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Author: Subject: NC boiled with NaHCO3, product dissapears partially?
Fantasma4500
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[*] posted on 2-9-2013 at 10:51
NC boiled with NaHCO3, product dissapears partially?


as the title hints..
i have seemingly been capable of removing NC in solution with NaHCO3 where it has been boiled at relatively low heat
what i see is that the solution darkens (carbon?)
and when its at this state you attempt to get the NC out, and then you realise its some strange consistensy slurry all of a sudden
upon drying you will realise its actually turned into a very fine powder

i took a small batch of NC, good quality, then i split the still wet product into halves
one half i wettened in ethanol and dried
other half i put in a 1000 mL beaker with approx 200 mL volume in total of approx 5% NaHCO3 solution (saturated, 20*C approx)
it was put on heat, as low as possible, it didnt boil..
next day i put it on heat again and it reached abit higher temperature, probably even 100*C
darkened and as observed first time with the dark solution, it was a slurry which i needed to actually filter

seemingly the product has a faster burnspeed, which is really good, it also looks much more pure
no residue in either of the products

but the important thing...
about 66% of the product 'disappears' in the NaHCO3 solution!!

ive been told the darkening would be from NO2 fumes, but i cant make sense out of this as NO2 + NaHCO3 > NaNO2 + H2CO3
or well thats what i understand of it.. anyhow, there shouldnt be impurities in the liquid, should there?




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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hossam6006
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[*] posted on 3-9-2013 at 02:17


I've always washed my NC with NaHCO3 solution, never noticed any loses in NC like 66% ! (never weighted, but the entire loss is 5% at most i guess)
when boiling with NaHCO3, NC texture softens a bit ... but when dried it returns as it was before.
It might be that the cotton you're using has short fibers? I usually use quality medical 500g cotton rolls.

about the darkening, well, It might also be H2SO4 residuals. don't really know what, but it's a nasty impurity that should be removed
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[*] posted on 3-9-2013 at 02:36


Need to know more about the nitration.

The reason should be obvious, there is no problem with neutralizing with bicarb, so standard troubleshooting dictates we investigate the stage before it.

DAS
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[*] posted on 3-9-2013 at 07:13


Quote:
. . .but the important thing...
about 66% of the product 'disappears' in the NaHCO3 solution!!

Incompletely nitrated cotton is more easily hydrolysed than a higher grade and even that is subject to some hydrolysis fresh from the pot, if subjected to 100°C in water . . .




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Fantasma4500
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[*] posted on 3-9-2013 at 22:23


hmh yes, i do have videos on its burnrate, and i can link to them here, sorry for taking so long time responding..

it was made with 27 mL H2SO4 +96% and 62% HNO3, 12.5 mL

but it might be due to H2SO4 residue..?
washing procedure: first plopped into a large amount of water; 1 litre approx
thereafter rinsing under running tap until it didnt feel hot from the acids reacting with water, plus abit more
then added to a 250 mL beaker and poured ~10% solution over (saturated, room temperature)
then washed and dumped in 1000 mL beaker on hot plate on low setting, bubbles was observed forming on the bottom, no discolouration tho

the other half i squeezed and wettened with ethanol whereafter i squeezed it again, heated oven and put it in (which was now off and surely wouldnt heat the NC to decomposition!!)

but.. is saturated solution at room temperature too concentrated? plante1999 mentioned that it was a VERY dilute solution that is industrially used, and NaHCO3 does act slightly alkaline..




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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