Sciencemadness Discussion Board - Short question / quick answer - Thread

Exist ( in some patent ) mixture NH4 NO3 + Al + water + guar gum + microballoons. It is watergel plastic explosive. Requiring booster, of course. And working only in bigger diameter, 70 mm and +. It is stabile with any stabilisator. Dr.

[Edited on 28-7-2016 by Laboratory of Liptakov]

I'm going to try something similar, with an hydrosoluble fuel (like urea or hexamine) instead of Al. When enough water is removed, you get a hard and castable explosive.

MineMan - 9-8-2016 at 10:05

Quote: Originally posted by kratomiter

I'm going to try something similar, with an hydrosoluble fuel (like urea or hexamine) instead of Al. When enough water is removed, you get a hard and castable explosive.

Ok, but please report back to us...on how this works, I would keep the Al though...

kratomiter - 9-8-2016 at 15:14

Quote: Originally posted by kratomiter

I'm going to try something similar, with an hydrosoluble fuel (like urea or hexamine) instead of Al. When enough water is removed, you get a hard and castable explosive.

Ok, but please report back to us...on how this works, I would keep the Al though...

Sadly I only got Magnalium, not pure Al. And Magnesium + water + oxidiser is a bad mix.

Bert - 9-8-2016 at 18:12

Can anyone point to a published velocity of detonation figure for a 70:1 nitromethane:hexamine solution as described here...

http://www.google.com/patents/US9175933

HMTD help

Isaacdude - 10-8-2016 at 09:09

Hi, would laundry detergent (Vanish) with hydrogen peroxide in it work for making HMTD? It says 5-15% hydrogen peroxide on the label, but I tried to make HMTD with HCl, and even after 48 hours no crystals formed. Does the detergent have something that prevents HMTD formation? Or should I use citric acid?

PHILOU Zrealone - 10-8-2016 at 09:32

Quote: Originally posted by Bert

Can anyone point to a published velocity of detonation figure for a 70:1 nitromethane:hexamine solution as described here...

http://www.google.com/patents/US9175933

Maybe take a look into the related patents...I couldn't download the pdf from your link so I went to the FPO website...
US9175933 via Free Patents Online
The related patents are a little below into the link.

The VOD should be essentially that of NM --> 6200-6400 m/s

[Edited on 11-8-2016 by PHILOU Zrealone]

Laboratory of Liptakov - 10-8-2016 at 10:17

Well, was be tested before month. Many variants, temperatures, ratios, purification etc. Not worked it. Detergent is reactive with acid, because he is Ph as NH4. And neutralize an acid. It is together very dirty impossible reaction. Dr.

Lotilko - 10-8-2016 at 11:13

I would abandon organic peroxides if I were you, I know it might seem as the best choice for an amateur, but please. A friend of mine had an accident where 30 grams of HMTD and about 200 mililiters of MEKP went off. Needless to say, he was lucky that he wasn't near. He said that the closet exploded with great violence and he could feel the shock wave 60 meters away. Try mercury fluminate if you are looking for a simple primary. Then move onto more complex ones.

Detonating the undetonable ANFO

Tricka90 - 14-8-2016 at 02:53

Did anyone manage to detonate ANFO?
I tried detonating 100 grams confined ANFO with a homemade cap filled with over one gram of Silver Acetylide but it didn't detonate. Should I try with two grams Silver Acetylide or more? Or I should just use a boost charge in the detonator cap such as Picric Acid or any other easier to detonate secondary?
Thanks to everyone will give me a suggestion.

hissingnoise - 14-8-2016 at 05:06

Most people would just google it ─ it cost me 10 seconds and 2 clicks?

MineMan - 14-8-2016 at 11:47

ANFO is cap sensitive when it is crushed, is yours? Also did you use 6% diesel? Add 2%-5% Al powder... that will help. Unfortunately SADS has a low VOD...

One gram of SADS, what are your yields, that would cost me about 2 grams of silver nitrate?

Picric Acid Sensitivity

Tricka90 - 14-8-2016 at 14:02

I'm currently studying picric acid synthesis and properties. Unfortunately there's not much information available online, expecially about its sensitivity. Do you have any direct experience with picric acid that you would like to share? Or can you suggest any informative resource (books, files, videos etc) which covers the proper and safe handling of picric acid and maybe some sensitivity test? I know it to be one of the safest secondary (excluding ammonium nitrate based explosives) but I'm trying to figure out how much safe it really can be (I know it's also very toxic) .
Thank you, have a nice summer.

[Edited on 14-8-2016 by Tricka90]

Nitrocellulose propellant

cryomancer - 14-8-2016 at 14:52

I have been wondering for a while if NC is plausible as a propellant for large objects like fireworks shells etc. but if you confine NC doesn't it explode?

Yet i think that i have heard that NC is used in a ring shaped format to be used as a booster charge in the 60mm and 81mm mortars that the military operates. Is this true and if not then could someone figure out what those rings are as my internet searches have come up dry so far.

Thanks, CM

zwt - 14-8-2016 at 15:04

Quote: Originally posted by careysub

The Disney Corporation uses nitrocellulose-based fireworks for their (thrice nightly) shows to drastically reduce air pollution from them.

Homeowners around Disneyland (who bought their homes there decades after the park opened and started the shows) have on occasion filed complaints and/or lawsuits against Disney for air pollution, but the Air Quality Management District has run tests and found that Disney's new fireworks don't pollute the air.

The cleaner burning compositions give better colors too with lower amounts of metals.

That thread was posted to just last week. I suggest practicing your Google-fu.

