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nitro-genes
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Jeezzz, I wish I could be there...
Seeing a you in full safety gear including gasmask, cautiously peeking from behind a plexiglass wall with highpower binoculars at this
evil-sucking-and-pumping-contraption you build to mass produce NG
"Hehehe,don't worry abbout me,I survivem more than you can imagine,99% not by my guilt!"
Personally, its the 1% that worries me most...
[Edited on 28-1-2010 by nitro-genes]
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mfilip62
pierced by a crossbow under a bridge while eating Billy goats
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English is not my first language,
and you seems to be illiterate one!
I didn't made 5kg NG/ENGD at once,nor did I said so!!!
Are you out of you mind!!!
Please explain me how can I be alive if I did that!?
No one sane should store more than 50g of primary
at once,it is suicidal.
Used to made around 100g of EGDN,and no more than 50g of NG
at once in my improvised blender.
I made this device to produce it faster in medium batches,now I changed to AN few years ago,which is almost perfect
for its price/safety/power ratio if you are making it in 10+kg
too bad it is so hygroscopic, and too bad there is no nitromethane here. Kerozene,flour,wax,Al,TNT,naphthalene,chorcoal...they all work good with
AN,but most of them are not allways cap sensitive. ( I am not actually synthetisig it,but separating it from fertilizer,but looks like I need to point
out obvious!)I still use NG/AN to set if off mostly.
Now I don't need too much HE-s, because I am not blasting seriously any more, but still do it for fun on the nice Sundays though! 
Good thing is that AN is not regulated in my country, so you can
"make" it in the tons if you want to!
What were the bigger booms you people made!?
Here people are not paranoid as much as in most of the EU and USA,
we didn't pissed off any terrorists, so you can blow 30+ kg at once without anyone seriously bitching.
I suppose you saw that youtube hit of 30kg ANNM gooing off in neighbor Slovenia. Well, people just don't care about!
Nitro-genes...No problem,
come over here and I will show you my lab!
How about 20kg blast!?
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Lord Emrone
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in the synth for NG, EGDN, Methyl nitrate, we can drop all the HNO3 in the H2SO4 at once, but in the ETN synth, it must be added dropwise. Why is that
?
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hissingnoise
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Hi Lord Emrone, mixed acid is normally used for the nitration of liquids.
For erythritol, according to Davis, the sugar is first dissolved in HNO3 and H2SO4 is added to precipitate the product; it's done dropwise to prevent
a temperature-spike that might cause runaway.
Liquids are simply added dropwise to the mixed acid.
When preparing mixed acid H2SO4 should be added to HNO3, not the other way round.
This is important when using 68% HNO3 because the water-content in 68% HNO3 can lead to unwanted heating of the solution.
[Edited on 6-2-2010 by hissingnoise]
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mfilip62
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Its not bad idea to cool acids down as much as you can
and add them as patiently as you can,in ANY nitration.
Most nitrations need further cooling of acid mix as well.
Take for example PETN.
Actual nitration will be smoother,safer and you will get better yield
and high qualitiy product.
Partial nitration is in over 90% cases result of impatience and
speeding things up.
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Lord Emrone
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Quote: Originally posted by hissingnoise  | Hi Lord Emrone, mixed acid is normally used for the nitration of liquids.
For erythritol, according to Davis, the sugar is first dissolved in HNO3 and H2SO4 is added to precipitate the product; it's done dropwise to prevent
a temperature-spike that might cause runaway.
Liquids are simply added dropwise to the mixed acid.
When preparing mixed acid H2SO4 should be added to HNO3, not the other way round.
This is important when using 68% HNO3 because the water-content in 68% HNO3 can lead to unwanted heating of the solution. |
So I can add all the erythritol to the HNO3 at once ? That would speed up the process a lot, but since the mixture, while adding H2SO4 must be kept
< 10°C it's still takes a lot of time.
I did a methyl nitrate synth last summer and it worked by adding HNO3 to H2SO4. I will do it reversed from now on. But the last months I failed to
make methyl nitrate and EGDN, even though I use the same acids, 60% HNO3 and 96% SA.
