Sciencemadness Discussion Board

Exotic Primaries - Complex Salts

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NeonPulse - 2-4-2016 at 23:28

I'm curious about this mentioned compound on the bottom of this page: https://sites.google.com/site/ecpreparation/nickel-hydrazini...
The author mentions a clathrate compound comprising of up to 10% AgN3 and the other 90% NHN. how do you think one would go about making such a clathrate? or is it more likely to be just a double salt of the two and not a true clathrate? it says the mixture is co-crystallized from a solvent, which is not mentioned.
Has anybody here heard of this compound before or had experience with it? it does sound interesting.

PHILOU Zrealone - 6-4-2016 at 07:45

Quote: Originally posted by a nitrogen rich explosive  
I have just synthesised 5 grams of zinc tetramine permanganate through the reaction of KMnO4 with an excess of a solution of 3% ammonia, zinc oxide and ammonium chloride. The temperature must be kept to a minimum without freezing, because the resulting product (Zn(NH3)4)(MnO4)2 decomposes with H2O. It is therefore unusable, with a shelf life of 1-2 hours, due to moisture in the air.

However, I was thinking: would it be possible to synthesise something like nickel tetramine permanganate (Ni(NH3)4)(MnO4)2 or cobalt/silver tetramine persulfate/nitrate? It would, but I don't know how energetic they'd be.

Any ideas?

Why posting the very same kind of questions in various treads of the energetic materials?
here and here too

If it is so sensitive to moist air, how do you cope with the 97% water content of your NH3?

No it would not!
If it does, Nickel will make a hexaamino complex and not a tetramino; so does Cobalt.
Silver will at best make a diamino complex.


[Edited on 6-4-2016 by PHILOU Zrealone]

PHILOU Zrealone - 6-4-2016 at 08:32

Quote: Originally posted by NeonPulse  
I'm curious about this mentioned compound on the bottom of this page: https://sites.google.com/site/ecpreparation/nickel-hydrazini...
The author mentions a clathrate compound comprising of up to 10% AgN3 and the other 90% NHN. how do you think one would go about making such a clathrate? or is it more likely to be just a double salt of the two and not a true clathrate? it says the mixture is co-crystallized from a solvent, which is not mentioned.
Has anybody here heard of this compound before or had experience with it? it does sound interesting.

I think it is a website from user AndersHoveland, sadly he hasn't post here since end 2013 and didn't show here since 2014.

Sadly also the website and its various clones, are a collection of ideas of AH himself and copy paste from various sources but usually without references...and just like its author a bit confuse and missing coherence/structure.
Anders was used to post weird receipts from obscure or unreferenced sources...

I even noticed in your link my own receipt for NiHN from mixing of alcoholic hydrazine and Ni(NO3)2 solutions, but of course omitting the source (me and this forum)...:mad::(

For the rest, any mixing of NHN with a compatible unsoluble sensitive primary will make a symbiotic mix beneficial to both compounds...lowering the sensitivity of the primary and sensitizing NHN making it more reliable for D2D; NHN will give its power and high VOD.
I have used silver nitrato acetylide complex.
I guess AgN3 would be even better.
I don't know how it would be done as a cocrystalisate...it all depends if Ni(N3)2 is unsoluble or not and how it will react with hydrazine...Ni(N2H4)3(N3)2 may form if I recall correctly.

Maybe mixing Ni(N2H4)3(NO3)2 with AgN3 in NH4OH will do the trick, but if I recall wel from my own experience ammonia destroys the hydrazino complex...but maybe I have mistaken solubilisation with destruction...because in theory Ni(N2H4)3(NO3)2 should be in equilibrium with Ni(NH3)6(NO3)2 and if the system is open while NH3 evaporates faster than N2H4, then the initial unsoluble complex will redeposit aside with AgN3.


[Edited on 6-4-2016 by PHILOU Zrealone]

kratomiter - 13-5-2016 at 08:48

Recently I made two batches of NHN. The first was blue and very impure, I think EtOH made Calcium Hydroxide precipitate along the NHN. The second batch, this time without EtOH, seems to be fairly pure and was washed 2 times with water. But I'm turning crazy trying to detonate it.
The only way I get a DDT was heating it in a 5mm diameter copper pipe, both sides sealed. It requires strong confination and behaves more like a nitrated polyol.
What's the best way to detonate it? Maybe flash powder? I could try to sensitize it with another primary, but I don't wanna mess with azides. At the moment I only could try mixing it with DDNP or DNPH.

Eosin Y - 13-5-2016 at 09:52

Detonation with some kind of super flash might be an idea.

Copper tetraammine azide/copper hydrazine azide might be interesting. However, I doubt that CuTA would be stable enough to not leak ammonia.

PHILOU Zrealone - 14-5-2016 at 09:22

Quote: Originally posted by Eosin Y  
Detonation with some kind of super flash might be an idea.

Copper tetraammine azide/copper hydrazine azide might be interesting. However, I doubt that CuTA would be stable enough to not leak ammonia.

How do you do to make Cu azide hydrazino complex?
And thus avoid the decomposition of the hydrazine (reducer) by the Cu(2+) oxydant?

PHILOU Zrealone - 15-5-2016 at 07:16

Quote: Originally posted by Eosin Y again  
I thought that the Cu2+ ion was only repellant to the O2 ion, and that copper hydrazino azide would stay together like copper peroxide.

Why "Eosin Y" and now "Eosin Y again" ?

Don't think, verify first!

Could you elaborate?
1°) Cu(2+) repellant to O2?
2°) O2 ion?
3°) Cu peroxide? How do you do this and stabilize it?

Eosin Y again - 15-5-2016 at 07:28

I'm surprised that you didn't notice the quad-trainwreck with me, Bert, Aga, and Blogfast that ended up in Bert going off in a rage and removing Eosin Y's posting priviledges.

https://en.wikipedia.org/wiki/Copper_peroxide

Schweizer's reagent and H2O2.

Bert - 15-5-2016 at 10:25

Rage was not involved. My mother was a psychologist, I only feel sadness when I run into the damaged people who act out on the net due to their mental health issues . And a desire to get them into a proper treatment regime where they may learn to act appropriately in public, perhaps eventually leading a normal life.

Why didn't you even bother to mask your ip while running the troll accounts this time? Before, you at least TRIED to hide. Using enormousdick@hotmail.com for a sign up email address, is it a cry for help, or merely the arrogance of a sociopath.

octonitrocubane, a nitrogen rich explosive, eosin-y and eosin-y again. Part of your psychopathology requires you to let others know that you have had them on and wasted their time? Or it's no fun to pretend to be an English schoolboy until you are caught?

[Edited on 15-5-2016 by Bert]

PHILOU Zrealone - 16-5-2016 at 04:44

I had a good intuition/feeling that those 4 pseudos were in fact the same person :).

PHILOU Zrealone - 16-5-2016 at 04:49

Quote: Originally posted by Eosin Y again  
I'm surprised that you didn't notice the quad-trainwreck with me, Bert, Aga, and Blogfast that ended up in Bert going off in a rage and removing Eosin Y's posting priviledges.

https://en.wikipedia.org/wiki/Copper_peroxide

Schweizer's reagent and H2O2.

So following your link CuO2 is just like I wrote unstable.
But CuO2 will have much gentle consequences than your putative Cu(N2H4)2(N3)2 because this last would be explosive.

KesterDraconis - 14-6-2016 at 09:20

So I tried the synthesis of NHN and I got a blue precipitate. However it did not change lilac purple, but instead stayed blue, even when I agitated the solution a bit and added more of the nickle nitrate solution. I'm letting it dry now, but its still not changing. Is there a reason for this odd/out of place color?

NHN

Laboratory of Liptakov - 14-6-2016 at 11:22

Will be better added hydrazine, not NiNO3. Small amount hydrazine = blue. Surplus Hydrazine = lila. If you has pure materials. If you has Hydrazine and NiNO3, is impossible any another reaction. Arises NHN. In a small surplus hydrazine hydrate. ...LL..:cool:

PHILOU Zrealone - 14-6-2016 at 12:39

Yes LL is right!
When adding Ni(NO3)2 to N2H5OH at first without agitation you get locally a blue flocculating precipitate (where the green concentrated drop of Ni(2+) crashes to the bottom of the beaker...
When you mix it, it turns lilac pink with the surrounding exces of N2H5OH.
--> You had too much Ni(2+) and too less/not enough N2H4.
Meaning you have transition/uncomplete complexation like Ni(N2H4)(NO3)2, Ni(N2H4)2(NO3)2 and maybe traces of Ni(N2H4)3(NO3)2 ...
But not plain Ni(N2H4)3(NO3)2.