[Edited on 14-8-2016 by zwt]

NeonPulse - 14-8-2016 at 17:23

There is a massive thread or two here on picric acid. You would find it to be less sensitive than you may think. It takes quite a kick to set it off. I'm not sure how much of a search you have done but in the forums library here you should check out a book The chemistry of powder and explosives by Tenney Davis or the 4 urbanski volumes. These books have a load of info on picric acid and other compounds. the books are free here in the SM library.

Tricka90 - 15-8-2016 at 04:21

There is a massive thread or two here on picric acid. You would find it to be less sensitive than you may think. It takes quite a kick to set it off. I'm not sure how much of a search you have done but in the forums library here you should check out a book The chemistry of powder and explosives by Tenney Davis or the 4 urbanski volumes. These books have a load of info on picric acid and other compounds. the books are free here in the SM library.

Thanks a lot for the advice, I downloaded the books you suggested and they definitely provide tons of informations about Picric Acid! However I just can't find the threads on the forum using Search function, can you please give me the links?

Tricka90 - 15-8-2016 at 04:24

ANFO is cap sensitive when it is crushed, is yours? Also did you use 6% diesel? Add 2%-5% Al powder... that will help. Unfortunately SADS has a low VOD...

One gram of SADS, what are your yields, that would cost me about 2 grams of silver nitrate?

Thank you for the suggestion, I didn't know that using Al powder would make ANFO more sensitive. Maybe it's just that I don't know much about ANFO properties and proper use yet, do you know any good source of information (maybe a good book) about ANFO?

Bert - 15-8-2016 at 07:27

Quote:

Maybe it's just that I don't know much about ANFO properties and proper use yet, do you know any good source of information (maybe a good book) about ANFO

There is a WONDERFUL source on this!
http://bfy.tw/7Dyd

Bert - 15-8-2016 at 07:58

Yes, that WAS snarky.

The last 3 threads from EM which I merged to "quick question, short answer" were all from a brand new user name, who immediately started new threads in EM on VERY heavily previously discussed subjects, without doing the bare minimum of research on their own. And they are making hash of legit short questions.

Sorry, if you do not show sources/links to how you came up with your information on whatever topic led to your question-

Or show credible lab notes documenting a procedure you claim to have performed and have questions about/want feedback on, with stoichiometry, source of information you started from, your own calculations, photos, video, etc.-

This type of zero effort thread will now be sent straight to beginnings, or detritus.

PHILOU Zrealone - 15-8-2016 at 08:34

Hint ... picric acid is also called TNP or 2,4,6-trinitrophenol.

James Ikanov - 16-8-2016 at 11:22

Does anyone know of a viable way to, on the small scale, compress gasses, for example for a CO2 cylinder? I have interest in pursuing an N2O based explosive (N2O is chhheeeeaaaappp and unrestricted) but I cannot seem to devise a reliable way to keep it under pressure in the presence of a fuel. Whipped cream cartridges seem like a viable jumping off point, as do beer keg charging systems, but I can't find much by way of a container that could hold up the pressures required and still intake the material. I have a bit of an understanding of pressure vessels but nothing leaps out to me as a good candidate for the purpose of condensing N2O.

I also considered liquefying the N2O into a liquid before hand but dry ice falls just short of being able to keep it liquid. I think a strong coolant might assist in keep in condensed while piping it or pouring it through a cooled funnel but that seems more like an afterthought. I suppose an alternative would be to find a method to cool below the melting point but that seems like it might take special equipment.

Astrolite G

MineMan - 16-8-2016 at 12:46

Is Astrolite G legit...? I just don't see how hydrazine could raise the VOD of AN more than NM...?

PHILOU Zrealone - 16-8-2016 at 13:00

Is Astrolite G legit...? I just don't see how hydrazine could raise the VOD of AN more than NM...?

NH4NO3(s) + N2H4(l) <==> N2H5NO3(s) + NH3(g)
Thus equilibrium reaction...

Hydrazine nitrate is more sensitive to shock and displays a VOD of 8900 m/s at max density vs the poor 3500 m/s of ammonium nitrate!

Dornier 335A - 16-8-2016 at 13:16

If you want VoD, hydrogen is the way to go. Basically, water increases the explosive gamma (adiabatic index) which gives a higher VoD for a given detonation pressure. Hydrogen rich explosives like hydrazine nitrate, hydrazine nitrate/hydrazine mixtures etc. have considerably higher VoD at a given density than say PETN or RDX.

For example:
21/79 Hydrazine/Hydrazine Nitrate
Density: 1.44 g/cm³
VoD: 8600 m/s (Mader)
Compared to:
RDX
Density: 1.46 g/cm³
VoD: 7600 m/s (Hobbs and Baer)

Even octanitrocubane at 1.44 g/cm³ reaches only 7990 m/s according to my calculations. So hydrogen is quite good!

MineMan - 16-8-2016 at 13:17

Ahh...

Why don't I see anyone using this compound... especially if it is a binary explosive and no synthesis is required....

I am guessing because of the toxicity of Hydrazine?

PHILOU Zrealone - 16-8-2016 at 15:31

You need dry N2H4 what is dangerous because flamable, volatile, endothermic, toxic, corrosive (to glass and to some metals what favourize decomposition) and vapour is explosive in a very large % with air, it burns very hot.

Dry N2H4 is expensive and regulated.

