Sciencemadness Discussion Board

nitroglycerin

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nitro-genes - 27-1-2010 at 20:12

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]

mfilip62 - 28-1-2010 at 08:09

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! :D

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!?:cool:

Lord Emrone - 5-2-2010 at 15:08

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 ?

hissingnoise - 5-2-2010 at 16:11

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]

mfilip62 - 5-2-2010 at 16:53

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.

Lord Emrone - 6-2-2010 at 06:57

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.

hissingnoise - 6-2-2010 at 07:35

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]

Lord Emrone - 8-2-2010 at 04:40

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.

The WiZard is In - 6-4-2010 at 07:15

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.

NUKE - 23-4-2010 at 06:38

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...

hissingnoise - 23-4-2010 at 09:55

Or acetone solution, strictly speaking - dispensing with acetone and dH2O just means extra swirling in a few changes of tap-water after neutralisation. . .


quicksilver - 23-4-2010 at 10:43

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]

The WiZard is In - 23-4-2010 at 13:41

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]

hissingnoise - 24-4-2010 at 03:06

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. . .


quicksilver - 24-4-2010 at 04:25

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.

The WiZard is In - 24-4-2010 at 06:04

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

The WiZard is In - 24-4-2010 at 06:44

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.

quicksilver - 24-4-2010 at 14:45

[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.

The WiZard is In - 24-4-2010 at 15:28

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.



The WiZard is In - 24-4-2010 at 16:05

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 928 times

J Putman a self-made man who had no use for theorists, among whom he classed all chemists

The WiZard is In - 24-4-2010 at 16:13

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.

franklyn - 24-4-2010 at 16:52

Quote: Originally posted by The WiZard is In  
Quote: Originally posted by quicksilver  
Quote: Originally posted by The WiZard is In  
you can DL this from the obvious US Gov. web site. Search for AD160636.
Unfortunately I couldn't find it. That would make for pretty interesting reading.
If I knew who to complain upon I would.

Dictionary of Explosives, Ammunition & Weapons ( German Section )
Links available here if you have access _
http://www.sciencemadness.org/talk/viewthread.php?tid=7518&a...

.

franklyn - 25-4-2010 at 13:59

Quote: Originally posted by quicksilver  
Unfortunately I couldn't find it. That would make for pretty interesting reading.

This could be why _
http://www.sciencemadness.org/talk/viewthread.php?tid=7518&a...

.

Formatik - 29-4-2010 at 10:48

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.

Quote: Originally posted by The WiZard is In  
... using an acid/glycerine ratio of approximately 6.


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).

Quote: Originally posted by S.C. Wack  
Drain cleaner? Technical grade materials too much?
For nitroglycerin?


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.

NUKE - 30-4-2010 at 00:33

@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.

Formatik - 1-5-2010 at 09:58

I know about the harmless runaways: nitrogen oxides, heat, no detonation. That's when it goes "good".

In the small scale, the violent runaway probably depends on how much nitro has already accumulated. At the start of nitration or dumping all the glycerin in at once might not allow the nitro to form, or decompose as or before it has even formed, alongside a vigorous oxidation of the glycerin.

Notice the example, from the poster I gave, it was towards the end where there was a runaway, so that means it was actually about 10ml which had formed, and detonated. Whereas your friend dumped all the glycerin in at once. That's not to say this will happen predictably, just my thoughts on the differences.

For: HNO3 + 2 H2SO4 = NO2+ + H3O+ + 2 HSO4-

Water is disadvantageous because of the protonation it causes (NO2+ and H2O form HNO3), and for which the sulfuric acid compensates. Sulfuric acid protonates the HNO3 which is what forms the NO2+. In pure nitric acid there is little NO2+, which is why it's combined with H2SO4. The hydronium sulfate is no good for the conversion to NO2+. With more water and more sulfuric acid, there will be less nitronium.

[Edited on 1-5-2010 by Formatik]

Cloner - 25-10-2010 at 11:56

Is it feasible to use a solvent such as DCM or petroleum ether during the synthesis of NG, to dilute it to inertness during the later stages of the reaction and the workup?

rbick - 28-10-2010 at 07:30

Thats a good question. Could you been more specific though? At what point would you dilute it? After it has formed on top of the nitrating mixture?

I know that NG can be transported more safely by diluting it with Acetone to a point where it is extremely hard to detonate, which I think starts somewhere around 70% NG to 30% acetone. I've never thought about trying it during a synthesis though. Sounds like a fun project.

Maybe you could add the acetone or whatever solvent with the NG to dilute before extracting it from the nitrating mixture with your separatory funnel. It could then be washed, neutralized and evaporated for a nice clean product. Being diluted and therefore less sensitive, it could make the synthesis and handling much safer. Any thoughts?


Microtek - 28-10-2010 at 13:27

Supposedly, DCM is a very good medium for aromatics nitration. I read somewhere that toluene was quantitatively nitrated to TNT by adding anhydrous nitric acid to a solution of it in DCM at 0 C. I haven't tried it myself though.

The WiZard is In - 28-10-2010 at 13:35

Quote: Originally posted by rbick  

I know that NG can be transported more safely by diluting it with Acetone to a point where it is extremely hard to detonate, which I think starts somewhere around 70% NG to 30% acetone. I've never thought about trying it during a synthesis though. Sounds like a fun project.



"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 nonexplosive mixture in tanks to places of work. There the
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 lives were lost in connection with NG and as long as most of
the workman were foreigners especially Chinese, the industrialists,
who care only for profits, did not introduce any safety regulations
until they were forced by the Government after establishing in 1910
the Bureau of Mines at Pittsburgh , Pennsylvania."

PATR 2700 me thinks.

Microtek - 29-10-2010 at 05:53

Surely, it must be possible to initiate a 15:85 mix of methanol and NG with a suitable detonator (I realize that the technology of detonators weren't very advanced at the time).

The WiZard is In - 29-10-2010 at 07:09

Quote: Originally posted by Microtek  
Surely, it must be possible to initiate a 15:85 mix of methanol and NG with a suitable detonator (I realize that the technology of detonators weren't very advanced at the time).



Nobel added methanol to prevent an accidental an explosions.

It wouldn't have been used mixed as an explosive... that would
have required larger bore holes to correct for the expanded
volume. Assuming it could have be detonated, which was
accomplished in the early days by flame only. Black powder
mixed with NG was also used.

Hudson Maxim
Dynamite Stories 1916
(A reprise can be had from www.fireworksnews.com )

HOISTED WITH HIS OWN PETARD
LIQUID nitroglycerin is still used to torpedo the oil-wells when they get old, in order to
give them a new lease on life.

There was one teamster in the old days who had become notorious as a hauler of the
dangerous explosive. The law does not permit the shipment of the liquid by freight or by
express, and for that reason this teamster had plenty to do in hauling nitroglycerin for long
distances. He was a great smoker and his old pipe was always alight, though he might be
riding on a ton of nitroglycerin with a few kegs of black gunpowder clinked into the load.

