Sciencemadness Discussion Board

Exotic Primaries - Complex Salts

 Pages:  1  ..  4    6  

twelti - 23-5-2019 at 09:19

Quote: Originally posted by wessonsmith  
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.

I have heard of it being done. Maybe alcohol or water, not a solvent, just a wetting agent, so just slightly moist.

MineMan - 23-5-2019 at 09:27

All. This looks like an amazing compound. Friction sensitivity is equal to PETN...

The only issue is I don’t know where to obtain the precursor that they say is commercially available.
Check it out. Share your thoughts.

https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6430815/#!po=46...

Laboratory of Liptakov - 23-5-2019 at 11:13

I readed this link. For professional use is it good. But the preparation is really not ecological. Starting with NaN3. Pretty hard poison. And tracked precursor. (holding can be criminal)
NaN3 is it the last, what I would need in my lab.....:cool:...LL
Final compound is maybe ecological. But preparation is for most researchs unavailable.

wessonsmith - 24-5-2019 at 07:12

Quote: Originally posted by Laboratory of Liptakov  
I readed this link. For professional use is it good. But the preparation is really not ecological. Starting with NaN3. Pretty hard poison. And tracked precursor. (holding can be criminal)
NaN3 is it the last, what I would need in my lab.....:cool:...LL
Final compound is maybe ecological. But preparation is for most researchs unavailable.


I agree with LL, Sodium azide is not a precursor I want to mess with. But the performance of that ICM-103 is VERY impressive and that article was a good read. But at some point, you have overkill. I can set off ETN based plastic explosive with 12% HTPB with only 180mg of anhydrous 25% / 75% NaNTz/NHN. So not sure what having that powerful of an initiator would do for most of us.

[Edited on 24-5-2019 by wessonsmith]

Static Sensitivity of Ni AG Perchlorate

twelti - 24-5-2019 at 19:45

I did an informal test of static sensitivity for Nickel Aminoguanidine Perchlorate. I used an electric fly swatter, with the wires pulled out. It actually is pretty repeatable. It charges internal cap depending how long you hold the button down. Ok, not terribly scientific, but the overall result is clear. The Nickel AG Perchlorate is much less sensitive than SADS. Will try Cu complex next.

Attachment: NiAGPerchlorate Static Sensitivity.mp4 (5.6MB)
This file has been downloaded 1002 times

Laboratory of Liptakov - 25-5-2019 at 12:13

NiAGP seems pretty low sensitive on electro. That's good message. I estimate, that CuAGP will similar. Good work....:cool:...LL

XeonTheMGPony - 23-7-2019 at 05:19

Quote: Originally posted by Laboratory of Liptakov  
I readed this link. For professional use is it good. But the preparation is really not ecological. Starting with NaN3. Pretty hard poison. And tracked precursor. (holding can be criminal)
NaN3 is it the last, what I would need in my lab.....:cool:...LL
Final compound is maybe ecological. But preparation is for most researchs unavailable.


Toxicity is only an issue if you are poor at material handling. The safety is in you, never the substance, even water is deadly if you are an idiot ;)

NaN3 is a bit of a pain to make, I'll be doing a scaled up run some point near future.

snooby - 10-8-2019 at 05:39

Okay guys,

ICM 103 is something nobody of us would like to try out. The pyrazole stuff seems inpossible to get hands on. However, I can buy IT and ship it around the world. Price is around 1000 dollars for 500 grams (WTF). And if I lower the price would increase (50 grams are 380 dollars). So, are there 3 or 2 other guys/girls who would like to share the costs? Price would be around 200 dollars for 100 grams. That's a LIFE supply. I AM willing to receiver the order and ship IT around our globe. Sent me an PM if you would like to join. Only first 3 guys can get involved.






Boffis - 11-8-2019 at 09:55

WTF is ICM 103? If you want someone to pay $200 for something then you will need to gives us an identity.

snooby - 11-8-2019 at 10:18

Okay first, shut your big attitude. Im trying to give people a chance like i woud like. If u are are interested, we can make An whatsapp groep. Tynenan is already in too..

MineMan - 11-8-2019 at 11:55

Snooby

Wow. Great job taking the lead on this. It would be quite a feat!!

snooby - 2-9-2019 at 10:42

Pm is open for the pyrazole. Grttt

snooby - 5-9-2019 at 08:34

Im struggling to get pure hno3 White. Im willing to trade IT for the pyrazole

Rosco Bodine - 5-9-2019 at 11:57

Quote: Originally posted by snooby  
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]


@snooby

Some earlier related information was posted by me and linked
http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...

You reported this Tris-Carbohydrazide Nickel Perchlorate is dangerously sensitive, confirmed by another member ....Who?

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


Anyway, I am thinking that sensitivity may relate to crystal size as can happen for many of the initiators that can still be useful when process control is applied to regulate crystal growth and produce a desirable mesh and density. Lower temperatures favor smaller more amorphous crystals of lower bulk density and likely lowered sensitivity while larger crystals are precipitated from warmer reaction mixture above 60 C. So process addition rate and temperature and stirring rate / agitation turbulence intensity may be all that is needed to achieve a product having desirable properties.

Other carbohydrazide metal complexes are known but it is unknown if any of these may form interesting double salts, and if they do what may be the properties of such double salts.

There seems also possible the formation of binary Metal Semicarbazide-Carbohydrazide Perchlorates which could be interesting, but are also a hypothetical complete unknown.

Attachment: prep_201400142_sm_miscellaneous_information.pdf (176kB)
This file has been downloaded 607 times

Attachment: Tris carbohydrazide nickel perchlorate (NCP).pdf (32kB)
This file has been downloaded 610 times

As an aside ...I hope our old friend nitro-genes knows intuitively and by GOOD evidence of many years contributions and discussions that I am a bona fide experimenter and researcher and not some gum shoe investigator / regulator or narc. I too have been on the receiving end of undeserved abuse and ripoff by corrupt government "types" and was never by intimidation "converted" into any like piece of evil shit to themselves. I have more self-respect than to be that kind of lowlife that are bottom feeding bottom of the sea lower than whale shit sub-human skin jobs that only pass for human on their best days :D

[Edited on 9/5/2019 by Rosco Bodine]

nitro-genes - 7-9-2019 at 07:40

Ah yes, it is all a coincidence…our meterpole is changed and I receive a U2U from Rosco about how their meterpole was changed. My 4 year old daughters toe gets pinched by me while sitting in our rocking chair and hours later a post appears mentioning “a low milage tail getting pinched by an ancient’s rocking chair”. The mention of roadkill was especially disturbing, as my wife and I had a conversation a while back indeed over if my daughter could play outside alone already, with that road right in front of our house. When we subscribe to a grocery delivery service called PICNIC, some bogus user called “picnic acid” appears in a thread that could very well be received by me as further personal intimidation and was locked by a moderator. Your whale shit comment is a nice touch though, considering I made an UNSENT U2U in which I was comparing agency presence here on this board with the presence of these agencies at a greenpeace meeting to watch carefully if no whales are shot.


