitrate impurities.
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[*] posted on 26-11-2015 at 17:17


Alright I attempted the synthesis again today, and have gotten much better results. It seems that I was right on both of my guesses, and both the short nitration length and the low temperatures were affecting my yields. To be honest, I don't know the exact weight of the product as it is still drying on the filter paper, but it has about 6 times more volume than my two gram yield. Also, I also used a different ratio of reactants, so that may have skewed my results.

My newer method:
I used the ratios mentioned by a member earlier in this thread, though his method used ammonium nitrate. I adjusted for the different molar weights by multiplying the amount of NH4NO3 by 1.07, to gain the amount of KNO3 needed. (I know this isn't stoichiometric either, but this adjustment was suggested by another post in this thread). I'll try to make this as compact as possible, as I'm sure the forum is already cluttered by many ETN "recipes" .
30 grams KNO3
50 ml H2SO4
8 grams erythritol
The nitrate salt was added to the sulfuric acid, kept below 25 degrees C (you know the drill). What I did differently here is, when all the nitrate salt was added, I allowed the solution to warm to room temperature. The solution was repeatedly stirred at room temperature, and placed back into the ice bath when needed. I believe this allowed more of the nitrate salt to react with the acid, as the higher temperature allowed the increasingly dilute mixture to completely react. The mixed acids were allowed to cool down again, about 15 degrees C. Erythritol was finely ground to a powder, and regularly added to the solution, keeping the temperature between 15 and 20 degrees C. To achieve this, the solution was brought out of the ice bath, and erythritol was added to the solution until the temperature started rising too much. It was then put back into the ice bath and stirred. Once all the erythritol was added, the solution was monitored at 20 degrees C for half an hour. After crashing and filtering as usual, the precipitate was washed with ammonia. I don't know the exact yield, but as I said above, the volume of precipitate was much greater than with other methods.

As the two above posters mentioned, the culprit was under-nitrated erythritol, which would simply disappear when it was crashed into water.

Hopefully some confused experimenter will find this useful, so I haven't simply posted another kewlish method which just spams the thread. Thanks guys

[Edited on 27-11-2015 by TheAlchemistPirate]




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[*] posted on 5-1-2016 at 18:59


Introduction:

Hello, Ironically I came to join due to a subject I was some how able to view in the whimsy sub-forum, the how or why I was able to is beyond me but I found it gripping but had to register to continue reading it. So here I am! So now I am all joined up I figured I'd share my synth and its quirks of ETN.

The Acid:

500Ml is poured into a 1L round bottom Pyrex flask to be purified/concintrated.

Like most of you I get my wonderful super mega high tech acid from the local big chain (Canadian Tire, any one wanna guess where I am?!?!) store here. It's called ro-tyme Drain opener (The actual name is all lower case!). Like most drain cleaners it is less then clear, to solve this I add 200Ml of 35% H2O2 in 2 steps, first addition of 100Ml is don with the acid cold (0c), the ensuing reaction will heat it up considerably hot and release ozone gas.

(I found the amount of peroxide to add by treating a small 100Ml sample then scalling it up for the main 500Ml batch, by adding peroxide and heating till it yielded clean clear acid in my sample)

I allow this reaction to go on un aided until it is to room temp with intermediate swirling every so oft, once at room temp I add the second 100Ml h2O2 @ 35% then I place on my heating mantle on low heat till no more bubbling is visible, then I increase heat to cook it off to a higher concentration (This process is less then scientific for me, I do about 4H at a volume of 700ml total (Acid + Peroxide) till I see the tell tail dense white acid fumes, I then take off heat and allow to cool to room temp. Then care fully weigh out a precise 100Ml then divide the result by 182 to get my % concentration (Usualy about 95 to 96%)

The end result is a near crystal clear amber fluid of nice viscosity!

The Synthesis:

I have followed the parameters that most have listed, after reading through all the related threads I have used the standard of 100Ml of H2SO4 @ 174grams per 100 Ml (apx 95%)

60grams NH3NO3 sourced from Tannerite, dried and crushed.