One day he was carrying, on runners, about two tons of nitroglycerin and a few odd
kegs of gunpowder, when something happened. There had been a fall of several inches of
light snow the evening before, and the scene of the eventuation was an open field which
he was crossing.

There was an enormous crater in the ground; the light snow around the crater was
besprinkled with a few shreds of horse and harness and a sliver or two of sled, but not a
trace of the driver was ever found.

Vist :—

Tallini Tales of Destruction www.logwell.com
..an amazing collection of historical stories involving nitroglycerin use in the oilfields.

For historical info on the early use of NG in the oil fields
consult the every suspenseful/interesting

VAn Gelder & Schlatter
History of the Explosives Industry in America
IME 1927
1132 well indexed pages.

I own a 1972 Arno Press reprint.

rbick - 29-10-2010 at 07:16

Microtek,

I bet it is too. If I'm not mistaken they were using compressed black powder to initiate dynamite until later in the 1800s?

Although I've never read about using Methanol, I know that a 70% NG/30% Acetone can be detonated although a booster must be used. I'm assuming it would be similar with Methanol since NG is listed as miscible with both Methanol, Acetone, and other organic solvents on the MSDS.

I read either a patent or an article (can't remember which if it was an actual patent or not) discussing the use of Acetone to dilute NG for safety reasons but the link and information was lost along with Rogue Sci :(. If anyone has the link, I'd like to see it!

EDIT: The Wizard and I posted at the same time. Looks like he found the info for the use of Methanol. Nice... :cool:

[Edited on 29-10-2010 by rbick]

The WiZard is In - 29-10-2010 at 07:58

Quote: Originally posted by rbick  

EDIT: The Wizard and I posted at the same time. Looks like he found the info for the use of Methanol. Nice... :cool:



Actually I found it years ago ...

Newsgroups: rec.pyrotechnics
From: "donald j haarmann" <haa...@mail.idt.net>
Date: 1997/06/01
Subject: Re: expendable labor!

"Before inventing his Dynamite in 1863, Alfred B. Nobel (1833-1896)

The WiZard is In - 29-10-2010 at 08:09

Quote: Originally posted by rbick  
Microtek,

I bet it is too. If I'm not mistaken they were using compressed black powder to initiate dynamite until later in the 1800s?



Eric Twitty in his book "Blown to Bits in the Mine: A History of Mining &
Explosvies in the United States, dates usage of RR powder [which version?]
from 1876 to 1930.

A curious version was made by the Giant Powder Company. Twitty cites
US Patent 183,764 of 1876 for the following:-

"Egbert Judson, on the of Giant Powder Company's visionary founding fathers,
duly noted the performance of the mixture of a small volume of nitroglycerine
absorbed in blasting powder, and its possible applications. In 1876 he patented
"Judson Powder", which consisted of a modified blasting powder thinly coated
nitroglycerine. The difference between Judson's product and earlier NG-coated
blasting powder formulas lay in the manufacturing process. Judson melted
the sulfur, added the other powder ingredients to the melt, cooled it, crushed it,
and classified the grains. Melting the ingredients made their surfaces glassy,
decreasing porosity and facilitating an even coat of nitroglycerine. In the making
of true blasting powder, there was no melting of ingredients. Judson's formula
required the grains be coated with 5%, 10%, or 15% nitroglycerine by weight."

Bismuth - 8-1-2011 at 05:19

I'm aware of the safer alternatives of NG (namely, EGDN/PGDN) but at one point or another, I want to synthesis some nitroglycerin. I simply deflagrate the secondaries I produce, so I'm not after making a large quantity at all. It's more just the experience and notoriety of synthesizing a little NG, so I can add a little first hand experience onto the knowledge I have accumulated from reading about it.

I began to think, nitrating 1ml of glycerin may pose more threat than a larger quantity. Not the consequences obviously, but an increased risk of an accident occuring. It would mean if I manually stirred it, there would probably be an increased chance of stirring rod to side of beaker contact. While I am definitely more inclined to use an aquarium pump, with these quantities it may prove to be a little annoying to do so. It also makes the whole experiment in colloquial language, "more fiddly".

It then brings me to, what glassware would be most suitable? Small beakers that could occupy such a small mix well aren't really abundant in a lab that usually does larger synthesis. I'm not keen to use a 25 x 150mm test tube, either. I gladly will go out and buy smaller beakers and other equipment to do the synthesis safely as I much rather pay with money than with eye loss or digit loss.

I've got my opinion in mind, but another from someone with a more practical knowledge couldn't hurt. I already know if I were to nitrate 20ml of glycerin, I would just use a suitable beaker, an aquarium pump to blow air over to create a whirlpool effect and all the other necessary precautions outlined in this thread and in literature. But for an amount where I only want to use 1ml? Would it just be an easier and safer process increasing it to 3, 4 or 5ml, just to make the whole procedure less of a nuisance?

hissingnoise - 8-1-2011 at 05:41

I use a thermometer as stirring rod and I flinch at every glass-on-glass clink!
Going at it as if you're beating eggs in a bowl is not the way to go.
Gentle (and I mean gentle) stirring shouldn't throw up "surprises" . . .


Mixell - 8-1-2011 at 10:18

Can anyone please post a link to the nitroglycerin producing method that was mentioned in the first post?
I can't manage to find it via the search option...

The WiZard is In - 8-1-2011 at 11:58

Quote: Originally posted by The WiZard is In  

Eric Twitty in his book "Blown to Bits in the Mine: A History of Mining & Explosvies in the United States, dates usage of RR powder [which version?] from 1876 to 1930.



Snelling and Storm
Bureau of Mines Bulletin 51
The Analysis of Black Powder and Dynamite
1913

GRANULATED NITROGLYCERIN POWDER.

When ordinary dynamite is used in blasting any material of a
consistency resembling that of earth or clay, little of the energy of
the explosive does useful work, because the soft and compressible
nature of the material blasted allows the greater part of the
energy of the explosive to be used in compacting the material and
in producing a cavity. Consequently, gunpowder has been largely
used in all places where earth, clay, or other soft material was to
be dislodged. In the blasting of the banks of railroad cuts there are
often places where a soft, but somewhat consolidated material,
intermediate between earth and hard rock, has to be blasted. Such
a material might be a soft shale, for example, or a friable and
easily crumbled sandstone, and for dislodging it neither ordinary
blasting powder nor ordinary dynamite is particularly suitable. In
the year 1876 E. Judson patented an explosive consisting of a low-
grade gunpowder made by heating and mixing together coal,
sulphur, sodium nitrate, etc., granulating the mixture, and then
coating this nonabsorbent granulated dope with a small amount of
nitroglycerin. The proportion of nitroglycerin used—often as little
as 5 per cent— was such that had it been absorbed by the grains
of explosive it would not have been capable of detonation, but by
remaining wholly or largely upon the surface of the grains the use
of a detonator brought about its explosion and the simultaneous
ignition of the gunpowder base which it covered. Such an
explosive, as a result of the detonation of the nitroglycerin,
produces an initial blow sufficient to crack and fissure the partly
consolidated material in which it is placed. The action of the
gunpowder mixture that forms the larger part of the explosive so
heaves and moves the broken-up mass as to make easy its
removal with steam shovels.

