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Laboratory of Liptakov - 7-4-2017 at 12:39

:cool:Thanks for link.....:cool:.....and oters....But is impossible, that on bottom will arise as firstly crystals NaClO3, because he has much highly solubility than NaCl. It is against logical. And if yes, on how temperature cooling ? On Zero Celsia? I read almost all about it, but still I do not know how to make apart both compounds. I need some tutorial: Take 100 grams NaCl/O3.
Dissolve in 100g (??) distill water. Heated on boiling point 100 C. Cooling on 63 C ??
Separation NaCl crystals on filter. Solution is pure NaClO3 (99%). Tutorial not exist.

yobbo II - 7-4-2017 at 12:55


Na Chlorate is more soluble and this means that for to get it to come out of solution you simply must have a greater concentration of it in the solution. It will they ppt out..
Keep running the cell and adding raw material (NaCl) and the concentration of chlorate will go up and up and solid material will start to be deposited on the cell floor.

http://www.sciencemadness.org/talk/files.php?pid=375539&...

https://www.sciencemadness.org/whisper/viewthread.php?tid=20...



[Edited on 7-4-2017 by yobbo II]

Attachment: Mut_Sol.zip (209kB)
This file has been downloaded 270 times


Laboratory of Liptakov - 7-4-2017 at 13:11

OK, I read all, it is system "salting out from the solution". Yet, that NaClO3 has highly solubility, is possible he get out from solution huge increase just simply NaCl. Absolut against reason.....:cool: It is as quantum physics. Nobody knows how is it possible, but work it. For sure I will rinsed in cell Schrödinger cat. Well, maximum simply method is increase NaCl + 10%, waiting on 70 C, again + 10% NaCl, again waiting on run temperature. ETC...
Until the cat climb out from solution....:cool:...LL

JJay - 7-4-2017 at 14:08

I noticed recently that it bumps horribly if you boil it down too fast. Nothing boiling saturated NaClO3 flying all over the place....

PHILOU Zrealone - 7-4-2017 at 16:55

Quote: Originally posted by Laboratory of Liptakov  
How apart NaClO3 from NaCl solution ? I have 100g mix NaClO3 + NaCl as dry crystals. This mix content : 50% NaCl + 50% NaClO3
Or also 10% NaCl + 90% NaClO3. It nobody know. Graph for NaCl is solubility 35g in 100g Water at 0 C. And 39g at 100 C.
For NaClO3 is graph solubility : 80g at 0 Cels. and 200g at 100 Celsia. Exist some method recrystallization. I look on all S-M, but not find describe exactly how to make. Especially making so, for relatively best purity on NaClO3. NaClO3 estimate stay as solution. But at how concentration create before heating on 100 C ? Dissolving 200g mix-salts in 100g H2O at 99 C ? And after what? Decrease slowly temperature on 50 C? And by 50 Celsius separe NaCl ? Or separe by zero Celsius all crysralls ? Thanks..........:cool:
Exist 1000 tutorials how to make KClO3 but nothing for NaClO3.

[Edited on 7-4-2017 by Laboratory of Liptakov]

@LL,
you didn't do your homework wel :mad: ...everything is into this forum and especially into a tread in which you have replied...:D;):cool::P(*)

1°) Simply dry all the NaCl/NaClO3 (and NaClO4 if ever present)

2°) Then extract with dry aceton or ethanol....leave the unsoluble NaCl (NaCl is almost unsoluble into aceton while NaClO3 is soluble and NaClO4 even more)...solubility of NaCl into ethanol is low while NaClO3 and NaClO4 are much more soluble.

3°) evaporate the aceton/or ethanol (avoid too much heat and favor the use of a closed system to avoid risk of fuel-air explosion of aceton/ore ethanol vapour-flame point is quite low so risk is high) and condense it to recover the valuable solvent for reuse and some economical turnover.

4°) Collect the dry crystals from solvent evaporation...it is NaClO3 and NaClO4 if present.

(*)
Here are some interesting solubility tables into ethanol I have gathered
tables provided by PH Z into NH4ClO3 tread

And here is a little later reply where I wrote:
***********QUOTED from myself*********
Side note:
It is to be noted that into the tables one may see that for the case of NaCl/NaClO3...the use of aceton is preconized to effect separation because NaCl is quasi totally unsoluble into aceton while NaClO3 is very soluble in it and NaClO4 even more...
Here it seems it is also the case with absolute ethanol that is quite a good solvent for that specific chlorate and perchlorate but not a good one for NaCl...
This is very interesting for all the old weed killer (60% NaClO3/40% NaCl) bags I own or for the purification from electrolysis chlorate cell from chloride...
*********END OF QUOTE***********
Quoted from here
A reply further into the same NH4ClO3 tread

[Edited on 8-4-2017 by PHILOU Zrealone]
I invite you to search into this http://chemister.ru/Database/properties-en.php?dbid=1&id... and the upper left "Search in database (English) " then you can type NaCl for example and get solubilities at various températures and sometimes into different solvents than water...

[Edited on 8-4-2017 by PHILOU Zrealone]

solubility

Laboratory of Liptakov - 7-4-2017 at 23:01

Thanks Philou.. However I am before put questions about separation making dissolving process and tested solubility my mix just in acetone. Into 50 ml acetone was insert 25,9g of mix salts. Heated on 50 C and cooling on 25 C. However after filtration and evaporate acetone, was on inert surface only 0,03g some. Practicaly nothing. I find and look on table on wiki. I are same digits as in your recommend tables about solubility. My opinion was, that on wiki are bullshit. Why it say: Because this mix, after mixing in sugar ( ratio 35 sugar / 65 ) burning very quickly, same as should by this mix, from pure NaClO3 + sugar. And according a lot videos with pure NaClO3 + sugar it seem, that I have almost pure NaClO3. However in acetone total not soluble. Ethanol (14,7g/100ml) was not tested yet. Go on it....:cool:...LL

yobbo II - 8-4-2017 at 05:26


US 3151935

has some discussion regarding subject.

If the acetone contains some water do you know what are the solubilities? or do they change much with a few % of water?

Laboratory of Liptakov - 8-4-2017 at 12:20

Good patent.. Very details about problematic solubility and next important things...Thanks...I´ve what for study on long times...:cool:...LL

PHILOU Zrealone - 8-4-2017 at 16:28

Quote: Originally posted by yobbo II  

US 3151935

has some discussion regarding subject.

If the acetone contains some water do you know what are the solubilities? or do they change much with a few % of water?

As a first approximation you may put the solubility of the salt into pure water and into aceton into a solubility as a function of the % of water and the % of aceton graph by putting the solubility at 100% water and 0% aceton on one side and the solubility at 100% aceton and 0% water on the other side...then draw a line between the two and you have a good idea of what might result from a few % water...this is observable into the link to graphs and tables into my previous post...but with the case of ethanol and different water content.

yobbo II - 9-4-2017 at 13:42


Would there be an issue with ignition with the mixture when drying. A small amount of acetone mixed with sodium chlorate sounds like stuff that might ignite with a spark?

separation NaClO3

Laboratory of Liptakov - 10-4-2017 at 10:45

The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL

yobbo II - 10-4-2017 at 14:08

Quote: Originally posted by Laboratory of Liptakov  
The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL


Did you mearure the amounts of NaCl and NaChlorate to get the 99% figure?
Will this process not depend on the amounts of Chloride and Chlorate (the ratio) that you have been starting off with.
If you have a mixed solid of 3% chloride and 97% chlorate will you have chloride being ppt out first?

The acetone would be much better for this kind of one off seperation.

Yob

AnWax

drifting_mine - 14-4-2017 at 04:24

Hi everyone,

I'm kinda new to the forum. This is my first post but i have already read through a lot of posts, my main source of other people's experiences.
I happen to have some pure paraffin lying around, and i was wondering what would be the best method to mix it with AN to obtain a AnWax mixture?
Correct me if i'm wrong, but i think some etn should be more than enough to detonate it?

Thanks for advices!

Ps. I apologize for any grammatical errors.

Laboratory of Liptakov - 14-4-2017 at 13:14

Of course, that ETN should be enough detonate any AN -WAX. Usually 3 grams is enough for AN-WAX , if is wax added as solution in gasoline and follow evaporate gasoline. Better is always add 2% Al. Much deminers has opinion, that main charge 1 Kg and more requires a big booster, for example 10g Hi - brisant EM. It is not pretty right. If is main charge medium sensitive, enough No.8. Or small booster 2 - 3g at it. For full strenght..........:cool:

Si Da Sci Guy - 25-4-2017 at 06:54

Is sulfur a better sensitizer for AN than aluminium ?

PHILOU Zrealone - 26-4-2017 at 01:31

Quote: Originally posted by Si Da Sci Guy  
Is sulfur a better sensitizer for AN than aluminium ?

No but the mix of the two mixes would be synergetical over the two appart.