I mix this at 0C to 5C during the nitrate addition, once all is added I allow to sit at room temp while I process the Erythritol (Grinding to fine powder and weighing out)

17 Grams Erythritol

Once the Erythritol is ground and weighed I place the acid in the ice bath till at 0C

I then start adding half a tea spoon at a time (I do not have a high accuracy scale so I use volumetric measures at this stage) I mix in fully then allow 1 minute to elapse while stirring between each addition.

Now here where there has been variables, Temp and nitration time ( am still adjusting these to zero in on best yield)

The results:

Out of the 17 I get a consistent 10grams yield!!! Mind you it is very good quality one, befor washing and recrystallizing you can see the nice platelets of the ETN shimmering in the acid!

I crash the mixed acids and products into 200Ml of ice cold distilled water, I then filter out on an unbleached coffe filter and wash with a further 400Ml distilled water then a final stage rinse of 100mL bicarb solution. I then proceed to air dry the crystals.

Recrystallization:

I take 70Ml of Methanol and warm to 40c, I add in some urea (3mL crushed) and stir till fully dissolved, I then take my now dried and powdered ETN and stir into the methanol/Urea mix (If required I filter this to remove any solid impurities and rinse the filter and funel with extra methanol).

Once dissolved and, filtered if needed, I then crash this into 100Ml distilled ice cold water with weak bicarb solution to precipitate out the crystals. This is placed in the freezer for a while to force out as much as possible. Then do the final filter stage.

Final result?:

Beautiful white shimmering platelets of ETN with a perfect melting temp of 61C and gives a solid report when heated and bound in Al foil! Sad part is the 10 gram yield out of 17!

Can any one shed some light on possible errors I am making?

Nitration #1 was half hour at room temp (being 15 degrees) #2 was at 1H after final addition at 5c, then for ten minutes at 20C, both produced 10g out of 17 grams starting material, Acid density/volume and nitrate amount remained static. Both times it was stirred every 5 minutes for 1 minute.

* Edited for clarity.
* Added details to peroxide volume to be added to clean acid and how it was determined
* Added details to the recrystalization section.

acid.jpg - 45kB etn.jpg - 76kB

[Edited on 6-1-2016 by XeonTheMGPony]

[Edited on 6-1-2016 by XeonTheMGPony]

[Edited on 6-1-2016 by XeonTheMGPony]
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wink.gif posted on 6-1-2016 at 12:32


ratio of nitrate to erythritol should be four to one.

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[*] posted on 6-1-2016 at 18:05


Thank you I calculated 68g Nitrate (NH4NO3) for 17g Erythritol, Does this sound correct? I'll increase sulfuric to 110Ml to help with viscosity.
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[*] posted on 6-1-2016 at 18:50


I won't comment on reagent ratios but your acid and reagent quality sounds fine to me. Of course when testing one variable you shouldn't change other ones while doing so. I would try letting the reaction mixture(with all reagents added) sit at one temperature for a longer period of time (maybe 45 minutes, an hour?).

Also, I'm unsure of what you meant about not having an accurate scale and adding half teaspoons at a time; are you measuring your total solid reagent amounts by volume? Or are you simply using a teaspoon to determine how much erythritol to add at a time? In the former case, I would implore you that a 0.1(or greater) gram scale is an essential piece of lab equipment, in my view the most important apparatus you should buy for home chemistry. Having a good scale can be (and frequently is) the difference between performing an excellent reaction and being able to repeat it, and never being able to repeat your results. In the case of the latter I don't think it matters too much how much erythritol you add at a time, as long as additions are consistent, not any more than about 1/4 of your total amount, and you stir and warm the solution to ensure it has all reacted.

I have only performed this reaction three times, but am getting closer to an efficient method. A big problem seems to be the water-soluble lesser-nitrated erythritols which appear in the reaction mixture, but vanish upon water crashing. If these manage to survive purification, they tend to make a less-powerful, less sensitive product. It sounds like you have managed to filter out (or more likely the opposite if that makes sense) these impurities, since your product explodes when heated on aluminum.