I suspected they were trying to build a legal case against me, and that is fine, but don't make provoking intimidations based on gathered intelligence towards members of my family!!! (I think J_Sum might also recall some of these as he was the one who removed them). I was not the one starting provocations on a personal level and family level Bodine and you know it! So don’t talk about my conscious to me for some of the provocations I made (that have actually never happened and also regret on a personal level). I would never do wrong to people, unless I really get the feeling that some people or agencies may pose a threat outside the boundaries of legal jurisdiction that would fuck me over. That is what happened…and towards your “I didn’t apologise” comment, I actually did by U2U, so is just a lie again.


Plaatje windmolens en Donquichotte - Copy.jpg - 166kB

[Edited on 7-9-2019 by nitro-genes]

Rosco Bodine - 7-9-2019 at 12:58

Quote: Originally posted by nitro-genes  
Ah yes, it is all a coincidence…our meterpole is changed and I receive a U2U from Rosco about how their meterpole was changed. My 4 year old daughters toe gets pinched by me while sitting in our rocking chair and hours later a post appears mentioning “a low milage tail getting pinched by an ancient’s rocking chair”. The mention of roadkill was especially disturbing, as my wife and I had a conversation a while back indeed over if my daughter could play outside alone already, with that road right in front of our house. When we subscribe to a grocery delivery service called PICNIC, some bogus user called “picnic acid” appears in a thread that could very well be received by me as further personal intimidation and was locked by a moderator. Your whale shit comment is a nice touch though, considering I made an UNSENT U2U in which I was comparing agency presence here on this board with the presence of these agencies at a greenpeace meeting to watch carefully if no whales are shot.


I suspected they were trying to build a legal case against me, and that is fine, but don't make provoking intimidations based on gathered intelligence towards members of my family!!! (I think J_Sum might also recall some of these as he was the one who removed them). I was not the one starting provocations on a personal level and family level Bodine and you know it! So don’t talk about my conscious to me for some of the provocations I made (that have actually never happened and also regret on a personal level). I would never do wrong to people, unless I really get the feeling that some people or agencies may pose a threat outside the boundaries of legal jurisdiction that would fuck me over. That is what happened…and towards your “I didn’t apologise” comment, I actually did by U2U, so is just a lie again.
[Edited on 7-9-2019 by nitro-genes]


You can look at clouds that look like animals or angels but that doesn't mean that rabbits or heaven's hosts are busy with some sort of mind altering messaging intended just for you. Get a grip will you. I can see you are making too much of pure coincidences by reading in some sort of meaning as a hidden message that simply isn't there.

Superstition and paranoia have a lot in common. Somebody breaks a mirror and has seven years bad luck and says See there! It's true. Another guy breaks a mirror and wins the lottery. Obviously for mirrors and luck there is an undeniable nexus. Or maybe people can just imagine there is some nexus between things where there isn't any nexus at all. I have no special insight into your unsent U2U drafts nor can I by some magical power read your secret thoughts and as everybody knows a tinfoil hat is a simple countermeasure found effective against "mind control". So should I provide instructions on tried and true, proven designs for tinfoil hats? My own tinfoil hat has proven to be most effective since none of the "hive mind" MK Ultra and beyond brainwash strategies of this cruel world that I have endured have ever been effective for controlling or intimidating me, and only succeeded at pissing me off instead.

Yes the world has had me too much in "school" of one sort or another all my life. But evidently I am just not college material, so wouldn't you just know it, I flunked every brainwashing class about the world's "meaning of life" ideology, while getting an A+ in that Sunday School where Jesus is the kind teacher. I am an actual peacenik at heart, all about peace and love. Actually it is true.

There hasn't been any effort by me to intimidate anyone or anyone's family. I am not some sort of socially dysfunctional malcontent or terrorist or irrational sociopath or psychopath.

https://www.youtube.com/watch?v=d6iXFMaxhQc

benjaminfranklin.bmp - 630kB

by my door.bmp - 1.6MB



Hurricane Michael aftermath crack and ash.bmp - 1.3MB

RJ2 - 7-9-2019 at 14:22

Quote:
[Quote]). I would never do wrong to people, unless I really get the feeling that some people or agencies may pose a threat outside the boundaries of legal jurisdiction that would fuck me over.
please don't act on a "feeling" for such serious matters. If it makes you feel better, you can be ready for all manner of disasters, but until you are confronted with a real life danger, you can't assume there is one.

I wouldn't consider those things you've listed as proof Rosco is threatening/spying on you, Nitrogenes. We all have potentially strange events, just by coincidence, in our lives, enough to seem suspicious once you start looking closely at them. Rosco is known to contribute interesting info on EMs, strong political and sometimes religious opinions, and sometimes, playful jokes about a "cunning linguist" or dieting by eating dog food until he started peeing on fire hydrants.

I wouldn't say the post about the cat's tail was especially out of character, particularly after suggesting curiosity dealing with a highly hazardous material. It only makes sense to say, "be a curious cat-but don't let curiosity kill you". The rocking chair metaphor was kinda odd, but, like I said, so is Rosco Bodine. I dare you to find somebody here who isn't odd.

Likewise, the meter thing seems to be something the power companies have been doing. I guess the new digital ones don't require meter readers to come onto your property. It rained last night were I live, but it's just a coincidence that you likely have a friend or relative in some place that also had rain last night.

The whale poo thing was, I thought , related to this movie.

At the same time, if you don't get paranoid sometimes... you likely don't breathe either. It's a natural human reaction to things that look like they could pose danger. The best you can do is be as ready as you can for all possible outcomes and wait for your paranoia fuel to crystallize into good news or fulminate into a real-life problem. I've seen you guys working together pretty well! Hopefully we will see it happen again.


Not to let my ship collide with RB's tin-fish nose, but I think both of you could take this advice.

[Edited on 7-9-2019 by RJ2]

nitro-genes - 7-9-2019 at 16:42

I tend to be a very logically oriented person person (as is generally evident from my posts I would think?), not taken anything for true unless there is substantial evidence. Sure, one event is odd, but as a scientist I tell you that statistically and logically the chances for ALL of these strange coincidental events and their timing to have happened as they did are INFINITELY small and in the end these events became increasingly more sinister and intimidating. The people showing up at our door, the first one in particular intimidating, were 100% sure members of the Dutch intelligence agency AIVD. Period.

I wish you all the best here at SMDB...






[Edited on 8-9-2019 by nitro-genes]

Rosco Bodine - 7-9-2019 at 16:47

Ancients connected the dots of the stars in the night sky as they saw the stars marking the outlines of various immortals. So it has been a long time that people have been "connecting the dots" to try to find some hidden meaning about things in the world.

Sometimes that kind of abstract analysis does pretty well and sometimes not so good.

https://www.youtube.com/watch?v=mT8bybL_DqY

RJ2 - 7-9-2019 at 17:18

True. You have a good point there, Rosco. And it's amplified by the fact that once you see someone do one thing that seems "suspicious", you will watch everything else and suspect each action more and more.

Anyhow, maybe you're right, NG. Hopefully not, though. I wouldn't write SM off just yet. If you're really worried, use a proxy server to just watch, and not post. If you get to a time when you know you're safe, you can go about posting as normal. RB's been guilty of paranoia in the past, (as have I in my personal life). He even accused one member of being an agent provocateur from MI5! It would be a loss to us all if either of you left over something that turned out to be a non-issue.

Edit: you might very well have had a cop at your door. He might even have came due to something you said on here, maybe. But that doesn't mean Rosco snitched on you. BTW, RB somehow strikes me as an American, after seeing him respond mostly to US political events. You said you're in Holland?