Granulated nitroglycerin powders, or "free-running" explosives,
have been very much used in the excavation of earth and are
commonly known as Judson powder (after the inventor), bank
powder, or railroad powder. In the analysis of low-grade granular
powder, moisture is determined by the standard method, and the
usual method of extracting with ether is followed. In the ether
extract are usually found large proportions of sulphur, rosin, etc.,
besides the nitroglycerin. The proportion of sulphur commonly used
in low-grade granular powder is so considerable that usually it is
not all removed by extraction with ether.

Explosive-DuPont-RR.jpg - 351kB Explosive-Judson-Powder-V&S-338.jpg - 441kB Explosive-Judson-Powder-V&S-681.jpg - 448kB

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DuPont is from the 1928 Edition of DuPont's Blasters Handbook,
the oldest edition I own. It is also in the 1934 ed. Not in the
1942 and following editions.

V&S is Vangelder and Schatler, History of the Explosives Industry
in America. IME 1927.


V&S

"[Egbert Putman] Judson [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 drying 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 shovelled into the
pan with wooden scoops and stirred by a white man with a
wooden rake until the grains appeared dry. Next it was shovelled
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."

* 40pts NG , 40 sodium nitrate, 6 rosin, 6 sulphur 8 kieselguhr.

As one wag noted some years ago when I posted this in
Sci.Chem... A chemist would have blow up the iron pan.


NG neutralization

Zinc - 12-1-2011 at 05:47

I have noticed NG can be difficult to properly neutralize.

Two times have I put NG under a NaHCO3 solution (once for 12 h, and once for more than 24 h, I have posted about the first attempt in this thread some time ago). After the time has elapsed I tested both the solution over NG, and the NG itself with litmus paper. The solution was basic but the NG was still acidic. Both times was the NG periodically swirled under the solution (not too much but quite a bit).

The second time I tried, after 12 h of staying under the NaHCO3 solution, I removed most of the solution, and added cca. 60 ml of acetone to the cca. 17-18 ml of NG and a small amount of the solution that remained over the NG (cca. 10 ml). The acetone and NG mixed and formed a layer that floated above the aqueous solution. After that I added cca. 150 ml of a NaHCO3 solution, swirled a minute or two, noticed some CO2 evolving, and added 500 ml of water. The water removed some acetone from the NG, but some (around half the volume) still remained mixed with the NG, so I added again the same amount of water. This removed almost all of the acetone. Then the third wash with half the volume of water was performed and the NG was tested with litmus paper, showing that it is non-acidic. After that I put the NG under an almost saturated NaCl solution to remove the water dispersed in the NG (it is milky-white). I forgot to write that all the water washes were performed with relatively warm water (hot tap water, how hot is it? Around 50 C?), in the hope that the extra heat would remove at least a small amount acetone through evaporation, and that the NaHCO3 solutions were both times moderately concentrated (don't know the exact conc. because I didn't weigh the NaHCO3), in the second attempt they were luke-warm, in the first room-temperature. I would also like to say that all of the washings reduced the final yield of NG (I don't know how much exactly because I never measured it, only eyeballed it. After the nitration I had around 20-23 ml (the batch was 200 ml of conc. H2SO4, 100 g of AN and 25 ml of glycerin), after the washings around 15-17 I believe.

All in all I can say that NG if more difficult to neutralize than I thought.

Are there some more effective methods? I do believe that constant stirring of the NG while under the basic solution would be much better, but I don't have the equipment for that. Perhaps simply letting it sit under the solution for several days would also work, but I would take a long time (not that I'm in a hurry but still :P)
Maybe it the problem where to dilute NaHCO3 solutions?

hissingnoise - 12-1-2011 at 06:28

Quote:

Are there some more effective methods? I do believe that constant stirring of the NG while under the basic solution would be much better, but I don't have the equipment for that.

What lack of equipment could possibly prevent you swirling the mixture by hand?
Wash water won't worm its way into the interior of the nitro by itself, you know!
And the bicarbonate solution should be no more than 5% . . .



Zinc - 12-1-2011 at 08:36

Quote: Originally posted by hissingnoise  

What lack of equipment could possibly prevent you swirling the mixture by hand?


Indeed, but don't think I could hand swirl it for several hours. It seems at the moment that the best thing to do would it be to leave it under a NaHCO3 solution for several days with periodic swirling.

Quote: Originally posted by hissingnoise  

And the bicarbonate solution should be no more than 5% . . .


Interesting. I thought the concentrated the better. Why is diluted better (I know strong bases would hydrolyze NG, but I don't think even a saturated solution of NaHCO3 is enough to do that, but I could be wrong)?

hissingnoise - 12-1-2011 at 13:25

Low bicarb concentrations lessen the possible contamination of nitro!
In practice, it's about 3%!
When you're swirling, time slows to a crawl . . .
Just reconnect with your dogged side and don't let your attention wander!



Microtek - 12-1-2011 at 14:02

Many kitchen appliances are made precisely for stirring, so I suggest that you buy a cheap hand mixer and use that. Just make sure that the rotating bits don't hit the sides of the vessel (mount the mixer in a fixed position eg. a drill press) and use a relatively soft plastic vessel just to be safe.
According to Urbanski, an emulsion of NG in relatively little water (on the order of equal volumes of water and NG IIRC; this is not a stable emulsion obviously) cannot be initiated even with a strong blasting cap.

Simply letting the NG stand under a bicarb soln is an excercise in futility. Try looking up diffusion and random walk. Even though you probably can't find diffusion coefficients for acid residue in NG, you can still get an idea of how long it could take. Depending on the batch size and the geometry of your vessel, it could take months or years for it to approach a neutralized state.

Jimbo Jones - 13-1-2011 at 10:18

…..or just use ordinary & improvised magnetic stirrer and soft plastic vessel.

quicksilver - 13-1-2011 at 10:34

Quote: Originally posted by hissingnoise  
I use a thermometer as stirring rod and I flinch at every glass-on-glass clink!
Going at it as if you're beating eggs in a bowl is not the way to go.
Gentle (and I mean gentle) stirring shouldn't throw up "surprises" . . .



Get an aquarium aerator and use those bubbles! Safe and will still keep your mix appropriate. In fact, if you take your time and bring your hose to the bottom of the beaker allow it to form a semi-circle around the bottom-base and you'll get a tiny gentle Whirlpool: perfect for continued mixing. By bringing the tubing to a smaller opening you can make a bubblier into a mild jet.
Take a few dollars and invest in a digital thermometer - much safer: sharper results.
Or take some tape and put VERTICAL & THIN stripes on a glass thermometer (all the way to the bulb!) to keep that banging from becoming a tragedy.

Never glass to glass because even if you're the "genteel hand in the West" the thermometer may weigh enough so that an accidental drop from your paw may do enough to start the train rolling; especially those real long ones because they naturally focus (in the bulb) at a point of sorts. Tape won't throw your readings off if you use very thin (vertical) strips.

If you should use a magnetic stir device - periodically examine the stir-bar. Occasionally the Teflon will wear down to the metal. A small piece of tape there is a good "peace of mind" utility.