EDIT: It might not have been clear, so I just wanted to say that these lesser-nitrated erythritols(or whatever the proper term is), which would have been ETN, will usually be lost during purification. Again, as the posters above stated, this is a very common reason for lack of product.

[Edited on 7-1-2016 by TheAlchemistPirate]

[Edited on 7-1-2016 by TheAlchemistPirate]




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[*] posted on 7-1-2016 at 04:25


Quote: Originally posted by TheAlchemistPirate  
I won't comment on reagent ratios but your acid and reagent quality sounds fine to me. Of course when testing one variable you shouldn't change other ones while doing so. I would try letting the reaction mixture(with all reagents added) sit at one temperature for a longer period of time (maybe 45 minutes, an hour?).

Also, I'm unsure of what you meant about not having an accurate scale and adding half teaspoons at a time; are you measuring your total solid reagent amounts by volume? Or are you simply using a teaspoon to determine how much erythritol to add at a time? In the former case, I would implore you that a 0.1(or greater) gram scale is an essential piece of lab equipment, in my view the most important apparatus you should buy for home chemistry. Having a good scale can be (and frequently is) the difference between performing an excellent reaction and being able to repeat it, and never being able to repeat your results. In the case of the latter I don't think it matters too much how much erythritol you add at a time, as long as additions are consistent, not any more than about 1/4 of your total amount, and you stir and warm the solution to ensure it has all reacted.

I have only performed this reaction three times, but am getting closer to an efficient method. A big problem seems to be the water-soluble lesser-nitrated erythritols which appear in the reaction mixture, but vanish upon water crashing. If these manage to survive purification, they tend to make a less-powerful, less sensitive product. It sounds like you have managed to filter out (or more likely the opposite if that makes sense) these impurities, since your product explodes when heated on aluminum.

EDIT: It might not have been clear, so I just wanted to say that these lesser-nitrated erythritols(or whatever the proper term is), which would have been ETN, will usually be lost during purification. Again, as the posters above stated, this is a very common reason for lack of product.

[Edited on 7-1-2016 by TheAlchemistPirate]

[Edited on 7-1-2016 by TheAlchemistPirate]


I most certainly agree, a 000.00 scale is critical, and I am waiting for it to arrive! ATM I have a scale with 1g resolution (Better then my refrigeration scale with a 10g res!) Some point I'd like to buy a good lab grade scale with a .0001g resolution, but that will be pricy but critical.

Ironically (Being as atm I do not have one my self (Yet!)) It is Vital to have an accurate high resolution scale! Experience can only compensate so much for lacking of the correct tools! But with care full grinding (All ways sieve what you grind for consistent particle size) and volumetric measures can at the very least be fairly consistent.

So for the additions, I am using volumetric measures for the Erythritol that has been sieved.

So the next synth I will use 110Ml of Sulfuric at 95%, 68g of NH4NO3, and the 17g Erythritol.

Mix nitrate and acid at 0c, then let sit for 30M @ 20C. Chill to 0C and then add my Erythritol at half a tea spoon per addition every 1 minute under constant stirring. After last addition will react at room temp (15c) for 1H with stirring every 5M.

I'll report back with final yield after weighing in on the dried recrystallized product.

M = Minutes
H = Hours
C = Celsius
G or g = Grams
Ml = Milliliters

As for the Lower nitrated amounts of material being lost, this I understand, what I do not yet quit get is why I am failing to get good nitration, but we'll see with the corrected nitrate to sugar ratio does, then I'll revamp procedure to a higher temp nitration (15C+ for the whole thing). Hope fully at the very least I'll break even on the sugar side and get 17g product for my 17grams sugar!

* Edit: Added table for abbreviations
* Spelling
* Added further paragraph.


[Edited on 7-1-2016 by XeonTheMGPony]

[Edited on 7-1-2016 by XeonTheMGPony]
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[*] posted on 7-1-2016 at 21:34


Perhaps report volumes in cc rather than obsolete Imperial volumes (teaspoons)... Try to give all measurement in SI?

https://en.m.wikipedia.org/wiki/International_System_of_Unit...