[Edited on 8-9-2019 by RJ2]

Rosco Bodine - 7-9-2019 at 20:01

Quote: Originally posted by RJ2  
True. You have a good point there, Rosco.


There is a complicated world in which we find ourselves "arrivals" originating from the abyss of non-existence, energized by sudden sentience becoming living souls, who ARE created, Yet who are ALL our progenitors? There is some heavy duty "meaning of life" kind of stuff there sufficient to perplex anyone who may waxe even a little philosophical about deep life questions.

And what trouble this imperfect world inhabited by imperfect people can be. And what exactly is HUMAN that is beyond having just the necessary number of chromosomes and looking like just another one of the "naked apes"? What higher qualities makes some people seem NOT REALLY human like they are cut from a different cloth. What puts a spark of the divine in some and a heavy dose of the demonic in others? Why are some kindly gentle loving souls, as if they were angels on loan from heaven here to deliver blessings, while others are delivering curses and calamity acting the role of evil deceitful minions of hell?

What is the point of it all? Where is the meaning to be found and the "big lesson" to be learned if life is for learning, and why is that class called LIFE sometimes such a brutal course? It all seems so truly incredible to me ...at times like yeah really...YMBFK me.
Actually I run into that regularly, being dismayed by just how much about "the world" makes no sense and seems to be truly insane.

Quote:

And it's amplified by the fact that once you see someone do one thing that seems "suspicious", you will watch everything else and suspect each action more and more.


There is a whole lot of EVIL afoot in the world and has been for a long time. Personally I try to avoid it.

Quote:

Anyhow, maybe you're right, NG. Hopefully not, though. I wouldn't write SM off just yet. If you're really worried, use a proxy server to just watch, and not post. If you get to a time when you know you're safe, you can go about posting as normal. RB's been guilty of paranoia in the past, (as have I in my personal life). He even accused one member of being an agent provocateur from MI5!

Yes I did because the shoe fit right down to the science supplies business that had been peripherally involved in a double murder.
My concerns about that vocal "pro-Palestinian" science "hobbyist" AND "supplier" was based on the PROFILE the man revealed and was NOT any "paranoia". In retrospect it is more likely any actual MI5 agent would have been more skilled at keeping a lower profile and becoming a public spectacle would not have been the norm for MI5 tradecraft. Then again we have the NOTORIOUS Christopher Steele (Russian blackmail peepee dossier) who certainly couldn't keep a low profile as a NOC either. Such absolute IDIOTS in British intel must be an embarrassing industry standard that runs counter to the glamorous James Bond 007 mythology for what could be generally ESPIONAGE associated idiots one and all.

Quote:

It would be a loss to us all if either of you left over something that turned out to be a non-issue.


Here here, I'll drink to that ....except I don't drink at all.

Quote:

Edit: you might very well have had a cop at your door. He might even have came due to something you said on here, maybe. But that doesn't mean Rosco snitched on you. BTW, RB somehow strikes me as an American, after seeing him respond mostly to US political events. You said you're in Holland?

[Edited on 8-9-2019 by RJ2]


You betcha I am American. My family here predate the chartering of the Penn Colony and I am part Dutch. My father was with the infantry that liberated Holland from the nazis in WWII. I have no use for nazis or bolsheviks or any of the "authorities" who act like such pieces of gestapo or thought police shit.

There is a lot of evil in the world, and I am on the "other" side and have no confusion about allegiances there, like some commie or fascist wearing a sheep's clothing. Old men or old lions didn't get to be old by being stupid. There is a lot of ageism type bigotry with which I contend where younger people just assume older people must be senile or unsophisticated or somehow just not up to date on all the technology or whatever trendy ideas that younger people think is just brilliant. I thoroughly enjoy bringing a sledgehammer down on that misconception when I encounter it.

God And Country.bmp - 675kB

woelen - 8-9-2019 at 12:27

@nitro-genes: I asked ore information from you and proof. I can see you read my U2U, but you did not respond to me, now several days ago. So, I would say, stop accusing other members of stalking you or even threatening you. Also, stop polluting this thread.

Herr Haber - 9-9-2019 at 03:31

Quote: Originally posted by nitro-genes  
The people showing up at our door, the first one in particular intimidating, were 100% sure members of the Dutch intelligence agency AIVD. Period.

I wish you all the best here at SMDB...

[Edited on 8-9-2019 by nitro-genes]


Oww those equatorial sativas Hissingnoise mentioned are waaay too trippy.

I dont know how I made it to your shitlist. Would be interested to know.

Rosco Bodine - 9-9-2019 at 08:52

A friend of mine who is an Old Mountain Goat said I could pass this along....

Equatorial sativas got nothing on Green Moroccan or Black Nepalese,
but for sativas the JTW is unmatched.....but what would I know :P .......
probably more than I should know, and positively way more than was ever
safe to know for sure

https://www.youtube.com/watch?v=8rhhf0OP2DE

Mountain-Goat-Soldier-on-a-Rock-Ledge.bmp - 926kB

https://www.youtube.com/watch?v=nBJYxPN8qIA

https://www.youtube.com/watch?v=Dn5Pbug5nRw

https://www.youtube.com/watch?v=FKWGSzxtcZA

https://www.youtube.com/watch?v=TWdSi0Xw4u0

I personally assembled and erected a power pole replacement that was made necessary, for being in the eye wall of a category 5 hurricane for half an hour at my location.



new meter panel and pole.bmp - 1.6MB hurricane snapped power pole.bmp - 1.6MB

[Edited on 9/10/2019 by Rosco Bodine]

RJ2 - 9-9-2019 at 21:37

I know this is all really off topic, (maybe this should all go in forum matters?) but I've just got to know. Where you are, what are the power company's rules for this kind of thing? It looks like a great build, but do they have to install one of their meters, or can you put one of your own in if it's accurate?

I suppose you still had to wait for them to get their lines and poles and generators back up. That generator in Cyprus needed quite the overhall after only only a very brief exposure to around 15-20 psi △P.

Which brings me to another question: in this video, it looks like the power poles are a lot tougher than the houses. So now I'm wondering, if that power pole laying on the ground is broken that badly, what does your house look like now?

[Edited on 10-9-2019 by RJ2]

Rosco Bodine - 10-9-2019 at 02:30

Quote: Originally posted by RJ2  
I know this is all really off topic, (maybe this should all go in forum matters?) but I've just got to know. Where you are, what are the power company's rules for this kind of thing? It looks like a great build, but do they have to install one of their meters, or can you put one of your own in if it's accurate?

I suppose you still had to wait for them to get their lines and poles and generators back up. That generator in Cyprus needed quite the overhall after only only a very brief exposure to around 15-20 psi △P.

Which brings me to another question: in this video, it looks like the power poles are a lot tougher than the houses. So now I'm wondering, if that power pole laying on the ground is broken that badly, what does your house look like now?

[Edited on 10-9-2019 by RJ2]


Hey it exceeds code and passed inspection at a reasonable cost :D

Yeah the main lines were down for 5 weeks and the missus and I lived in a hotel from which I commuted the hundred miles distance every couple of days to do debris clearing and essential repairs. It is a 200 amp Square D panel and the meter was salvaged from the old panel and was still operational though it had to be reset / rebooted because the surge when the grid went down caused an anomalous reading of 114 MW/hours used in a service period of 1 millisecond :D and I complained that it would be impossible for me to afford that bizarre "light bill".