Methanol in Ammonium Nitrate synthesis

Tricka90 - 16-8-2016 at 22:51

This is the procedure for synthesising Ammonium Nitrate found in The Preparatory Manual Of Explosives. As you can read, after reacting nitric acid with ammonia, it suggests to recristallize ammonium nitrate from methanol, but only if it is going to be alloyed with picric acid or similar. In other synthesis procedures I've found, ammonium nitrate is made just by reacting nitric acid with ammonia, without the methanol recrystallization at the end. In others ethanol is used instead of methanol. Do you know what exactly methanol/ethanol should do? I'm wondering if maybe is used to remove any substance which can react with picric acid, producing unstable products, or to dilute any impurity found in commercial ammonia.

[Edited on 17-8-2016 by Tricka90]

ecos - 17-8-2016 at 00:36

maybe this can help : http://pubs.acs.org/doi/pdf/10.1021/ie50459a028

NeonPulse - 22-8-2016 at 17:31

A couple of days ago me and a friend were talking and he had this idea that the energy released from a bit of exploding potassium or sodium would be enough to set off ETN or another sensitive explosive. I thought it sounded crazy but after watching some videos on the tube of alkali metals exploding and seeing how they can break glass and blow water into the air it really does look like it is a plausible idea. I'm not really keen to attempt such a dangerous stunt so it is purely theoretical. So what do you think? Maybe a gram of ETN wrapped in 1 layer of foil wrap with 1g of Na metal taped to it tightly with metal exposed, and throwing it into a puddle. Would the ETN explode? If not from the shock or the metal exploding but maybe the heat of the metal reacting with water?

Laboratory of Liptakov - 23-8-2016 at 07:35

If heating 10 grams Pb(NO3)2 on 300 - 400 C arises this compounds: 6,74g PbO + 2,78g NO2 + 0,04g O2. It is theory. Question: If will be both gases (after cooling) Introducing into ice water, for example 5 Celsius: Arises HNO3 ? The attempts show that yes. It is fact, was try it, and worked. Weak acid, but yes. Is in this method some problem? I am asking therefore, that Lead nitrate is possible easy prepare from NH4NO3 + Pb. A huge amount during 2 hours. Will be described later.
But I am curios not for lead nitrate, but on preparation HNO3. Thanks... :cool:

....Dr.

kratomiter - 23-8-2016 at 08:56

A couple of days ago me and a friend were talking and he had this idea that the energy released from a bit of exploding potassium or sodium would be enough to set off ETN or another sensitive explosive. I thought it sounded crazy but after watching some videos on the tube of alkali metals exploding and seeing how they can break glass and blow water into the air it really does look like it is a plausible idea. I'm not really keen to attempt such a dangerous stunt so it is purely theoretical. So what do you think? Maybe a gram of ETN wrapped in 1 layer of foil wrap with 1g of Na metal taped to it tightly with metal exposed, and throwing it into a puddle. Would the ETN explode? If not from the shock or the metal exploding but maybe the heat of the metal reacting with water?

Na or K in contact with chloroform detonates, see COPAE page 403: there's an improvised shock-sensitive device made this way.

PHILOU Zrealone - 23-8-2016 at 09:01

If heating 10 grams Pb(NO3)2 on 300 - 400 C arises this compounds: 6,74g PbO + 2,78g NO2 + 0,04g O2. It is theory. Question: If will be both gases (after cooling) Introducing into ice water, for example 5 Celsius: Arises HNO3 ? The attempts show that yes. It is fact, was try it, and worked. Weak acid, but yes. Is in this method some problem? I am asking therefore, that Lead nitrate is possible easy prepare from NH4NO3 + Pb. A huge amount during 2 hours. Will be described later.
But I am curios not for lead nitrate, but on preparation HNO3. Thanks... :cool:

....Dr.

Process is known for lab production of NO2 and NxOy from heavy metals nitrates.

What would be more interesting instead of Pb metal use ...would be to recycle the PbO with NH4NO3 to get NH3 + H2O (on one side) and Pb(NO3)2 (on the other) to produce PbO and NO2,O2, NxOy...then HNO3 and HNO2.

PbO + 2NH4NO3 -heat-> Pb(NO3)2 + 2NH3(g) + H2O(l)
Pb(NO3)2 -heat-> PbO + NO2(g) + NxOy(g)
NO2 (g) + NxOy(g) -H2O-> HONO2 + HONO
2 HONO <--==> N2O3(g) + H2O

PbO will react easier with NH4NO3 than Pb...

Same could be done with Cu(NO3)2 but the recycling may pose problem...heating CuO and NH4NO3 is like heating TAC(u)N (Cu(NH3)4(NO3)2...
So better avoid metals that complexate NH3...

[Edited on 23-8-2016 by PHILOU Zrealone]

PHILOU Zrealone - 23-8-2016 at 09:12

The Na or K could be reactive enough to decompose the ETN...with a lot of heat and maybe fire...so explosion may result...yes.
But this would be unpractical, dangerous, uneconomical and a big waste of valuable Na or K.

HNO3

Laboratory of Liptakov - 23-8-2016 at 09:32

Thanks, for flash answer. However it is work with poisons. Therefore will be this type preparation HNO3 examined later. As last event. Best thing, is recyclation PbO and NH4NO3. In this time, is all only on theoretical level. I am looking for in patents this type preparation HNO3, but nothing find. Again thanks... :cool:

...Dr.

nux vomica - 24-8-2016 at 15:55

Thanks, for flash answer. However it is work with poisons. Therefore will be this type preparation HNO3 examined later. As last event. Best thing, is recyclation PbO and NH4NO3. In this time, is all only on theoretical level. I am looking for in patents this type preparation HNO3, but nothing find. Again thanks... :cool:

...Dr.