A digital scale with 10 milligram resolution is cheap, and quite good enough for what you're trying to do.

http://www.amazon.com/Frankford-205205-Parent-Arsenal-Reload...






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[*] posted on 8-1-2016 at 03:57


Quote: Originally posted by Bert  
Perhaps report volumes in cc rather than obsolete Imperial volumes (teaspoons)... Try to give all measurement in SI?

https://en.m.wikipedia.org/wiki/International_System_of_Unit...

A digital scale with 10 milligram resolution is cheap, and quite good enough for what you're trying to do.

http://www.amazon.com/Frankford-205205-Parent-Arsenal-Reload...




I know what SI is how ever to properly describe what I am doing is to well, accurately describe it, is this perfect most certainly not how ever it is a true rendition of the events taking place

Here is more functional link then that generic description Of the SI system:
http://www.metric-conversions.org/volume/teaspoons-to-millil...

As for the scale issue if you have a re-read you'll see that one has all ready been ordered with said resolution, how ever that is not good enough for my liking, Accuracy is every thing,

BTY This is all off topic to the parrent thread.

For those whom may be interested apx volume of a tea spoon is 5Ml rounded to the highest and the apx range of a half tea spoon would be 2 to 3 Ml (I was not doing very precise measures hence my choice of a generic figure of "half teaspoon") All other measures for weight are within .5grams

[Edited on 8-1-2016 by XeonTheMGPony]

[Edited on 8-1-2016 by XeonTheMGPony]
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[*] posted on 14-1-2016 at 09:20


After some further reviews I committed the error of not paying close enough attention! Turns out the Erythritol I was using included Stevia extract!

Following the procedure laid out here: http://www.sciencemadness.org/talk/viewthread.php?tid=26679

I successfully recrystallized a much more pure feed stock.

I used the same 100Ml of 95% sulfuric acid and I kept the 60G of NH4NO3 measures intact so I can track the efficiency better

I Nitrated for 2H, started the first hour at low temp of 0C to 10C, then the final hour at 17C to 20C

I used 17G of The purified Erythritol, and yielded raw dry powder weighing in @ 22.57G and after recrystallizing a Net of 19.9G with 2.67g loss due to spillage and entrapment in the filter media (New scale arrived so I can track losses n such much better now!)

Crystals are free flowing with a nice snow white color!

Thank you all for your help, I will now do the next synth following the 4 Nitrate to 1 Erythritol rule, to see what changes that makes to nitration time.

Out line of procedure:

100Ml Sulfuric acid @ 175.5G per 100Ml
60G of Ammonium Nitrate
17G purified Erythritol

Acid was chilled to -10c, a salted ice bath was prepared during this time.

Acid removed from freezer then placed in the salted ice bath, half a teaspoon (ruffly 1 - 3Ml)(Yes still doing this ruff shot for expediency) of nitrate is added, and stirred vigorously till all is dissolved befor the next addition, First half of the addition is don every 1.5m then after that I go as fast as it will dissolve with out raising temp.

After last addition I stir for 2 additional minutes then place to the side to warm to room temp as I weigh out and mill the Erythritol, I reweigh the Erythritol post milling to adjust for losses.

With the Erythritol milled and weighed, I place the acid mix back in a fresh salted ice bath and stir till at or below 0C, I then add half a teaspoon (1 to 3Ml apx) whilst stirring, Once dissolved I wait 1m befor next addition. Repeat till it is all added.

Once all is added I stir for 5m then let rest and stir in 5 minute intervals for 1H. After the one hour has elapsed I remove from ice bath and allow to rise to room temp and stir every 5 minutes for another hour. (Please note that the ice bath IS NOT discarded at this point, it will be required should temps rise more then 20c)

After 2Htotal time (Including addition of the Erythritol time) I crash in 200Ml iced distilled water while stirring the water.

This is then filtered and washed with 500ml distilled water, then with 1l of RO (Revers Osmosis) water. Once water is drained it is placed in a warm air bath @ 30C to fully dry.