That small gray box on the pole next to the ground is the gigabit digital data feed that was out for 4 months while I was forced to use in the alternative satellite and wireless for coms.

We are still "digging out" 11 months later from what was a truly surreal experience.
The level of damage from a cat 5 hurricane is so great it is a terrain altering event
that is like a visit from a supernatural force that simply flattens the whole countryside as far as the eye can see and more distance miles beyond the horizon. It takes an hour to drive across the path of destruction after the roads are finally cleared and everything is either substantially damaged or totally destroyed. Even steel and concrete buildings like banks and hospitals are demolished, and much of what remains standing is knocked out of plumb and is later condemned and bulldozed because the damage is too great to simply repair. Most of what remains is damaged so badly that if it was a wrecked vehicle it would be "totaled" by the insurance company and sent to the crusher. 4 dozen people were reportedly killed outright but I think there were actually a lot more unreported. A few days later the smell of decomp filled the air over the entire area. More than a hundred square miles smelled like bloated roadkill. I stayed way for nearly a week to let the stench of death dissipate so I could continue with cleanup and repairs.

You asked about the house/s...well ...:D ....they are coming along and eventually repairs should be completed ...:D

[Edited on 9/10/2019 by Rosco Bodine]

RJ2 - 10-9-2019 at 03:26

So your house was probably 100% blown off the foundation? Whoa, Wow, and props to you for not only replacing it, and your power pole and panel but also finding the runaway meter:D 5 weeks to restore power? I'm surprised they got it on that quick. I'm also amazed that it would damage concrete buildings. I guess about 2 psi dynamic presure for minutes on end will do the same damage as 10-20 psi dynamic (and 20-30 something overpresure) for a few seconds.

Glad you mae it in one piece! Glad I don't live in hurricane territory!

Edit: it also gives me confidence that if people can survive that and rebuild, we should be able to survive a nuclear war no problem. Just evacuate to the countryside, and then rebuild somewhere that hasn't became radioactive:D

[Edited on 10-9-2019 by RJ2]

Rosco Bodine - 10-9-2019 at 04:26

The air pressure differential doesn't compare with the reality that is more like hydraulic mining or water jet cutters ....the moving air is carrying a load of liquid and solids which changes the kinetic energy considerably ....like a whole order of magnitude increase.
What would be just "wind" becomes a scythe in the hands of the grim reaper. It is like being the earthworm on the ground when the lawn mower passes overhead, but decides to just stop there and run for awhile that begins to seem like forever. It is a "religious" experience that creates an eagerness for prayer in all sinners,
and leaves sphincter cramped fannies trying for a week to relax for a return to regularity. :D On the anxiety scale of 1 to 10 it is an 11.

My properties are pretty banged up and damaged but still livable, with repairs continuing for months and incrementally delayed with delivery delays caused by suppliers sold out / out of stock and other "supply system overload" everywhere in the impact area. For immediate most essential repairs I was hauling materials that could be gotten only in distant unimpacted areas before shortages hit there also, which didn't take very long. Electrical supplies got sold out in a few days. A hurricane overwhelms all the materials and services vendors and months or even years delays are the new normal for what were before routine ordinary things.

Trying to get replacement windows can take six months because the factory is backlogged with more orders than can be filled same story everywhere about every common item. Everything that was taken for granted as a common item can become scarce when the usual supply and demand balance no longer applies in a disaster area.

It is an interesting experience to see what a great "equalizer" a disaster can be when nobody escapes the "shock and awe" that is 100% a full attention getter provided by an overwhelming force of nature that is humbling to endure, and leaves survivors counting their blessings really just to still be alive, and appreciating that as a miracle which it just could be. There really is no way to describe in words what the eye wall of a cat 5 is like ....it is just surreal and jawdropping what the intensity of energy is like there and it isn't just a lot of moving air.....it is multidimensional ...for lack of a better term. For one thing, a person can easily see through what is just a lot of moving air...like looking out of an airplane window.
But there is zero visibility in the eye wall of a cat 5 and you can't see 2 feet through it ...it is like being in a car wash times ten, and being hammered with stuff that looks like ground up mulch coming out the discharge chute of one of those limb chipper shredders. The air is like a semi-liquid semi-solid paste that the atmosphere has become, that is so thick it would choke a person to try to breathe....and so abrasive it will sandblast paint from metal. It literally will tear bark from snapped trees and will tear skin and flesh even more easily. Exposed in the open it would cut a living animal or person to pieces.

I never thought I would have or need to own 5 chain saws of different sizes .....but now I do. And I have been wanting a #6 that has "more power" for Santa Claus to bring me. :D

One glorious fringe benefit is that it seems women have generally become a lot more friendly, I suppose to encourage men to play their natural roles as protector / provider / hero / ect. and to keep up their morale .....which curiously is a very arousing change of disposition by the females, which I have been enjoying immensely. There is bound to be a spike in the birth rates that should correlate to the time of a disaster that will be similar to the uptick in births associated with blizzards and that sort of thing that results in "what are we going to do now" ....I know, let's be busy bees :D Isn't love wonderful ? God bless those caring women for doing their part and doing what comes naturally. See, nature is not all bad. :D

[Edited on 9/10/2019 by Rosco Bodine]

MineMan - 10-9-2019 at 15:10

Makes sense that a disaster can blow through the PC we have been taught and encourage men and women to fulfill their natural roles and despositions. Women may say they don’t want a hero, a provider and a manly man... but what is more important is what they feel... not what they want :)

This is interesting rosco... you could have a very interesting sociology and physiology paper on your hands...

Vomaturge - 10-9-2019 at 20:00

Quote: Originally posted by Rosco Bodine  
The air pressure differential doesn't compare with the reality that is more like hydraulic mining or water jet cutters ....the moving air is carrying a load of liquid and solids which changes the kinetic energy considerably ....like a whole order of magnitude increase.
What would be just "wind" becomes a scythe in the hands of the grim reaper. It is like being the earthworm on the ground when the lawn mower passes overhead, but decides to just stop there and run for awhile that begins to seem like forever. It is a "religious" experience that creates an eagerness for prayer in all sinners,
and leaves sphincter cramped fannies trying for a week to relax for a return to regularity. :D On the anxiety scale of 1 to 10 it is an 11.

My properties are pretty banged up and damaged but still livable, with repairs continuing for months and incrementally delayed with delivery delays caused by suppliers sold out / out of stock and other "supply system overload" everywhere in the impact area. For immediate most essential repairs I was hauling materials that could be gotten only in distant unimpacted areas before shortages hit there also, which didn't take very long. Electrical supplies got sold out in a few days. A hurricane overwhelms all the materials and services vendors and months or even years delays are the new normal for what were before routine ordinary things.

Trying to get replacement windows can take six months because the factory is backlogged with more orders than can be filled same story everywhere about every common item. Everything that was taken for granted as a common item can become scarce when the usual supply and demand balance no longer applies in a disaster area.