I dont know if this is of any use liptakov, i pulled this out of a old 1860,s book i was reading on google books but i cant remember witch one it was

anyway they are useing sodium nitrate and boracic acid heated together to produce nitric acid .

By the patent process of M. Mallet, dried nitrate of soda is decomposed by dried or monohydrated boracic acid, by heating the two together. The products are liquid nitric acid, which distils over, and biborate of soda (borax), which remains in the retort. The crude coloured nitric acid of commerce (aquafortis) was originally prepared by distilling a mixture of nitre and copperas, and is still sometimes obtained in this way.

Cheers nux.

HNO3

Laboratory of Liptakov - 25-8-2016 at 01:19

Thanks Nuxy, interesting method. Good note for all. ... :cool:

...LL

PHILOU Zrealone - 25-8-2016 at 06:46

Maybe helping with the old chemical names like nitre and copperas old-common-chemical-name

Bert - 25-8-2016 at 11:22

Quote:

i pulled this out of a old 1860,s book i was reading on google books but i cant remember witch one it was

Now THAT is of some interest... As in USA, sodium nitrate is available for meat curing, fertilizer and other uses OTC, with boric acid (boracic acid is an old fasioned name) being available at any hardware store and/or drug store.

One might assume that using anhydrous or nearly so chemicals could produce a fuming, possibly darn near anhdrous nitric acid?

Checking heats of fusion, and solubility of the residual borax left in one's distilling flask...

(Edit)

Boric acid, MP 179 C.

Sodium nitrate, MP 308 C.

Borax decahydrate would be the easily soluble form of borax, apparently anhydrous borax (as this residue would be) is only very slowly soluble in comparison. But probably still do-able, if one was not in a great hurry to use the retort again.

One could assume the reaction to begin at the MP of boric acid? A shot bath or sand bath for heating and ordinary pyrex glassware could do for the aparatus.

One potential issue with the use of glass aparatus might be the well known fluxing action of borax in a glass melt?

This calls for a quick experiment.

[Edited on 25-8-2016 by Bert]

[Edited on 25-8-2016 by Bert]

nux vomica - 25-8-2016 at 16:55

Quote: Originally posted by Bert

Quote:

i pulled this out of a old 1860,s book i was reading on google books but i cant remember witch one it was :( anyway they are useing sodium nitrate and boracic acid heated together to produce nitric acid .

By the patent process of M. Mallet, dried nitrate of soda is decomposed by dried or monohydrated boracic acid, by heating the two together. The products are liquid nitric acid, which distils over, and biborate of soda (borax), which remains in the retort.

Hmm i have boric acid and sodium nitrate at home i wonder if you mix the reactants in equal molar amounts or need a excess of one, as usual these old science books are a bit vague on detail..
They also mention earthen ware retorts and cast iron retorts in other parts of the book if i remember right .
I might mix and heat some of the chems up in a test tube to see if something happens and what the borax does to the glass tube.

(Edit)
I had a small scale test of heating boric acid and sodium nitrate together in a test tube there was a vapor condencing on the test tube walls and also red fumes comeing off when i heated the tube strongly, ph test paper held in the vapors went red as well so acid fumes are being generated.

I looked for the book with the text i copyed but i havent found it yet but i did find some informaton from a book that was published in 1830 its called the chemistry of the arts by Arthur t Porter and this is what the book says about aqua fortis .

Aqua Fortis. To obtain the common nitric acid called aquafortis, equal parts of well purified nitre and copperas, or green vitriol, are taken. The nitre is dried, and the vitriol is calcined to red ness. These two substances are well mixed together. The mixture is then put into an earthen retort, or an iron pot, with a stone-ware head, of such a size that they may be but half full. The retort, if used, is set in a reverberating furnace, and in either case, a large glass receiver, having a small hole in its body, stopped with a little lute, or a safety-pipe, is ap plied. This receiver is luted to the retort with the fat lute, and the joint covered with a slip of canvass, smeared with lute made of quicklime and the white of an egg. The vessels are heated gradually; the receiver is soon filled with very dense red vapours. In order that the redundant vapours may be let out, the small hole in the receiver must be opened from time to time. Towards the end of the operation, the fire must be raised so that the ves sel is made red. When it is found, even if the retort be red hot, that nothing more comes over, the vessels are left to cool, and the receiver is unluted, and, without delay, the liquor it contains is poured into a bottle. This liquor, being nitrous acid, is of a reddish-yellow colour, smokes exceedingly, and the bottle containing it is constantly filled with red fumes, like those observed in the distillation. By this process a very strong and smoking spirit of nitre is obtained. If the precautions of drying the nitre, and calcining the vitriol, be neglected, the acid that comes over, greedily at tracting the water contained in these salts, will be very aqueous, will not smoke, and will be almost colourless with a very slight tinge of yellow, and is sold by the name of single aqua fortis. The fumes of highly concentrated nitrous acid, such as that obtained by the above process, are corrosive, and very dangerous to the lungs.

[Edited on 26-8-2016 by nux vomica]

nux vomica - 26-8-2016 at 22:04

I just gave the synthesis a go but on a small scale i used equal molar amounts of reactents..

Then ran my new heating mantle flat out the first droplets formed in 10 minutes .

After reaction was over.

The final result was just over 3mls of fuming nitric acid there was more droplets in the condencer but they were too hard to recover.

The acid in a beaker reacting with copper.