[Edited on 13-1-2011 by quicksilver]

User - 14-1-2011 at 03:05

Ive always wondered about the potential effect of the stirbar..
2 of my stirrers carry very strong magnets, some scratching effect may occur.
Probably not enough to do serious damage , still there is no real way of actually knowing.

[Edited on 14-1-2011 by User]

quicksilver - 14-1-2011 at 08:57

Air has been used in plant production for decades and is more than just a "peace of mind" issue for most. It's a very flexible methodology and is "wear resistant".

We know that the majority of these materials are not as sensitive as characterized but both the fluids and the solid polyols / esters CAN provide a gateway to a tragedy from their very characteristics: fluids can seep into tight places, particulate can grind against itself.
If I were ever to synthesis NG I would ALWAYS err on the side of over-caution.



[Edited on 14-1-2011 by quicksilver]

Zinc - 16-1-2011 at 05:37

My NG has now been 4 days under the NaCl solution. Already after the first day it almost completely cleared.

But I notice there are quite a lot of bubbles in the NG. How much do they sensitize the NG? And what would be the best way of removing them?

I was thinking perhaps simple swirling and decantation to an another container would work?

hissingnoise - 16-1-2011 at 07:06

I'd be a bit concerned if I saw lots of bubbles appearing . . .
I'd wash it further; simply tilting the container, which could be fairly large, so that the blob of NGl rolls around the bottom is probably as good as swirling, not to mention safer.


Zinc - 16-1-2011 at 12:05

I washed the NG with an another portion of conc. NaCl soln. and transported it with a syringe into a measuring cylinder. Final yield is 23.5 ml, much more than I thought. A few ml were lost during washing, so it is possible that the yield was over 25 ml. Also I doubt that there is acetone left from the neutralization, the NG has a weak smell, I believe if there is some acetone left, the smell would be much stronger.

Almost all of the bubbles were removed by the final washing and during transportation from the jar to the measuring cylinder. Although a small amount of some powder like material remained on the surface of NG, perhaps some salt (a small amount of water could have evaporated from the NaCl soln. causing some NaCl to precipitate), but the quantity is extremely small (I don't think it is more than a few mg).

Also I have tested it again with litmus paper, it is still neutral :D

Zinc - 21-1-2011 at 11:04

Sorry for the double post, and if the question is too "practical".

I was thinking about trying NG/DNT mixture (perhaps with some paint grade Al powder), and I know NG mixtures often contain a small amount of CaCO3 to neutralize any acid that may be in the mix.

As I don't have access to pure CaCO3, and don't like the idea to use impure ground rocks, could perhaps NaHCO3 be used instead of it?

I believe that NaHCO3 is a stronger base than CaCO3, and that it can react with AN quite easier than CaCO3 (to form NaNO3 and ammonium bicarbonate, that easily decomposes to NH3 and CO2), so is perhaps that the reason that it isn't used (at least I didn't find any information on it being used)?

As the NG/DNT (perhaps some Al) doesn't contain AN, could NaHCO3 be safely added (perhaps 1-2 %) to the mixture?

And I know that Al can react with bases, but I don't think that NaHCO3 is a strong enough base to penetrate the Al2O3 layer on the surface of the Al (and my Al seems to be coated with some form of resin or "plastic", don't know how much of that is on it) especially if it is so "diluted" with NG and DNT.

Microtek - 21-1-2011 at 14:15

Why don't you just make some CaCO3? Surely you must have access to a soluble calcium salt (CaCl2 or maybe Ca(NO3)2). Then just combine the solutions with stirring and if it doesn't precipitate right away (depending on the exact nature of the salts you may get a gel at first) just keep stirring (or boil the mix) until you get a suspension of fine precipitate. Filter, wash, dry.

maxidastier - 22-1-2011 at 10:32

Honest answer: Is it really so dangerous when I stir with a glass thermometer that it even could explode? :o:(

hissingnoise - 22-1-2011 at 11:16

I've stirred the reactants with a thermometer on a few occasions but I'll not do it again!
When it comes to nitro you can't be too careful . . .


Jimbo Jones - 22-1-2011 at 12:00

http://img11.imageshack.us/i/15129161.jpg/

http://img812.imageshack.us/i/43034.jpg/

I have no problems with this setup. The “addition funnel” is very handy, because you can mesure the alcohols directly in the syringe.

[Edited on 22-1-2011 by Jimbo Jones]

Zinc - 24-1-2011 at 03:24

Yesterday I tried to set off a mix of 40g DNT, 30g NG and 5g paint-grade Al powder and cca. 1g of NaHCO3 (I don't know how safe it is to use NaHCO3 instead of CaCO3, but as the time from mixing to the time of detonation was only around 1.5 h I took the risk). When prepared the mixture is a very dense and viscous shiny liquid.

Unfortunatley, I had no better primary than MEKPAP/AN.

My MEKPAP was contaminated with unreacted acetone/MEK, so it wouldn't DDT alone in a small glass test-tube (volume 5 ml), forcing me to mix it with AN and put it in a small plastic bottle (the bottle is 15 ml, filled with cca. 2.5g of AN and 4 ml of MEKP/AP). Even then it detonated quite weak compared to pure MEKPAP/AN, but I thought that as the mix contains so much NG it would be enough.

Well it wasn't and the mix went low-order. I know that the VOD at wich NG detonates is very dependent on the strenght of the detonator, but as I didn't have anything else, and didn't want to store the NG/DNT/Al mix I used what I have.

maxidastier - 25-1-2011 at 10:18


Quote:

I've stirred the reactants with a thermometer on a few occasions but I'll not do it again! When it comes to nitro you can't be too careful . . .


Again, glyceryl trinitrate is quite sensitive, no doubt, compared to PETN oder RDX.
But I insist it will never detonate when a glass rod hits the beaker...
And I've also NEVER read about that so far in any reliable sources, but you still should bear in mind proper safety precautions.

But you can still convince me with data about what energy releases a glass rod hitting a beaker and if that is enough to detonate NG regarding to the given sensitivity data.



[Edited on 25-1-2011 by maxidastier]

hissingnoise - 25-1-2011 at 11:53

Quote:
But I insist it will never detonate when a glass rod hits the beaker...

You're making a very dangerous assumption here, maxidastier!
It's the kind of attitude anyone handling these compounds should guard against . . .
Much better to err wildly on the side of safety at all times!



maxidastier - 26-1-2011 at 06:15

You are right. But I just can't believe that something like a little "cling" from a glass rod can make NG to explode. If that's the point, I would never handle with it again. :(

Jimbo Jones - 26-1-2011 at 09:35

Very interesting! Maybe a remote controlled old kitchen mixer and some big ass stirring rod will solve the problem. This is impossible for me, but anyone with nice place for tests is wellcome. Some things like the NG sensitivity in acid suspensions and the temperature are very interesting to me, because in the beginning I heavily used the thermometer for stirring rod. Then I totally switched to the magnetic stirrer & teflon bar combo. So, can “a little "cling" from a glass rod make NG to explode”. It’s time for some mythbusting…….