There might be storage issues between Al/NH4NO3/S due to air moisture and hygroscopicity of NH4NO3, mild acidity of S (air oxydation leads to SO2 and SO3 traces or it is trapped inside the S crystal matrix) and mild acidity of NH4NO3...thus chewing protective oxyd layer of the aluminium

--> generation of H2 gas (flamable),
--> generation of much heat that may accelerate decomposition if in larger enough quantity to allow for good heat dissipation.

The powder will invariably loose power upon storage since untreated Al powder will be oxydised and the amount of active metal will be less.

Into hermetical container, pressure may rise upon storage.

Si Da Sci Guy - 26-4-2017 at 06:27

Thank you for your response PHILOU Zrealone.

So throw them all in, maybe 2.5%S 2.5%Al 95% NH4NO3.

What do you make of adding an AN decomposition catalyst in like ammonium chloride, will that help during the detonation?

Si Da Sci Guy - 26-4-2017 at 11:31

I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?

clearly_not_atara - 26-4-2017 at 11:48

It looks high for a small molecule, but compare it to an equal weight of methane, with ∆H ≈ 890 kJ/mol. Methane's molar mass is 16 g/mol, so approximately 18.3 moles of methane has equal weight to one of myristic acid. 18 moles of methane combustion is worth about 16 megajoules.

I wonder if AN/paraformaldehyde might have a better oxygen balance than ANFO. Possibly AN/polyoxymethylene?

[Edited on 26-4-2017 by clearly_not_atara]

DubaiAmateurRocketry - 26-4-2017 at 20:14

Quote: Originally posted by Si Da Sci Guy  
I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?


You can judge from the structure.

Acetyl group + a carbon backbone chain.

Just a combustible compound, like any other organic compound, nothing "energetic" in the sense of EM

[Edited on 27-4-2017 by DubaiAmateurRocketry]

PHILOU Zrealone - 27-4-2017 at 17:34

Quote: Originally posted by yobbo II  

Would there be an issue with ignition with the mixture when drying. A small amount of acetone mixed with sodium chlorate sounds like stuff that might ignite with a spark?

No risks since aceton is too volatile and will cool down by evaporation the NaClO3 below its decomposition temperature.

PHILOU Zrealone - 27-4-2017 at 17:46

Quote: Originally posted by Laboratory of Liptakov  
The problem with splitting, separating NaCl from NaClO3 resolved. Both substances were dissolved in the smallest possible amount of water, at temperature 20 C. The water is brought to a boil. Observing, watching level boiled solution. If on surface arises a gray coating - fine crystals, the solution is immediately (maximum hot) filtered.
Upstairs in the filter, during process filtering, arises crystalls NaCl. In solution bottom filter in flask, arises next crystalls NaCl, (after cooling to 20 Celsius. ) The solution is filtered or decantated at 20 C. We have Pure solution NaClO3 + water, in purity 99%. Done. For best purity is possibe process repeated again.
Self / answer sytem....Liptakov.....:cool:...LL

True!

The solubility of NaClO3 was contradictory into several documents I have found...so I did test it...was 1,6g / liter aceton (coherent with US patent 3151935A what mentions 1,7 g/L). This is 8 times better than NaCl...so in principle with a Sohxlet extractor, one could extract more selectively NaClO3 from a NaCl/NaClO3 mix...

Based onto that patent solubility of NaClO4 is 216 times better than NaClO3 and 1840 times better than NaCl.

Into the "traité de chimie minérale" about sodium and lithium...they expose the solubility of NaClO3/NaCl mix saturated into water as function of the T°. The NaCl is usually dropped out of the solution by the mutual ionic effect since while NaCl almost doesn't increase its solubility when warming; NaClO3 does it exponentially...so more Na(+) and NaCl kicked out of the solution faster (at a lower concentration than when alone)...Solution if filtrated warm, then slowly cooled down and almost pure NaClO3 are collected...
--> That is the process LL has used/reinvented ;-)

PHILOU Zrealone - 27-4-2017 at 17:54

Quote: Originally posted by Si Da Sci Guy  
Thank you for your response PHILOU Zrealone.

So throw them all in, maybe 2.5%S 2.5%Al 95% NH4NO3.

What do you make of adding an AN decomposition catalyst in like ammonium chloride, will that help during the detonation?


That composition may work for a detonation process but (is it stoechiometrical? --> if not then) not for a good burning composition (like rocket or deflagrating banger).

Nearly anything catalyses the decomposition of AN into a detonation process -->nearly anything is a sensitizer of AN.
AC will of course be.

The mix AN/AC (NH4NO3/NH4Cl) may be troublesome for corrosive reasons towards container especially if metallic... moisture will probably set some traces of nitrosyl chloride free and be kind of a solid form of an unefficient aqua-regia.

PHILOU Zrealone - 27-4-2017 at 18:02

Quote: Originally posted by Si Da Sci Guy  
I know I'm jumping in here and asking lots of questions but here is another quick one:

is 8675.9 kJ/mol ( 8.675 MegaJoules ) high for a standard enthalpy of combustion. The molecule is Myristic Acid and has a molar mass of 228.38 g·mol−1.


I mean is that a lot of energy ?

Nearly about the same as any organic oïl...
and a little less than same lenght mineral oils (paraffins) because part of the myristic molecule (an organic carboxylic acid) is already oxydised (-CO2H terminated)...

-->compare the heats of combustion of ethane, ethanol, ethanal and ethanoic acid to understand this.
(or the ones from methane, methanol, methanal, formic acid and carbonic acid)...

Carbonic acid has no more energy to be combustible on its own (to the contrary...it will extinguish fire).

PHILOU Zrealone - 27-4-2017 at 18:09

Quote: Originally posted by clearly_not_atara  


I wonder if AN/paraformaldehyde might have a better oxygen balance than ANFO. Possibly AN/polyoxymethylene?

[Edited on 26-4-2017 by clearly_not_atara]

The OB depends onto the % of fuel vs oxydizer so the question has no sense per se. ;)

But if the % of paraformaldehyde/polyoxymethylene and mineral oïl are the same in both compositions; then yes ;) the (-CH2-O-)n variant will be higher in OB than the (-CH2-CH2-)n one...

But the detonic parameters have to be analyzed to determine which of the two will be more potent...fuel oïl contains more energy but is lighter...POM is denser but contains less energy...stil a decent amount....
Into a detonation process POM may depolymerise into CH2=O and react instantaneously with NH4NO3 to make "virtually" hexamine dinitrate equivalent (7000 m/s VOD) or Methylamine nitrate equivalent (6500 m/s VOD) thus better than ANFO (3500 m/s at best)...

[Edited on 28-4-2017 by PHILOU Zrealone]

MineMan - 29-4-2017 at 10:47

Hi All,

Google has continued to become worse and worse of a search engine these last few months... showing things that are not relevant.

Anyways, I am looking for a PETN Synth using sulfuric acid and a nitrate like ammonium nitrate. I cant find this. can someone point me to the correct source?

XeonTheMGPony - 30-4-2017 at 05:17

quite a few in the energetic forum, just got to read though it all!

MineMan - 2-5-2017 at 14:38

Quote: Originally posted by XeonTheMGPony  
quite a few in the energetic forum, just got to read though it all!



That was so helpful! ok, now back to the real world, not the world:D of sarcasm!

That was literally the worse answer pyro guy

Beware

Laboratory of Liptakov - 6-5-2017 at 06:55

Beware of this seller. Sells very low quality platinum anodes.
http://store.theamateurchemist.com/platinum-titanium-anode-2...
All describe here: https://www.youtube.com/watch?v=xV-SaP2iv7s

PbO2 anode

Laboratory of Liptakov - 7-5-2017 at 03:10

Has anyone recommendation on seller for Lead dioxide anode PbO2 - beta ? Some experiences ? Thanks.............:cool:..........LL

PHILOU Zrealone - 8-5-2017 at 02:18

Quote: Originally posted by Laboratory of Liptakov  
Has anyone recommendation on seller for Lead dioxide anode PbO2 - beta ? Some experiences ? Thanks.............:cool:..........LL

Hi L(o)L ;),

The joinded document explain how to make alfa- and beta-PbO2 anodes and their properties.

It seems that the alfa is better but not wel studied.

Enjoy ;) and continue the good job and experimentation.

PHZ

Attachment: Unsoluble anode lead dioxide coated on titanium for electrosynthesis of sodium perchlorate.pdf (267kB)
This file has been downloaded 334 times


PbO2 alpha type

Laboratory of Liptakov - 8-5-2017 at 07:14

Great , thanks. But in tutorial is absence concentration KOH. What is (4M) ? Others prepare conditions seems pretty easy. And maybe preparation Lead acetate can be problem, of course is necessary study how make him. 40g per liter solubility in KOH electrolyte. Clear ratio. But basic concentration KOH is describe not.
Next question is, why everybody not use from year 1990 only alpha type PbO2 anode. Everywhere is prefer beta PbO2.
Maybe is only same , as with prefer the primer Lead azide. Commerce conditions are cheapest for acid bath or some so. ...:cool:...LL



[Edited on 8-5-2017 by Laboratory of Liptakov]

PHILOU Zrealone - 8-5-2017 at 07:46

Quote: Originally posted by Laboratory of Liptakov  
But in tutorial is absence concentration KOH. What is (4M) ? But basic concentration KOH is describe not.