[Edited on 14-6-2016 by PHILOU Zrealone]

KesterDraconis - 14-6-2016 at 20:07

Ah, this actually makes sense, on a second attempt I noticed it was lilac purple for a bit, then turned blue and stayed that way. When this precipitate was dried, I found myself with a substance that did not burn very well, but surprisingly made a nearly unnoticeable popping sound when confined. I will try again tomorrow and do the reverse by adding the hydrazine to the nickle nitrate, and add it in greater quantity (though I'm trying to keep things very small here, for obvious reasons).

I will report back here with results in a few days, thanks!

NHN

Laboratory of Liptakov - 15-6-2016 at 00:45

Well, here is difference between not complete reaction (1) and result complete reaction with surplus hydrazine (2) Use HH 80%....LL...:cool:

nhn.jpg - 323kB

KesterDraconis - 19-6-2016 at 17:45

I would like to thank all the members here for all the contributions to my successful synthesis of NHN, particularly PZ and LL here. It really is a wonderful color change (one of my favorite colors is lilac purple actually), and I was very impresses and pleased with the explosives characteristics. If I were one to set off large charged (which I am not, I prefer tiny bits of smaller things, for experimentation) I would probably use this, low friction and impact sensitivity, but high enough flame sensitivity to be useful in the amounts necessary to act as a primary. Very good all around it seems.

Thanks again for the help guys, I can finally check this off my list of "things I would like to synthesize and experiment with". (about time too, its been on the list a year!)

NHN

Laboratory of Liptakov - 20-6-2016 at 01:14

Well, NHN is beauty and even has nice smell. Thus my experience. Pretty silent a flame. As nitrocellulose, but still speeding. Until detonation. (huhaha). But my experience is difficult transfer to fully velocity on 7000 m/s. At 1.7g /cm3. However, is it the way, it is development. ..:cool:...LL

PHILOU Zrealone - 20-6-2016 at 03:49

Yes!
Unlike other primaries NiHN is not reliable in too low/tiny quantities...this means that the D2D transition is not effective below a certain amount that is quite large vs real primaries.:(

NiHN doesn't detonate unconfined except in even larger quantities displaying enough self-confinement.:(

When wrapped in Al foil (confined) and heated by a flame it deflagrates/detonates with a very loud report and huge fire ball.
When 100 mg of such wrapped stuff is trown into a camp fire, after a second or more, it makes a fire ball of about 40 cm diameter and trows incandescent charcoal all arround a few meters away!:D;):P:)

I use the co-mix of SADS/SANC (silver acetylide double salt, silver acetylide nitrato complex) with NiHN to circumvent this lack of reliability (mix SADS/NiHN 1/3 to 1/4 by weight).
Since both are unsoluble clayish stuffs (white creamy and lilac pink...the resulting mix is paler lilac pink).
This is synergetic co-mix because SADS offers immediate D2D and flame sensitivity even in minute amount, while NiHN offers its brisance, higher VOD, and energy output.:cool::cool::cool:

I'm more than eager to follow the results of Laboratory of Liptakov about the improvement of NiHN D2D without help of a conventional primary (NPD detonator) like/based on the now famous Berta kind he designed/invented...:o:o:o;):)

NHN

Laboratory of Liptakov - 21-6-2016 at 03:35

Well, well... Thanks. Was making next 3 tests, about NiHN. Without SADS mixing, but with partially using copper hexamine perchlorate, respectively was used this mix: Tetraamine Copper Perchlorate 88% + 6% hexamine + 6% NH4ClO4. Boiled together by 100 Celsius, evaporated by 60 C. The Grain 1x1mm. For NiHN (DDT segments) was used this mix: NiHN 94% nitrocellulose 4% magnesium 2%. Nitrocellulose is necessary for making aglomerate 1x1 mm, for best function of detonation transfer. (DDT) Magnesium should by increase DDT also.

Next. First attempt (red 1) was used for output segment pure NiHN 0,3 grams, it see on scheme. Other segments are NiHN mix described. From result is clearly, that NiHN was detonated, or partially detonated. This is the sharp edge around in steel 2mm thickness. Thus DDT worked. But not much power. But good detonation (power) for using next secondary segment ETN.

Second attempt, (red 2) was used same output segment from NiHN (0,3 pure grams), but other material in next segments was CHP (described up) . Again from aglomerate basically large by 1x1 mm. It see, that energy was bigger. It maybe was a full detonation NiHN.

For comparsion was (red 3) using only CHP for all segments. Thus system Berta on Copper hexamine perchlorate (CHP) based. All attempts are not in system NPED, because NiHN and CHP are primary substance. But both compounds has much more safety, than HMTD and relatives. All others important is in scheme, how I hope. ...LL...:cool:









NHN results123a.jpg - 167kB

NHN scheme Berta a.jpg - 64kB

[Edited on 22-6-2016 by Laboratory of Liptakov]

KesterDraconis - 21-6-2016 at 17:18

Quote: Originally posted by PHILOU Zrealone  

I use the co-mix of SADS/SANC (silver acetylide double salt, silver acetylide nitrato complex) with NiHN to circumvent this lack of reliability (mix SADS/NiHN 1/3 to 1/4 by weight).
Since both are unsoluble clayish stuffs (white creamy and lilac pink...the resulting mix is paler lilac pink).
This is synergetic co-mix because SADS offers immediate D2D and flame sensitivity even in minute amount, while NiHN offers its brisance, higher VOD, and energy output.:cool::cool::cool:


I actually like this idea, since it helps to get rid of the one con of SADS, which is its low power. :D If only I could make some more to experiment with, but alas, I used up the last of my hydrazine, and have no time to make more before my university summer classes begin. I will save it for Christmas break I think. :(

I also appreciated the experiments LL! I find it odd that the NHN doesn't seem to be producing very much power and detonating fully. I noticed the batch I made was very very reluctant to detonate at all, but I'm still surprised that it doesn't detonate in the manner you are using it. Perhaps it would simply be best as you said, to use something like number 2, and an ETN secondary. You could then use that as your booster for larger charges, and still have some of the safety of the NHN.

Rosco Bodine - 21-6-2016 at 21:51

@Laboratory of Liptakov please edit and limit image width to 650 pixels because it destroys the page format for 4X5 aspect ratio monitors, when larger images are placed inline.

Thanks for the image resizing. It looks better now.

NHN is critical diameter sensitive for DDT and should transition upward in velocity with a significant jump in brisance at a larger charge diameter, and I'll have to check my references to confirm but IIRC it was in the area of 9-10 mm. It isn't uncommon for slow self accellerating primary explosives, and there are several others that show the same sluggishness, but above a certain diameter and above a certain critical mass, which for some might even be several grams ....will get the job done when they do go high order.

It could be a different method of synthesis could produce a more dense crystalline form of NHN that would perform better.

I have wondered if instead of using hydrazine hydrate, maybe try hydrazine nitrate in presence of ammonia as the hydrazine value.

Possibly just take hydrazine sulfate and render more soluble as the neutral dihydrazine salt by adding an equivalent of ammonia, then add a solution of calcium nitrate to precipitate the sulfate as calcium sulfate and filter out leaving a solution of hydrazine nitrate. Simultaneously add gradually nickel nitrate and additional ammonia in separate streams dropwise with stirring and low heating. Such an approach might allow for crystal growth of the low solubility NHN, if it will form under such conditions as I am thinking it will form by a more gradual and slower reaction.

It may be possible also to simultaneously form and introduce some azide content by utilizing a nitrite of nickel in mixture with the nickel nitrate, possibly forming the nickel nitrite by adding sodium nitrite to react with some of the nickel nitrate solution.

In the alternative, putting an azide like sodium azide in solution with the ammonia to be added dropwise separately, parallel with the nickel nitrate solution, to the ammoniated hydrazine nitrate solution. Possibly some azide content in the NHN could improve its self accelleration and small diameter performance.

[Edited on 6/22/2016 by Rosco Bodine]

NHN

Laboratory of Liptakov - 22-6-2016 at 01:00

If you have ETN and NiHN is easily do it prepare DDT mix: ETN 70% + NiNH 25% + 5% nitrocellulose for better agglomerates 1x1 mm. All is mixed in acetone, a few a drops. Arises paste, through the sieve do it agglomerate and slowly dry process evaporate acetone by 40 Celsius. This deflagration - detonation mix is filled according scheme. Only output segment is from pure ETN. His Pressing can be higher cca 100 Kg on 6mm diameter. This construction worked perfectly always. Ratio ETN-NiHN for DDT segments can be pretty free arbitrary. For example even 50 : 50. And worked it. Necessary is content (4 - 7%) nitrocellulose, commerce grade, thus with content nitrogen 12 - 12,6 %. I not recommend homemade NC, because is usually with residuum acid...:cool:...LL

Rosco Bodine - 22-6-2016 at 01:41

ETN has a good but limited shelf life ~4-5 years and is not so good at warmer temperatures, so for long term storage devices ETN is not viable. You have an expiration date on anything in which you use ETN. In the alternative, there are other more stable materials for which the shelf life is indefinite, perhaps even hundreds of years. PETN would be better for long storage, and likely p-DDNP would be better also, though the power output would be reduced compared to ETN or PETN....as an OTC material p-DDNP could have advantages over ETN if there was need for long storage endurance.