[Edited on 26-1-2011 by Jimbo Jones]

maxidastier - 26-1-2011 at 11:14

Veery funny!

DNA - 27-1-2011 at 02:10

Yes I also think this should be tested because I am also of the opinion that NG wont detonate from a glass rod hitting the wall of a flask.
Neither will a stirrbar detonate NG.

If you see how much force is needed with a hammer to detonate NG when it is placed on an anvil....

quicksilver - 27-1-2011 at 08:55

I would have thought that I would NEVER have to consider saying this but we are talking about safety and ethics so.....

It's NOT just the impact of glass to glass but friction as well.; what's more there can be issues of hot-spots sensitizing minute droplets moving about the acid bath w/ it's possible temp fluctuations. We are also speaking to the phenomenon of the "expls TRAIN" concept where in a small pop sets off the rest. MY GOD! There is no correlation between an active nitration and a competed synthesis and during any nitration that has consistently provided documented proof a hideous disasters from what is termed a "run-a-way", if that phenomenon were to be examined it would be clear to some who has low levels of knowledge in chemistry that NG (as an example) has certain anomalies that can render it hyper-sensitive. The level and amount of unintended explosions has been documented to such a degree that if ANYONE wanted to venture into this with an open mind they would find EVERY reason to employ EVERY safety precaution available.

Anyone who has professional level chemical training does not dismiss safety issues with a "first person all encompassing statement". Just because something had not happened to you yet, does not mean it cannot occur. First hand single level experiences are just that: experiences. That is NOT science.

There is a great difference between a product that is in the process of nitration and one that has been completed, washed, stabilized, cooled, neutralized, & isolated. The correlation of an actively nitrated material's impact sensitivity and one that is currently being nitrated is dissimilar.

The warning of "glass to glass" impact during NG synthesis is VERY old and has been the course of many tragedies. (I actually can't believe I'm writing this.....)
One of the MAJOR rules of energetic synthesis is that you 1st minimize the possible sources of ignition stimulation. Hasn't ANYONE EVER STUDIED THIS? There is NEVER any valid reason for testing the limits of safety.

The two major areas wherein tragedies have happen were when someone "forgot" a simple procedure (i.e. grounding oneself and related areas to minimize static) and when they IGNORED those safety precautions ("I've done this all the times I've made it and it never........")

Let's just cut right to the chase here. Let's stop the bullshit. If anyone wants to CUT DOWN on their safety precautions (for whatever reason) make a sworn promise with yourself that you WILL come back and post what had happened when you had a tragedy! Remember.....it's NOT an "accident" it's negligence: as you have been amply warned about impact, friction, static, & other forms of stimulus. Not some post that I did this and nothing happened; but when you went to the Emergency Room!
I have heard too many of these things. I have confidence in one thing; unpredictability if formats of consistent precautions in the face of potential injury are ignored. It may not happen for 3x or 100x but eventually, if a person works with energetic materials CUTS DOWN on their safety procedures, they will eventually pay a price.

Ask yourself WHY even manual stir rods are coated with Teflon? Then ask yourself what is the pay off for LIMITING safety precautions rather than tightening them? Then ask yourself how many times you are willing to experiment with the possible loss of sight and limbs, finger, tendon tissue, etc?

Frankly I am very surprised & disheartened to read this thread. I had thought with so MANY years of history of tragedies behind it, that energetic synthesis would have simply been a standard [example of] EVERY lab precaution possible. And to find I was WRONG on that point makes me VERY leery of ever contributing an active, workable synthesis to this section of the Forum again. I would be willing to bet I am NOT alone in this thinking as well!
If what I have just written doesn't make sense to someone or someone wants to "debate" the issue; I simply won't go there but I will leave one statement of fact that should be considered ASIDE from the loss of eyes,, limbs, & flesh. The very idea of REDUCING safety measures when working with energetic materials would actually get you FIRED from most every vocational position dealing with any aspect of this subject.

Some folks wants to diminish their safety precautions: be my guest! I am VERY curious how many would be man enough to come back and speak to typing w/ one hand, or loosing their depth perception AND ESPECIALLY - HOW THEY WERE DEAD WRONG in not taking advise on the side of safety!

I say this with such emphasis because rationalization & intellectualism have caused SO much harm.....there IS NO getting through that emotional defense mechanism. Logic DOESN'T HELP.......So go for it.



[Edited on 27-1-2011 by quicksilver]

maxidastier - 27-1-2011 at 09:12

I'm sry.
Will it be ok then, when I wrapp my glass thermometer with some Teflon coil? Will it give valid temperatures?
Can I also use a magnet stirrer with PTFE rods?

quicksilver - 27-1-2011 at 09:29

The use of a thermometer is generally to be a stationary tool. Your best readings are made when it consistently it set up to encompass the fluid, gas etc; it's movement may cause more poor readings than anything else. It is NOT designed to BE a stirring utensil.

The common method of stirring NG both in plant-level and lab was with the use of air. There was a VERY good reason for that. It disbursed the material for better nitration and it made no contact of surface to surface agenda. I had already written that however. So I suppose I'm repeating myself.

[Edited on 27-1-2011 by quicksilver]

maxidastier - 27-1-2011 at 09:52

But since I'm not the owner of a pump to blow air trough the mix, what can I do?

The WiZard is In - 27-1-2011 at 10:20

Quote: Originally posted by quicksilver  

The warning of "glass to glass" impact during NG synthesis is VERY old and has been the course of many tragedies. (I actually can't believe I'm writing this.....)
One of the MAJOR rules of energetic synthesis is that you 1st minimize the possible sources of ignition stimulation. Hasn't ANYONE EVER STUDIED THIS? There is NEVER any valid reason for testing the limits of safety.

Let's just cut right to the chase here. Let's stop the bullshit. If anyone wants to CUT DOWN on their safety precautions (for whatever reason) make a sworn promise with yourself that you WILL come back and post what had happened when you had a tragedy! Remember.....it's NOT an "accident" it's negligence: as you have been amply warned about impact, friction, static, & other forms of stimulus. Not some post that I did this and nothing happened; but when you went to the Emergency Room!
I have heard too many of these things. I have confidence in one thing; unpredictability if formats of consistent precautions in the face of potential injury are ignored. It may not happen for 3x or 100x but eventually, if a person works with energetic materials CUTS DOWN on their safety procedures, they will eventually pay a price.


If you are not going to boil anything ... use plastic. Preferable
soft plastic. If you can find them for powders ... conductive
rubber containers.

Bert - 27-1-2011 at 10:22

You could use methods designed to not require stirring, merely swirling the reaction vessel.

With appologies to Boomer, who posted this for another kid who was going to do it anyhow...

