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Author: Subject: Sodium Ethyl Sulfate
sulfuric acid is the king
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[*] posted on 18-2-2017 at 08:23


Hmmm so you have done it by acid alcohol methode...
Great.But can you tell me some details...Percentage by mass of the acid,was alcohol anhydrous?How long did reflux take?After reflux you neutralised acid with water?How much?Please tell me details...I am so obssesed with it i will not stop...It takes me days etc...I have improvised equipment but...
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[*] posted on 18-2-2017 at 10:04


Reflux was 24 hours on a boilng water bath, 200 ml 95% sulfuric acid, 600 ml anhydrous ethanol.

The reflux is probably counterproductive; you might want to just heat it to 70 C for 10 minutes. I am still unsure as to the best neutralization method.




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[*] posted on 18-2-2017 at 13:16


Really?Nice then...I must try...
I added calcium carbonate but it was mess...
You have good expirience with buslulfate method?It should work fine...
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[*] posted on 18-2-2017 at 16:19


Adding calcium carbonate is a mess... and you have to stir it to prevent wasting calcium carbonate. I have used the bisulfate method but never got nearly the yields claimed.



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[*] posted on 18-2-2017 at 21:59


I'm halfway tempted to give this another shot knowing what I know now. I'd like to know the melting point of its anhydrous form (which I assume exists), and it would be good to know its solubility curve in water by temperature....

I imagine that good results detailing its solubility would be accepted for publication in a respectable journal.




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[*] posted on 19-2-2017 at 03:45


I found this "With excess sulfuric acid, the equilibrium can
be shifted to the right."
But how much excess?Next time i will try 2:1.
Yes i also need that physical properties,but it's very hard to find anything...

[Edited on 19-2-2017 by sulfuric acid is the king]
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[*] posted on 19-2-2017 at 05:20


I've actually never tried using excess sulfuric acid, but I've seen that recommended in a couple of places.



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[*] posted on 21-2-2017 at 17:24


Ok,when you have calcium ethyl sulfate,how you add sodium carbonate,in solution or in powder form?
I have improvised equipment and everything,i do not have ph indicators etc,it's very dificult for me,but...
I plan to pour sodium sulfate already in solution to solution of calcium ethyl sulfate,and hope for calcium carbonate forming or "snowing" that can be only indicator for me,or?

[Edited on 22-2-2017 by sulfuric acid is the king]
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[*] posted on 21-2-2017 at 20:21


That might work well, actually, but I've never tried it.

I have used sodium carbonate and sodium bicarbonate solution, saturated, sometimes adding powder first, and finishing off with saturated sodium carbonate to a pH of at least 9. The pH seems to decrease slightly when solutions of sodium ethyl sulfate are concentrated over heat unless they are already acidic... in which case the pH decreases rapidly. Exactly why that happens, I'm not sure, but it seems to be some sort of hydrolysis.

Concentrating the solution under vacuum might keep that from happening. The crystals of impurities obtained while concentrating a solution of sodium ethyl sulfate, for me, have had different properties... some have been deliquescent, some have had basically neutral pH, some have been sludges that are hard to filter, some flakes, some crusty substances that creep up the side of the flask, etc. In general, if it remains a solid above 86 C, it's an impurity and should be removed.

As the solution gets concentrated, any excess calcium salts will slowly precipitate out. Calcium carbonate forms a complex with carbon dioxide that is actually pretty soluble in water, and there can be a surprisingly large amount of this, especially if you used sodium bicarbonate for the neutralization. When the solution starts to get very concentrated, unless you somehow magically have absolutely 0 unwanted sodium salts in solution, the excess sodium salts will precipitate out. When this started happening, you'll want to remove the water slowly--I've usually used a boiling water bath for this but low heat on a hotplate works ok too--and remove the salts periodically while checking the specific gravity. It will climb very slowly at times with the elimination of of a lot of salt material, and at other times it will climb very quickly with the elimination of little salt material. Once you have a saturated solution, the specific gravity will be around 1.33-1.34, and removing water at 100 C won't change the volume of the solution much or cause precipitation of salts. In fact, it will look like nothing is happening unless you allow the solution to cool, in which case a crystalline mass of sodium ethyl sulfate will form around the outer parts of the beaker, encasing the solution in a manner reminiscent of partially frozen ice cubes.




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[*] posted on 22-2-2017 at 04:47


I use marble as a calcium carbonate source,i hope that's not a problem,i tested it disolving in hydrochloric acid it fully disolved,so it's chloride now.But i don't know if using crushed marble is good,when i added it to solution of sulfuric acid etc. it formed clumps...Maybe couse i was to fast adding it.
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[*] posted on 22-2-2017 at 04:54


That probably won't work well... the calcium carbonate needs to be very finely powdered and added slowly with strong stirring so that it doesn't get coated with nonreactive calcium sulfate. You can use finely powdered chalk if it is actually calcium carbonate. It is also easy to prepare it from calcium chloride and sodium carbonate.

Edit: Oh, crushed marble. That might work, actually. It needs to be very finely powdered.

[Edited on 22-2-2017 by JJay]




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[*] posted on 22-2-2017 at 14:58


@JJay
This is from the first try that i mentioned before,solution with misterios ultra soluble salt is evaporated by half and now at 10C crystals!
What do you think?


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[*] posted on 22-2-2017 at 15:46


I would check the specific gravity of the solution to be sure, but it looks like that might be sodium ethyl sulfate.



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[*] posted on 22-2-2017 at 15:46


Nah...It's to easy... :/
I just touched crystals to get them out,poured remained liquid first,and they are liquidy...Hah...Probably that's just some sulphate monohydrate or something...
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[*] posted on 22-2-2017 at 16:00


What i know so far is that it has no pungent smell like sulphate when i made it by h2so4/nacl methode,substance is nearly without smell,and i think smell is more deep,basic.
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[*] posted on 22-2-2017 at 16:02




[Edited on 23-2-2017 by sulfuric acid is the king]
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[*] posted on 22-2-2017 at 16:05


That very well could be.

I thought about saving sodium sulfate when it is generated as a side product but so far have always decided it isn't worth it.




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