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hissingnoise
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| Quote: |
So I can add all the erythritol to the HNO3 at once ? |
No! That would lead to runaway very quickly!
Heat is produced when organic substances are added to HNO3 and if the temperature passes a certain point runaway is likely to occur.
Mixing the acids first and adding erythritol a little at a time with constant stirring would speed things up but the reaction mixture thickens as the
reaction proceeds and efficient mixing becomes difficult.
It might be a good idea to have a look at "The Chemistry of Powder and Explosives" by Davis - it's in the site library.
You should always use 98% H2SO4 for nitration and your HNO3 should be 68% or better.
An excess of H2SO4 should be used with 68% HNO3 to bind up the 32% water it contains!
[Edited on 6-2-2010 by hissingnoise]
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Lord Emrone
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| Quote: Originally posted by hissingnoise |
It might be a good idea to have a look at "The Chemistry of Powder and Explosives" by Davis - it's in the site library.
You should always use 98% H2SO4 for nitration and your HNO3 should be 68% or better.
An excess of H2SO4 should be used with 68% HNO3 to bind up the 32% water it contains! |
Ok, thanks, I also tried it with AN, failed too. Strange.
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The WiZard is In
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| Quote: Originally posted by Microtek |
When doing the hammer test, the NG must be absorbed into a piece of toilet paper. Otherwise, the hammerblow will more likely just scatter the NG
as little droplets.
------
You could boil it.
Nitroglycerin — Ascanio Sobrero
" On one occasion a small quantify of an ethereal solution of nitroglycerin as allowed to evaporate in a glass dish. The residue of nitroglycerin was
certainly not more than 2 or 3 centigrams. On heating the dish over a spirit lamp a most violent explosion resulted, and the dish was broken to atoms.
On another occasion a drop contained in a test tube was being heated when it detonated with great violence, and pieces of glass cut my face and hands
severely and also injured others standing some distance away in the room."
Ascanio Sobrero "Some New Fulminating Products Obtained by the Action of Nitric Acid on some Vegetable Organic Substances." Torino. Mem. Acad. (1847),
195-203.
In: GW McDonald "Historical Papers on Modern Explosives." Whittaker & Co. 1912
Byda ... I have an original copy, you can DL McD's book from the obvious site.
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NUKE
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Here I will publish some of my findings:
Nitro isn't even remotely close as sensitive and super duper dangerous as people say it is. So stop being "NG racists"...
I have tried synthesizing nitroglycerin with both >99.5% HNO3 and 65%. And I have to say product is identical! Density is very close to 1.6 in each
case only the yield is slightly increased with use of 99.5% HNO3.
200mL >99.5% HNO3
300mL 96% H2SO4
112mL glycerine
Yield was ~180-190mL of nitro both times.
100mL C3H8O3
454mL 96% H2SO4
318mL 65% HNO3
Those ammount yield approximately 100mL of NG.
From my experiences... NG does not detonate as a liquid when struck with a hammer it only splatters around. It must be absorbed in some material in
order to detonate by hammer blow and even then it needs a much stronger blow than most primary explosives (namely HMTD, lead azide, silver azide, lead
styphnate).
When NG is dropped on hot metal plate an interesting and rather amusing effect is observed. Lovely blueish white flames are observed with small
ammount of sound evolution. NG on flat thin Al surface only burns. When small ammount of it is put in Al foil and folded it explodes on heating.
Ok here I will describe an example of H2SO4, HNO3 (>99.5% and 65%) synthesis.
H2SO4 and thermomether (-30°C to 150°C interval) were placed in 1L flat bottomed florence flask and put into the salt/ice bath untill temperature
reaches approximately -5°C.
HNO3 is added in portions with occassional swirling so the max. temperature mixture reaches is 35°C. After all the HNO3 is added temperature is
allowed to drop to 10-15°C.