It looks like this method works but not wanting to heat my flask with a flame i dont know if yields would be higher with more heat.
Cheers nux

[Edited on 27-8-2016 by nux vomica]

NeonPulse - 27-8-2016 at 18:28

Very interesting experiment there nux. Did you measure the density of the resulting liquid? Just curious to see the estimated concentration. Heating with a flame would probably not work the greatest due to decomposing the acid but very nice result of a method I haven't seen before.

Laboratory of Liptakov - 28-8-2016 at 00:14

Perfectly photos. Only 3 cm 3 HNO3 ? Thus 4 grams? From 8,4g KNO3 + 6,1 Boric a., I mean, a good attempt. ...
Without vacuum apparatus. Good result. Very easy method. Dr.

nux vomica - 28-8-2016 at 04:34

Very interesting experiment there nux. Did you measure the density of the resulting liquid? Just curious to see the estimated concentration. Heating with a flame would probably not work the greatest due to decomposing the acid but very nice result of a method I haven't seen before.

I didnt measure the acids density as i was a bit cocky and thought i would nitrate some homemade Pentaerythritol i made recently.
I got a small amount of petn when i diluted the mix at the end but i think the acid wont nitrate properly without sulfuric acid by the looks of things.
It also slightly eroded the bottom of the flask so i dont want to damage the flask anymore than it is so i won't try that reaction again.

nux vomica - 28-8-2016 at 04:38

Perfectly photos. Only 3 cm 3 HNO3 ? Thus 4 grams? From 8,4g KNO3 + 6,1 Boric a., I mean, a good attempt. ...
Without vacuum apparatus. Good result. Very easy method. Dr.

Yes not a great result but you can only give it a go.

PHILOU Zrealone - 28-8-2016 at 05:38

Quote: Originally posted by nux vomica

@ Nux Vomica, very nice OTC HNO3!
HNO3 for the crowd!

Strange that it eroded your flask...especially if you didn't overheated into a flame.
Normally NaNO3, HNO3 are inoffensive towards glass.
Maybe B(OH)3 (H3BO3) or borax are somehow integrating into the glass...borosilicate glass is known...but without strong heating (red heat) it seems strange.

For the rest if it is really a problem, one could use aluminium or iron since those are inert/passivated towards strong HNO3...but for iron, avoid contact with other metals (like copper) what may depassivate it instantly.

Adding a little water into the reactor may increase the yield of HNO3 recovery (of course of lower concentration) but for some applications very concentrated is not needed (like amine nitrate salts).

Increasing the amount of reactants will also increase the yield since a lot of drops are stuck into the retort.

Increasing the heat or vaccuum or the cold trap would also increase the yield.

Just two ideas! H3BO3 can be dehydrated to B2O3 above 300°C.
1°)So maybe that mixing intimately NaNO3 and B2O3 then subjected to strong heat and cold trapping (eventually under vaccuum) may lead directly to anhydrous nitric acid anhydride (N2O5)...
NaNO3 + B2O3 --> Na2B4O7 (or NaxByOz) + N2O5

2°)Alternatively if first doesn't work, at least:
B2O3 + HNO3 -heat-reflux below200°C-> N2O5 + H3BO3(s)
or
HNO3 (dil) + B2O3 -heat reflux-> HNO3 (conc) + H3BO3(s)
It should be a way to increase concentration maybe up to the anhydride...

H3BO3 should be insoluble crystaline into HNO3 and thus easily separated by filtration or decantation/pipeting!

[Edited on 28-8-2016 by PHILOU Zrealone]

PHILOU Zrealone - 28-8-2016 at 05:44

Perfectly photos. Only 3 cm 3 HNO3 ? Thus 4 grams? From 8,4g KNO3 + 6,1 Boric a., I mean, a good attempt. ...
Without vacuum apparatus. Good result. Very easy method. Dr.

That is not bad given the low quantity of material and maybe not optimum stoechiometry.
Theorically one could get 5,3g HNO3 from 8,4g KNO3 so 4g is nearly 80%...

PHILOU Zrealone - 28-8-2016 at 07:13

I have done the maths and worked out the stoechiometry:
2 NaNO₃ + 4 H₃BO₃ --> Na₂B₄O₇ + 2 HNO₃ + 5 H₂O

MM NaNO₃ = 85
MM H₃BO₃ = 62,8
MM Na₂B₄O₇ = 201,2
MM HNO₃ = 63
MM H₂O = 18

So from 170 gr dry NaNO₃ (sodium nitrate) mixed with 251,2 gr dry H₃BO₃ (boric acid); one should get:
201,2 gr of Na₂B₄O₇ (borax)
126 gr of HNO₃ (nitric acid)
90 gr of H₂O (water)

Since the water and the nitric acid will distillate under the process conditions (over 450°C borax initially decahydrated, becomes anhydrous), one should get 216 gr of 58,33% HNO3 solution.

Thus from 100 gr of initial mix (40.36% Na nitrate and 59.64% boric acid) one gets theorically 51.28 gr of nitric acid of 58.33% concentration.
From this information it is obvious that the trial of Nux Vomica misses quite some H₃BO₃ to get optimum yield...for 8,4 gr Na nitrate he should have used 12,41 gr boric acid instead of 6,1 gr...a double dose.