Recrystallization:

100Ml of Methanol Hydrate is measured into a beaker, to this 225mg of Urea is added (I find this number by multiplying the raw product dry weight by 1%). The methanol and Urea are mixed in a hot water bath at 60C till all is dissolved, I then add my dried product till all is dissolved thoroughly.

I then filter into 200ml of room temp (16c) distilled water that had 225mg of Urea and 5ml of sodium bicarbonate dissolved into it.

This is then filtered and further washed with 200ml of cool distilled water, befor final drying.

As the old saying goes, Pics or it didn't happen! First one is the Nitrated product, the other is the purified Erythritol!

Thanks for such an awesome forum and the help people!

ETN.jpg - 70kB pure Erythritol.jpg - 117kB

[Edited on 14-1-2016 by XeonTheMGPony]
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[*] posted on 14-1-2016 at 09:50


Pretty crystals. Maybe you should post a copy to the crystal growing thread-

http://www.sciencemadness.org/talk/viewthread.php?tid=64907

Could you take photo on graph paper and state division size, or put a mm scale in picture? Curious how big those are.




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4. Only then are you permitted to say so much as a word of rebuttal or criticism.

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[*] posted on 14-1-2016 at 11:07


Sadly no graph paper but I'll dig through what is left in my drafting box, I should have a ruler some where in there! Will take another pic with the ruler for ya. They where what was left in the mother liqueur (I do cooking too, so saved the tailings for sweetener and they grew over night!) Nice not having wasted any of it!


Test result one; Compressed in foil then heated:

New purified feed stock had a 5 fold increase in power! finger is sore from a very very small amount!

I think that was my main issue was the Stevia contaminant!

Only had a good imperial one but here it is. All so posted in sugested thread.

[Edited on 14-1-2016 by XeonTheMGPony]

Purifide Erythritol crystals-Size 02.jpg - 123kB

[Edited on 14-1-2016 by XeonTheMGPony]
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[*] posted on 14-1-2016 at 15:45


That's strange, when purifying my erythritol from stevia I found that very little impurities were on the filter paper, and questioned the necessity of purification in the first place...
Honestly I'm still having trouble with this reaction, I'll have to try out your method.




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[*] posted on 14-1-2016 at 16:16


first 3 synths where with unpurified truvia, the color was off white and piss poor yield but good power.

The synth with the purified dried Erythritol produced pure white product and the power was magnitudes higher! a tiny amount completely shattered the aluminium foil shell and shock wave hurt my finger! With very good yield.

So I can say with out doubt the purification is vital!

I regret not taking a premix picture showing the color difference between this synth and the last 3.

during the purification there was zero residue from the truvia, well aside from the sugar its self.

But the recrystallization of the ETN the residue is large amounts of fur! amazing how it gets every where! Along with some Ammonium sulfate that didn't get washed out during the first stage.

If you are referring to the filter paper in the picture they are just fines that where statically stuck to the paper, and where not worth the head ache to recover every super fine particle.

I need to work on my recrystallization method to make a larger denser crystal, that will resolve the post processing losses due to ultra fine crystals.

[Edited on 15-1-2016 by XeonTheMGPony]

[Edited on 15-1-2016 by XeonTheMGPony]
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[*] posted on 15-1-2016 at 06:13


Quote: Originally posted by XeonTheMGPony  


I need to work on my recrystallization method to make a larger denser crystal, that will resolve the post processing losses due to ultra fine crystals.



Instead of filtering the hot concentrated recristallisation solution (ETN+MeOH or EtOH) and letting it drip into water you could just filter it into another container and then cool it down in deep freeze to percipitate the product as dense transparent flakes. Then separate the cold solvent by filtration and wash the product with plenty of water. This procedure yields a very nice flake form that compresses easily and effortlessly.




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[*] posted on 15-1-2016 at 08:17



Quote:

a tiny amount completely shattered the aluminium foil shell and shock wave hurt my finger! With very good yield.


You deliberately cooked off a high explosive- with hands close enough for that to happen. :o

I suggest you stop doing that, use a ring stand or similar and get away.