Glycerine is added (10-20mL at a time) temperature is kept at approximate interval of 15-21°C while constantly vigorously swirling and immersing the
reaction mixture into ice bath to prevent localised overheating. All the glycerine can be added (no matter the ammount) in as little as 15 minutes if
good enough ice bath and vigorous swirling is employed. And temperature would never exceed 21°C (industrial processes use higher temperature anyway,
and runaway in small batches don't present significant detonation hazard). After all the glycerine is added mixture is swirled for some time and put
into a seperatory funnel (at temperature ~15°C). Mixture is left there for hour, two or however long neccessary for acid layer (bottom) to seperate
from NG layer (top) and above mentioned temperature is kept during the seperation process. As much acid layer as possible is seperated from NG.
When NG is almost "acid free" warm (45°C) NaHCO3 solution is added and swirling is used (to increase the surface area of NG) without closing of the
seperatory funnel (*cough*, *cough* tried that too but got a "headbursting" NG/solution fountain).
After some time when bubble evolution decreases NG is washed again with similar solution until it contains even less acid remains.
After letting it settle on bottom of seperatory funnel a NG equivalent volume of acetone is measured into a beaker and few mililiters of 25% NH3
solution is added to it and stirred.
NG is seperated directly into the beaker with as little leftover water as possible. Whole mixture is thoroughly stirred using a glass rod. And pH
paper is used to determine if it's in alkaline range.
Clear but slightly yellowish solution is formed and small ammount of heat is evolved.
Whole mixture of acetone/NH3/NG is dumped into approximately 5 times it's volume of distilled water and whole thing is violently shaken so as much
acetone,NH3 as possible is seperated from NG (I used HDPE vessel for that purpouse). Mixture is let to sit for a hour or two so as much NG as possible
settles on bottom. As much clear layer as possible is decanted off and NG is again transfered into a seperatory funnel.
As much warm distilled water is added to NG in seperatory funnel and violent swirling is employed untill yellowish NG changes colour to "milky white".
After that happens NG is let to settle down, seperated with as little water as possible and transfered into a vessel for drying purpouses.
NG is left for approximately 24h on a warm place (40-50°C) and it's milky appearance dissapears. After "drying" process it's completely colourless.
No need for dessicator...
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hissingnoise
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Or acetone solution, strictly speaking - dispensing with acetone and dH2O just means extra swirling in a few changes of tap-water after
neutralisation. . .
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quicksilver
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| Quote: Originally posted by NUKE |
After letting it settle on bottom of seperatory funnel a NG equivalent volume of acetone is measured into a beaker and few mililiters of 25% NH3
solution is added to it and stirred.
NG is seperated directly into the beaker with as little leftover water as possible. Whole mixture is thoroughly stirred using a glass rod. And pH
paper is used to determine if it's in alkaline range.
Clear but slightly yellowish solution is formed and small ammount of heat is evolved.
Whole mixture of acetone/NH3/NG is dumped into approximately 5 times it's volume of distilled water and whole thing is violently shaken so as much
acetone,NH3 as possible is seperated from NG .........
As much warm distilled water is added to NG in seperatory funnel and violent swirling is employed untill yellowish NG changes colour to "milky
white"........... |
Avoid your swirling with a glass rod. I had Emailed (back & forth) a fellow who lost a thumb and eye to NG in that being a liquid within a liquid
(not acetone solution which is a wise move), it is difficult to see the small droplets which - when impacted, "train the other NG" within the vessel
to mass ignition. The proximity was less than six inches from the flask of 40 ml NG & at that distance the violence of over an ounce of NG will
tear tissue and the glass shards had come up under the goggles to sever cornea and eyelid. This fellow was NOT a jackass or unskilled. He was simply
negligent of the issue of glass to glass impact on a droplet.
A Sep-funnel's petcock should never be dry or even "sticky". If a proper Teflon petcock is used the device should have solutions drawn through it
prior to the introduction of NG supported solutions.