It is under the 4M secret code information.....:cool:

But only initiated chemist know that...;):P:D:)
It is common chemical writting ... 4M is "4 molar concentration" what means 4 moles per liter solution. ;)

************************************
You of course know what a mole is?

In biology it is an underground digger mamal that destroys green grass gardens by making tiny soil bumps everywhere as aeration holes. ;):P:)

But in chemistry it is a number defining a group/a number/amount of atoms or molecules that provide a workable quantity linked to the Avogadro's number (6,022 140 857 × 1023 units)...

So when mixing the two biological and chemical notion you have
6,022 140 857 × 1023 moles is a mole of moles :D;):P:)... (Chemical joke).

Si if you have 2 shoes you have a pair of shoes, if you have 12 shoes you have a dozen of shoes or 6 pairs of shoes...and if you have 6,022 140 857 × 1023 shoes, you have a mole of shoes...convenient isn't it?
It is a hurge number but when applying it to molecules and atoms what are very tiny and weights nearly Nothing if furnish you the quantities to work at our scale and to allow us to react together réactants to get products whith the help of the periodic table of the elements and the atomic masses...this is stoechiometry what links equations containing number of molecules that interacts; their molecular/atomic weight and multiplied by the Avogadro's number to get it as a mass of réactants...;):P

As an example:
So 2g H2 gas contains (approx) 1 mole of H2 molecules but two moles of H atoms.
So 32g S contains (approx) 1 mole of S atoms.
By warming the two
H2(g) + S(s) --> H2S(g)
You get 34g H2S or (approx) 1 mole ...
Smokey....Stinky :D;):):P

[Edited on 8-5-2017 by PHILOU Zrealone]

Laboratory of Liptakov - 8-5-2017 at 09:05

Only one thing, what I am understood, that I had 6 pairs of stinky shoes. And on the garden 4 the moles. Thanks for explanation.
Well...concentration 1 M is less than 4 M. However, still is not clear, how much KOH is need insert, in order that arise solution 4M KOH....Shoes are clear. Everybody the Mole are also in their holes. Schrödinger´s cat in the box. But KOH stay top secret.
........:cool: LL

PHILOU Zrealone - 8-5-2017 at 09:38

Quote: Originally posted by Laboratory of Liptakov  
Only one thing, what I am understood, that I had 6 pairs of stinky shoes. And on the garden 4 the moles. Thanks for explanation.
Well...concentration 1 M is less than 4 M. However, still is not clear, how much KOH is need insert, in order that arise solution 4M KOH....Shoes are clear. Everybody the Mole are also in their holes. Schrödinger´s cat in the box. But KOH stay top secret.
........:cool: LL

:cool::):D;):P You got everything right ;-)

Molar Mass KOH = 56,1056 gr/mol (1 mole of KOH weights 56,1056 grams)

So 1M is 1 mole/L or 56,1056 gr into 1 L volume solution.
So 4 M is 4 mole/L or 4*56,1056 gr = 224.4224 gr into 1 L volume solution.

Laboratory of Liptakov - 9-5-2017 at 00:18

Oh not...So easy...? Well...Thus, is necessary use 700g pure water and insert 224,5g KOH and after pour water on volume 1dm3. Not on 1 kg, because it not it same. OK, last problem is solved, done. Thanks for superchemical counting..........:cool:....LL

drifting_mine - 9-5-2017 at 02:24

Hi everyone

I've lately been experimenting with etn, and about a month ago i prepared some with H2SO4 (95%) and NH4NO3. I then washed it with distilled water and NaHCO3 solution but this time I didn't recrystallize it. Yeld was about 11 grams of a fine white powder with some minor lumps that I divided into smaller batches and placed in various containers in different places: I even left a small amount (0.25 g) in direct contact with sunlight. The result is that after a month in none of the samples any sign of degradation is noticeable, with sensitivity tests remaining the same as it was just prepared, even in poorly packed samples or left in open air (and without any recrystallization).

QUESTIONS: Should degradation of etn affect its sensitivity? Is degradation even an issue? (I know it has a long shelf life)
I now plan on recrystallizing some of the samples by dissolving it in hot ethanol, filter it and then dumping it in cold water as I usually do: is this a good method or should etn be allowed to slowly crystallize as the solution cools to room temperature?
Should I add some NaHCO3 solution to the etn solution befor recrystallization?

*I apologize for any language mistake*

Thanks!

[Edited on 9-5-2017 by drifting_mine]

[Edited on 9-5-2017 by drifting_mine]

greenlight - 9-5-2017 at 06:53

It is quite hard to find any test results for ETN as no one has really conducted many. Probably due to the fact that PETN found more use as a commercial/military explosive so all the testing was done on it instead.

I am fairly sure that ETN is quite similar in storage stability to PETN and you should have no worries if it is recrystallized and acid free . The only information I could find was on wikipedia about a 4 year storage stability test but you don't know how much truth there is to it as I can't find any info on it anywhere else. Here is the transcript :

"Studies that directly observed the crystalline structure saw no signs of decomposition after four years of storage at room temperature."

As for the recyrstallisation, I usually dissolve in alcohol and pour slowly into heavily stirred ice-water to get sand like granules. You can add small amount of sodium bicarbonate and ammonia if you wish. This process is documented somewhere else on the forum.

drifting_mine - 9-5-2017 at 08:10

Quote: Originally posted by greenlight  
You can add small amount of sodium bicarbonate and ammonia if you wish. This process is documented somewhere else on the forum.

Thank you for the answer greenlight, I do remember reading about that procedure on the forum but i couldn't find it.

FeedMe94 - 17-5-2017 at 02:29

Quote: Originally posted by greenlight  


As for the recyrstallisation, I usually dissolve in alcohol and pour slowly into heavily stirred ice-water to get sand like granules. You can add small amount of sodium bicarbonate and ammonia if you wish. This process is documented somewhere else on the forum.


I can only aquire 2 types of ethanol. The first one is 93% ethanol denatured with turpentine and methanol also is colored with methylene blue.
The other one is 95% and its denatured with water and glycerin.

Can i use any of these to recrystalize ETN ?

I cant find anything about purifying these and distillation wont work at least this is what they told me.

PHILOU Zrealone - 17-5-2017 at 03:12

Quote: Originally posted by feedme94  
Quote: Originally posted by greenlight  


As for the recyrstallisation, I usually dissolve in alcohol and pour slowly into heavily stirred ice-water to get sand like granules. You can add small amount of sodium bicarbonate and ammonia if you wish. This process is documented somewhere else on the forum.


I can only aquire 2 types of ethanol. The first one is 93% ethanol denatured with turpentine and methanol also is colored with methylene blue.
The other one is 95% and its denatured with water and glycerin.

Can i use any of these to recrystalize ETN ?

I cant find anything about purifying these and distillation wont work at least this is what they told me.

I would go for the second one because less ingrédients and of lower impact to the ETN.

Strange that this second alcohol cannot be purified by distillation because glycerine is quite non volatile and sticks well to water...so in principle...a simple evaporation 1 plate should get you nearly pure ethanol and leave H2O and glycerine behind...

testing the chlorate ph

underground - 19-6-2017 at 15:42

I have read that the ph of chlorate cell cant be measured directly cause hypochlorite will bleach the paper, this can be solved by boiling the solution. Can i just use h202 to destroy the hypochlorite then test it with a ph paper ? or will h202 affect the ph ?

PHILOU Zrealone - 20-6-2017 at 06:02

Quote: Originally posted by underground  
I have read that the ph of chlorate cell cant be measured directly cause hypochlorite will bleach the paper, this can be solved by boiling the solution. Can i just use h202 to destroy the hypochlorite then test it with a ph paper ? or will h202 affect the ph ?

Hard to tell...

*Hypochlorite/bleach water is usually quite basic (holding a few % of NaOH for stability

*If you start from NaCl...the media will also turn basic because some Cl2 is lost into the process as Cl2...

*Bleach and H2O2....different compounds same fight....
H2O2 may have acidic or basic stabilisators...it is also a strong oxydiser (just like hypochlorite)...as such it will aswel discolor the pH paper.

I think that if you work/read fast...you may use the paper strip for both H2O2 and ClO(-)...the discoloration is not always instantaneous (depends onto quantity, concentration and heat)

Better use a drop of the solution on one specific place of the strip...so you may use the paper strip several times for a multiple pH determination at different moments.

underground - 20-6-2017 at 12:47

Thank you PHILOU for your valuable help, i really appreciate that. I will take them into consideration

[Edited on 20-6-2017 by underground]

PHILOU Zrealone - 23-6-2017 at 12:50

Quote: Originally posted by underground  
Thank you PHILOU for your valuable help, i really appreciate that. I will take them into consideration

[Edited on 20-6-2017 by underground]

De nada...my plaisure.