RECYCLING:
The beauty of this OTC process is that the boric acid can be recycled from borax and OTC-ish HCl (chlorhydric acid) or H₂SO₄ (sulfuric acid).
Na₂B₄O₇+ H₂SO₄ + 5 H₂O ----> 4 H₃BO₃ + Na₂SO₄
Na₂B₄O₇+ 2 HCl + 5 H₂O ----> 4 H₃BO₃ + 2 NaCl

[Edited on 28-8-2016 by PHILOU Zrealone]

nux vomica - 28-8-2016 at 19:27

Quote: Originally posted by PHILOU Zrealone

I have done the maths and worked out the stoechiometry:
2 NaNO₃ + 4 H₃BO₃ --> Na₂B₄O₇ + 2 HNO₃ + 5 H₂O

MM NaNO₃ = 85
MM H₃BO₃ = 62,8
MM Na₂B₄O₇ = 201,2
MM HNO₃ = 63
MM H₂O = 18

So from 170 gr dry NaNO₃ (sodium nitrate) mixed with 251,2 gr dry H₃BO₃ (boric acid); one should get:
201,2 gr of Na₂B₄O₇ (borax)
126 gr of HNO₃ (nitric acid)
90 gr of H₂O (water)

Since the water and the nitric acid will distillate under the process conditions (over 450°C borax initially decahydrated, becomes anhydrous), one should get 216 gr of 58,33% HNO3 solution.

Thus from 100 gr of initial mix (40.36% Na nitrate and 59.64% boric acid) one gets theorically 51.28 gr of nitric acid of 58.33% concentration.
From this information it is obvious that the trial of Nux Vomica misses quite some H₃BO₃ to get optimum yield...for 8,4 gr Na nitrate he should have used 12,41 gr boric acid instead of 6,1 gr...a double dose.

RECYCLING:
The beauty of this OTC process is that the boric acid can be recycled from borax and OTC-ish HCl (chlorhydric acid) or H₂SO₄ (sulfuric acid).
Na₂B₄O₇+ H₂SO₄ + 5 H₂O ----> 4 H₃BO₃ + Na₂SO₄
Na₂B₄O₇+ 2 HCl + 5 H₂O ----> 4 H₃BO₃ + 2 NaCl

[Edited on 28-8-2016 by PHILOU Zrealone]

Thanks for the maths bit PHILOU Zrelone im more of a nuts and bolts type of person i started to try and work it out and couldent get it to balance.
My instinct was to go with twice as much Boric acid but i decided to keep them equal instead.
With your info i might try a larger reaction to get more acid to measure its density when ive a free hour or so.
Nux.

Bert - 28-8-2016 at 21:09

Quote:

Since the water and the nitric acid will distillate under the process conditions (over 450°C borax initially decahydrated, becomes anhydrous), one should get 216 gr of 58,33% HNO3 solution

I wonder, with careful process control, keeping the heat to just that required to melt the boric acid and drive the reaction, could the borax formed serve to at least somewhat dehydrate the acid... The questions being, what temperature is REQUIRED for the reaction to proceed, and at what temperatures does borax hold how many molecules of water of crystalization?

Nice start there, it is good to know that fairly strong nitric acid is available to those without access to OTC sulfuric acid. No place I know of controls sale of boric acid, the least objectionable of roach poisons.

James Ikanov - 28-8-2016 at 22:42

Would it be plausible to use a similar method to produce perchloric acid?

I'm not sure about whether such a thing could be advised, I'm simply curious if it's plausible.

PHILOU Zrealone - 29-8-2016 at 03:16

Quote: Originally posted by James Ikanov

Would it be plausible to use a similar method to produce perchloric acid?

I'm not sure about whether such a thing could be advised, I'm simply curious if it's plausible.

Good question.
In principle, I see nothing against it since HClO4/H2O is also distillable...sole difference between HClO4 and HNO3 is the acidity (HClO4 is even more acidic than HNO3 itself much more acidic than H3BO3).

Of course here in no way should the B2O3 / NaClO4 be attempted...the putative anhydrous HClO4 and Cl2O7 being heat sensitive explosives.

Microtek - 29-8-2016 at 23:23

I could see the much higher boiling point of HClO4 causing some trouble, but maybe with a sufficient vacuum...

PHILOU Zrealone - 30-8-2016 at 04:32

I have done the maths and worked out the stoechiometry:
2 NaClO₄ + 4 H₃BO₃ --> Na₂B₄O₇ + 2 HClO₄ + 5 H₂O

MM NaClO₄ = 122,5
MM H₃BO₃ = 62,8
MM Na₂B₄O₇ = 201,2
MM HClO₄ = 100,5
MM H₂O = 18

So from 245 gr dry NaClO₄ (sodium perchlorate) mixed with 251,2 gr dry H₃BO₃ (boric acid); one should get:
201,2 gr of Na₂B₄O₇ (borax)
201 gr of HClO₄ (perchloric acid)
90 gr of H₂O (water)

Since the water and the perchloric acid will distillate under the process conditions (over 450°C borax initially decahydrated, becomes anhydrous), one should get 291 gr of 69,1% HClO4 solution. (Boiling point should be arround 200-203°C vs 120°C for the HNO3)

Thus from 100 gr of initial mix (49,38% Na perchlorate and 50,62% boric acid) one gets theorically 58,65 gr of perchloric acid of 69,1% concentration.

RECYCLING:
The beauty of this OTC process is that the boric acid can be recycled from borax and OTC-ish HCl (chlorhydric acid) or H₂SO₄ (sulfuric acid).
Na₂B₄O₇+ H₂SO₄ + 5 H₂O ----> 4 H₃BO₃ + Na₂SO₄
Na₂B₄O₇+ 2 HCl + 5 H₂O ----> 4 H₃BO₃ + 2 NaCl

[Edited on 30-8-2016 by PHILOU Zrealone]

Short question: Sensitivity when wet

Tricka90 - 31-8-2016 at 02:51

Can primary as well as secondary explosives (such as silver acetilyde or picric acid as an example) be considered completely unsensitive when wet?
Of course friction and impact sensitivity would decrease due to lower friction between grains and damp impact provided by water. Flame and heat sensitivity would also decrease because of water heating inertia. But do you think solid explosives are really 100% stable and just can't detonate under water? Do you have any direct experience?