[Edited on 6/22/2016 by Rosco Bodine]

NHN

Laboratory of Liptakov - 22-6-2016 at 02:31

In system Berta of course worked also PETN. I had to write directly together upstairs, sorry. One different is only this, that content of nickel hydrazine nitrate must be (in DDT mix) between 50 - 40 %. Lower content shows on some failed. At 20% for example. All others parameters are same, prepare, pressing according the scheme here upstairs. ...:cool:...LL

Rosco Bodine - 22-6-2016 at 03:26

The thought I was describing above about a possible alternative synthesis approach could result in a coprecipitation or possible double salt of nickel hydrazine nitrate and nickel hydrazine azide described on the preceding page by Mr.Greenix

http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...

I don't know if this has ever been tried before or proposed as an experiment

PHILOU Zrealone - 22-6-2016 at 03:34

@Rosco and LL,
If I remember correctly (IIRC) LL has made a comparative study of various copper detonators diameters with NiHN against witness plate... 4, 6, 8 mm that indeed showed that too low a diameter resulted in unefficient detonation...

Correct?

Rosco Bodine - 22-6-2016 at 03:46

There was a patent GB821586 I posted early in the thread that claimed IIRC the diameter had to be above a certain range for the DDT of the NiHN to be assured.

http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...

Adding some silver nitrate and sodium nitrite with the nickel nitrate being added to the hydrazine nitrate could result in silver azide being produced concurrently and copreciptated in the NiHN .....and that could be interesting too if it works

[Edited on 6/22/2016 by Rosco Bodine]

MineMan - 26-6-2016 at 16:18

LL and Rosco,

ETN has proved to be very impact sensitive from my experiments... just a light hammer tap (8oz hammer) while NiHN is 80cm drop with a 2kg weight. Both of you already know this, but my point is aren't we going backwards if we use ETN as a base, or a mix? Certainly it is better than HMTD and AP... but that is not saying much.

LL I don't have any NIHN so could you try a experiment for me for a NEPD?;)

Mix 1 gram of:
.8-NiHN
.15-Potassium Perchlorate
.05-Mg Power (preferably 1000mesh or below)

Then take .2grams of this mixture and place it in the center of a 4cm x 4cm piece of aluminum foil and insert a fuse in the center of the mixture and fold the corners of the foil square around the fuse and twist around the fuse and compress with the fingers.

After this, take 6cm x 6cm piece of Al foil and place .5 to .8grams of the above mixture in the center, then place the above made initiator inside of this and fold the corners around the fuse and twist (like above) and compact with the fingers. The resultant should be the shape of an over sized raindrop/teardrop, with the tail being the fuse. Then wrap 1 or 2 more pieces of Al foil around this and compact with the fingers, then wrap some electrical tape around it for further confinement.

I am hoping this will produce a completely safe NEPD which forces the mixture (in the outer layer) to go from DDT because of the resulting pressure from the inner mixture:D

MineMan - 26-6-2016 at 17:10

Right after I typed the above I decided to go into the garage and perform some more sensitivity test with ETN to "prove" my conviction that ETN should still be avoided.

Oftentimes a flick of the wrist with a hammer (8oz) will set a few milligrams off when folded in Al foil and set on another hammer, sometimes fully, sometimes partially. And sometimes it will not set it off...but that still bothers me... maybe it is an OCD thing but I would like to avoid ETN altogether.

LL I hope you are willing to perform the above experiment for me, and even more so, I hope it works...!

PHILOU Zrealone - 28-6-2016 at 02:45

Quote: Originally posted by MineMan  
Right after I typed the above I decided to go into the garage and perform some more sensitivity test with ETN to "prove" my conviction that ETN should still be avoided.

Oftentimes a flick of the wrist with a hammer (8oz) will set a few milligrams off when folded in Al foil and set on another hammer, sometimes fully, sometimes partially. And sometimes it will not set it off...but that still bothers me... maybe it is an OCD thing but I would like to avoid ETN altogether.

LL I hope you are willing to perform the above experiment for me, and even more so, I hope it works...!

Hand hammer testing is not reliable since:
-you get a mix of shock and friction (slight twisting from the wrist)
-the speed of the hammer and the strenght you apply on it is hard to evaluate
-multiple hits heats the substrate that becomes more sensitive (usually when the first strike doesn't work, people hit several times)
-the effective surface contact of the hammer and angle of percussion is hard to evaluate and to repeat precisely...often hammer surface is curved by use so if the sample is perfectly centered it will get more energy (pressure per surface) than a little asside

For all those reasons it is better to use a machine for the testing following the recommandations of international testing normalisation.

Also impact sensitivity testing is a mather of statistics...usually defined as the 50% out of 10 trials that crackled, took fire, deflagrated or detonated after impact...
So for example if IS is 20cm for 2kg weight (roughly 20 N for 0.2m or 4 Nm); this means that:
-5 trials out of 10 where positive by using 2kg weight falling from 20 cm
-increasing the weight or the height will increase the chances of positive result ...
For example
at 21 cm 6+/10 trials,
at 22 cm 8+/10 trials
and at 23 cm 99+/100 trials
-decreasing the weight or the height will reduce the chances of firing...
For example
at 19 cm 3/10,
at 18 cm 1/10,
at 17 cm 1/100,
and at 16 cm 1/1000.

[Edited on 29-6-2016 by PHILOU Zrealone]

MineMan - 28-6-2016 at 18:00

PH Z,

you make some great points and I agree with them all. But I don't have an apparatus to test as such, and I think the hammer test still gives a good indication of whether a EM is:

-Will never go off through impact (ANFO)
- Extraordinarily stable (TNT, ANAl)
-Stable (RDX)
-Sensitive (PETN)
-More sensitive (ETN,SADS)
-Very Sensative (Lead Azide)
-Then substances such as HMTD and AP

I would love to see some official numbers for ETN and SADS though...

PHILOU Zrealone - 29-6-2016 at 02:18

Quote: Originally posted by MineMan  
PH Z,

you make some great points and I agree with them all. But I don't have an apparatus to test as such, and I think the hammer test still gives a good indication of whether a EM is:

-Will never go off through impact (ANFO)
- Extraordinarily stable (TNT, ANAl)
-Stable (RDX)
-Sensitive (PETN)
-More sensitive (ETN,SADS)
-Very Sensative (Lead Azide)
-Then substances such as HMTD and AP

I would love to see some official numbers for ETN and SADS though...

Some forum members have made nice devices...search for the tread.
When I will have time (after my ex-girlfriend has left home) I will for sure build one such device...imperative if you want to test energetic materials qualitatively.

MineMan - 30-6-2016 at 13:44

PH Z,

I look forward to seeing the results, please share with us all!

Iron (III) Acetate Oxide Persulfate Trihydrate (?)

Σldritch - 30-7-2016 at 10:14

I tried to prepare the compound in the title and i think i have suceeded.
The name is kind of crazy so i will just say it is the persulfate salt of basic iron (III) acetate, also im not even sure about the name of the title but thats my best guess.

Anyway it was prepared from basic iron (III) acetate dissolved in water wich was mixed with sodium persulfate solution and then diluted with denatured alcohol. The resulting precipitate was filtered off and dried.

It is obviously not very energetic considering the poor oxygen balance, the water, carboxyl groups and iron but it fizzles when a burning match is held above it. It also gives an ocasional pop but it just melts itself too a yellow-ish goop.

Anyway ill try making the nitrate but i think i read somewhere it is very unstable but i can not find the document.

PHILOU Zrealone - 30-7-2016 at 11:20

Quote: Originally posted by Σldritch  
I tried to prepare the compound in the title and i think i have suceeded.
The name is kind of crazy so i will just say it is the persulfate salt of basic iron (III) acetate, also im not even sure about the name of the title but thats my best guess.

Anyway it was prepared from basic iron (III) acetate dissolved in water wich was mixed with sodium persulfate solution and then diluted with denatured alcohol. The resulting precipitate was filtered off and dried.

It is obviously not very energetic considering the poor oxygen balance, the water, carboxyl groups and iron but it fizzles when a burning match is held above it. It also gives an ocasional pop but it just melts itself too a yellow-ish goop.

Anyway ill try making the nitrate but i think i read somewhere it is very unstable but i can not find the document.

The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...

Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.

[Edited on 30-7-2016 by PHILOU Zrealone]

Σldritch - 30-7-2016 at 11:50

Quote: Originally posted by PHILOU Zrealone  

The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...

Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.



I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.

Replacing the water with ammonia might be doable but i dont think it would make much of a diffrence when the oxygen balance is so bad anyway.

I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with perchlorate
would probely improve it the most IMO

EDIT: Think i found the document http://scholarsmine.mst.edu/cgi/viewcontent.cgi?article=8134&context=masters_theses.