MineMan - 23-6-2017 at 13:59

Does anyone know the optimum ZPP ratios for max VOD.

I have no experience with ZR KclO4 mixtures, and I know that if we just followed stiochiometry for flash powder the resulting 65/35 mix is very weak.

Does anyone have hands one experience with ZPP?

Uriel - 8-7-2017 at 10:37

Hello guys,

I tried to suppress NO2 and NOx gas from H2SO4+HNO3 solution but I have some problems.

I often make a nitrating mixture of 40g of pure NH4NO3 + 100g of H2SO4 >96% and I have a slightly brown color in the obtained liquid.
More the acids are "brown" (still slightly) more my yield decrease. I fall from 95 to 87% for my ETN.

Recentlly, I have add 0.4g of urea : many bubble appeared and my mixture overflowing with foam at room temperature.
Another time, at cold temperature (-5°C) little bubbles still appeared when I move the beaker after 24H of rest.
And the coolor is still the same, slightly brown/yellowish :(

Do you know if urea nitrate react with ammonium sulfate or anything ?
Do you know how can I remove NO2 gas from my nitrating bath ?

Thank you !


[Edited on 8-7-2017 by Uriel]

kratomiter - 9-7-2017 at 03:49

Quote: Originally posted by Uriel  
Hello guys,

I tried to suppress NO2 and NOx gas from H2SO4+HNO3 solution but I have some problems.

I often make a nitrating mixture of 40g of pure NH4NO3 + 100g of H2SO4 >96% and I have a slightly brown color in the obtained liquid.
More the acids are "brown" (still slightly) more my yield decrease. I fall from 95 to 87% for my ETN.

Recentlly, I have add 0.4g of urea : many bubble appeared and my mixture overflowing with foam at room temperature.
Another time, at cold temperature (-5°C) little bubbles still appeared when I move the beaker after 24H of rest.
And the coolor is still the same, slightly brown/yellowish :(

Do you know if urea nitrate react with ammonium sulfate or anything ?
Do you know how can I remove NO2 gas from my nitrating bath ?

Thank you !


[Edited on 8-7-2017 by Uriel]


When I do a nitrating bath with KNO3 and SA (drain cleaner), the solution turns completely clear when I heat it to 80ºC.

PHILOU Zrealone - 9-7-2017 at 10:40

Quote: Originally posted by Uriel  
Hello guys,

I tried to suppress NO2 and NOx gas from H2SO4+HNO3 solution but I have some problems.

I often make a nitrating mixture of 40g of pure NH4NO3 + 100g of H2SO4 >96% and I have a slightly brown color in the obtained liquid.
More the acids are "brown" (still slightly) more my yield decrease. I fall from 95 to 87% for my ETN.

Recentlly, I have add 0.4g of urea : many bubble appeared and my mixture overflowing with foam at room temperature.
Another time, at cold temperature (-5°C) little bubbles still appeared when I move the beaker after 24H of rest.
And the coolor is still the same, slightly brown/yellowish :(

Do you know if urea nitrate react with ammonium sulfate or anything ?
Do you know how can I remove NO2 gas from my nitrating bath ?

Thank you !


[Edited on 8-7-2017 by Uriel]

Blow dry air into the solution...it will take the NxOy away with the gas flow into a few minutes...

Alternatively add some dry urea nitrate (UN - united nations ;-)into your reaction vessel...
It will provide some anhydrous HNO3...destroy the NxOy and sadly also generate some water...that's why the HNO3 taken with it is good for to diminish the impact of the water of oxydation

NH2-CO-NH2 + 3 O (from NxOy) --> N2 + CO2 + 2 H2O

So the overal added HNO3 via UN is equivalent to "HNO3 . 2 H2O" (or HNO3 63%)...so better not use too much of it and only the required amount...in a way not to dillute too much the reaction media.


[Edited on 10-7-2017 by PHILOU Zrealone]

Joint grease for the grignard reaction?

Assured Fish - 14-7-2017 at 22:34

Hi all.
I was wondering if it was alright to use Vaseline grease for ground glass joints in a grignard reaction, i know Vaseline is quite hydrophobic but i wasn't sure if perhaps some of the other components of Vaseline could react with or degrade a grignard reagent. Refluxing ether will likely pull a small amount of grease into the boiling flask and im not too bothered about Vaseline contaminants provided they don't lower yields.

Thanks

PHILOU Zrealone - 15-7-2017 at 01:43

Quote: Originally posted by Assured Fish  
Hi all.
I was wondering if it was alright to use Vaseline grease for ground glass joints in a grignard reaction, i know Vaseline is quite hydrophobic but i wasn't sure if perhaps some of the other components of Vaseline could react with or degrade a grignard reagent. Refluxing ether will likely pull a small amount of grease into the boiling flask and im not too bothered about Vaseline contaminants provided they don't lower yields.

Thanks

Depends onto the contaminants...if you have fatty acids or esters...those might be interracting with a Grignard.
For example into candle wax/paraffine you have sometimes stearic acid and stearates amongst other stuffs....
You may have non ionic-detergents (thus fatty alcohols, ketons, ....)

Vaseline must be mainly if not completely alcanic thus:
-Straight aliphatic chains
-Branched aliphatic chains
-Branched cycloalcanes
==> CxH(2x+2)


Assured Fish - 17-7-2017 at 16:21

Ok thanks PHILOU Zrealone, the Vaseline that i have states no other components except petroleum jelly, it doesn't have a smell or taste so im pretty confident of its purity, I will try and purchase some proper vacuum grease at some point but for this particular reaction ill try using Vaseline.
I was just wondering if other people used Vaseline for the grignards.

PHILOU Zrealone - 18-7-2017 at 13:06

Quote: Originally posted by Assured Fish  
Ok thanks PHILOU Zrealone, the Vaseline that i have states no other components except petroleum jelly, it doesn't have a smell or taste so im pretty confident of its purity, I will try and purchase some proper vacuum grease at some point but for this particular reaction ill try using Vaseline.
I was just wondering if other people used Vaseline for the grignards.

Then the vaseline is good for the Grignard reaction you intend to do...

agent_entropy - 27-7-2017 at 05:25

How stable is potassium permanganate / aluminum flash powder (with a touch of fumed silica anticake)?
Need I be concerned about moisture/acid/storage as a finished device?

greenlight - 27-7-2017 at 11:35

KMNO4 is a quite reactive, powerful oxidizer and there are much safer oxidizers you can use for flash. It likes to react with things (especially hot fuels) and makes powerful flash even with aluminium powder that won't burn hardly with perchlorate.
It will do if you are very careful with it but there are much safer options.
It has a bit of a bad rap in the flash powder world like acetone peroxide with primaries.

I used to make KMNO4, atomised Al, S flash quite often as a filling for small fire crackers but only a gram at a time, use that and diaper up another gram.
I never had the finished devices around for longer than a day or two though but they were fine for that.
I wouldn't be exposing it to any moisture though.

If you really must use it be careful of static electricity and friction and make small gram batches that can't self confine and explode.





agent_entropy - 28-7-2017 at 04:38

I see, thank you, I'll avoid using it then. I was mostly just curious because KMnO4 is so easily available.

agent_entropy - 17-8-2017 at 13:47

I'm aware that storing silver fulminate under water is standard practice, but is there any more volatile fluid or solution under which it could be stored with relative safety and stability? I'm interested in applying a slurry to a surface and having the storage fluid evaporate quickly.

greenlight - 17-8-2017 at 19:23

Are you trying to make a touch explosive of sorts out of it?

I don't think relative safety and stability can be used in the same sentence as silver fulminate. :)

It is extremely sensitive and maintains the same sensitivity even if it is wet.

Ammonia will dissolve silver fulminate but when you apply it to a surface, I think it would eventually detonate just from the stress of crystallization from the solvent evaporating.
I have heard of the weight of crystals on top of crystals causing initiation and add in the fact that bonds forming during crystallization is an exothermic process. It would be a slower crystallization than the initial precipitation during manufacture which means larger crystals and more internal stress.

If you did manage to apply it to a surface in dissolved solution, I think it would detonate prematurely.


[Edited on 18-8-2017 by greenlight]

I am NOT planning to try this but...

physics inclination - 20-8-2017 at 13:08

Since acetylene dissolves in acetone, what would happen if one tried to make TATP from acetylene-enriched acetone? Would the acetylene instantly react with the hydrogen peroxide? If not, would it get trapped in the precipitate, or bubble out of the acetone as it turns into a solid that can't dissolve the gas?

physics inclination - 20-8-2017 at 16:40

Actually now I have another idea that might not be as dangerous (but still not certain its safe): what if you dissolved nitrocellulose in acetylene-enriched acetone? Could it make some enhanced-power or higher-detonation-velocity nitrocellulose lacquer? I just remember Darian Berg made a video about nitrocellulose lacquer that was mixed with Al-KClO3 flash powder and it could detonate, so I wonder if acetylene could do anything similar, assuming it doesnt bubble out of the acetone when NC is added.

