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Fantasma4500
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i would say etn as initiation aswell, you dont need a primary for that, you can shock initiate it and use rocket candy for it, aswell as using rocket
candy as the fuse
an ammonal alike charge would be preferred.. sugar dynamon works well with 85 15 AN:Sugar
85 10 5 AN Su Al can be used instead which should be more sensitive, and you already got aluminium anyways
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chemcam
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Quote: Originally posted by caterpillar  |
I started with NC too, but later I realized that PA is more interesting and its preparation is no more complicate than preparation of NC (gun cotton).
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I never got bored with NC, but anyway, what synthesis are you following that makes it as easy as NC? I have read a few online ones that wouldn't
actually yield TNP, rather, DNP or lower.
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Hennig Brand
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I am not necessarily bored with NC either, maybe to a large extent because I have other interests as well. "Variety is the spice of life"
I guess there is always some DNP present in a sample of TNP and the amount can be quite large if strong enough acids aren't used and proper procedure
isn't followed with regard to temperature, etc.
TNP requires much more knowledge, skill and technique to perform properly than does NC. The amount of actual attention and effort required with a NC
synthesis is a fraction of what is required in running a decent TNP synthesis, IMHO.
[Edited on 5-6-2013 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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caterpillar
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Well, boys, for both of you. NC has some problems- fibrous cotton's nature causes large amount of mixed acid. And then one has to press NC strongly or
to dissolve it in an appropriate liquid. About PA- I dissolve phenol in sulfur acid. Then by means of hot water bath keep it at 100 Celsius for one
hour. Cool it. I mix KNO3 (or NaNO3) with sulfur acid. Cool this mixture and add in small portions solution of phenol in sulfur acid. temperature must
not be above 30 Celsius, therefore this process takes some hours. At the next day I put reaction vessel into water bath and slowly increase its
temperature up to 100 Celsius and keep at this temperature for one hour. Then I put it into water with crushed ice, filter precipitate and wash with
two small portions of cold water. That's all. 250 gr phenol + 800 gr of H2SO4 - it gives me sulfophenol and nitration mixture- 1000 gr of KNO3 + 1600
gr of H2SO4. I do not think that this process is very complicate. Just for beginners. Yeah, if you want to make kalium or ammonium picrate, add some
water to PA and add K2CO3 or NH4HCO3 respectively to this slurry, mixing it with plastic. I used 92-94% sulfur acid.
Women are more perilous sometimes, than any hi explosive.
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chemcam
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Yeah I guess we just have different views on easy processes and amounts of mixed acids. But nevertheless explosions are explosions no matter what HE
you choose. But like member Hennig Brand says, "variety is the spice of life."
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papaya
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caterpillar, as you use KNO3 for nitration how is that you get pure PA and not potassium picrate (insoluble if I'm right)? I have no experience with
this, just asking.
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Hennig Brand
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KHSO4, is what precipitates along with the TNP mostly I think.
"Potassium picrate requires 260 parts of cold or 14 parts of boiling water for solution" from "An Introduction to the Practice of Commercial Organic
Analysis: ... - Page 331". Potassium bisulfate solubility in water at room temperature from Wikipedia (their usually right), 490g/L. Looks like you
have a point about the solubility.
The acidic medium will convert potassium picrate to picric acid, or prevent formation of it. I think it will also reduce the solubility of the acid
salt KHSO4.
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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papaya
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Or you just can't tell what you get just from appearance  Could caterpillar
somehow test for potassium in the product ? Also what about ammonium nitrate? Sodium must not cause problems. It is interesting question what can
replace nitric acid without giving byproducts, always wanted to see some PA in my hands, but no way to obtain phenol and ascorbic from tablets is not
practical 
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chemcam
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| Quote: Originally posted by papaya | | It is interesting question what can replace nitric acid without giving byproducts, always wanted to see some PA in my hands, but no way to obtain
phenol and ascorbic from tablets is not practical |
Ascorbic acid? If you mean acetylsalicylic acid it is very practical. Cheaper than buying phenol.