There IS a profoundly realistic set of reasons why NG was feared over the decades. It's liquid form made it difficult to contain & easy to get
between bearing surfaces. This is NOT to say that it has the sensitivity of Iodine "fly-killer", but that it does present a difficulty in visually
determining it's whereabouts. What's more as NG moves from temp to temp and from flat - to containing bubbles, it's level of sensitivity changes. We
have all heard how when NG is frozen and thawed it becomes uniquely sensitive; there is more to that issue than "meets the eye".
Another issue that's tricky is accurate assessment of ph. The problems made me invest in a digital meter. The issue with NG is to avoid getting
anything BUT the NG on the paper - lest you get a false reading from the surrounding alkali solution (while the proper NG remains slightly acidic).
As a nitric ester it's imperative that it be neutralized and the fact that the "original batch" of NG is "cleaned up" every so often gives rise to the
question of it's demand for proper climate control, etc. Glycerin was dropped from industrial blasting in favor of Ethelyn Glycol for some very good
reasons.
Ethelyn Glycol offers much wider safety margins & is really worth the effort to use it instead.
There is a difference between being reasonable with regards to respect for energetic materials and overly fearful. In either end of the spectrum;
being overly confident or overly fearful is not a great place to be. Discussions of safety procedures are never a "put-down" but often meant to
illustrate how to avoid stepping into the "dark side".
The guy who lost an eye still gets around with the hobby. But he freely tells the story so that other folks won't make that mistake. He once said
something I really take to heart....He said that if he doesn't "feel sharp" & knows what he's going to be doing exactly, etc....He puts off any
synthesis till he's on target.
[Edited on 23-4-2010 by quicksilver]
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The WiZard is In
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| Quote: Originally posted by Lord Emrone |
I did a methyl nitrate synth last summer and it worked by adding HNO3 to H2SO4. I will do it reversed from now on. But the last months I failed to
make methyl nitrate and EGDN, even though I use the same acids, 60% HNO3 and 96% SA. |
High technology terrorism - L. Paul Bremer address - transcript
US Department of State Bulletin, July, 1988
Statement before the Subcommittee on Technology and the Law of the Senate Judiciary Committee
on May 19, 1988. Ambassador Bremer is Ambassador at Large for Counter-Terrorism.(1)
"In some cases, the bombs themselves have changed. The Czech plastic explosive Semtex, more
powerful and less detectable than traditional explosives, is becoming very popular with those groups
which can gain access to it. Lebanese terrorist Mohammed Ali Hammadei, accused of helping direct
the hijacking of TWA #847 in 1985, was captured last year trying to enter the Federal Republic of
Germany with the volatile liquid explosive methyl nitrate concealed in liquor bottles."
http://www.findarticles.com/p/articles/mi_m1079/is_n2136_v88...
--
djh
------
Tuez-les tous, Dieu
reconnaîta les siens.
Amalric Arnaund
(?-1225),
Abbé of Citeaux.
At the the sack of Béziers (1209)
[Edited on 23-4-2010 by The WiZard is In]
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hissingnoise
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Yeah, I can see someone with bottled methyl nitrate acting jumpy.
It's more brisant and more powerful than nitro and its high volatility adds an extra dimension. . .
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quicksilver
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The history of methyl nitrate in WWII was a tragic and nightmarish one. Slave labor was used to man the production facilities in Nazi Germany; the
explos. being used in landmines and aerial bombs. The production facilities were segregated from the management and over-seers, allowing the mistakes
to take their toll undisturbed.
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The WiZard is In
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| Quote: Originally posted by quicksilver | | The history of methyl nitrate in WWII was a tragic and nightmarish one. Slave labor was used to man the production facilities in Nazi Germany; the
explos. being used in landmines and aerial bombs. The production facilities were segregated from the management and over-seers, allowing the mistakes
to take their toll undisturbed. |
"Before inventing his Dynamite in 1863, Alfred B. Nobel (1833-1896)
proposed a rather safe method of transporting liquid NG. He mixed it with
15-20 parts of anhydrous methyl alcohol and transported the resulting
non-explosive mixture in tanks to places of work. There NG was precipitated
by adding water and the supernatant dilute methanol removed by decantation.