EDIT 2: Forgot to mention that nitrosyl metal complexes might make good explosives or add extra oxidizer too compounds with bad balance. Maybe something like Copper (II) Butyndiolate Nitrosyl?

[Edited on 30-7-2016 by Σldritch]

PHILOU Zrealone - 31-7-2016 at 10:32

Quote: Originally posted by Σldritch  
Quote: Originally posted by PHILOU Zrealone  

The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...

Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.



I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.


I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with perchlorate
would probely improve it the most IMO

Fe(III) and formate anion are stable together except under heating...

Formic acid is relatively stable with H2O2 as long as you don't heat it.

The oxygen balance will be better for most of the proposed compounds vs acetic acid...don't forget that most are diacids not monoacids like acetic:
Monoacids: (multiplied by 2 to get valid comparison with diacids)
2 HO2C-CH3 = C4H8O4 needs 8 O to completely burn
2 HO2C-C#C-H = C6H4O4 needs 10 O to completely burn
2 HCO2H = C2H4O4 needs 2 O to completely burn
Diacids:
HO2C-CH=CH-CO2H = C4H4O4 needs 6 O to completely burn
HO2C-CHOH-CHOH-CO2H = C4H6O6 needs 5 O to completely burn
HO2C-C#C-CO2H = C4H2O4 needs 5 O to completely burn

One may even consider oxalic acid...
HO2C-CO2H = C2H2O4 needs 1 O to completely burn

****************

Adding Nitrosyl ligand might indeed be interesting for OB.

The use of perchlorate anion would of course make a big difference even if the mix doesn't form a complex ... the binary stoechiometrically balanced mix of iron III perchlorate and any iron III organic acid fuel salt would be energetic and cocrystalization will make a molecular level intimate mix prone to D2D from heating or shock.

kratomiter - 1-8-2016 at 07:19

Quote: Originally posted by Σldritch  
Quote: Originally posted by PHILOU Zrealone  

The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...

Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.



I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.

Replacing the water with ammonia might be doable but i dont think it would make much of a diffrence when the oxygen balance is so bad anyway.

I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with perchlorate
would probely improve it the most IMO

EDIT: Think i found the document http://scholarsmine.mst.edu/cgi/viewcontent.cgi?article=8134&context=masters_theses.

EDIT 2: Forgot to mention that nitrosyl metal complexes might make good explosives or add extra oxidizer too compounds with bad balance. Maybe something like Copper (II) Butyndiolate Nitrosyl?

[Edited on 30-7-2016 by Σldritch]


You can replace water with DMSO. Lots of metal perchlorates and nitrates form high explosives that way (patent). Mixing it with AN or AP improve the OB.

Amine complex with cobalt and nickel

symboom - 4-1-2017 at 03:34

Trying to synthesize tetramine cobalt nitrate

Materials
Cobalt nitrate
Ammonium nitrate
Ammonium hydroxide
Ethanol
Tetramine cobalt nitrate
Is what color im getting a brown powder
I can't tell if I keep getting the hydroxide
No crystals??

Attempting amine nickel complex
Maybe better results

Also nitro complexes should be interesting
Like ammonium hexnitrocobaltate

And ammonium hexnitronickelate




symboom - 11-3-2017 at 04:18

Attempted ammonium based complex salts

Tetramine nickel perchlorate is very easy to synthesize
No ethanol to help it percipitate
Hexamine nickel sulfate is added to ammonium perchlorate
A purple percipitate forms after the addition of ammonium perchlorate

Tetramine copper perchlorate
Ethanol is needed for the percipitation
Copper sulfate is not used due to that also being insoluble in ethanol also the tetramine copper sulfate is also insoluble

So copper oxide is added to ammonium hydroxide
With ammonium perchlorate after a day the solution goes from black fine percipitate to tge tetramine complex blue color
Solution is deep blue once it is added to ethanol purple precipitate forms

Next step to add hexamine to tetramine copper perchlorate
In ammonia solution
To hopefully form copper hexamine perchlorate



[Edited on 11-3-2017 by symboom]

DraconicAcid - 11-3-2017 at 10:13

Tetramine nickel? Surely it's the hexamine- nickel is usually octahedral, unless you've got bulky ligands (to make it tetrahedral) or strongly splitting ligands like cyanide (to make it square planar). And the perchlorates are crappy ligands, unlikely to displace ammonia.

CHP

Laboratory of Liptakov - 11-3-2017 at 13:50

Copper hexamine perchlorate is good material. His VoD is 7590 m/s ( at 1,91g/cc) and pressure 260 000 Bar. Therefore his preparation was reported and delete admin from my youtube channel..........:cool:.....Dr.

symboom - 11-3-2017 at 17:00

Quote: Originally posted by Laboratory of Liptakov  
Copper hexamine perchlorate is good material. His VoD is 7590 m/s ( at 1,91g/cc) and pressure 260 000 Bar. Therefore his preparation was reported and delete admin from my youtube channel..........:cool:.....Dr.



That is the procedure im following is Laboratory of Liptakov
Great work also is your vaccum funnel homemade? I hope it isnt deleted :-(

And for cerealkiffer
For the synthesis of hexamine nickel perchlorate

Complex salts are very interesting
Such as

Chromium
Cobalt
Nickel
Copper
Zinc

Videodemolitions also is another interesting youtube channel

Diamine zinc perchlorate?

[Edited on 12-3-2017 by symboom]

[Edited on 12-3-2017 by symboom]

TACP NH4ClO4

Laboratory of Liptakov - 18-3-2017 at 04:17

Next interest is it, that in Liptakov converter for preparation double salt (especially TACP) is possible preparation TACP directly from NaClO4 + NH4Cl + Cu wire + NH3 water. Yield is basically quantitative on NaClO4 (strategic salt). Basic charge for attempt are :
NaClO4 monohydrate 22g + NH4Cl (dry) 20g + Cu wire 8g + NH3 100g water 24%. Dissolving salts by 30C, insert to Liptakov converter. After 150 minute at 20 - 25 C running temperature we have in glass (after drying) 18,5g dry TACP (non hydrate) Crystals from this reaction is pretty big, about cca 1 mm. All others is dissolved in solution: NaCl, residuum NH4Cl and NaClO4 + Cu wire 1g. Reaction requires better counting ratios between NaClO4 xH2O + NH4Cl for better yields. However I recommend use small overlap NH4Cl, because is cheap and free available. 100g ammonia water is minimum, on edge for dissolving.
Next:
This method is possible use for preparation NH4CLO4 and not for TACP. Copper respectively his ligand bonding on NH4. Arises crystals, in relatively high purity. When you need NH4ClO4, simply dissolved TACP in distill water and separe fine CuO powder. After boiling and evaporate all water we have NH4ClO4. Advantage this method is it, that we not need use crystallization process between different solubility salts NaClO4 (as residuum) + NH4Cl (as residuum) + NaCl (production from reaction) + NH4ClO4 (product) which are all in one solution. Copper coordinate ligand helping get out NH4ClO4 in pure form, without multiple recrystallization. All is try again and again, confirmed.
Dr.........:-)

NeonPulse - 5-4-2017 at 03:30

I could find only a little information on cesium picrate and was not even sure it could be made.
so i decided to find out for myself. i simply took a boiling hot solution of picric acid maybe a gram and neutralized it with Aq CsOH added dropwise. it got to the point of being neutralized and i accidentally added an extra drop so the solution was slightly basic PH 7.5 -8 oops. it did not seem to affect the product though and it crystallized gradually in tiny orange needle shaped crystals. these were separated via gravity filtration and rinsed with ice water and set out to dry.

Here is my experiment in forming this picrate: https://www.youtube.com/watch?v=MtUXoU_sjVg

Formed in much the same way as one would prepare potassium picrate, with the resulting product looking much the same, perhaps a little more orange.
upon heating the salt on foil over an alcohol burner it first melted then deflagrated in a nice puff of bright blueish violet light and black smoke.
i did attempt to set it off via friction and impact but these failed.
it did detonate with an oK report at first so i used several more layers of foil and gently pressed the foil hard which in turn increased the density of the picrate.
the reports from these little amounts -50-100mg in the pressed foil was much more satisfying and actually quite loud and spread glittery foil particles all over the place.

Once i can get to retrieving my stash of styphnic acid i really would like to see if i can form cesium styphnate to see how this performs

IMG_2645 (Edited).PNG.jpg - 67kB

005.JPG - 981kB

PHILOU Zrealone - 6-4-2017 at 16:00

Quote: Originally posted by NeonPulse  
I could find only a little information on cesium picrate and was not even sure it could be made.
so i decided to find out for myself. i simply took a boiling hot solution of picric acid maybe a gram and neutralized it with Aq CsOH added dropwise. it got to the point of being neutralized and i accidentally added an extra drop so the solution was slightly basic PH 7.5 -8 oops. it did not seem to affect the product though and it crystallized gradually in tiny orange needle shaped crystals. these were separated via gravity filtration and rinsed with ice water and set out to dry.