Just use salicylic acid. You can use asperin as well but purification is recommended. I actually prefer to make salicylic acid from acetylsalicylic
acid because its so damn cheap and its good fun. 
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papaya
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Acetylsalicillic, sorry, but I asked what nitrates would be best (taking in mind the question about possible picrate formation), does ammonium nitrate
yield PA or picrate ?
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Hennig Brand
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Ammonium picrate like potassium picrate is kept from forming, or converted to picric acid, by the acidic reaction mixture.
Sodium nitrate is best I think. Sodium nitrate gives a thinner more easily stirred reaction mixture than potassium nitrate does. A thinner reaction
mixture allows for better mixing and a more efficient nitration, also the sulfate by-product is less problematic, I think, during separation and
purification. Potassium nitrate can also work quite well, but produces a thicker mixture. Ammonium nitrate seems to be the least suitable and I am not
exactly sure why. I obtained a low yield of impure product when using ammonium nitrate, but then again I was just learning about picric acid and the
ammonium nitrate I used was most likely unpurified fertilizer grade. I should try it again sometime with purified stuff (recrystallized from water).
BTW, sodium nitrate can be made rather easily from ammonium nitrate and sodium bicarbonate or hydroxide.
Edit:
You know this has all been covered to death in several other threads about picric acid. Oh, Nerd Rage on You Tube has a good video on making sodium
nitrate from ammonium nitrate (if its still up). Seek and ye shall find.
[Edited on 6-6-2013 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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caterpillar
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| Quote: Originally posted by papaya | | Or you just can't tell what you get just from appearance Could caterpillar
somehow test for potassium in the product ? Also what about ammonium nitrate? Sodium must not cause problems. It is interesting question what can
replace nitric acid without giving byproducts, always wanted to see some PA in my hands, but no way to obtain phenol and ascorbic from tablets is not
practical |
Sulfur acid is much stronger than PA, therefore do not worry about K (or Na) salts during preparation, if you use some salt of nitric acid instead of
nitric acid itself. But I have to warn you: once I tried to use NH4NO3 instead of usual KNO3. I got a runaway (not intensive, however), significant
amount of NO2 and what was the worst I got foam, which fulfilled my reaction vessel and slowly moved to my hot water bath. I think that mixed acid can
be replaced with some salt of HNO3 + H2SO4 everywhere, except preparation of nitramines (RDX, HMX). ASA (aspirin) could be used too instead of phenol,
but I never used it (I had phenol and therefore no reasons to use substitutes)
Women are more perilous sometimes, than any hi explosive.
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papaya
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| Quote: Originally posted by Hennig Brand | Oh, Nerd Rage on You Tube has a good video on making sodium nitrate from ammonium nitrate (if its still up). Seek and ye shall find.
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Sure, but why waste Na2CO3, when theoretically the same reaction must go with AN ? I'm always trying to keep number of stages and wasted chemicals as
less as possible.
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Finnnicus
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Umm, not sure about you, but Na2CO3 is 4$ for 500grams (hydrated). Sorry if this doesn't apply to you, but it's sold as letric soda at the
supermarket.
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papaya
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| Quote: Originally posted by Finnnicus | | Umm, not sure about you, but Na2CO3 is 4$ for 500grams (hydrated). Sorry if this doesn't apply to you, but it's sold as letric soda at the
supermarket. |
Yes, but again WHY? Reformulating the question - does anybody know why AN should not work itself? (some said here they got runaways). As I know nitric
esters form without complications with AN, so is there something special with picric?(yes I know it's not an ester )
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caterpillar
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| Quote: Originally posted by papaya |
Yes, but again WHY? Reformulating the question - does anybody know why AN should not work itself? (some said here they got runaways). As I know nitric
esters form without complications with AN, so is there something special with picric?(yes I know it's not an ester ) |
Try and see what will happen.
Women are more perilous sometimes, than any hi explosive.