Next, will you will tell us how long your (unprotected) ears rang? Or that there are bits of foil in your eye because you were not wearing safty glasses/face shield?





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[*] posted on 15-1-2016 at 12:43


that is the point hand was not that close! and when I say very small I do mean small, I've worked with HE's in the field so I know their power and abilities quite well, I was in no danger of injury, just surprised by the power increase over the last few runs!

FYI Remember what assumptions make you ;)

In the remote logging camps you mess up you die, just that simple, being I am still here with all parts attached means I been doing some thing right!

Usually I use a candle but I figured the scrappings from the table and being smaller then the size of a salt grain the risk of using a bic lighter was marginal. FYI The charge was held in pliers, it was the hand with the lighter that felt it hurt is the wrong word for it but it is the closest discriptor I can think of.

In terms of safety I'll be posting pics in one of the threads dedicated as such for others to illustrate how unforgiving these substances are with a cow thigh bone (Got them for the dogs, but they since abandoned them).

I do not take risks! (Not even speeding!)


[Edited on 15-1-2016 by XeonTheMGPony]
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[*] posted on 23-1-2016 at 07:52


Batch #5

17.03 grams erythritol purified from Truvia
68.05 grams Ammonium Nitrate
110 Ml Sulfuric acid @ 178.23g/100ml

Process:

Weighed out the sulfuric acid into beaker then placed in freezer.

Weighed out ammonium nitrate prills, Sieved out the finer particles then placed remaining material in mortar, crushed and sieved till all was equal in particle size (Mortar was warmed in oven to help reduce moisture up take)

Weighed out Erythritol (recrystallized), sieved and then milled in mortar (Same process as nitrate)

Rechecked weights of material after processing.

Prepared ice bath (Large container of snow saturated in a weak salt solution)

Placed my acid into ice bath, Added nitrate at 5ml increments, each addition was don after the first had fully dissolved, after slightly over half of the nitrate was added and when each addition no longer caused a temperature spike I removed from ice bath.

After the last addition had fully dissolved I continued stirring for 5 minutes and allowed it to come to room temp (15c) at this point I allowed to sit for 30 minutes at 15c.

After 30 minutes elapsed I then stirred for 1 minute then began adding the erythritol in 5ml increments, following the same method as for the nitrate, once the each addition had fully dissolved and the temp spike started to drop I'd add the next one, with the exception is I did it at a sufficient pace to drive the temp to 20c and I held it here through the addition phase.

After last addition I stirred for 5 minutes continuously then allowed it to rest with a stir every 5 minutes for a total time of 1.5h measured from the start of the erythritol additions.

I then crashed into 200ml distilled water, stirred for 5 minutes, added an additional 100Ml then filtered out the crystals, this is then washed with 1.5L of RO water with a final wash of 500ml distilled water.

After drying gross yield is 22g
After recrystallizing 20.3g (With some remaining in the methanol/water mix that I'll recover upon next batch)

Note: Recrystallization was don with 1% urea as stabilizer and acid scavenger in both the methanol phase and water phase for a total of 2% of the gross weight of etn.

It seems the feed stock (Truvia) was my issue all along! The final crystals of E.T.N where beautiful snow white and free flowing, still very light and fluffy so a small loss was incurred by particles clinging to surfaces n such but over all huge success!

So this is the second batch following the purified feed stock with stellar results, the only change was the nitrate ratio, I went from 60g to 68 grams, the only real difference I saw was a slightly shorter nitration time but that could been altered by the higher nitration temps.

Next batch will be don the same but this time I will again use only 60g of nitrate to try and see what the difference is! I placed an order for 1pound of pure Erythritol at a local health/hippy supply store so if I can get same results with less nitrate usage it will pay off nicely.

So again Thank you to the members suggestions and tips, and for this whole thread, it was instrumental in be developing the procedure and fine tuning it!
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[*] posted on 24-1-2016 at 18:17


batch 6:

60g nitrate all ells remained the same, 13g yield, so one must follow the 4 to 1 rule of nitrate to sugar! T get full yield as has been reported.
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