Here is my experiment in forming this picrate: https://www.youtube.com/watch?v=MtUXoU_sjVg

Formed in much the same way as one would prepare potassium picrate, with the resulting product looking much the same, perhaps a little more orange.
upon heating the salt on foil over an alcohol burner it first melted then deflagrated in a nice puff of bright blueish violet light and black smoke.
i did attempt to set it off via friction and impact but these failed.
it did detonate with an oK report at first so i used several more layers of foil and gently pressed the foil hard which in turn increased the density of the picrate.
the reports from these little amounts -50-100mg in the pressed foil was much more satisfying and actually quite loud and spread glittery foil particles all over the place.

Once i can get to retrieving my stash of styphnic acid i really would like to see if i can form cesium styphnate to see how this performs


Very nice work NeonPulse...

Now I imagine Lithium picrate (more soluble) --> red flash :D

What would be the deflagrating colour and properties of Rubidium picrate?

For your health safety don't play with Francium picrate ;) would stil be theorically interesting because probably more unsoluble and more sensitive.

Now you can also play with Calcium, Strontium and Baryum picrate to get colorized flame from deflagro-detonating stuffs. :cool:
Ca --> pink orange
Sr --> deep red
Ba --> green

Remain the copper --> blue/green?

greenlight - 7-4-2017 at 02:19

Excellent work Neonpulse, I can't find any information on Cesium picrate at all except for what you have provided.

I have made potassium picrate from picric acid and potassium carbonate before so surely carbonates of Strontium, Barium and copper could be used.
Very interesting.

James Ikanov - 7-4-2017 at 14:15

I was under the impression metal picrates were "too dangerous" (I recall stories of people booby trapping old munitions in a low tech way by smearing picric acid on exposed metal threads of UXO and just waiting for metallic salts to form after it was threaded back in) but it seems there's some consensus that that danger was overstated?

PHILOU Zrealone - 7-4-2017 at 17:14

Quote: Originally posted by James Ikanov  
I was under the impression metal picrates were "too dangerous" (I recall stories of people booby trapping old munitions in a low tech way by smearing picric acid on exposed metal threads of UXO and just waiting for metallic salts to form after it was threaded back in) but it seems there's some consensus that that danger was overstated?

Depends strongly of the "metallic" cation involved...
Some are less sensitive others are more sensitive...copper and calcium may be amongst the worst IIRC.

Also there is a difference between heat sensitivity, shock sensitivity and friction sensitivity...for picrate the 3 are not always wel correlated...

symboom - 26-6-2017 at 08:34

Does anyone know the soubility and extraction of hexamine cobalt chlorate and nitrate
https://m.youtube.com/watch?v=PsdJ99qiCRs

[Edited on 26-6-2017 by symboom]

PHILOU Zrealone - 26-6-2017 at 15:58

HACo(II)N is quite soluble and red like Co(NO3)2.
Extraction and synthesis similar to TACuN and HANi(II)N.

I guess HACo(II)C is similar to HACo(II)N in solubility and synthesis.

But here maybe it is the Co(III) that is concerned...thereover I have no clue or info.

The video is no proof of anything...only claims that are dubious:
*Odorless...and NH3 is it odorless?

*Not detectable by any means? And spectrometry? All complexes display specific absorption and emission spectra...

*Vod 7500m/s...really...hard to believe...proof of oscilloscopic or high speed camera measurement? No.

*Several order of power magnitude stronger than peroxyde explosive...HMTD...is quite powerful and I doubt a dead weight metalic holding molecule can beat a purely CHNO explosive material onto energetic content.

*Any molecule holding NH3 and ClO3 onto a catalytic metallic core can't be an unsensitive safe ternary explosive...it must by definition perform easy D2D...and as such is a primary or at best a secondary

Strontium picrate

greenlight - 15-7-2017 at 06:46

I was inspired by neonpulse experiment with cesium picrate on the previous page that I decided to try and make strontium picrate.

I made a thick slurry of strontium carbonate due to the insolubility problems and added it with a dropper to boiling hot picric acid solution until neutral.
Nothing crystallised when room temperature was reached and still nothing after chilling in the freezer. Strangely, I poured the strontium picrate solution into a fresh evaporating dish and it instantly started crystallising on the sides and was filtered soonafter.

Its looks very similar to potassium picrate with the crystals needle-like structure but slightly darker in colour (see uploaded photos).
I was unable to intiate it with shock or friction at all.
When ignited it burns similarly to potassium picrate very fast with a slight crack leaving black residue behind. It emits a deep red colour when ignited or exploded which proves the existence of the strontium cation. When confined in foil and heated in flame it explodes with a loud report.
I will have to try the barium version.

It doesnt take fire from a fuse really at all though or only partially burns if it does.
If this was not an issue, considering the low sensitivity I think it would be a suitable more colourful replacement for the colored Mg flash compositions for firecrackers which usually get washed out.

Photo on bottom shows about 50mg strontium picrate confined in foil and heated with a flame exploding.


[Edited on 15-7-2017 by greenlight]

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[Edited on 15-7-2017 by greenlight]

[Edited on 15-7-2017 by greenlight]

[Edited on 15-7-2017 by greenlight]

[Edited on 15-7-2017 by greenlight]

Laboratory of Liptakov - 15-7-2017 at 08:51

Beautiful. In foil exploded ? That's a good message....:cool:........LL

symboom - 15-7-2017 at 23:37

I want to add a couple more energetic complex salts
Perticularly

Diamine zinc perchlorate
They dissolve in alcohol. Salvadori has obtained the hydrates Zn(ClO4)2.6H2O and Zn(ClO4)2.4H2O, and the compound Zn(ClO4)2. 4NH4. Both hydrates are strongly hygroscopic, and decompose on heating before all water is eliminated. The ammonia compound is not very stable.

Diamine zinc iodate
3Zn(IO3)2. 8NH4, are obtained by dissolving zinc iodate in concentrated ammonia solution, and either adding alcohol or allowing the solution to evaporate spontaneously. Another compound with ammonia, insoluble in water and stable in air, has been obtained by slow evaporation of an ammoniacal solution of zinc iodate. It decomposes explosively at 150° C. Dry powdered zinc iodate absorbs ammonia gas to form Zn(IO3)2.4NH4.

Less stable diamine zinc bromate
Deliquescent, unstable crystals of Zn(BrO3)2. 3H2O.2NH4 were obtained by adding ammonia to a solution of the salt. Zinc bromate is soluble in its own weight of water at 15° C.

Zinc hexamethylenetetramine (hexamine)nitrite ZHN
Colourless prismatic crystals of Zn(NO2)2.2H2O.C6H12N4 are obtained by adding sodium nitrite to the solution of a zinc salt containing hexamethylenetetramine. Zinc nitrite also occurs in the hygroscopic yellow crystalline double salt, 3KNO2.Zn(NO2)2.3H2O, obtained by acting with nitrous acid on zinc hydroxide suspended in potassium nitrite solution, and in the similar salt, 2KNO2.Zn(NO2 )2.H2O, prepared by mixing solutions of potassium nitrite and zinc chloride

Update sucess made ZHN its a dark yellow compound
Once sodium nitrite was added to the solution the yellow color
ZHN is insouble in water settled to the bottom it seems like a fine percipitate small bubbles are forming not sure if it is decomposing in water or its stability
all reagents are soluble in alcohol so a reaction could take place in alcohol then precipitated slowly with water to cause bigger crystals to form havnt done any flame tests

Excerpt from atomistry.com/zinc
This website is great shows many exotic compounds such as sodium aluminum perchlorate , sodium hypoborate, and diamine silver bromate

[Edited on 16-7-2017 by symboom]

[Edited on 16-7-2017 by symboom]

PHILOU Zrealone - 17-7-2017 at 03:56

Quote: Originally posted by greenlight  
I was inspired by neonpulse experiment with cesium picrate on the previous page that I decided to try and make strontium picrate.

I made a thick slurry of strontium carbonate due to the insolubility problems and added it with a dropper to boiling hot picric acid solution until neutral.
Nothing crystallised when room temperature was reached and still nothing after chilling in the freezer. Strangely, I poured the strontium picrate solution into a fresh evaporating dish and it instantly started crystallising on the sides and was filtered soonafter.

Its looks very similar to potassium picrate with the crystals needle-like structure but slightly darker in colour (see uploaded photos).
I was unable to intiate it with shock or friction at all.
When ignited it burns similarly to potassium picrate very fast with a slight crack leaving black residue behind. It emits a deep red colour when ignited or exploded which proves the existence of the strontium cation. When confined in foil and heated in flame it explodes with a loud report.
I will have to try the barium version.

It doesnt take fire from a fuse really at all though or only partially burns if it does.
If this was not an issue, considering the low sensitivity I think it would be a suitable more colourful replacement for the colored Mg flash compositions for firecrackers which usually get washed out.