==================================================

OK, I cannot stop you anyway, so here is a very safe method: Your ratios were not bad, I mix 75ml of 96% sulphuric acid with 50g AN and put it in the deep freezer set to max. power (-25C) overnight. During the next morning, I add 11ml of glycerine in four portions with good swirling, and put it back for 1-2 hours each time. Even if you SHOULD add ONE portion very fast, the temp will only shoot from –25C to –10C each time, that’s why it is safe (thermal mass cannot jump to 30C). Of course you WILL add them SLOWLY and WATCH THE TEMP to get a feeling for the process. You have a thermometer, ehh?
I give it a few good shakings over the afternoon (putting it back in the freezer each time), and in the evening pour it into a litre of cold water. The NG settles at the bottom and can be sucked out, washed again with water, with bicarb, with water… look the process up on the above sites again before you start.
The reason you only saw a few drops is that most is suspended in the thick liquid. Yield for this method is around 50% of theory or 10ml of neutralised NG.

And SCALE IT DOWN the first time, please!

maxidastier - 27-1-2011 at 11:18

Thanks for the method, but yield is rather bad. Anyway, is magnetic stirrer also to dangerous?

"If you are not going to boil anything ... use plastic"

I thought nitric acid and plastic don't work together? What specific sort of plastic do you suggest apart from "soft plastic"?

Jimbo Jones - 27-1-2011 at 12:00

http://www.tpp.ch/technical_information/raw_materials/Resist...

maxidastier - 29-1-2011 at 01:25

Well, but where can you get a stirring rod made of PE oder PP???

grndpndr - 29-1-2011 at 02:14


Adequate air volume should be available from an aquarium air pump.Mine was free from a friend who no longer owned an aquarium.Even new I cant imagine there an awful lot of $ given the increased piece of mind.The aquarium pump really agitates a 500ml beaker full of mildly viscuous fluid.As I dont yet own an overhead stirrer or mag stirrer/hotplate its very useful for relieving tired arms while still keeping the synthesis well stirred.

Im not sure if in high humidity climes it might be wise to try to use air coming off a source of dry heat,electric heater!?

[Edited on 29-1-2011 by grndpndr]

[Edited on 29-1-2011 by grndpndr]

Bert - 29-1-2011 at 08:55

Quote: Originally posted by maxidastier  
Well, but where can you get a stirring rod made of PE oder PP???


There are PE and PTFE (Teflon) stirring rods and small spatulas available.

http://www.labsafety.com/search/HDPE+stir+rod/24550628/

That took 10 seconds to find. Google...

Quote: Originally posted by grndpndr  


Im not sure if in high humidity climes it might be wise to try to use air coming off a source of dry heat,electric heater!?



Heating air only lowers the relative humidity, it doesn't REMOVE any water vapor.



[Edited on 29-1-2011 by Bert]

Microtek - 30-1-2011 at 10:57

I have always found that air agitation stripped off too much of the nitric, giving huge clouds of fumes. For this reason I have used swirling or magnetic stirring. If anyone has a method that reduces stripping, I'd like to hear it.

quicksilver - 30-1-2011 at 11:40

Take your tubing and curve it on the very bottom of the beaker, into the edge and about 120deg. of circumstance. Use a valve OR a clam to allow a small amount of pressure to escape. There is a "timing issue" here and if you open the valve up you get a whirlpool effect that is VERY gentle. Hard bubbles appear to be the problem; the idea is to make the movement very gentle and avoiding "hard aeration". Another technique I've sen is to point the air tube directly down into the flat bottom of the beaker & lighten up the pressure; this creates a "pebble-in-a-pond" effect which is very effective. The issue is generally TOO MUCH pressure rather than slight amounts. You just want to have the acid move about in a continuum.

If a magnetic unit is used (IMO) it's always best to use those tiny "capsule" sized ones as they just barely move the acid in a gentile swirl (the same as air if reduced in pressure, etc).

maxidastier - 2-2-2011 at 04:51

Quote: Originally posted by Microtek  
I have always found that air agitation stripped off too much of the nitric, giving huge clouds of fumes. For this reason I have used swirling or magnetic stirring. If anyone has a method that reduces stripping, I'd like to hear it.


Yes, but bubbling dry air through it can help to convert red fuming HNO3 into white fuming, doesn't it

4 NO2 + O2 + 2 H2O ---> 4 HNO3

MetalNeko - 10-5-2011 at 18:55

Hi, all! This is my first post - although I would like to point out that I've been reading the forums for four to five years and I've nitrated a handful of different nitric esters as well as some other things along with pyrotechnics. I haven't done much in the past two years in regards to chemistry, but I've sort of picked up the hobby again.

----end introduction!---

Alright, I'll make this short and sweet: I nitrated some glycerol/glycerin recently using pure NH4NO3 and Clear Line drain opener (which I believe is around 97% H2SO4). The nitration, crashing and neutralization all went swimmingly and I'm left with a nice little vial sample of the batch. Here's a photo of it:

[img]http://i176.photobucket.com/albums/w185/devaughn357/NG.jpg?t=1305082383[/img]

In case you cannot view the photo, the nitro is an off-white color, mostly translucent.

I'm posting to ask if anyone knows if those little bubbles are a problem? Thanks in advance.


[Edited on 11-5-2011 by MetalNeko]

hissingnoise - 11-5-2011 at 02:35

Couldn't find the picture, but if bubbles are visible in your nitro then neutralisation isn't complete!
If you're talking about a slight milkiness - that's normal.
The milkiness of freshly prepared nitro is caused by a small quantity of entrained water and it disappears in a few days by evaporation . . .


MetalNeko - 11-5-2011 at 08:20

I crashed in 10 gallons of water, added an icecream container of sodium bicarb water, let it sit for a few days, sucked up the NG with a syringe, then flushed the container it was in with about 6x the amount of water.

I placed some sodium bicarbonate solution directly into a little drop of NG and observed no reaction, Hmm, is it possible for it to bubble like this from being too basic?

hissingnoise - 11-5-2011 at 10:06

10 gal seems excessive unless you're doing litre batches . . .
And letting nitro simply sit in water isn't sufficient for washing!
All of the interior of the nitro must be exposed to the washwater by gently swirling it around the bottom of the container for several minutes.
I'd rewash it in ~10 times its volume of cool water . . .


My two cents...

albqbrian - 26-5-2011 at 23:37

I've just got on this site and it's been eye opening. I'll confess up front; I haven't made NG nor do I plan on it. But there are some obvious safety things I feel need mentioning.

I have some background in the area: pyro as kid, college chem deg, lots of work in orgo syn & biochem labs, taught explosive use in military, made hundreds of pounds of composite rocket fuel as a recent hobby, and I lived long enough to have mainly gray hair. I don't want to start out my career here as an a**hole, but jesus...

Most of you are scary cavalier about this stuff! You're making something where a few ml can permanently f**k you up. And you're using stump remover? You're worrying about when you're glass rod hits the side of the reaction vessel? Where is any mention of shielding/armor? Of remote control ops (the air bubble thing certainly sounded like a minimum precaution), etc.

You want to make NG? OK. But let's be clear. In the US anyway you are seriously breaking the law. No if, ands, or buts. Everyone has to make their own risk/reward calculations here, but be very cognizant of this. You don't want the ATF on your ass. Ask Randy Weaver or those two dozen kids burned alive in Waco. But that's who does explosive stuff in US LE. You're making NG? You'd better have a serious plan.