Tin man - 22-8-2017 at 11:49

I believe in either case, you would make a flammable liquid.

joseph6355 - 23-8-2017 at 03:18

I'm planning on using ETN in order to detonate ANNM (95:5).

Assuming that the main charge (ANNM) weighs about 250g, how much ETN should I use?
What about the blasting cap?
I read something once about ETN that it would react somehow with aluminum and increase its sensitivity in a dangerous level. Would the same reaction occur with steel?

Regarding the ANNM.
Would a 90:10 mixture make any significant difference (sensitivity, brisance...)?

[Edited on 23-8-2017 by joseph6355]

physics inclination - 26-8-2017 at 23:30

So Ive seen lots of good information on metal complex salts that are primary explosives, and I was wondering if there are any similar complex salts that are more like booster or secondary explosives.
Like, I only need a list of compound names, and I can UTFSE from there :P

And sorry to kinda put two questions into one, but this is also related to metal ion complexes: has anyone tried making complex salts with iodate or bromate as the anion? Both would probably be unstable but I'm just curious.

PHILOU Zrealone - 27-8-2017 at 01:46

Quote: Originally posted by physics inclination  
So Ive seen lots of good information on metal complex salts that are primary explosives, and I was wondering if there are any similar complex salts that are more like booster or secondary explosives.
Like, I only need a list of compound names, and I can UTFSE from there :P

And sorry to kinda put two questions into one, but this is also related to metal ion complexes: has anyone tried making complex salts with iodate or bromate as the anion? Both would probably be unstable but I'm just curious.

I guess you will find more info than you wish for into the dedicated tread Exotic Primaries - complex salts

and also some into New Energetic Materials - Current Research

Tin man - 27-8-2017 at 12:10

Look into complexes of DMSO and metal nitrates/perchlorates. Fe+3(DMSO)6(NO3-)3 was the only one of the nitrates I could get to precipitate. I did not try any perchlorates.

greenlight - 2-9-2017 at 03:25

Just a quick question.
I made a small batch of PVA-coated lead azide for primary charge in dets. After I had pressed all I needed I left a small sample out to make sure it was storage stable. It is now four months later.
The only thing is that whatever part of the pile is in contact with the air becomes darker brown in colour from the original white of the batch and dearlens more on prolonged storage. I habe noticed this with other batches as well as I only make a small amount at a time.
I have attached a photo below after I transferred it onto a new piece of paper.
Maximum temp it has been exposed to is about 25 C.

Anyone know what causes this or if it affects sensitity or performance?

[Edited on 2-9-2017 by greenlight]

20170902_184440.jpg - 2MB

Bert - 2-9-2017 at 08:07

Lead azide left exposed to air and especially to light will get a thin layer of litharge on the surface. Litharge is brown.


physics inclination - 2-9-2017 at 19:52

What is this compound's name, if it has one? I've tried searching under several different names I thought it might be, but couldnt find any instance of it. Is it known to exist, and if so, is it usefully stable?


I want to believe its real.png - 8kB

ninhydric1 - 2-9-2017 at 21:47

@physics inclination
Correct me if I'm wrong, seasoned members, but I believe the name of this compound is 2-nitrotriazane. The compound N3H5 is named triazane systematically. Assuming the naming is the same as alkanes, the nitro group substitutes the hydrogen on the middle nitrogen and therefore would be named 2-nitrotriazane.

greenlight - 2-9-2017 at 22:20

Quote: Originally posted by Bert  
Lead azide left exposed to air and especially to light will get a thin layer of litharge on the surface. Litharge is brown.



Thanks bert.

PHILOU Zrealone - 4-9-2017 at 02:41

Quote: Originally posted by greenlight  
Just a quick question.
I made a small batch of PVA-coated lead azide for primary charge in dets. After I had pressed all I needed I left a small sample out to make sure it was storage stable. It is now four months later.
The only thing is that whatever part of the pile is in contact with the air becomes darker brown in colour from the original white of the batch and dearlens more on prolonged storage. I habe noticed this with other batches as well as I only make a small amount at a time.
I have attached a photo below after I transferred it onto a new piece of paper.
Maximum temp it has been exposed to is about 25 C.

Anyone know what causes this or if it affects sensitity or performance?

[Edited on 2-9-2017 by greenlight]

Pb(N3)2 when left into the air will hydrolyse...via two pathways:
1°) Pb(N3)2 + H2O --> Pb(OH)2 + 2 HN3(g)
2°) Pb(N3)2 + H2O + CO2 --> PbCO3 + 2 HN3(g)

The HN3(g) is toxic/poisonous and volatile just like HCN (cyanhydric acid).

Upon time sensitivity and performance will drop down...

PHILOU Zrealone - 4-9-2017 at 02:53

Quote: Originally posted by physics inclination  
What is this compound's name, if it has one? I've tried searching under several different names I thought it might be, but couldnt find any instance of it. Is it known to exist, and if so, is it usefully stable?

As mentionned Ninhydric1... 2-nitrotriazane
or alternatively
==> N,N-diamino-nitramide (nitramide is H2N-NO2)

If it ever exists it will only be as a transient species...even the lower members of the family are not that stable:
-nitro-hydrazine (H2N-NH-NO2) is not stable (adding an extra NH2 will not help at all)
-nitramide (nitro-ammonia H2N-NO2) has limited stability and very fast decompose autocatalytically to H2O, N2 and O2... apparently it is not stabilised by NH4(+) or N2H5(+) salt formation.

This is to be expected with free nitroazanes...
==> so not "uselfully stable"

Same applies to dinitramide (HN(NO2)2) what display only moderate stability...on its own ...
but here it can be greatly improved by NH3 or N2H4 salt formation...and this comes from the stabilizing effect of the second nitro group...and resonances structures of the dinitramide anion...

[Edited on 4-9-2017 by PHILOU Zrealone]

physics inclination - 4-9-2017 at 14:26

Quote: Originally posted by PHILOU Zrealone  

As mentionned Ninhydric1... 2-nitrotriazane
or alternatively
==> N,N-diamino-nitramide (nitramide is H2N-NO2)

If it ever exists it will only be as a transient species...even the lower members of the family are not that stable:
-nitro-hydrazine (H2N-NH-NO2) is not stable (adding an extra NH2 will not help at all)
-nitramide (nitro-ammonia H2N-NO2) has limited stability and very fast decompose autocatalytically to H2O, N2 and O2... apparently it is not stabilised by NH4(+) or N2H5(+) salt formation.

This is to be expected with free nitroazanes...
==> so not "uselfully stable"

Same applies to dinitramide (HN(NO2)2) what display only moderate stability...on its own ...
but here it can be greatly improved by NH3 or N2H4 salt formation...and this comes from the stabilizing effect of the second nitro group...and resonances structures of the dinitramide anion...

[Edited on 4-9-2017 by PHILOU Zrealone]


Thanks for good information, and yea I didnt expect it would be very stable, at least not on its own. But for similar compounds, if anyone's curious, I do have a few papers saying that some salts and metal complexes of them are somewhat stable:


Attachment: method of synthesizing triazanium perchlorate monohydrate.pdf (256kB)
This file has been downloaded 282 times

Attachment: synthesis characterization and crystal structures of Cu Ag and Pd dinitramide salts.pdf (156kB)
This file has been downloaded 377 times

Attachment: structure and stability of trinitramide.pdf (202kB)
This file has been downloaded 502 times

[edit: added another paper]

[Edited on 9-4-2017 by physics inclination]

Attachment: synthesis and modes of coordination of energetic nitramine ligands in copper 2 nickel 2 and palladium 2 complexes.pdf (1.7MB)
This file has been downloaded 294 times


PHILOU Zrealone - 4-9-2017 at 23:40

Quote: Originally posted by physics inclination  
Quote: Originally posted by PHILOU Zrealone  

As mentionned Ninhydric1... 2-nitrotriazane
or alternatively
==> N,N-diamino-nitramide (nitramide is H2N-NO2)

If it ever exists it will only be as a transient species...even the lower members of the family are not that stable:
-nitro-hydrazine (H2N-NH-NO2) is not stable (adding an extra NH2 will not help at all)
-nitramide (nitro-ammonia H2N-NO2) has limited stability and very fast decompose autocatalytically to H2O, N2 and O2... apparently it is not stabilised by NH4(+) or N2H5(+) salt formation.

This is to be expected with free nitroazanes...
==> so not "uselfully stable"

Same applies to dinitramide (HN(NO2)2) what display only moderate stability...on its own ...
but here it can be greatly improved by NH3 or N2H4 salt formation...and this comes from the stabilizing effect of the second nitro group...and resonances structures of the dinitramide anion...



Thanks for good information, and yea I didnt expect it would be very stable, at least not on its own. But for similar compounds, if anyone's curious, I do have a few papers saying that some salts and metal complexes of them are somewhat stable:

Nice articles, thanks.

I really like the triazane perchlorate one...