As this method was time-consuming and rather wasteful (because it did not
pay to recover methanol), it was seldom used in the USA.
"Here, where everything is done in a hurry and as cheaply as possible, it
was preferred to transport NG in liquid form, although it was more
dangerous, Many accidents occurred and many live were lost in connection
with NG and as long as most of the workmen were foreigners, especially
Chinese, the industrialists, who care only for profits, did not introduce
any safety regulation until the were forced by the Government after
establishing in 1910 the Bureau of Mines, at Pittsburgh, Pennsylvania."
PATR 2700
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The WiZard is In
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| Quote: Originally posted by quicksilver | | The history of methyl nitrate in WWII was a tragic and nightmarish one. Slave labor was used to man the production facilities in Nazi Germany; the
explos. being used in landmines and aerial bombs. The production facilities were segregated from the management and over-seers, allowing the mistakes
to take their toll undisturbed. |
A description of the use of Myrol (methyl nitrate — methyl nitrate/methanol) of which during the 2nd half of
WW II German production was "as high as 20,000 metric tons a month" can be found in :—
DICTIONARY OF EXPLOSIVES, AMMUNITION AND WEAPONS (GERMAN SECTION)
Fedoroff, Basil T Aaronson, Henry A Clift, George D Reese, E...
PICATINNY ARSENAL DOVER NJ
Page Count: 359 page(s)
AD Number: AD0160636
Report Date: 07 JUL 1958
In theory you can DL this from the obvious US Gov. web site. Search for AD160636.
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quicksilver
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[rquote=176472&tid=949&author=The WiZard is
In theory you can DL this from the obvious US Gov. web site. Search for AD160636.
[/rquote]
Unfortunately I couldn't find it. That would make for pretty interesting reading.
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The WiZard is In
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| Quote: Originally posted by quicksilver | [rquote=176472&tid=949&author=The WiZard is
In theory you can DL this from the obvious US Gov. web site. Search for AD160636.
[/rquote]
Unfortunately I couldn't find it. That would make for pretty interesting reading. |
I have never-ever had trouble finding it. HOWEVER, I have
never even after a dozen attempts succeeded in DL'ing a PDF
that could be opened!
I have had others that took 4-5 DL's before they could be opened,
this one ..... never.
Had a series of failure to connect this AM, then I could connect.
If I knew who to complain upon I would.
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The WiZard is In
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| Quote: Originally posted by andrea | | Hi guys, I'm gonna make some nitroglycerin for the first time. I've got only 65-70% concentrated HNO3 and 96-98% concentrated H2SO4. In the
megalomania's procedure they use 98% HNO3 and 98% H2SO4 in a 2:3 ratio. I wanna know if using a nitrating mixture with a different ratio of HNO3/H2SO4
I will be able to get successfully some NG. If yes what ratio of HNO3/H2SO4 should I use (with 65-70% HNO3)? Thanks for your answers
|
Me again, you know the analogue guy with all the books.
This from one of four that I own that I am amazed I have
never seen mentioned. One of them is in the
library, however, if I were king, it would not be!
Someday when I have time I'll figure out how to DL
JPS or same such here, therefore the PDF.
Attachment: NG.pdf (203kB)
This file has been downloaded 942 times
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The WiZard is In
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J Putman a self-made man who had no use for theorists, among whom he classed all chemists
| Quote: Originally posted by andrea | | Hi guys, I'm gonna make some nitroglycerin for the first time. I've got only 65-70% concentrated HNO3 and 96-98% concentrated H2SO4. In the
megalomania's procedure they use 98% HNO3 and 98% H2SO4 in a 2:3 ratio. I wanna know if using a nitrating mixture with a different ratio of HNO3/H2SO4
I will be able to get successfully some NG. If yes what ratio of HNO3/H2SO4 should I use (with 65-70% HNO3)? Thanks for your answers
|
"[Egbert Putman] a self-made man who had no use for theorists, among whom he
classed all chemists [b. 9 August 1812 patented Giant Powder No. 2* in
1873] was a self-made man who had no use for theorists, among whom he
classed all chemists. Although he was the proprietor of the largest chemical or
acid works in San Francisco, he never employed one of these creatures. Since
the first Judson powder was rather sticky and would not run readily down bore
holes, he conceived the idea of dryin the grains or "driving the nitroglycerine
into the grains" by heating them to about 200o F. He built a jacketed iron pan, about
5 by 12 feet in size which held about a ton of powder and was heated
by steam to the desired temperature. The powder was then shoveled into the
pan with wooden scoops and stirred by a white man with a wooden
rake until the grains appeared dry. Next it was shoveled out on the floor to cool.