It is an interesting experience to see what a great "equalizer" a disaster can be when nobody escapes the "shock and awe" that is 100% a full attention getter provided by an overwhelming force of nature that is humbling to endure, and leaves survivors counting their blessings really just to still be alive, and appreciating that as a miracle which it just could be. There really is no way to describe in words what the eye wall of a cat 5 is like ....it is just surreal and jawdropping what the intensity of energy is like there and it isn't just a lot of moving air.....it is multidimensional ...for lack of a better term. For one thing, a person can easily see through what is just a lot of moving air...like looking out of an airplane window.
But there is zero visibility in the eye wall of a cat 5 and you can't see 2 feet through it ...it is like being in a car wash times ten, and being hammered with stuff that looks like ground up mulch coming out the discharge chute of one of those limb chipper shredders. The air is like a semi-liquid semi-solid paste that the atmosphere has become, that is so thick it would choke a person to try to breathe....and so abrasive it will sandblast paint from metal. It literally will tear bark from snapped trees and will tear skin and flesh even more easily. Exposed in the open it would cut a living animal or person to pieces.

I never thought I would have or need to own 5 chain saws of different sizes .....but now I do. And I have been wanting a #6 that has "more power" for Santa Claus to bring me. :D

One glorious fringe benefit is that it seems women have generally become a lot more friendly, I suppose to encourage men to play their natural roles as protector / provider / hero / ect. and to keep up their morale .....which curiously is a very arousing change of disposition by the females, which I have been enjoying immensely. There is bound to be a spike in the birth rates that should correlate to the time of a disaster that will be similar to the uptick in births associated with blizzards and that sort of thing that results in "what are we going to do now" ....I know, let's be busy bees :D Isn't love wonderful ? God bless those caring women for doing their part and doing what comes naturally. See, nature is not all bad. :D

[Edited on 9/10/2019 by Rosco Bodine]


So here I was thinking you evacuated and came back to a "Grade A Damage" neighborhood, but it looks like you saw the storm a bit (or a lot) too close for comfort! Wow. Just wow.

On the difference of dynamic pressure vs particle debris, I see how even 1% rock by volume (30 kg/m3) would turn 100M/Sec wind into a truly devastating force. 20 psi dynamic is a only a hair less than you would experience a mile from a megaton explosion. Of course seeing is believing, and I'm not sure I need to that badly. The best photos I can send for "extreme weather" is the odd late May snow.;)
Screenshot_20190910-190851-320x200.jpg - 15kB

Screenshot_20190910-190856-320x200.jpg - 12kB
One more question on the meter, did you find it in your yard or did you have to look around. Could it have been from a comercial or industrial building and just been lifted into a higher level of the cloud. I don't know about meters, but I recently had to recycle a few rusty old meter bases; this entailed separating the insulated plastic socket from the sheet metal enclosure. The quickest way, turns out, was to slam them on the ground. A couple 15m/sec straight-down impacts with asphalt broke the socket's plastic around every screw, and separated it nicely. I suppose the meters themselves must be a whole lot tougher!

@RJ2: I too am amazed at how quickly they got the power back on. I guess that's the difference between an island like Cyprus, where that one power plant supplied half the nations electricity, and the lower 48 United States where if you can run a long enough powerline, you can always find a power station with energy to spare. That linked picture of that power plant didn't look that bad, though. All the framework and internal equipment looked basically undamaged. I'm still surprised that it took the Cypriots so long to get it back online.

Screenshot_20190910-190851.jpg - 148kB

[Edited on 11-9-2019 by Vomaturge]

Rosco Bodine - 11-9-2019 at 02:22

The old meter base and panel I built also 35 years ago was laying on the ground but the meter was a recent replacement about 5 years ago, was still sealed and appeared to be okay, and was still plugged into the old meter base. I unplugged it and reinstalled it in the new panel and it powered up okay. The conductors 4/0 X 3 triplex have about a 4 metric ton breaking strength and the cable was snapped like sewing thread from tension failure that also snapped the 2 power poles that supported them. The picture before only shows one pole. A second larger pole was snapped at the ground also.


snooby - 12-9-2019 at 09:52

Thanks rosco, for more info about the carbo stuff.
I Will try again..

For now we almost got everything for the icm103.. IT Will posted.
The nickel amino perchlorate still rules. Only waiting for the White hno3 :)

Rosco Bodine - 13-9-2019 at 11:06

Quote: Originally posted by snooby  
Thanks rosco, for more info about the carbo stuff.
I Will try again..

For now we almost got everything for the icm103.. IT Will posted.
The nickel amino perchlorate still rules. Only waiting for the White hno3 :)


No problem, have a ball with it and stay safe.

Another idea generally regarding the nickel carbohydrazide perchlorate and analogous complexes is the possibility of a compound salt / double salt with nickel glycine perchlorate or the analogous copper or perhaps zinc or other complex salts that could control the sensitivity. Betaine perchlorate is another possibility for formation of a potential complex salt.

snooby - 20-9-2019 at 12:49

We only got one synthesis right now which is this one :

https://www.nature.com/articles/s41467-017-00286-0

The first reflux was not a succes, but, this does not meab the next Will Be not too... However, the synth is not very detailled and therefore i did a lot of research for more detailled synths. However, i did not found Anyone... If someone does have more info, pls let me know... Thank you in advance and we Will keep you updated.


Mr.Greeenix - 22-9-2019 at 05:48

Aminoguanidin Ligands

Quote: Originally posted by Tyneman  
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.


Going back to the Aminoguanidin Ligands and the requiered perchlorat salts.
Does someone have a few papers on the pechloric salts and their preparation?

Is it possible to get (pure) nickel perchlorat by using sodium perchlorat and nickel sulfate ?

Thanks for the help I cant really find much on this.

Tyneman - 22-9-2019 at 10:53

No papers, but can tell you how I did it.

Take your cheapest, most soluble Ni-salt. Weigh it and put in water. Then add a stoichiometric amount of Na2CO3. (A little extra won't hurt, is cheaper then Ni-salt and excess will be washed away)
NiCO3 will percipitate out. Filter off and wash 2 times with cold dH2O. Dry.
Take some (dilute) perchloric acid, slowly and with stirring add NiCO3. When bubbling (CO2) subsides use very small portions. When there is no more CO2 to be seen you have a solution of Ni-perchlorate. Check for acidity with some pH paper.
Slowly evaporate the water and harvest your Ni-perchlorate crystals.

I wasn't using Na-perc though but perchloric acid.
Hope this at least helps a little, although it's not a true answer to your question.

snooby - 9-10-2019 at 08:28

I came by this:

new initiating explosive-tetraamminediazido cobalt(III) perchlorate(DACP) was synthesized. Its structure was characterized by the IR, HNMR etc. And the main properties were measured by the various methods. The results show that DACP is an excellent primary explosive similar to tetraamminebis (5-nitrotetrazolato) cobalt (III) perchlorate (BNCP) in functions. Synthetic method of DACP is much simpler than that of BNCP. In some initiating devices, DACP may be a substitute for BNCP and Pb(N3)2...

The ctcn is goed to make:
The synthesis conditions are: concentration CTCn suspension was: 5% to 7% (by mass); raw CTCN: 5-HT: molar ratio of HC104 is 1: 2.2: 2.7, reaction temperature was 8
..but i really cannot rond anyy good syth...