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Bot0nist
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I never had trouble with runaways using ammonium nitrate in a PA synth. Rosco and Quicksilver were discussing a while back about how using alkali
nitrates over ammonium nitrates, and even differences between sodium nitrate and potassium nitrate. Differences beyond solubility and stoichiometric
amounts of -NO3 per gram. It is tried and true that NaNO3 gives better yield and less DNP in the PA synth. I can not seem to find a definitive reason
for this, but it has been discussed in many past threads.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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papaya
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The reason MAY be that sodium sulfate can take up to 10xH2O into complex Na2SO4x10H2O which if is true will be a huge advantage (dessication effect)
over other nitrates. A similar effect I observed while getting H2O2 out of percarbonate, look ''Leaching H2O2 from percarbonate'' thread. But the
thing is all this is not proven directly, just easy explanation of an observed effect.
[Edited on 6-6-2013 by papaya]
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Armistice19
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First baby step
UPDATE:
Materials for NC synth. Have been ordered. Improvised equipment was no longer an option in my mind due to safety/quality of final product. Thus lab
equipment was worth the heavy price IMO.
MATERIALS ORDERED:
nitric acid 70%
sulfuric acid 98%
Urea
Sodium hydroxide
Beakers
Glass stirring rods
Graduated cylinders
Mortar and pestle
pH test strips
Analytical balance 300/0.001
Everything was purchased from Ebay. I will use NaOH as my dilute aqueous base for acid neutralization, and will be adding 0.5% urea to my acetone
laquer as an added safety precaution. During the delivery time I will continue in depth research of NC. I Would have loved to have purchased some Hg
if I ever decided to attempt fulmination down the road, however what I have found so far online is much too expensive. Perhaps there is another
primary option for sometime in the future?
Comments? Criticizm?
[Edited on 8-6-2013 by Armistice19]
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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golfpro
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Holy COW!!!!
I bet you get a firm knock on your door/kicked down instead of these things ever being delivered. Good luck.
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hyfalcon
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I don't see a thing in that list to get excited about golfpro. I ordered 4-2.5l bottles of 68% Nitric from a biodiesel supply house. I use it to
reclaim silver from scrap.
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golfpro
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As many news stories I see now of homes being raided and "explosive devices found," I won't order anything more than a glass beaker and thermometer
maybe a stirring rod, I'm probably a bit on the cautious side though
I think that would be cool though if you did mercury fulminate, I am trying to fugre what is the easiest inroganic primary (or non organic peroxide).
You should post your next order you make too if you order more.
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chemcam
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Purchasing nitric acid and sulfuric acid at the same time is not too wise because anyone with a little chemistry knowledge knows it is for nitration.
What they would think by reading your list is that you want to make nitrourea which is fairly powerful.
I get my mercury from medical equipment and switches. Just look around and you'll find it for free.
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Armistice19
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chemcam, thanks for the purchasing advice, I just wanted to let everyone know that each of the acids were bought from separate sellers, however this
does not negate the fact that everything shows up on my Ebay account. In all seriousness, should I be worried? Is big brother on his way? I personally
am not too worried at all. My impression was that chemicals are legal, but what you do with them may not be. Is my shopping list probable cause? If it
is, I only have chemicals, no explosives. Wouldn't I have to be in the process of making NC, transporting it, or storing it for it to be illegal?
“Imagination is more important than knowledge. For knowledge is limited to all we now know and understand, while imagination embraces the entire
world, and all there ever will be to know and understand.” -Albert Einstein
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chemcam
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If you purchased a large amount of the acids I would be slightly worried but if <1000mL you should be okay. And yes you are right the chemicals are
legal, however if law enforcement saw your purchases and the same dates they probably wouldn't come to your door until a couple days after you
received the packages to try and catch you red handed nitrating things. In actuality though I would not worry, you should be okay. Just in the future
be more aware of what you buy online.
There is a law in the USA, sort of vague law, that says having the chemicals needed to make drugs or explosives is enough to make an arrest. Meaning
if somebody owns acetone, H2O2, and acid they can be arrested, obviously about every house has that so it is likely during trial you would have
charges dropped. I believe this law is there to allow law enforcement more time to prove intent and gather other evidence. So in actuality for that
charge you WOULD go to jail but only until your trial, in USA that means usually a month but up to one year. Don't let that scare you from
experimenting.
[Edited on 6-10-2013 by chemcam]
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