Several charges had been made when the workman who was doing the work
was taken sick with a headache, caused, so he said, by the red fumes coming
from the powder. As he was alone, Judson having just gone, be went to tell
Judson and get some fresh air. This saved his life. He had not gone two hundred
feet when there was a flash. All that remained of the building was the iron pan."
As one wag noted in the past - a chemist would have also destroyed the iron pan.
* 40pts NG , 40 sodium nitrate, 6 rosin, 6 sulphur 8 kieselguhr.
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franklyn
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Dictionary of Explosives, Ammunition & Weapons ( German Section )
Links available here if you have access _
http://www.sciencemadness.org/talk/viewthread.php?tid=7518&a...
.
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franklyn
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This could be why _
http://www.sciencemadness.org/talk/viewthread.php?tid=7518&a...
.
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Formatik
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| Quote: Originally posted by NUKE | I have tried synthesizing nitroglycerin with both >99.5% HNO3 and 65%. And I have to say product is identical! Density is very close to 1.6 in
each case only the yield is slightly increased with use of 99.5% HNO3.
200mL >99.5% HNO3
300mL 96% H2SO4
112mL glycerine
Yield was ~180-190mL of nitro both times.
100mL C3H8O3
454mL 96% H2SO4
318mL 65% HNO3
Those ammount yield approximately 100mL of NG. |
That's a big difference in yield. Though pure nitric acid can be used itself to nitrate the glycerin, it requires a large excess. The sulfuric acid
will completley convert the nitric acid to nitronium ion (NO2+), which is the nitrating species. Selenic or perchloric acid do the same, but I
wouldn't use those in an ester nitration. When combined with pure nitric acid, other dehydrants have been used in place of H2SO4, like P2O5 or
Ca(NO3)2, yielding more or less pure NG as described by Tenney Davis. Oleum will reduce the water content even further, and so some of the highest
yields have been reached as mentioned by Urbanski.
| Quote: | | ... runaway in small batches don't present significant detonation hazard |
Maybe not, maybe so. A poster in this thread lost a hand and an eye from a mere 10ml of nitroglycerin runaway reaction
despite noting adequate temperature control.
| Quote: | | Whole mixture of acetone/NH3/NG is dumped into approximately 5 times it's volume of distilled water and whole thing is violently shaken so as much
acetone,NH3 as possible is seperated from NG (I used HDPE vessel for that purpouse). |
Shake it violently in an insolubilized (suspended) state? I'd rather not.
Federoff states a mixed acid of less than 80g per 10g glycerin tends to give an explosively unstable waste acid. The ratio given by Stettbacher is
just under this (7.5 parts acid per part glycerol).
Urbanski mentions the H2SO4 (or oleum) should be free from Fe- and Pb- sulfates, since these make separation of nitroglycerin and acid difficult.
Drain cleaners and car battery acid likely contain such contaminants in significant amounts.
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NUKE
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@Formatik
I was being very approximate at estimation of the yield. There was a difference tho. I believe it could be attributed to HNO3 not being completely
free of dissolved NOx (long storage).
Regarding the runaway hazard: A friend of mine purpousely remotely dumped few 10mL of glycerine at once into a room temperature acid mixture and
nothing but a large evolution of NO2 and boling of mixture resulted. No detonation occurred.
Even after shaking NG always contains fair ammount of acetone so it's not entirely pure NG that's being shaken.
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