Rosco Bodine - 10-10-2019 at 14:10

Quote: Originally posted by snooby  
I came by this:

new initiating explosive-tetraamminediazido cobalt(III) perchlorate(DACP) was synthesized. Its structure was characterized by the IR, HNMR etc. And the main properties were measured by the various methods. The results show that DACP is an excellent primary explosive similar to tetraamminebis (5-nitrotetrazolato) cobalt (III) perchlorate (BNCP) in functions. Synthetic method of DACP is much simpler than that of BNCP. In some initiating devices, DACP may be a substitute for BNCP and Pb(N3)2...

The ctcn is goed to make:
The synthesis conditions are: concentration CTCn suspension was: 5% to 7% (by mass); raw CTCN: 5-HT: molar ratio of HC104 is 1: 2.2: 2.7, reaction temperature was 8
..but i really cannot rond anyy good syth...


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

Rosco Bodine - 13-10-2019 at 08:22

Quote: Originally posted by Rosco Bodine  
A similar complex to Diazidodiamminocopper(II) described on page 8 of this thread is a related Trimethylamine complex or compound salt trimethylammoniumpentazidodicuprate

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

Quote: Originally posted by Taoiseach  
was prepared according to

CuSO4*5H2O + 2NH3 + 2NaN3 ---> [(NH3)2(N3)2Cu] + Na2SO4 + 5H2O

NH3 was added to a solution of CuSO4 until the precipate of Cu(OH)2 redissolved. A saturated warm solution of NaN3 was added. Upon cooling and addition of an equal volume of ethanol, a nice crop of [(NH3)2(N3)2Cu] precipated.

Green-blue glistering crystals. Unlike copper azide these are not friction sensitive. Explodes upon flame contact.

Obviously the compound is oxygene-deficient, so addition of a strong oxidizer should increase its power.



trimethylammoniumpentazidodicuprate is a similar compound about which I can find very little information. It is unclear to me if this type complex or compound salt is strictly limited to the example of trimethylamine azide forming a complex salt with copper azide, or if other trimethylamine salts such as the perchlorate may also form a complex or mixed salt with copper azide. It would seem possible that different metals may also form analogous compounds as does copper.

See attached excerpt from PATR for description of

trimethylammoniumpentazidodicuprate

(CH3)3N-HN3-2[Cu(N3)2]


Trimethylammoniumpentazidocuprate.bmp - 456kB



Attachment: straumanis 1943.pdf (733kB)
This file has been downloaded 685 times

[Edited on 10/13/2019 by Rosco Bodine]

JohnDoe13 - 13-10-2019 at 09:04

https://sci-hub.tw/10.1002/zaac.19432520102

ethanolamine bis-cupric azide

Rosco Bodine - 15-10-2019 at 06:07

Even more interesting for experiments would be the ethanolamine complex that bridges 2 copper (II) azides. Federoff indicates that this complex forms an non-explosive hydrochloride salt, which suggests that other salts may also be possible, that would likely be energetic, such as a nitrate or perchlorate. This complexed cupric azide would also be a candidate for coprecipitation complex salt schemes with glycine complexed copper perchlorate.

Ethanolamine-Tetrazido-Copper  Ethanolamine bis-Copper Diazide.bmp - 652kB

ethanolamine complexed bis-cupric azide.bmp - 428kB

ethanolamine complexed bis-cupric azide 2.bmp - 284kB

Attachment: Straumanis II 10.1002@zaac.19432510405.pdf (792kB)
This file has been downloaded 658 times

[Edited on 10/15/2019 by Rosco Bodine]

Period 4 transition metal ammine complexes

franklyn - 25-10-2019 at 09:05

Inorganic Nitrates.jpg - 76kB


The first row transition elements , period 4 metal nitrates and other anion radicals are the basis for complex forming species and moities.
I have compiled below some links from previous posts of this thread and other sources as well along with some ideas for investigation.
• • D O T S identify forum downloads

Anhydrous , Chromium III nitrate Cr(NO3)3
similarly to Magnesium nitrate Mg(N03)2 , or Titanium nitrate Ti(N03)4 , readily hydrates but has higher dissociation temperature than the others.
Can it form a peroxide H2O2 addition compound ? That would be one super duper oxidizer.
Peroxidates of ionic Nitrates discussed here => www.sciencemadness.org/talk/viewthread.php?tid=1778&page...
suggests Hydrogen Peroxide can substitute the water of the hydrate to form an adduct.
http://chromium.atomistry.com/chromium_trioxide.html

http://en.wikipedia.org/wiki/Chromium(III)_nitrate
Forms an ammine complex comparable to TNT in explosive strength.
www.sciencemadness.org/talk/viewthread.php?tid=1778&page...
A peroxidate of this would enhance performance.

Preparation of Hexammine Chromium (III) Nitrate with Liquid Ammonia
http://alpha.chem.umb.edu/chemistry/ch371/documents/Labrepor...

Synthesis and Characterization of Hexammine Chromium (III) nitrate
www1.lasalle.edu/~prushan/IC-articles/experiment%201%20-AIC....

Thermal dissociation of Hexammine Chromium (III) complex , prep on page 5
https://ttu-ir.tdl.org/bitstream/handle/2346/16612/312950150...

Peroxidation can be tried on Nickel Hydrazine Nitrate
https://en.wikipedia.org/wiki/Nickel_hydrazine_nitrate

www.sciencemadness.org/talk/viewthread.php?tid=1778&page...
Maybe anhydrous hydrazine would instead yield a hydrazine complex

Hydrazine complexes of transition metals as prospective explosives
• • www.sciencemadness.org/talk/files.php?pid=301489&aid=264...
https://pdfs.semanticscholar.org/7ed5/24109f55815dc81cf1e7c3...

Synthesis and Characterisation of Metal Hydrazine Nitrate , Azide and Perchlorate Complexes
• • www.sciencemadness.org/talk/files.php?pid=274667&aid=223...

Hydrazine salts of Nickel , Cobalt
• • www.sciencemadness.org/talk/files.php?pid=275559&aid=224...
http://nowa.pirotechnika.one.pl/hedm/nhn1.pdf

Inorganic Hydrazine Derivatives
http://chemistry-chemists.com/chemister/Neorganika/inorganic...


.

Rosco Bodine - 25-10-2019 at 16:33

Recently I was reading a probably recent patent or journal article that described the easy cheap synthesis of Zinc Peroxide useful as a stable and practical oxidizer in primer compositions. It was simply made by precipitation from aqueous H2O2 using IIRC ordinary zinc oxide as the precursor, simply stirring the mixture ...or possibly it was a different method used...I should have saved the reference and tagged it but I was busy with something else and did not save the reference.

The complexation of copper by ethanolamine acting as a bridge for 2 copper salts like the azide could also be of interest for copper perchlorate, which would very probably be energetic.

[Edited on 10/26/2019 by Rosco Bodine]

Synthesis and Complexation of Nitrogen-rich Materials

franklyn - 27-10-2019 at 00:59

Download here _
https://ruor.uottawa.ca/bitstream/10393/33162/1/Sebastiao_El...
pdf page 68 ( page 47 in paper ) charts metal nitrate complexes having Hydrazine ligands. I wonder if peroxidation of these can occur at all given hydrazine itself hypergols with hydrogen peroxide. The author here ( Ph.D candidate ) outlines energetic polymer derivatives from the aforesaid , interesting. ( I had speculated in an earlier time using formaldehyde could serve this purpose ) Center of post here _
www.sciencemadness.org/talk/viewthread.php?tid=1778&page...
This is just that one section , lots more fun stuff discussed in the other sections of the dissertation.