Photo on bottom shows about 50mg strontium picrate confined in foil and heated with a flame exploding.


[Edited on 15-7-2017 by greenlight]

Nice...Greenlight that makes RED Lights :D;):):P:cool:
Great info for picrate lovers and picrate information, thank you...
Lithium may also find uses for the red color...

You experienced the overfusion effect...the compound is into sursaturation state...and a sudden temperature change or a scratch/dust into a glas recipient may induce fast crystalization...

Instead of carbonate you could also have used the hydroxyde....what must be slightly more soluble...but the advantage of the carbonate is that it fizzes showing there is stil some picric acid...and the excess carbonate is easy to observe and to separate from the picrate salt.

PHILOU Zrealone - 17-7-2017 at 04:01

Quote: Originally posted by symboom  
I want to add a couple more energetic complex salts
Perticularly

Diamine zinc perchlorate
They dissolve in alcohol. Salvadori has obtained the hydrates Zn(ClO4)2.6H2O and Zn(ClO4)2.4H2O, and the compound Zn(ClO4)2. 4NH4. Both hydrates are strongly hygroscopic, and decompose on heating before all water is eliminated. The ammonia compound is not very stable.

Diamine zinc iodate
3Zn(IO3)2. 8NH4, are obtained by dissolving zinc iodate in concentrated ammonia solution, and either adding alcohol or allowing the solution to evaporate spontaneously. Another compound with ammonia, insoluble in water and stable in air, has been obtained by slow evaporation of an ammoniacal solution of zinc iodate. It decomposes explosively at 150° C. Dry powdered zinc iodate absorbs ammonia gas to form Zn(IO3)2.4NH4.

Less stable diamine zinc bromate
Deliquescent, unstable crystals of Zn(BrO3)2. 3H2O.2NH4 were obtained by adding ammonia to a solution of the salt. Zinc bromate is soluble in its own weight of water at 15° C.

Zinc hexamethylenetetramine (hexamine)nitrite ZHN
Colourless prismatic crystals of Zn(NO2)2.2H2O.C6H12N4 are obtained by adding sodium nitrite to the solution of a zinc salt containing hexamethylenetetramine. Zinc nitrite also occurs in the hygroscopic yellow crystalline double salt, 3KNO2.Zn(NO2)2.3H2O, obtained by acting with nitrous acid on zinc hydroxide suspended in potassium nitrite solution, and in the similar salt, 2KNO2.Zn(NO2 )2.H2O, prepared by mixing solutions of potassium nitrite and zinc chloride

Update sucess made ZHN its a dark yellow compound
Once sodium nitrite was added to the solution the yellow color
ZHN is insouble in water settled to the bottom it seems like a fine percipitate small bubbles are forming not sure if it is decomposing in water or its stability
all reagents are soluble in alcohol so a reaction could take place in alcohol then precipitated slowly with water to cause bigger crystals to form havnt done any flame tests

Excerpt from atomistry.com/zinc
This website is great shows many exotic compounds such as sodium aluminum perchlorate , sodium hypoborate, and diamine silver bromate

[Edited on 16-7-2017 by symboom]

[Edited on 16-7-2017 by symboom]

Thank you for the informations....;)

Barium picrate

greenlight - 18-7-2017 at 05:20

Thanks LL and Philou

[/rquote]
Nice...Greenlight that makes RED Lights :D;):):P:cool:
[/rquote]

Here I will try make the green light haha:D:)

I used the same synthesis method as for the strontium picrate and the same overfusion effect happened when I crystallised it.
The crystals are much finer smaller needles than the Sr salt and leave the same black soot behind after being burnt which seems to be common for picrates.

It is insensitive to friction and shock the same as the strontium picrate.

Although the green colour is not as strong as the Sr picrate it makes up for it in power and brisance when confined.
Unlike the strontium picrate, the top crystals of a small pile first melt and then initiate the whole pile with a loud whooomp when ignited with a flame.
It cannot be initiated without first going through a melt-phase of the surface.
It takes longer to explode when confined in foil because of this as well.

The report is louder than Sr and the foil is reduced to smaller pieces even under slight confinement by making a small Al foil cup it explodes loudly blowing a hole in the bottom and unravelling the whole top.
The amounts used were the same as the tests with Sr picrate.
The left picture is confinement in foil under the same conditions as the Sr salt and the right picture is burning of an small unconfined pile

[Edited on 18-7-2017 by greenlight]

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[Edited on 18-7-2017 by greenlight]

[Edited on 18-7-2017 by greenlight]

Exotic silver amine complexes

symboom - 20-7-2017 at 21:25

Exotic silver complexes
Diamine silver nitrite
Silver nitrate to sodium nitrite form Silver nitrite
Double compounds with ammonia of the formula
AgNO2,NH3; AgNO2,2NH3; and AgN

Diamine silver bromate
Potassium bromate precipitates silver bromate from Silver nitrate.Its solution in ammonium hydroxide yields crystals of the formula Ag(NH3)2BrO3.

Diamine Silver chlorate
The Silver chlorate, AgClO3, can be prepared by dissolving the monoxide in chloric acid, or by passing chlorine through a suspension of the monoxide in water, the hypochlorite being an intermediate product.produces shock-sensitive dark crystals. A use for silver oxide batteries unfortunatly the silver oxide is very stubborn to desolve in chlorine water due to calcination.
Its solution in ammonium hydroxide yields prismatic crystals, Ag(NH3)2ClO3, melting at 100° C.


And mercury
Trimercury chlorate acetylide
Mercuric nitrate; sodium chlorate; acetylene or calcium carbide

And copper
Tetraaminecopper chlorate
ammonium hydroxide, copper sulfate, sodium chlorate, alcohol

Exotic amine nickel
Nickel Bromate, Ni(BrO3)2.6H2O, may be prepared by double decomposition of barium bromate and nickel sulphate solutions. It crystallises in unstable octahedra which are green in colour. From its solution in aqueous ammonia, alcohol precipitates the diammoniate, Ni(BrO3)2.2NH3.

Popular hexamine nickel perchlorate
If a piece of blotting or filter paper is moistened with a solution of nickel perchlorate and introduced into the tip of a Bunsen flame, a series of small detonations ensues.

the hexammoniate, Ni(ClO4)2.6NH3.

Also never understood the zinc amine complexes are never very stable and decompose such as the diamone zinc permangante and diamine zinc perchlorate

Too bad alumunum chlorate doesnt form a complex but aluminum perchlorate does form a double salt

Aluminium perchlorate, Al(ClO4)3.6H2O, is a colourless, crystalline salt, soluble in water. Its aqueous solution gives, with sodium perchlorate, a crystalline precipitate of aluminium sodium perchlorate, AlNa(ClO4)4.12H2

Info on the chlorate
Kind of off topic but it does produce chlorine dioxide
Aluminium chlorate, Al(ClO3)3.9H2O, prepared by mixing aluminium sulphate and barium chlorate, removing the barium sulphate, and evaporating the cold solution over sulphuric acid, is very soluble in water. From a hot solution it separates as the hexahydrate. The salt is easily decomposed by heat, and explodes when slowly heated.

Im guessing due to chlorine dioxide gas being produced

[Edited on 21-7-2017 by symboom]

symboom - 22-7-2017 at 21:10

Persulfates of Divalent Metals.
From google books


From this apparently pyridine and hexamine (Hexamethylenetetrammine) can form complexes with persulfates also makes me think of other combinations with pyridine perchlorate or chlorate I have been trying to form stable chlorate complexes no luck oh well so heres a list of persulfate complexes


Crystaline persulfates of the divalent metals are difficult to obtain because of their great solubility and instability.

Tetrammine-zinc persulfate,
large transparent prisms, precipitates only from very concentrated solutions formed by double decomposition between a concentrated solution of ammonium persulfate and a concentrated NH3 solution of the metal sulfate the corresponding NH3 compound separates as a crystaline percipitate

Hexammine-cadmium persulfate, CdS208.6NH3, forms white microscopic crystals, less soluble than the zinc analog Strong NH3 odor, decomposes on standing in moist atmosphere

Hexammine-nickel persulfate, NiS208.6NH3, clear blue-violet crystals, strong NH, odor. Becomes black in moist air; H20 soln. is blue, turns cloudy, percipitates NiO When dried over CaCl, it turns gray, then green, with loss of ammonia and oxygen and forms a double sulfate. In vacuum over H2SO4 it turns dirty yellow.

Tetrammine-copper persulfate dark blue-violet needles, more stable than the precededing. All the above compoinds luae ammonia and oxygen on standing some time, and explode when strongly heated or when struck.

---------------------------------------

By replacing amine with pyridine one obtains stable compounds

The Pyridine compounds are similarly prepared using 8-10 mol. Pyridine to 1 mol. metal sulfate.

Tetrapyridine-zinc persulfate glittering prisms, forms slowly from very concentrated solution Decomp. readily, turning yellow.