[Edited on 31-8-2016 by Tricka90]

Lotilko - 31-8-2016 at 11:43

Well, sensitive secondaries like PETN are very stable, however for some primaries like organic peroxides and nitrogen halides water won't really help. Water makes the explosives more resistant to physical disturbance. But when there are unstable bonds in the molecule it's a whole different story.

Maker - 1-9-2016 at 04:53

Why is potassium nitrate used as an oxidizer in pyrotechnic compositions when sodium nitrate has more nitrate ions per gram?

Metacelsus - 1-9-2016 at 04:59

Sodium will make a yellow color, obscuring any other coloring agents. Also, it's a lot more hygroscopic than potassium nitrate, so it's bad for storage purposes.

kratomiter - 2-9-2016 at 08:04

Can primary as well as secondary explosives (such as silver acetilyde or picric acid as an example) be considered completely unsensitive when wet?
Of course friction and impact sensitivity would decrease due to lower friction between grains and damp impact provided by water. Flame and heat sensitivity would also decrease because of water heating inertia. But do you think solid explosives are really 100% stable and just can't detonate under water? Do you have any direct experience?

[Edited on 31-8-2016 by Tricka90]

Some sensitive secondary explosive like picric acid or DNPH when wet are considered enough unsensitive that no special cautions are considered for transport and storage (I'm talking about quantities lower than 1 kg, AFAIK).
But I have no idea about primary explosives.

One question: I'm looking for a inner coating for copper tubes. I use it for making detonators, but copper can be form dangerous salts with some explosives and make them more sensitive. Is there a cheap way to make an inert coating? Maybe cyanocrilate?

MineMan - 2-9-2016 at 10:08

Why copper, why not just switch to Al or graphite??

Maker - 2-9-2016 at 13:25

Quote: Originally posted by kratomiter

Why not just use a glass tube?

[Edited on 2-9-2016 by Maker]

Maker - 2-9-2016 at 13:47

How do you decide what length vigreux column to use for fractional distillation? Is it a case of the bigger the better or is there more to it than that?

aga - 2-9-2016 at 13:53

I got two vigreux columns, 300mm-ish.

Not enough headroom in the hood to put one on top of the other, so it's always 300mm-ish.

If you calculate (based on theoretical plates etc) a 40m tall column, it won't work.

Basically you got to go with what you have.

If it does not resolve your B.P.s sufficiently well, you got to distill it again.

Maybe many times.

[Edited on 2-9-2016 by aga]

kratomiter - 3-9-2016 at 07:53

@MineMan @Maker I used copper tubes because they're available where I live, but I'll try aluminum tubes if I find them. I didn't know the existence of graphite tubes until now. As for glass, it's more difficult to work with it and also it can't handle high pressures to ensure that explosives like TACP undergo DDT.

MineMan - 3-9-2016 at 17:13

Are you trying to make a DDT detonator? Yes, graphite from arrows. However, maybe the arrows are two small (about 6mm id) because 70mg of SADS keeps on failing for me. I really hate approaching duds, even after waiting for a while...

system Berta

Laboratory of Liptakov - 4-9-2016 at 11:22

In aluminium TACP worked, but only in diameter 8 mm. Wall 1mm Al. Again reccomend basic construction system Berta. Thus Copper, because is heavy. During process DDT arises dynamic resistance of copper against increase pressure inside. Thus, not aluminium, glass, papper, plast and similarly. Only copper, steel. It is system NPED. Required solid cavity. Always. Not softly shit. From the shit is impossible making any detonator NPED. Next:
TACP is not much sensitive. With wax very low sensitive. Therefore is use in system Berta. However pure TACP can have difficult DDT in diameter 6mm. Therefore is better using CHP. It is TACP 88%, HMTA 6% NH4ClO4 6%. Mixing under a few drops NH4OH on porridge, get on surface 80 C and evaporate. Arises soft material, partially crystals, partially as rubber. CHP worked in diameter only 4,3 mm. In copper cavity. General universal scheme is on Vimeo or YT system Berta. Berta detonator is possible trashing blow help the hammer on the anvil. Without explode, of course. Not try it, everybody. ... :cool:

...Dr.

[Edited on 4-9-2016 by Laboratory of Liptakov]

MineMan - 4-9-2016 at 13:10

Ahh yes, thank you for the additional information LL, I was wondering how to convert TACP to CHP. Yes, I think that my TACP with 3% wax may just be to insensitive for 6mm dia. I suspect no amount of SADS will do the job in that diameter with a thin (sub 1mm) graphite tube.

LL, I like fuses over electrical ignition, but it seems that for the Berta it must be ignited in the middle first, how is this possible with a fuse?

I am really impressed with TACP so far, small amounts can detonate ANNMAL and with small amounts of wax it is nearly immune to impact and friction ( it will still go off easily is placed on a rough rock and hit with a hammer, but steel on steel it is very resistant to blows). The best part, is no acids and no neutralization and filtering!

LL, is HMTA Hexamine??

kratomiter - 4-9-2016 at 19:26

Interesting, I thought CHP was more insensitive than TACP, thanks for the info.