Any serious experiment, or cooking for that matter; requires the best ingredients. You need high quality NA? Then buy it (hard granted) or distill it. If you can't successfully distill NA I'd say you shouldn't be making NG. What sort of shield is between you and the reaction vessel? A bit of NG in a small glass container won't need much, but it needs something. If you're smart enough to make NG aren't you smart enough to find a way to turn/shake your reaction vessel without holding it in your hand?? Wow, holding something glass in my hand while it has a dangerous quantity of HE and who knows what impurities. Is that about right? Shiver. What about your dry runs? With colored water or whatever standing in for the chems while you do all the tasks required of your synthesis. I'd do that at least a couple of times. No way you'll do a complex task exactly correctly the 1st time. If you need a simple example to convince you; go pick out an unfamiliar recipe (for food) and make it. You'll see.

OK, I'll stop now. I found this thread to be very educational. Certainly as a life long pyro I've always wondered about the nuts and bolts of making NG. I've learned a lot. But I strongly feel that what I said needed saying. If you want to boot me from here; I'll understand.

In the future I'll post some positive stuff. I don't want you to think I'm just some nasty old a**hole :)


hissingnoise - 27-5-2011 at 01:47

Quote:
Wow, holding something glass in my hand while it has a dangerous quantity of HE and who knows what impurities. Is that about right? Shiver.

You've spent time in the army, blowing shit up, and you're this overly paranoid about a substance that has been produced in tonnage quantities since Nobel's day?
Are you, perhaps, taking the 'Hollywood model' at little too literally?



HN...

albqbrian - 27-5-2011 at 07:17

I don't want get into a pi**ing contest here. But you can't equate industrial production with the methods being discussed here. That's not what this thread is about. It's about one person, most likely at home, by hand, making a somewhat sensitive HE.

What just jumped out at me was the lack of a big picture, process perspective. The checklist, the practice runs, another person who can save you if something bad happens, etc. All I saw was is this pure enough, how much of that ingredient. Those things are important; but you need an overall plan to successfully get you to your objective.

In the Army using explosives was pretty regimented; not always, but mostly. And if you had to do something dangerous; one person did it; while a rescue crew waited nearby.

I'll leave this topic be now. Thanks for listening.

hissingnoise - 27-5-2011 at 10:15

I wasn't having a go at you albqbrian, but there are tried syntheses of more sensitive and dangerous compounds than nitro on the board . . .
Nitro certainly commands respect but once the synthesis is known any careful amateur can prepare it without incident.
I'd recommend a reading of COPAE; "The Chemistry of Powder and Explosives" by T.L. Davis - it's in the site library.



quicksilver - 27-5-2011 at 13:38

Gentlemen please take a moment and realize that you're closer in your manner of thinking than it may superficially seem.

All too often the printed word cannot convey the undertones that body-language and facial expressions do.

That being said; an individual considering experimenting with nitric esters who does not do substantial background study is obviously opening themselves up to a serious set of problems. [Baker 1909 US patent] siting the stability-longevity of glycerin when compared to glycol; the choice is obvious. I believe it was the Nitro-Nobel Corp. offices maintain an original sample which they periodically test and neutralize; yet glycols have met shelf life stability of decades.
Polyester+ stabilizer pelletized NG in firearm's propellants have (in some cases) maintained stability for close to 100 yrs.
However the common testing batch sizes used by the USBoM maintained at or below 40gr as a standard. Controlling acidity and related issues of stability in sizes measured in grams is common & achievable.

I was going to set legal issues aside; however there are (written into law) levels of experimental unit sizes of energetic materials that can and do amount to common research and are not infractions of US Federal law. The popular "Orange Book" is very old at this point & cannot be depended upon for clarification of Federal statutes in this regard. However they may be infractions of State law & the best thing is to do one's legal research before anything chemical.
Realistically, there is a difference between "kitchen chemistry" and graduate and post-doc research in energetics. It's not my place to second-guess what any other individual is doing with physical materials. While any "picture' could just as easily be table salt or mineral oil, any discussions can be confabulation; I prefer to not assume anything & realize that our dialogs are a 1st Amendment Right and NOT aimed at the "practical implementation" of energetic materials application. This is NOT the E&W forum.

hissingnoise - 28-5-2011 at 02:10

Apropos of nothing in particular, a dark question I've asked myself more than once is; if when holding a beaker containing, say, nitro, an unscheduled detonation occurred, would it be preferable that the batch would be the usual quantity, a quantity which would have the energy to pretty well fuck me up physically for the remainder of my life, or should there be 'enough', the concussion of which would take me out - instantly . . .
I'm fairly certain this 'uncomfortable' question lurks in the recesses of the minds of a few other people interested in HEs, posting here!

[edit] I seem to remember Sidney Alford once saying; "Think of the hospital bills you'd save" . . .




[Edited on 28-5-2011 by hissingnoise]

quicksilver - 28-5-2011 at 05:15

That IS pretty dark.

Reminds me of a WWII concept wherein the Allies were using booby-traps in field telephone made from one (single) blasting cap in the ear-piece of the phone. Result was generally instantly lethal due to placement.
It's a lot like realty and home sales...."Location, location, location".

hissingnoise - 28-5-2011 at 06:46

And the Wehrmacht, of course, weren't exactly slouches when it came to thinking up methods to produce this type of nasty little, er, 'surprise'!


nitromethano - 30-9-2011 at 14:35

Hi, I'm new to the forum, I had all kinds of explosives usually high order for about 5 years, I'm from Argentina, do not speak good English, so I use a translator, I hope you understand.

My concern is: I always spoil nitroglycerin, in a short time. My NG fresh, is translucent, practically colorless (very similar to EGDN), its sencibilidad is correct, its viscosity, and pH.

After completing the chemical reaction, wash it 5 times, with big quantity, solution of sodium bicarbonate (2 liters of saturated solution of bicarbonate to 20 ml of NG). Then dried.
In this NG, is translucent, colorless, with a faint odor, slightly oily, and is supposed to be neutral. PURE NG
After a month, begins to turn yellow-green, as the weeks go more green, at 3 months and is green with some small bubbles.
As the months pass, it becomes dark green and some small crystals are formed on the shore.
After a year and some months, take this photo, where liquid is transparent, with jelly crystals. ¡¡¡¿¿??!!!

[Edited on 30-9-2011 by nitromethano]

[Edited on 30-9-2011 by nitromethano]

ng.JPG - 127kB

[Edited on 30-9-2011 by nitromethano]

bonelesss - 30-9-2011 at 15:27

I am a bit confused why You store such a volatile explosive so long period? Are You making some kind of test? I would not even stand near that.

hissingnoise - 1-10-2011 at 02:47

Quote:
My concern is: I always spoil nitroglycerin, in a short time.

For starters, the neutralising wash should contain no more than a few per cent bicarbonate and and all traces of the salt should be washed from NGl by two or three further clean-water washes!
Properly stored, purified NGl should remain unchanged indefinitely . . .


quicksilver - 1-10-2011 at 09:51

Hay muchas cosas que son muy imporante!
* - Sabía usted tome una lectura de pH después de neualization?
* - El "lavado de carbonato" se debe a totalmente en la solución por lo tanto, sólo necesita una pequeña cantidad de "carbonato" a un mayor volumen de agua.