Tetrapyridine-cadmium persulfate, sharp glittering needles, less soluble than the Zn salt.

Tetrapyridine-nickel persulfate, thin, clear, blue microscopic needles, forms only from very concentrated solution

Tetrapyridine-copper persulfate, masses of blueviolet microscopic needles, insoluble in presence of excess Pyridine and ammonium persulfate
------------------------------------
Hexamethylenetetrammine compds. were similarly prepd., using 2 mol. Hexamethylenetetrammine to 1 mol. metal sulfate. The compounds obtained should be quickly separated. and washed with ethanol since they decompose rapidly when moist but are more stable when dry.

BisHexamethylenetetramine-magnesium persulfate-octahydrate forms colorless silky scales.

BisHexamethylenetetramine-manganese persulfate-octahydrate - colorless scales.

BisHexamethylenetetramine-cobalt persulfate-octahydrate rose-colored scales.

BisHexamethylenetetramine-nickel persulfate-octahydrate, green scales.
The above 4 compounds are all isomorphous.


[Edited on 23-7-2017 by symboom]

Peter Lustig - 21-9-2017 at 00:48

I have noticed that SADS is not stabel in contact with NHN ! After 3/4 year it beckame black and lost its effect. I guessit is reducing by hydrazin...

PHILOU Zrealone - 21-9-2017 at 04:07

Quote: Originally posted by Peter Lustig  
I have noticed that SADS is not stabel in contact with NHN ! After 3/4 year it beckame black and lost its effect. I guessit is reducing by hydrazin...

I have no such troubles with it...
==> May be due to some traces of exces free hydrazine into the NiHN ...
==> Or to unstable SADS (traces of Cl(-), of OH(-), exposure to light, uncomplete washing with demi-water)...

Was your SADS white/ cream colored, wel dried and washed with demineralized water several times?
Was it (the SADS alone thus) stable upon storage into the very same conditions?

[Edited on 21-9-2017 by PHILOU Zrealone]

dave321 - 21-9-2017 at 11:30


maybe it is simply the sads changing colour due to light exposure

specialactivitieSK - 6-1-2018 at 00:27

Experimented someone with BISMUTH ?

symboom - 21-4-2018 at 21:24

Complex salts list

Hexamine nickel perchlorate

Silver chlorate
Aluminum chlorate

Copper hexamethylamine  perchlorate
Tetramine copper persulfate
Diamine silver nitrite
Diamine silver bromate

Trimercury chlorate acetylide

Tetramine copper chlorate
Tetramine zinc chlorate
Tetramine zinc persulfate
Tetramine Lead nitrite
Diamine zinc permanganate

snooby - 23-1-2019 at 07:34

I came by this two documents about NiCP. Sensitivity looks promising. Furthermore easy synthesis, except for carbohydrazide (relatively non toxic btw). But this compound can be bought quite easy. Nickelperchlorate should be doable also I guess.

I was looking on BNCP (its quite difficult to get it properly working in a det ( but sometimes it works however, but not really reliable, about 50/50). But it is really not sensitive towards beatings with hammer, about same as ETN. So thats really good. But in anoher patent wich i cannot find anymore
- I mean fuck yeah found it:

http://www.niscair.res.in/sciencecommunication/ResearchJourn...

https://www.sciencedirect.com/science/article/pii/S030438940...

http://www.allindianpatents.com/patents/253659-process-for-p...

So, what you guys think bout this? Im only confused because why bothering the BNCP synthesis that takes agesi
In the end, while probably NiCP alone can also initiate tetryl, and prob also Petn/ETN and RDX maybe to.

So yeah thats why i start asking bout the NiCLO4. I am really hoping to hear some thoughts from u all. Bye

[Edited on 23-1-2019 by snooby]

CHP

Laboratory of Liptakov - 24-1-2019 at 11:46

Safe initiation with perchlorate salt has been resolved before 4 years. Tetraamine copper perchlorate pure, or + 6% hexamine. Thus CHP. (copper hexamine perchlorate) Which is much better.

system Berta 4mm.jpg - 33kB
Works even in cavity 4 mm only.....Of course, that you can deploy for example booster from 500mg ETN......:cool:

snooby - 6-4-2019 at 07:47

NiCP tested. Fucking sensitive, not usefull as a primary. This is confirmed by another member btw. Also the cobaltversion, dont waste any money it..


I also worked two whole days to make:

Di-Silver Aminotetrazole Perchlorate. Synthesis should not be difficult: just react silverperchlorate (tricky and a lot of work to make though) with 5-ATZ monohydrate. I got a nice clean white precipiate that wont dissolve in wother, washed it 10.00 times. Only one time it managed me to make a product that actually detonated by flame instantly, and loud. I tried 4 more times, and now I am done with it, my whole house turned black and messy.:mad::mad:

[Edited on 6-4-2019 by snooby]

Laboratory of Liptakov - 6-4-2019 at 08:00

Haha...Di- silver ATZ -perchlorate ? :o.....Only from the formula are my hair from fear up!...(or out) ...:D.......LL

snooby - 6-4-2019 at 08:34

It was not so sensitive to impact. Much less then LA or double.salts or whatsover. It looked really promissing, but I havent made up why it just worked once. The silver perchlorate was nice and clean. Now my product each time looks like chalk. And they burn and fizzle a lil bit but not much. Silver perchlorate is makeble: react agno3 with sodium carbonate. Use a lot of water. Excess Yellow silvercarbonate react with HCLO4. Filter of excess carbonate and evaporate. Hope someone will give it a shit too!

Lol give it a shot too.

[Edited on 6-4-2019 by snooby]

[Edited on 6-4-2019 by snooby]

Attachment: 20190406_184139_1.mp4 (5.6MB)
This file has been downloaded 365 times


Laboratory of Liptakov - 6-4-2019 at 10:38

Nice sharp blow. The mad formula. Great work, Snooby....:cool:....LL
The spoon got a pretty blow....(muhaha)

snooby - 23-4-2019 at 11:50

Another one: double salt of am guanidine bicarbonate and nickelperchlorate. Very easy to make, just boil components and filter of crystals. Sensitivity tests has yet to come though! Sorry for doublr post. In confinement this stuff detonates.

Attachment: videocompress-045-20190423_211507.mp4 (3.4MB)
This file has been downloaded 299 times


aminoguanidine ligands

Tyneman - 7-5-2019 at 06:51

Inspired by Snooby and Mineman I decided to try my hand at some amino guanidine ligands. Namely the copper and nickel variants. To show you a bit of my journey here's the synthesis and sensitivity tests for Cu (II) (Monoaminoguanide) diperchlorate.

http://pyrobin.com/files/Cu-gua-perc%20lq.mp4

Nickel took some more work. I will follow-up when that report is finished.

Laboratory of Liptakov - 7-5-2019 at 11:48

@Tyneman.....One from best video editing and quality and full info in 2 minute.....:o..... Thanks for sharing.....:cool:..... We all thanks for perfect work.
I estimate, the reaction runned by lab. temperature? Only on table ?
It has very similar properties as CHP. I see low friction sensitivity and suoer speed of burn. Hammer test show also almost same power. Very good material. Is it neutral salt? Because CHP is alkaline = disadvantage in some mixtures CHP/xy ...LL

Tyneman - 7-5-2019 at 12:59

@LL.. Thank you for your kind words.:D

As stated in video synthesis was ran @ room temperature, around 20C. This resulted in a steady foaming and good rate of reaction. So there was no need for heating.
First I ran it on the table, when more precipitate was formed I used a magnetic stirrer without heating applied.

I believe it is a neutral salt, but with these ligands and other big molecules I find it hard to know for sure. I hope someone who is more chemically educated can answer this one.

Laboratory of Liptakov - 7-5-2019 at 13:28

We all look forward to the nickel ligand on same base.....:cool:...LL

Tyneman - 9-5-2019 at 05:22

As promised, here the results of the Nickel ligand.
It is definetly a bit more (impact) sensitive then it's Cu brother. And I believe a bit more powerful.

http://pyrobin.com/files/Ni-gua-percLQ.mp4

Also the patent states it is neutral.
Quote:
Furthermore, the explosives of the invention is neutral, d. H. Neither acidic or alkaline. Therefore it is compatible with both acidic and basic compounds having, in particular secondary explosives, d. H. There will be no decomposition reactions with other explosives during storage. The complex salt is also highly soluble. This also avoids other explosives unwanted decomposition reaction.


Next will be penetration tests. To be continued!