CHP

Laboratory of Liptakov - 4-9-2016 at 23:28

HMTA = hexa methylen tetra amin. Hexamin. CHP - producing described here, thus on hot surface method, is very low sensitive on friction and pretty low on hammer. Because is it soft material. MInimum hard crystals. At filling to cavity is it clearly feeling. Nothing sound at crushing. At pressing is hear nothing. Similarly as at pressing the flour. Between fingers is feeling his soft consistence. The soft consistency is well made CHP. And minimal risk with handle care. With Bickford fuse type is possible this. Diameter Bickford is usually 5,6 - 6 mmm. This making with CHP. Not confirmed for others mixes. Dr.

[Edited on 5-9-2016 by Laboratory of Liptakov]

MineMan - 5-9-2016 at 09:21

Ok, but mirror ignition seems impossible with a fuse...Isn't the mirror ignition necessary for reliable DDT of CHP?

Laboratory of Liptakov - 5-9-2016 at 13:22

Not. For CHP and Bickford fuse is posible use this scheme. Without mirror effect. Running it. Dr.

MineMan - 5-9-2016 at 14:26

Ahh good to know Dr. But different density loading is required I presume, a long with a strong metal case.

system Berta - fuse type

Laboratory of Liptakov - 6-9-2016 at 01:14

All is described in scheme. Tube can be also steel. For classic Bickford fuse is best diameter of cavity 6 mm.

Dr.

Picric Acid Toxicity

Tricka90 - 6-9-2016 at 03:23

The toxicity of Picric Acid is well known.
But is its toxicity a real concern even when dealing with very small quantities like one gram or two, for use just as a booster charge?

[Edited on 6-9-2016 by Tricka90]

greenlight - 6-9-2016 at 04:46

I wouldn't think so as long as you wear gloves and don't eat the stuff.
The most annoying thing when you make it occassionally is the yellow staining if you touch it or any of the solutions it was in contact with.

I found a pdf with some tests on the toxicity of trinitrophenol:

https://toxnet.nlm.nih.gov/cgi-bin/sis/search/a?dbs+hsdb:@te...

[Edited on 6-9-2016 by greenlight]

Tricka90 - 6-9-2016 at 12:30

Thank you greenlight, that was very interesting.
By the way, I'm a bit confused about picric acid ingredients when using aspirin. Two different recipies are found on the internet and in this forum.
According to the first one the ingredients should be aspirin, sulfuric acid and nitric acid, according to the second one ingredients should be aspirin, ethyl alcohol, sulfuric acid and sodium/potassium nitrate.
Which recipie do you think is correct? Are they both effective?

Lotilko - 6-9-2016 at 13:05

I am no expert on picric acid synthesis, but the first procedure should be the mixed acid nitration of aspirin whereas the second one uses sulfuric acid and a nitrate salt. The ethanol is to remove any impurities from the aspirin, so you'll have pure acetylsalicylic acid. I think the second route is more feasible for the amateur chemist because nitric acid is not a readily available reagent in some places.

greenlight - 6-9-2016 at 18:58

I have heard of both of those processes for the synthesis of TNP. Lotliko is right, the ethanol is needed in both of them to extract the acetylsalicylic acid from the aspirin tablets.
In the potassium nitrate method, the nitric acid is formed in the flask during the nitration whereas the second method it is one of the reagents. I prefer using the straight 70% nitric acid/98% sulfuric acid method as for me better yields are achieved.

[Edited on 7-9-2016 by greenlight]

Tricka90 - 7-9-2016 at 01:17

Thank you for all your help Lotilko and greenlight.

Greenlight, when making TNP with 70% nitric acid and 98% sulfuric acid do you prefer using phenol or aspirin (after reaction with ethanol to get acetylsalicylic acid)?

greenlight - 7-9-2016 at 02:45

I have never made it straight from phenol as I never have had any...
I always used to make it from the cheap aspirin tablets but the straight phenol method would be exactly the same but a bit shorter as you don't have to sulphonate the acetylsalicylic acid into phenol first.

Amount of acid for nitroglycerin

Gemlingur - 7-9-2016 at 02:49

I have often made nitroglycerim in the past, with varying success, and I was wondering hoe much glycering you can use per amount of acid mixtute? I use oleum and 68% nitric acid so that i get 1:1 waterfree mixture. If i woulf use more concentrated oleum, might that get rid if the water that forms when the glycerin gets nitratrated? And how much nitro can you make per amount of the acid mixture?

hissingnoise - 7-9-2016 at 03:13

IIRC, the ratio is about 1 to 6 by wt.─ that is essentially anhydrous MA containing 40% HNO₃!

Bert - 7-9-2016 at 05:51

Nitroglycerin and Nitroglycerin Explosives- Phokion Naoum

Go to the library and read. Ask short questions with no documentation of sources here, or in a related, existing thread in the future.

And where are you obtaining "oleum"?

MineMan - 7-9-2016 at 16:13

Has anyone on this forum used dinitrogen pentoxide for nitration? Apparently it is the new thing, and industry is now using it as it provides higher yields than HNO3 and can nitrate substances HNO3 is reactive towards.

I could not find any dinitrogen pentoxide for sale...

Lotilko - 8-9-2016 at 07:55

One could prepare it from distilling a mixture of anhydrous nitric acid and phosphorus pentoxide under vacuum. The dinitrogen pentoxide is then trapped in a condenser cooled with ice.

The reaction is:

2 HNO₃ + P₂O₅ = N₂O₅ + 2 HPO₃

[Edited on 2016.9.8 by Lotilko]

NeonPulse - 8-9-2016 at 17:22