While on the topic , can the cited inorganic nitrates form a complex with Nitroguanidine which tends to be as basic as Urea. I once discussed that at length here _
www.sciencemadness.org/talk/viewthread.php?tid=9443#pid17013...

.

Rosco Bodine - 27-10-2019 at 06:37

The patent reported semicarbazide complex analogue of Nickel Hydrazine Nitrate being possibly more stable as the undescribed and unreported perchlorate variant that would be Nickel bis-Semicarbazide Diperchlorate is another perhaps novel "unknown" that may not have same instability and treacherous sensitivity as its notorious Nickel Hydrazine Perchlorate analogue that has made news for traumatic amputation maimings of curious but careless college student experimenters.

Mixed complexes are also possible where bridged complexation may have a complexing agent pair in parallel for example where a bis or poly complexation involving two or more amines is a case where the two or more amines are not the same amine, for example the case where a tetra ammonium complex forms first, and then upon addition of methylammonium, some of the ammonium is displaced and replaced by methylammonium.....a strategy which can lead to Oxygen balance .....as would be the case with Copper Tetra-ammonium Diperchlorate dissolved in aqueous ammonia being
converted to Copper ( bis-ammonium / bis-methylammonium ) Diperchlorate .....Also novel and unreported......gotten by simply adding 2 mole equivalents of methylamine as hydroxide or nitrate or perchlorate to the reaction mixture. Comparative lower solubility for the methylammonium substituted complex should preferentially precipitate the heavier and lower solubility complex.

Analogously, instead of methylammonium, dimethylammonium, trimethylammonium, tetramethylammonium, hydrazinium, semicarbazide, aminoguandinium, ethanolamine, or betaine, may serve to function as similar substituent agents for partial or complete displacement of the ammonium from an ammonium complexed precursor, producing the desired higher molecular weight shared complex or higher mole weight complex, when that direction of reaction is favored by a lower solubility of the desired product which crystallizes and precipitates.

Have a greatly blessed Sunday my friends ......

https://www.youtube.com/watch?v=KShGGElRsxU Angelis - (Latin) Angels

Angelis - Sanctus Dominus - Our Holy Lord.bmp - 481kB

Attachment: Angelis - Libera.mp3 (6.3MB)
This file has been downloaded 710 times

https://www.youtube.com/watch?v=eBLyk6yOTnU How Shall I Sing That Majesty

https://www.youtube.com/watch?v=P-akN9q8ks0 From A Distance

[Edited on 10/27/2019 by Rosco Bodine]

papaya - 4-9-2020 at 15:19

Anyone is still after TACN ? Dig your own !

Enjoy.

https://www.researchgate.net/publication/281488300_Shilovite...

"Shilovite, natural copper(II) tetrammine nitrate, a new mineral species The new mineral shilovite, the first natural tetrammine copper complex, was found in a guano deposit located on the Pabellón de Pica Mountain, near Chanabaya, Iquique Province, Tarapacá Region, Chile. It is associated with halite, ammineite, atacamite (a product of ammineite alteration) and thénardite. The gabbro host rock consists of amphibole, plagioclase and minor clinochlore, and contains accessory chalcopyrite. The latter is considered the source of Cu for shilovite. The new mineral occurs as deep violet
blue, imperfect, thick tabular to equant crystals up to 0.15 mm in size included in massive halite.
...
The idealized formula is Cu(NH3)4(NO3)2.
....

"

NHN from hydrazine sulfate - is it worthwhile?

dangerous amateur - 1-10-2020 at 07:15

@papaya:
haha nice find :D


I had given this up for a very long time, and unfortunately lost my lab notes from few years ago.
I used hydrazine sulfate with barium/sodium hydroxides, and my NHN yields where always to low for further experimentation. Now my fingers are itching to try this again...

Did anybody here ever got a decent yield with low concentrated hydrazine from freebasing? I'll never get the commercial 60% stuff some people are using, so I might as well abandon the whole thing...



Another question:
Did anybody ever tried cobalt hydrazine nitrate?
There's little information out there... I wonder if this has the same flaws as NHN, lazyness in DDT, large critical diameter except with superstrong confinement...

Laboratory of Liptakov - 4-11-2020 at 03:19

I read it all. Great news about TACN. When I go there to tear a rock, I'll only take a detonator and a piece of wire with me....:D

Laboratory of Liptakov - 4-11-2020 at 03:27

@dangerous amateur...NHN works reliable in mixture with ETN 1:1 Density about 1 - 1,2g / cc in solid cavity. Simply dry mix of powders.

dangerous amateur - 5-11-2020 at 01:25

@LL:
Great to have you back. If it's really you.....?

I do not doubt the mixture works in your copper tubes. It might be a good solution.

But my question 3 posts upwards was about making NHN from low concentrated hydrazine. Until now I failed with that.
Should I pursue this any further or rather look for commercial 60% solution?

B(a)P - 5-11-2020 at 01:45

I have had good success making NHN using hydrazine free based from hydrazine sulfate.
Can you describe your process?
My approach has been as follows:
- make sure everything is as dry as possible to start and stir stir stir stir stir then stir the whole way, also keep everything cold at all times.
- add NaOH in two portions
- after the first portion of NaOH add 1 ml of cold DH2O, if the reaction does not take off add another 1 ml.
- add ethanol once the reaction is proceeding
- at this point the solid portion will be sticky, add the second portion of NaOH, this makes the sodium sulfate go to sodium bisulfate and pull a bunch of water out with it.
- wash twice with ethanol and you have fair concentrated hydrazine in ethanol.

Laboratory of Liptakov - 8-11-2020 at 03:07

Interesting process. Two dry powders? A like fine powder? Drying NaOH can be problem. Any ratios between Hydrazine sulfate and NaOH? Basic weight of both compounds? For 1- 2 ml DH2O ? I estimate, vacuum Buchner was used? How much ethanol?
Thanks.

MineMan - 15-11-2020 at 16:07

He’s back!!

B(a)P - 16-11-2020 at 01:08

Quote: Originally posted by Laboratory of Liptakov  
Interesting process. Two dry powders? A like fine powder? Drying NaOH can be problem. Any ratios between Hydrazine sulfate and NaOH? Basic weight of both compounds? For 1- 2 ml DH2O ? I estimate, vacuum Buchner was used? How much ethanol?
Thanks.


Sorry for the slow reply, I missed your message. I just dug out out my lab notes from last time I did this.
10 g of hydrazine sulfate
17 g EtOH start with 10 g then use 7 g for the second rinse
6.15 g NaOH added in two equal portions as described above
1.5 mLs dH2O

I did not use a funnel or filtration I simply decanted the ethanol/hydrazine liquid from the sodium bisulfate once it had settled.

Edit - Yes both solids as fine dry powders stored in a desiccator bag prior to use.

[Edited on 16-11-2020 by B(a)P]

Laboratory of Liptakov - 19-11-2020 at 03:45

Thanks BP....interest method...:cool:

dangerous amateur - 6-2-2021 at 08:49

Sorry for the late answer ;)

Sadly I did not find my old notes, but I used Barium hydroxide back then. But I concluded that it's not working ;)
I will try it again this year.