Too bad into most characterization they don't give interesting datas for detonics properties... except density... :(
==> Heat of formation, Enthalpy of decomposition, Calculated VOD, Temperature of decomposition, Impact sensitivity, ...

XeonTheMGPony - 5-9-2017 at 03:59

Quote: Originally posted by greenlight  
Just a quick question.
I made a small batch of PVA-coated lead azide for primary charge in dets. After I had pressed all I needed I left a small sample out to make sure it was storage stable. It is now four months later.
The only thing is that whatever part of the pile is in contact with the air becomes darker brown in colour from the original white of the batch and dearlens more on prolonged storage. I habe noticed this with other batches as well as I only make a small amount at a time.
I have attached a photo below after I transferred it onto a new piece of paper.
Maximum temp it has been exposed to is about 25 C.

Anyone know what causes this or if it affects sensitity or performance?

[Edited on 2-9-2017 by greenlight]


As others stated it is decomposing to lead oxide

For long term storage stable caps your components must be well dried and the cap hermetically sealed, as must your primaries!

A well dried cap is a very long storage stable cap!

Bert - 5-9-2017 at 10:12

There is considerable information available for high explosives based on mixtures of Potassium chlorate and nitrobenzene or of ammonium nitrate and nitromethane.

Do any know of data on mixtures of Potassium chlorate and nitromethane? VOD, impact and friction sensitivity? (high, one assumes...) STABILITY? Was there ever any industrial use made of this mixture?

A quick Google search shows some amateur experimental uses, and at least one video.

PHILOU Zrealone - 6-9-2017 at 01:33

Quote: Originally posted by Bert  
There is considerable information available for high explosives based on mixtures of Potassium chlorate and nitrobenzene or of ammonium nitrate and nitromethane.

Do any know of data on mixtures of Potassium chlorate and nitromethane? VOD, impact and friction sensitivity? (high, one assumes...) STABILITY? Was there ever any industrial use made of this mixture?

A quick Google search shows some amateur experimental uses, and at least one video.

The main problems with nitromethane (NM) are:
1°) It is near perfect OB
CH3-NO2 --> CO2 + 3/2 H2
3/2 H2 + 3/4 O2 --> 3/2 H2O
OB = -19,6%

This means that for perfect OB one needs 50% KClO3 and 50% NM (halve a mole of KClO3 to get 3/2 O vs 1 mole of NM thus 61g and 61g)

This will cause fast sedimentation of the KClO3...unless some active thickener gellig agent is used ==> Nitrocellulose is a good gelling agent.

Into ANNM and ANFO the % of liquid vs solid is low thus it can be held by capilarity forces into place without too much segregation.


2°) It is of low density... Nitrobenzene (NB) is slightly higher in density and DNB or DNT oils are much denser thus increasing VOD and detonic parameters of the oxydiser/fuel mix

3°) NB contains a lot more fuel (C and H atoms/bad OB) to burn so the heat of combustion per kg is much higher than NM...also one will need more solid vs the liquid to acheive a perfect OB mix and one will be closer to conventional ANNM/ANFO mixes with regards to solid/liquid ratio.

4°) NB has a higher viscosity, a lower inflamability and lower volatility than NM; viscosity will help in holding the mix stabler with regard to sedimentartion segregation; the other parameters will help for storage safety...

*************************************************
The problem with KClO3 is its dead weight counterpart... solid KCl into the detonations products...

NH4NO3 has the advantage to increase the overal gas generated during detonation process and thus the explosion mechanical work or blast pressure.

So better oxydisers would be (eventually with help of active/or energy rich fuel gelling agents stables vs the oxydisers):

A) Ammonium perchlorate ==> AP/NM
AP has a low VOD but a very high density; the low VOD is caused by its overoxygenation...adding NM will reveal its maximum power...

B) Hydrazinium nitrate ==> HN/NM

C) Hydrazinium pechlorate ==> HP/NM

D) Hydroxylamine nitrate ==> HAN/NM

E) Hydroxylamine perchlorate ==> HAP/NM

F) Urea perchlorate ==> UP/NM

G) Other oxydisers based on nitroform or dinitramide
==> HNF/NM (hydrazinium nitroformate (stable?)-NM)
==> ANF/NM (Ammonium nitroformate-NM)
==> HANF/NM (hydroxylaminium nitroformate (stable?)-NM)
==> UNF/NM (urea nitroformate (stable?)-NM)
==> HDN/NM (hydrazinium dinitramide (stable?)-NM)
==> ADN/NM (Ammonium dinitramide-NM)
==> HADN/NM (hydroxylaminium dinitramide (stable?)-NM)
==> UDN/NM (urea dinitramide (stable?)-NM)

******************************************
Sensitivity to impact or friction of KClO3/NM mix should be driven by the weakest explosive link... what is NM... thus not exceptionnal except if some conventionnal basic media is present to help.

Storage stability should be of no concern if KClO3 and NM are pure enough...and exempt of water...
KClO3 is uncompatible with acidic compounds... and NM is moderately acidic and only express its weak acidity if water is present... and KClO3 is not hygroscopic at all...it crystallizes/precipitates without water of hydration...


********************************
The use of higher homologues of NM like 1,2-dinitroethane (DNE) or 1,2,3-trinitropropane (TNPr) will bring more density to the mixes and allow those to reach regios of VOD (between 8,0-10 km/s) and very high brisance...



[Edited on 6-9-2017 by PHILOU Zrealone]

EM Short Question

UkAmateur - 13-9-2017 at 05:42

I hope these questions aren't regarded as overly kewlish and whilst they have probably been answered previously I have utse and read numerous posts with out a definitive answer being apparent.

But given this is the short question/quick answer thread I thought I may as well ask.

1, How much A.P. (acetone peroxide) is required to successfully initiate detonation of E.T.N (ethryitol tetranitrate)?

The ETN will be sensitized by addition of 15%(b.w) of aluminum powder. Containment will be a thin walled aluminum tube approx 6mm diameter.

2, How much ETN is required to successfully initiate detonation of nitrocellulose?
(Trinitrate, properly washed, neutralised, stabilized, dried and pressed to optimal density) containment varied.

I apologise in advance if these questions aren't suited to this thread and am happy for a moderator to delete or move to the appropriate thread or subsection if deemed necessary.

Many thanks in advance.

E2a I realise AP is less than an ideal primary and I loath to synth it again (been several years since I last did on account of a Darwin award worthy mistake on by behalf which very nearly lost me two fingers) but unless my UTC source of sodium azide comes through soon my options are limited to AP/HMTD. Its worth saying that both questions are at this point hypothetical. As I am still unconvinced that AP is worth the risk. Its amazing how convincing our little accidents can be eh..

Anyways just wanted to clarify as I'm not some 14yr old kid and have the appropriate respect for the compounds in question.

Again, many thanks
[Edited on 13-9-2017 by UkAmateur]

[Edited on 13-9-2017 by UkAmateur]

James Ikanov - 13-9-2017 at 19:52

I'm not often the sort to suggest this kind of thing, but if you can find an older car (I think pre-2004? google might be more informative) with intact original airbags, those systems primarily used sodium azide. You can gut them and strip them for sodium azide if you use the right tools and are very gentle about removing the gas generator.

I should clarify I've never personally attempted this method of procurement. But I read about it in a text written by someone I would qualify well as an expert in the field.

Either way, I'd say making Nickel Hydrazine Nitrate or a nitroguanidine derivative would both be highly preferable to AP. If neither could be produced, perhaps you could consider the MnO2 thermite initiator produced by another member of this forum?

j_sum1 - 13-9-2017 at 20:24

IIRC, Panache is our resident expert on airbag systems. And again, IIRC he does not recommend disassembly to recover NaN3.

Corrosive Joeseph - 13-9-2017 at 20:34

I once spent a night reading about obtaining sodium azide from airbags and came to the conclusion it was just too dangerous.


/CJ

NeonPulse - 13-9-2017 at 20:41

Quote: Originally posted by Corrosive Joeseph  
I once spent a night reading about obtaining sodium azide from airbags and came to the conclusion it was just too dangerous.


/CJ

I do this on video for my YT channel. The biggest bastard is separation of the KNO3 from the NaN3 which I have not succeeded in doing yet- not that I have really attempted to though. I dismantled two different airbags from two different car makers and there is a marked difference in construction of each unit but the idea is the same.

PHILOU Zrealone - 14-9-2017 at 02:00

Quote: Originally posted by UkAmateur  
I hope these questions aren't regarded as overly kewlish and whilst they have probably been answered previously I have utse and read numerous posts with out a definitive answer being apparent.

But given this is the short question/quick answer thread I thought I may as well ask.

1, How much A.P. (acetone peroxide) is required to successfully initiate detonation of E.T.N (ethryitol tetranitrate)?

The ETN will be sensitized by addition of 15%(b.w) of aluminum powder. Containment will be a thin walled aluminum tube approx 6mm diameter.

2, How much ETN is required to successfully initiate detonation of nitrocellulose?
(Trinitrate, properly washed, neutralised, stabilized, dried and pressed to optimal density) containment varied.