[Edited on 9-5-2019 by Tyneman]

Laboratory of Liptakov - 9-5-2019 at 09:29

Hahaaa...!....Incredible beautiful color. And properties also are great from video. Thanks very much....:cool:.....Still some test on pressing into cavity......:D...... I believe, that nexts examinations bring sure great results. I believe in this sure. For someone can be problem availability of HClO4. But it seems that exact ratios is not need. Only excess of HClO4. And something will precipitate always....:cool:...LL

strategic mixtures

Laboratory of Liptakov - 9-5-2019 at 09:59

Safe mixtures for detonators have existed long ago. They have long been developed and tested. There may be dozens of relatively safe compounds for detonators. But they are not meant for amateurs. They are locked in the vaults of national laboratories. Like many other strategic information. Similar to CHP, which bridges the gap between primary and secondary materials. To date, there is no single official study for TACP and its features. Where it would be officially written: Yes, TACP + fuel can provide a detonation pressure of up to 25 GPa. And has an easy D-D Transition. Therefore, the S -M community must (or can) discover and test many materials in amateur conditions. Again. Without the support of national laboratories. No support because it is a strategic information and material.

guanidine ligands

Tyneman - 16-5-2019 at 05:20

Finally got around to some testing.

I made 5 small detonators, an average CHP det to the side for comparison. (pic1)
Dimensions were 4mm x 6mm Al tubes 35mm long.

Contents:
1: 0,1g PETN @ 30Kg - 0,05g PETN @ 15Kg - 0,02g NiQP @ 5Kg
2: 0,1g PETN @ 30Kg - 0,05g PETN/CHP 50/50 @ 15Kg - 0,02 NiQP @ 5Kg
3: 0,1g PETN @ 30Kg - 0,05g PETN @ 15Kg - 0,02g CuQP @ 5Kg
4: 0,1g PETN @ 30Kg - 0,05g PETN @ 15Kg - 0,05g NiQP @ 5Kg
5: 0,15g PETN @ 15Kg - 0,02g NiQP @ 5Kg

All detonators placed perpendicular on a 4mm Al plate.

Results:
Topside, see picture 2

Backside, see picture 3

Measurements:
1: Indent 0,1mm.
2: Indent 1,5 mm.
3: Full penetration, diameter hole 4mm.
4: Full penetration, diameter hole 3mm.
5: 90% penetration, 3,5mm bulge on backside.

Debris recovered after detonation, see picture 4.

Comments and discussion are welcome




detsLQ.jpg - 2.2MB topLQ.jpg - 2.3MB backLQ.jpg - 1.4MB debrisLQ.jpg - 836kB

Laboratory of Liptakov - 16-5-2019 at 06:54

3. Looks good. So was use aminoguanidine copper perchlorate? Or only guanidine copper perchlorate? I am confused from all the ligands....:D
Any way, great a piece of work. Finaly someone, who tested something really...:cool:....LL

Tyneman - 16-5-2019 at 23:23

Full name should be Ni (II) di(monoaminoguanidin) diperchlorate. But hey, what's in a name? I thought Q was the abbreviation for aminoguanidin, is it just guanidine?
Is there a common abbreviation for this 'thing' ?

Microtek - 17-5-2019 at 01:46

Well, nitroguanidine is NQ, so logically aminoguanidine should be AQ. However, I think I have seen Ni (II) di(monoaminoguanidin) diperchlorate abbreviated as ANP...

MineMan - 17-5-2019 at 23:37

So the copper ligand is better? Anyone have any other metal ligand that might work even better, like silver? What is the synth for the copper ligand and how does the sensitivity compare to the Ni? I am beyond greatly interested in your answers.

Thank you

Mineman.

Tyneman - 18-5-2019 at 07:08

Synth for the copper ligand is posted on previous page. Aswell as some friction and impact tests.
I will make a little comparison side by side this week.
Cobalt is allso an option, but patent states it gives some thick liquid as result from which it is hard to separate crystals. But might give that one a try to. Silver is also stated to work, but I can't find any info on that one, only one way to find out I guess...

twelti - 18-5-2019 at 09:34

Quote: Originally posted by snooby  
Another one: double salt of am guanidine bicarbonate and nickelperchlorate. Very easy to make, just boil components and filter of crystals. Sensitivity tests has yet to come though! Sorry for doublr post. In confinement this stuff detonates.

I made a little of the nickel complex, it detonates even wo confinement (and how!). Copper complex seems to need it. Are you washing it with anything? I just poured mine on to a paper towel, since there is so little liquid.

Tyneman - 18-5-2019 at 14:14

Quote:
Are you washing it with anything?

I washed twice with cold dH2O and once with cold EtOH.

Quote:
So the copper ligand is better?

At first glance I thought it was actually less powerful then the Ni counterpart. It is less friction and impact sensitive for sure IMO. Deto tests showed the Cu to be more powerful. Wich was not what I expected. If it is indeed more powerful and less sensitive that would make it better yes.

Please compare the tests in my two vids I posted.
I will be doing more testing soon, aswell as try to make Ag and Co ligands.

Laboratory of Liptakov - 18-5-2019 at 22:21

Very interesting results from Tyneman testing. It confirmed old rule, that behaviour on air is (almost always) some else than in solid cavity. Basic energetic properties is necessary measured in conditions, which will use. As final applications. And not repeatedly between two stones as troglodyte. Or dancing around it and throw into flame. A like an shaman. You won't find out anything....:cool:....LL

(OK, copper ligand is best)

Microtek - 19-5-2019 at 11:07

You need more than one repetition of a test to find out which one is best.

Tyneman - 19-5-2019 at 13:41

You are very right there Microtek!
That is why
Quote:
I will be doing more testing soon,

These are just first results, but they seem viable enough to try and get others to test them too. Even if I test more, other peoples results may differ and shed a new light.
So I hope to get others to synthesise and test them. Which can only be done by showing what I have done sofar.

twelti - 19-5-2019 at 14:18

I have been making some small batches - both Ni and Cu. It seems that in the patent it says to boil for 5 minutes and then cool to RT for four hours. I tried that and got needles. Is some other batches where I went straight to ice bath, I got smaller crystals. I guess that is not surprising. I wonder what else I could do to reduce crystal size.

I'm also not sure how much water I should be adding and when to add. Should I add more as the reaction continues, and how much will I lose in a water wash during filtration?

Is there any way of desensitizing it? It seems very powerful, but not as insensitive as I'd hoped, at least so far.

Microtek - 19-5-2019 at 22:59

When you have boiled the mix, and it is time to let it cool down and precipitate the product, just keep on stirring it (preferably not by hand). This will prevent the formation of large crystals, but will still give a product that is easy to filter and handle.

You should not add any more water during the course of the reaction, just what is needed in making the solutions in the first place.

Tyneman - 19-5-2019 at 23:13

To get smaller crystals you could try to let it cool whilst stirring. Agitation should reduce Cristal size.

I only used water at the beginning, slurry the aminoguanidine, and dissolve the NiPerc in a little (10mL) dH2O. No further additions.


Rosco Bodine - 20-5-2019 at 09:03

A suggestion I have about the copper and nickel compounds is to experiment with a synthesis that produces *both* at the same time from their mixture of precursors, to see if a complex compound salt or double salt may form having different crystalline and physical form that may be an improvement.

Microtek - 20-5-2019 at 12:38

Yes, I have used that strategy before with some of the "green primaries" based on nitrotetrazole transition metal complexes. I doped the nickel salts with a little silver in order to co-precipitate a small amount of silver nitrotetrazolate. This increased the DDT ability and lessened the requirement for confinement without too much increase in sensitivity.

Very safe and powerful detonator composition.

wessonsmith - 22-5-2019 at 05:07

below

[Edited on 23-5-2019 by wessonsmith]

MineMan - 22-5-2019 at 13:09

Wessonsmith. Confused we are by your post.

twelti - 22-5-2019 at 14:49

I think he put his comment inside the html quote.

Can you not press any primary wet, then allow to dry?

wessonsmith - 22-5-2019 at 17:09

My detonator mix has two parts. 1) A composition consisting of 500mg 65% Nickel Hydrazine Nitrate (NHN) / 35% Sodium Nitrotetrazole Dihydrate (NaNTz) which is intimately mixed together then pressed into detonator tube (I press the comp to 1.7 g/cm³ using an Irwin vise) and heat-treated at 107°C (225°F) for 4hrs. The heat treatment drives off the water of crystallization of the NaNTz Dihydrate leaving behind NHN tightly packed with the anhydrous version of NaNTz.

Since the Dihydrate version of the composition is VERY insensitive, there is no fear of loading it. 2) 50mg NHN added on top of the heat treated mix to help the Visco fuse in setting it off.

What you have is a detonator composition that is “green”, set off with Visco fuse, very powerful, safe to load, not reactive to metals or plastics and can sit on a shelf for a decade or more.


[Edited on 23-5-2019 by wessonsmith]

[Edited on 23-5-2019 by wessonsmith]

wessonsmith - 22-5-2019 at 17:14

Quote: Originally posted by twelti  
I think he put his comment inside the html quote.

Can you not press any primary wet, then allow to dry?


My primaries are not wet. NaNTz Dihydrate has the water of crystallization that is being removed to make the anhydrous form of NaNTz. Not sure how pressing actually wet primaries would work. Probably make quite a mess.

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