Usted debe leer litererature de la ciencia antes de hacer esto para que sepa de todas las técnicas de laboratorio apropiadas y peligros. Muchas personas se han visto afectados por no leer lo suficiente la calidad de la ciencia (the chemistry) libros sobre explosivos. Almacenamiento no es una buena idea para el "nitric ester". There are different tipos o "diseños de productos químicos (de explosivo). And they have different "REQUISITOS" (sp?) in the storage. First you must understand those requirements.
Obtener el libro de "Química de la Pólvora y Explosivos", escrito por "Tenny Davis". Sí, es en Inglés, pero se puede traducir y la síntesis de explosivos de la ciencia - no solo la discusión. It is free: you can download it here in the "Los Alamos" book section at the start of the Forum.

Esto es muy peligroso. Hacer sus preguntas en español, está bien. Pero LEER y estudiar los libros de ciencia alidad. Usted recibirá respuestas sólidas aquí, pero cualquiera puede cometer un error Y con este tema, esta actividad, un error y usted perderá sus ojos y manos.



[Edited on 1-10-2011 by quicksilver]

hissingnoise - 2-10-2011 at 04:10

Looks interesting, but I'm too old to start learning Spanish . . . any chance of a translation, QS?



quicksilver - 2-10-2011 at 06:20

Of course.
I asked if he had tested his pH ( at his point of completion of neutralization - so that he knew from the outset that it had moved from being acidic.)
I mentioned (as you did) that a small amount of anti-acid [properly in solution] was the best way to create a means of dealing w/ acidic nitric esters.
I attempted to communicate the requirements (requisitos - I'm not sure if that's the correct spelling) of nitric esters in shelf life

Then I addressed the importance of obtaining source material and pitched Davis' book. And that - although it was in English he could work with it just as he was dealing with the language issue here (& elsewhere) bit by bit. I also mentioned cautionary elements (especially with esters) and how it's all to easy to loose your eyes and hands. Basically, I reiterated the need to "READ" before proceeding with energetic chemistry; to study the science of chemistry. That's about it.



It's been my belief that many people naturally believe that the more experience; the greater the learning. We know that in this agenda it's potentially a serious danger to use experience as a guide alone without a background of prior study: more toward lab technique, safety issues, & potential "red flags" in a synthesis. I also think it's natural to some degree for an individual to assume that reading about a subject is less instructive than actively engaging in it. Some people especially with natural analytic, athletic or mechanical backgrounds often enjoy an active engagement in a subject. Some may believe that reading about it is somewhat "arm-chair experience" & wouldn't apply the same to other hobbies or areas of interest. Many, if not most people like a "hands-on" approach. But in this area it could end up being a hands off tragedy.
I push Davis' book a lot because it's available, proven, & easily understood. It also has well understood sections that could be translated with little problem. One difficulty with some of the more expensive & in-depth texts are that they are scanned as a graphic. That does not allow a "cut & paste" to use in Google's translator or a non-English dictionary conversion program.

hissingnoise - 3-10-2011 at 04:56

Quote:
Basically, I reiterated the need to "READ" before proceeding with energetic chemistry; to study the science of chemistry. That's about it.

Thanks QS --- yes the 'need to read' would seem to be self-evident but apparently it isn't clear to all.
Let's just hope he takes the message on board while he's still in one piece . . .



Ral123 - 9-2-2012 at 13:18

I haven't made NG and I'm kinda wandering would I ever http://www.youtube.com/watch?v=5tlvDTPxwEY&feature=relat...

quicksilver - 9-2-2012 at 14:24

Utube is great for getting guitar lessons.....but that was enough NG to tear the upper part of the individual's body apart. The best favor anyone could do is leave the videos alone for information regarding a subject such as that. Nitric esters need to be totally acid free and in many instances, re-evaluated for spoilage. In many instances a stabilizer could provide some help or warnings (diphenylamine turning blue in response to nitrus, etc) but purity in synthesis is not a kitchen chemistry issue.
If I am correct some of the original nitroglycerin on display at Dynamit-Nobel is periodically checked for purity. many esters have long shelf lives but a great deal of knowledge and research was put into that agenda. Putting 250ml+ in a screw top jar is not a good sign for longevity.....

Ral123 - 9-2-2012 at 15:19

That is NG. And I'm supposed to handle such a thing in a beaker till I wash it? How you guys do it? I feel stupid for being afraid of nicely washed, neutralised egdn at home.

quicksilver - 10-2-2012 at 08:44

First of all a mid-size jar of NG open on a table would give a new user a nitro headache he would not soon forget. That generally needs to be remembered as the adrenaline rises and your head is pounding....And one of the reasons to work with a tiny amount as well. But there are methods.....
Once NG is synthesized many people retain it under water that has been deeply saturated with common salt (Na or KClO2) and an anti-acid such as Calcium Carbonate or even baking soda. This is a simple method of drying the NG and freeing it from any remaining acids. The introduction of water ALSO keeps the head-ache factor at bay. Nitro head-aches can be very nasty and can disturb concentration. After about 3-5days of working with nitro (glycerin or glycol) the body gets "used to" the extreme vaso-dilation and the headaches go away. In fact some people have a strange reaction AFTER they have worked with NG for a long period and get head-aches once again when the NG is REMOVED!

NG can be a serious toxin for some and the proper protective gear should be worn at all times when working with NG. notice in the uTube video the young person had nothing to protect himself from a glass jar of about 250ml+ of nitro. If that blows up the wave would most likely kill him outright. but if he had some distance the room would be filled with a great deal of fast moving projectiles. NG is still one of the "kings" of seriously powerful explosives: substantially faster than TNT, TNP, most all primaries, etc.

NG is difficult to contain as a screw-top jar is really a stupid place to store it. Anything with friction or grinding is to be avoided. That was one of the basic reasons why dynamite was developed. If one MUST work with liquid NG, keep the levels low (in the single gram(s) level) & don't use glass if you don't have to.Many stores with perfume have sample bottles that contain about one gram and have a polymer seal top. This may be coated with wax on the top contact of the polymer top and lower friction to a moderate level. A single gram may still have the strength to knock a finger off but you would live if something unfortunate occurred.

AND -=DON'T=- FEEL STUPID about being apprehensive over potentially dangerous materials. Trepidation, anxiety, fear, and apprehension are emotions we have that provide self preservation. Poisonous snakes are often handled with a snake-stick for a REASON - and the finest Herpetologists in the world don't let their samples slither around their homes. We have these emotions for a damn good reason.

Edit:

Nauom wrote some of the best materials you can get for exploring some testing - Book was titled "Nitroglycerin & Nitroglycerin Explosives". Old but interesting and a fast read. Modern dynamites however (when used) generally use glycol - less sensitive but the headache is fairly serious. Many nitric ester are now used for heart conditions, even PETN.

[Edited on 10-2-2012 by quicksilver]

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