I apologise in advance if these questions aren't suited to this thread and am happy for a moderator to delete or move to the appropriate thread or subsection if deemed necessary.

Many thanks in advance.

E2a I realise AP is less than an ideal primary and I loath to synth it again (been several years since I last did on account of a Darwin award worthy mistake on by behalf which very nearly lost me two fingers) but unless my UTC source of sodium azide comes through soon my options are limited to AP/HMTD. Its worth saying that both questions are at this point hypothetical. As I am still unconvinced that AP is worth the risk. Its amazing how convincing our little accidents can be eh..

Anyways just wanted to clarify as I'm not some 14yr old kid and have the appropriate respect for the compounds in question.

Again, many thanks
[Edited on 13-9-2017 by UkAmateur]

[Edited on 13-9-2017 by UkAmateur]


Above the critical mass of detonation of the explosive into that diameter under the given density... but like many explosive material... it is not reliable D2D explosive...
==> This is the case of ETN / CTAP (cyclo-tri-aceton-peroxide)... depends on too many factors...
==> Trial error and better too much than too little... but that is not nice with regards to the inherent danger of CTAP...

It is said that ETN may be thermaly pushed to D2D with help of Aluminium under heating... so maybe a mild heating mix may do the trick (or a stronger one like exploding CuO/Al thermite.

Again ETN is not easy to D2D reliably especially in tiny amounts...

Better shift to SADS/SANC (Silver acecytlide double salt/ Silver acetylide nitrato complex)... pretty OTC and very easy to detonate even from minute amounts (without confinement what CTAP or ETN hardly do in so tiny amounts) by flame or heat > 180 °C.
==> When using KMnO4/glycerine... it detonates before the mix has the time to burst into flame...

[Edited on 14-9-2017 by PHILOU Zrealone]

UkAmateur - 14-9-2017 at 04:33

Thanks for the replies guys. I think I'm gonna shelve the AP idea for now. Even in minute amounts its just to dangerous (to handle/manipulate, the synthesis itself is easy and measures can be taken to reduce risks but when it comes to handling the dry product.. Well I don't need to elaborate)

I'll concentrate on acquiring the required reagents for other primaries first. And maybe look into docs method of detonating ETN caps too at the same time..

I've got plenty of chlorates available (and my cell can easily produce perchlorate too) so the perchlorate primaries are perhaps another option as well.

I was hoping to acquire sodium azide via the car airbag route as I have a friend in the car breaking business but reading a couple of the above posts it may not be as simple as I first hoped..

As is often the case, less speed = more haste.

This isn't the kind of hobby where rushing things brings you any medals. In fact, often the opposite.

I'll keep reading.

Again, many thanks.

Rosco Bodine - 14-9-2017 at 09:59

For sluggish, low efficiency / low impulse / slow DDT / slow self accelleration initiators there is a very real constraint of critical diameter that works against a practical design at below about 3/8" inch diameter for the initiator column. TCAP is only very marginally usable as an initiator even at that 3/8" diameter in an amount of several grams topped off with a first fire "kicker" of AP / bullseye putty as a low press loading "hand pressed" firing train. HMTD performs a little better, and DDNP still better. At a 1/4" inch column diameter, from my tests, which were not done on ETN or other sensitive base charge, none of the sluggish initiators will perform like they should. Reported by others NHN and other sluggish initiators are going to also require the larger diameter charge columns to be useful loadings.

As for the perchlorates, triaminoguanidine perchlorate over guanidine perchlorate could be an interesting combination of initiator and base charge.

PHILOU Zrealone - 15-9-2017 at 04:57

Quote: Originally posted by UkAmateur  
Thanks for the replies guys. I think I'm gonna shelve the AP idea for now. Even in minute amounts its just to dangerous (to handle/manipulate, the synthesis itself is easy and measures can be taken to reduce risks but when it comes to handling the dry product.. Well I don't need to elaborate)

I'll concentrate on acquiring the required reagents for other primaries first. And maybe look into docs method of detonating ETN caps too at the same time..

I've got plenty of chlorates available (and my cell can easily produce perchlorate too) so the perchlorate primaries are perhaps another option as well.

I was hoping to acquire sodium azide via the car airbag route as I have a friend in the car breaking business but reading a couple of the above posts it may not be as simple as I first hoped..

As is often the case, less speed = more haste.

This isn't the kind of hobby where rushing things brings you any medals. In fact, often the opposite.

I'll keep reading.

Again, many thanks.

Why not make hydrazine hydrogeno sulfate the conventionnal way (ammonia or urea and NaOCl (bleach)) and convert it to NaN3... plenty of receipe and info here into the forum or elsewhere on YouTube...

PHILOU Zrealone - 15-9-2017 at 05:05

Quote: Originally posted by Rosco Bodine  
For sluggish, low efficiency / low impulse / slow DDT / slow self accelleration initiators there is a very real constraint of critical diameter that works against a practical design at below about 3/8" inch diameter for the initiator column. TCAP is only very marginally usable as an initiator even at that 3/8" diameter in an amount of several grams topped off with a first fire "kicker" of AP / bullseye putty as a low press loading "hand pressed" firing train. HMTD performs a little better, and DDNP still better. At a 1/4" inch column diameter, from my tests, which were not done on ETN or other sensitive base charge, none of the sluggish initiators will perform like they should. Reported by others NHN and other sluggish initiators are going to also require the larger diameter charge columns to be useful loadings.

As for the perchlorates, triaminoguanidine perchlorate over guanidine perchlorate could be an interesting combination of initiator and base charge.

Nice data/infos Rosco :);)

The NiHN (Nickel nitrate hydrazino complex) is indeed too much on the edge between a primary/Secondary... that's why I developped the synergetical mix with SADS/SANC (1/1 to 2/1)... so:
1°) initiability of of the mix is strongly improved vs NiHN alone
==> reducing the needed amount and critical diameter of detonation allowing for a lower diameter detonator and shorter one (development distance of the D2D much shorter)
2°) overal power of the mix is improved vs SADS alone since NiHN is more brisant and display a higher VOD.

Hence the synergy :cool:;)

joseph6355 - 1-10-2017 at 05:12

I need a primary explosive that won't kill me easily, is chemically stable, can be synthesized at a home lab and is not TOO expensive to make.
HMTD is cool, but it is not chemically stable.
I need an explosive to make a blasting cap for my Dunnite. :)

Lead azide is not an option for me. It is very time demanding and expensive to make.

kratomiter - 1-10-2017 at 05:47

Quote: Originally posted by joseph6355  
I need a primary explosive that won't kill me easily, is chemically stable, can be synthesized at a home lab and is not TOO expensive to make.
HMTD is cool, but it is not chemically stable.
I need an explosive to make a blasting cap for my Dunnite. :)

Lead azide is not an option for me. It is very time demanding and expensive to make.


SADS, without any doubt.

kratomiter - 1-10-2017 at 08:30

I tried to sensitize nitromethane with a 5% epoxy curing agent based on polyamine. The PLX-like explosive is green, I put 6 grams inside a syringe I tried to detonate it with SADS/MHN (500 mg) without success. Should I add a booster or switch to another amine? EDA is hard to get.

PHILOU Zrealone - 1-10-2017 at 11:15

Quote: Originally posted by kratomiter  
I tried to sensitize nitromethane with a 5% epoxy curing agent based on polyamine. The PLX-like explosive is green, I put 6 grams inside a syringe I tried to detonate it with SADS/MHN (500 mg) without success. Should I add a booster or switch to another amine? EDA is hard to get.

What polyamine?
Maybe the amine group into your product is not basic enough to force the nitromethane to its nitronate form...
==> The nitronate form is responsible of the sensitivity.

joseph6355 - 1-10-2017 at 15:01

Quote: Originally posted by kratomiter  
Quote: Originally posted by joseph6355  
I need a primary explosive that won't kill me easily, is chemically stable, can be synthesized at a home lab and is not TOO expensive to make.
HMTD is cool, but it is not chemically stable.
I need an explosive to make a blasting cap for my Dunnite. :)

Lead azide is not an option for me. It is very time demanding and expensive to make.


SADS, without any doubt.

Hi! Thanks for answering.
By SADS you mean silver acetylide?
Doesn't seems hard to make. I can buy silver nitrate locally and recrystallize it, and then generate some acetylene gas.

How stable is it? Will it decompose or change its chemical structure in contact with metals, light, time?
I'd like to know more about it.

How much SADS would be required to detonate, lets say, 300g of dunnite?

kratomiter - 2-10-2017 at 06:13

Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by kratomiter  
I tried to sensitize nitromethane with a 5% epoxy curing agent based on polyamine. The PLX-like explosive is green, I put 6 grams inside a syringe I tried to detonate it with SADS/MHN (500 mg) without success. Should I add a booster or switch to another amine? EDA is hard to get.

What polyamine?
Maybe the amine group into your product is not basic enough to force the nitromethane to its nitronate form...
==> The nitronate form is responsible of the sensitivity.


Sorry, it wasn't a polyamine, it was a polyetheramine, so maybe is not basic enough. Next amine to try is hexamine.

kratomiter - 2-10-2017 at 06:15

Quote: Originally posted by joseph6355  
Quote: Originally posted by kratomiter  
Quote: Originally posted by joseph6355  
I need a primary explosive that won't kill me easily, is chemically stable, can be synthesized at a home lab and is not TOO expensive to make.
HMTD is cool, but it is not chemically stable.
I need an explosive to make a blasting cap for my Dunnite. :)

Lead azide is not an option for me. It is very time demanding and expensive to make.


SADS, without any doubt.

Hi! Thanks for answering.
By SADS you mean silver acetylide?
Doesn't seems hard to make. I can buy silver nitrate locally and recrystallize it, and then generate some acetylene gas.

How stable is it? Will it decompose or change its chemical structure in contact with metals, light, time?
I'd like to know more about it.

How much SADS would be required to detonate, lets say, 300g of dunnite?


My SADS is stable enough stored under ethanol in a dark place. I think dunnite is quiet insensitive, maybe you need a booster to detonate it, like picric acid.

joseph6355 - 2-10-2017 at 08:31

Quote: Originally posted by kratomiter  

My SADS is stable enough stored under ethanol in a dark place. I think dunnite is quiet insensitive, maybe you need a booster to detonate it, like picric acid.

Nice.
Since you mentioned solubility, how soluble is SADS in ethanol, acetone and other solvents? The wikipedia article states that it is insoluble in water.
If it is insoluble in ethanol, it is indeed a good choice of chemical, since it would dry the SADS much faster than water.

How much SADS can I store safely together, in the same container?

Thanks! :D

PHILOU Zrealone - 2-10-2017 at 17:00

Quote: Originally posted by kratomiter  
Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by kratomiter  
I tried to sensitize nitromethane with a 5% epoxy curing agent based on polyamine. The PLX-like explosive is green, I put 6 grams inside a syringe I tried to detonate it with SADS/MHN (500 mg) without success. Should I add a booster or switch to another amine? EDA is hard to get.

What polyamine?
Maybe the amine group into your product is not basic enough to force the nitromethane to its nitronate form...
==> The nitronate form is responsible of the sensitivity.


Sorry, it wasn't a polyamine, it was a polyetheramine, so maybe is not basic enough. Next amine to try is hexamine.

Polyetheramine are in principle basic enough, but everything depends onto the molecular structure of it some have very large carbonaceous counterpart vs the amine moiety; hence the amount of product to acheive same sensitizing effect as ammonia or ethylene diamine will be much higher than 5% by weight can be 10, 15, 20% or even more for very high MW polyetheramine with little amino groups unit per molecule...

Hexamine is not basic enough... you can eat it...
It was used as ancient cure for urinal infections hence the name of urotropine... this effect is obtained by the slow hydrolysis of the hexamethylenetetramine and slow release of formaldehyde (bactericide but also carcinogen) and of basic counterpart.
Hydrolysis only occure into waterous media...

You will have more chance to allow some NM (nitromethane) to react with formaldehyde to get dinitropropane, nitroethanol, nitroethene, 2-nitropropandiol or nitroisobutyltetrol...then reduce this by SnCl2/HCl to get the amines from it and to allow this to mix after isolation with NM...

PHILOU Zrealone - 2-10-2017 at 17:11

Quote: Originally posted by joseph6355  
Quote: Originally posted by kratomiter  

My SADS is stable enough stored under ethanol in a dark place. I think dunnite is quiet insensitive, maybe you need a booster to detonate it, like picric acid.

Nice.
Since you mentioned solubility, how soluble is SADS in ethanol, acetone and other solvents? The wikipedia article states that it is insoluble in water.
If it is insoluble in ethanol, it is indeed a good choice of chemical, since it would dry the SADS much faster than water.

How much SADS can I store safely together, in the same container?

Thanks! :D

SADS is pretty much insoluble in any solvent except very basic or acidic ones...

SADS is silver acetylide double salt or SANC silver acetylide nitrato complex... it is related to silver acetylide but it is not the same.

SA = Ag2C2
SANC/SADS = Ag2C2.xAgNO3 or Ag2C2.xAgNO3.yHNO3

The fact SANC/SADS contains nitrate into its complex structure allows form more energetic output and power... since the oxygen will help burning part of the acetylen carbonaceous fuel... but not all as proven by the fact that the addition of KClO3 increases the power up to 40% by weight vs plain SADS/SANC ==> so not enough oxydizer present for perfect OB (oxygen balance)

There are plenty of info about it all over the energetic section ==> Use the search engine ;)
==> The safe amount to handle depends onto the operator, his ability to make the product pure following good procedures and onto the container.

I have had more than 15 grams stored at the same place under a granulated form with finer powder parts for long time.

Avoid light exposure for too long especially strong halogen ones and UV (like from the sun)... avoid too much friction, shock and heat... 150°C can set it off.

[Edited on 3-10-2017 by PHILOU Zrealone]

joseph6355 - 2-10-2017 at 17:17

Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by joseph6355  
Quote: Originally posted by kratomiter  

My SADS is stable enough stored under ethanol in a dark place. I think dunnite is quiet insensitive, maybe you need a booster to detonate it, like picric acid.

Nice.
Since you mentioned solubility, how soluble is SADS in ethanol, acetone and other solvents? The wikipedia article states that it is insoluble in water.
If it is insoluble in ethanol, it is indeed a good choice of chemical, since it would dry the SADS much faster than water.

How much SADS can I store safely together, in the same container?

Thanks! :D

SADS is pretty much insoluble in any solvent except very basic or acidic ones...

SADS is silver acetylide double salt or SANC silver acetylide nitrato complex... it is related to silver acetylide but it is not the same.

SA = Ag2C2
SANC/SADS = Ag2C2.xAgNO3 or Ag2C2.xAgNO3.yHNO3

The fact SANC/SADS contains nitrate into its complex structure allows form more energetic output and power... since the oxygen will help burning part of the acetylen carbonaceous fuel... but not all as proven by the fact that the addition of KClO3 increases the power up to 40% by weight vs plain SADS/SANC ==> so not enough oxydizer present for perfect OB (oxygen balance)

There are plenty of info about it all over the energetic section ==> Use the search engine ;)
==> The safe amount to handle depends onto the operator, his ability to make the product pure following good procedures and onto the container.

I have had more than 15 grams stored at the same place under a granulated form with finer powder parts for long time.

Avoid light exposure for too long especially strong halogen ones and UV (like from the sun)... avoid too much friction, shock and heat... 150°C can set it off.

[Edited on 3-10-2017 by PHILOU Zrealone]

Thanks for the info.
Do I synthesize SADS from SA or I have to approach it differently?

PHILOU Zrealone - 3-10-2017 at 04:04

Quote: Originally posted by joseph6355  
Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by joseph6355  
Quote: Originally posted by kratomiter  

My SADS is stable enough stored under ethanol in a dark place. I think dunnite is quiet insensitive, maybe you need a booster to detonate it, like picric acid.

Nice.
Since you mentioned solubility, how soluble is SADS in ethanol, acetone and other solvents? The wikipedia article states that it is insoluble in water.
If it is insoluble in ethanol, it is indeed a good choice of chemical, since it would dry the SADS much faster than water.

How much SADS can I store safely together, in the same container?

Thanks! :D

SADS is pretty much insoluble in any solvent except very basic or acidic ones...

SADS is silver acetylide double salt or SANC silver acetylide nitrato complex... it is related to silver acetylide but it is not the same.

SA = Ag2C2
SANC/SADS = Ag2C2.xAgNO3 or Ag2C2.xAgNO3.yHNO3

The fact SANC/SADS contains nitrate into its complex structure allows form more energetic output and power... since the oxygen will help burning part of the acetylen carbonaceous fuel... but not all as proven by the fact that the addition of KClO3 increases the power up to 40% by weight vs plain SADS/SANC ==> so not enough oxydizer present for perfect OB (oxygen balance)

There are plenty of info about it all over the energetic section ==> Use the search engine ;)
==> The safe amount to handle depends onto the operator, his ability to make the product pure following good procedures and onto the container.

I have had more than 15 grams stored at the same place under a granulated form with finer powder parts for long time.

Avoid light exposure for too long especially strong halogen ones and UV (like from the sun)... avoid too much friction, shock and heat... 150°C can set it off.

[Edited on 3-10-2017 by PHILOU Zrealone]

Thanks for the info.
Do I synthesize SADS from SA or I have to approach it differently?

As explained the search engine is your friend...
Ag2C2.x AgNO3 - SADS - SANC

Armstrong's mixture, powerful primary ?

Hexogen - 10-10-2017 at 12:00

I understand the instability of Armstrong's mixture due to it composing of a strong oxidizer and red phosphorous.

Would it be possible to set off a mix of 9:1 mix of KClO3 and PIB
(Polyisobutylene) ?

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