Quote:

10 g of hydrazine sulfate 17 g EtOH start with 10 g then use 7 g for the second rinse 6.15 g NaOH added in two equal portions as described above 1.5 mLs dH2O


Could you somehow judge the yield somehow? How do you know it was
Quote:

fair concentrated

?



[Edited on 6-2-2021 by dangerous amateur]

Hens2 - 26-9-2021 at 05:43

You can weigh out the sodium sulfate thats left behind and do some maths. calculate the theoretical amount of sodium sulfate which should be synthesised in the procedure. than check it with the one that was left behind. dont forget to add the small amount which is desolved in etoh (solubility of na2so4 is about 0.44g/100g of etoh (100%)). with that you should be able to calculate the mass percentage of the hydrazine in your etoh solution.. correct me if i am wrong.;)

night429 - 28-12-2021 at 22:05

I've seen it mentioned once in this thread, but I made (what I believe to be) tetraamminecopper (ii) picrate. I made this by adding a solution of excess tetraamminecopper (ii) sulfate to a solution of warm ammonium picrate with a bit of ammonia to ensure the complex didn't fall apart. Immediately, a flaky gold-colored precipitate formed. Upon filtering, the filtrate remained the typical color of the tetraamminecopper (ii) ion, indicating that the complex hadn't fallen apart. Drying caused the precipitate to "mat", and I chopped it up while damp with a metal spatula.

20211228_235948.jpg - 239kB

The properties of the product are typical with both a copper salt and a picrate. Upon exposure to flame, a green color is observed, indicating copper is present. The product then melts, followed by vigorous and rapid burning; a noise and flame are both present. To prove the compound I made wasn't just copper (ii) picrate, I made the latter by adding copper (ii) chloride to a concentrated sodium picrate solution. A green precipitate formed, which was filtered. The properties of this precipitate, not only color, are different than the compound I made. Burning is less vigorous, but it burns more readily and doesn't melt beforehand.

Comparison of the supposed tetraamminecupric picrate (left) and cupric picrate (left):
20211229_002933.jpg - 130kB

So, the only conclusion I could come up with was that the product I have is tetraamminecopper(ii) picrate, considering its properties are quite different than both ammonium picrate and copper (ii) picrate, and I don't think that a product could've been made that wasn't this one, given the conditions I performed the reaction in.

Raid - 26-3-2023 at 10:27

i did the same thing as night429 but instead of the sulfate I did a nitrate and it makes a nice dark forest green complex. its somewhat energetic, I'm going to do some more large scale tests with it later.

Raid - 31-3-2023 at 07:14

I found this in a patent for NiHN and CoHN and it says that adding KCLO3 or LFCN (Lead Ferrocyanide) reduces the friction sensitivity, I'll post a screenshot of the chart here if you want to see it. I'm wondering if this is even worth doing since they don't show the effects on DDT velocity. They did say that the NiHN is an almost oxygen balanced compound and I'm thinking that maybe the KCLO3 may help the DDT a bit, but since the KCLO3 is not Incorporated in the molecule i'm not so sure.


Screenshot 2023-03-31 9.51.30 AM.png - 26kB

papaya - 31-3-2023 at 13:08

I've created a whole new thread since your question raised some memories... btw can you provide a link to that patent, since it sounds like parallel to my own experiments? https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

[Edited on 31-3-2023 by papaya]

Raid - 3-4-2023 at 06:16

I have uploaded the patent in the "NHN based improved primary composition" that you have just made.

papaya - 3-4-2023 at 09:50

Quote: Originally posted by Raid  
I have uploaded the patent in the "NHN based improved primary composition" that you have just made.
Thanks a lot!

specialactivitieSK - 23-4-2023 at 05:07

Can 500g TACN ignite standard granulated ANFO?

[Edited on 23-4-2023 by specialactivitieSK]

MineMan - 24-4-2023 at 23:35

Quote: Originally posted by specialactivitieSK  
Can 500g TACN ignite standard granulated ANFO?

[Edited on 23-4-2023 by specialactivitieSK]


Can this get removed? It puts this place in a bad name and is low effort. Has nothing to do with exotic primaries which are used sub gram

Laboratory of Liptakov - 25-4-2023 at 08:24

I am also for remove 500g TACN question.

dettoo456 - 30-5-2023 at 15:15

I may or may not have made some sodium 3-nitro-1,2,4-triazolate recently and now I can’t figure out what to do with it. It is reasonably powerful on its own (unconfined heating from under Al foil causes melting and a flash/poof similar to organic peroxide ignition). The Ag salt is like more powerful tetrazene - same smokey, poofy decomp but can actually deflagrate or detonate in the right confinement. I want to make the Cu (i) and (ii) salts when I get a chance and they should act as a sort of insensitive booster EM.

Anyways though, I wanted to know if making the triazole variant of BNCP would likely bear any fruit? It’s already extremely stable, so would replacing the 1 N with C just make it kind of overly insensitive and therefore useless?

Microtek - 30-5-2023 at 22:29

I would request that you examine solubilities of the salt as well as the free acid (I know that doesn't sound very exciting, but many contemporary papers don't bother to do that, and it can really help with preparation and identification if you know how soluble your product is). Then I would be interested in salts of nitrogen containing bases (ammonia, hydrazine, hydroxylamine, etc.). How did you synthesize the material?

dettoo456 - 31-5-2023 at 12:51

Since I had some old, yellowing AGB lying around, I refluxed it in >90% CH2O2 for about 3-4hrs until the acid smell stopped and the mixture was a yellow, transparent liquid. Then I evaporated it down under gentle heat (this took a long time and even then, the final off-white goop formed a hygroscopic gel - I assume this material is 3-amino-1,2,4-triazole with impurities of formylaminoguanidine.

With the assumption being by that the product is mostly Amitrole, I followed the PacSci Oxidative nitrosation in US9598380B2 (prep for 5-NaNTz) but modified by mole scale to 3-Amino-1,2,4-triazole. The reaction was about the same as for 5-ATz but it generated what seemed like larger amounts of NOx. The product (assumed to be Sodium 3-nitro-1,2,4-triazolate) precipitated in the crude rxn mix even in stirring and above 60C. Rxn miz was then allowed to cool, product filtered, dried, then extracted with Acetone to get rid of Na2SO4 and bisulfate.

The final product (Na-3-NTiz), crystallizing out of acetone, presents as bright yellow, opaque ‘petal-like’ shapes. It does seem to be modestly hygroscopic on standing in an open vessel at rt.

I’m busy right now but I’ll try to give more info and pictures later on.

[Edited on 1-6-2023 by dettoo456]

Microtek - 1-6-2023 at 08:15

I think you are supposed to react the product of the acetylization (from heating the guanidine derivative with carboxylic acid) with aqueous base. Sodium- or potassium carbonate seem popular from the papers I have read.



Attachment: kurzer1963(1).pdf (1.6MB)
This file has been downloaded 275 times


dettoo456 - 1-6-2023 at 11:10

I know that Amitrole is produced industrially via formylation and cyclization of AGB, but there are very few papers on the prep of 3-nitrotriazole. One paper (https://onlinelibrary.wiley.com/doi/10.1002/047084289X.rn020...) lays out a synth starting from amitrole but i had issues in the past trying to replicate it, so I used the modified 5-ATz oxidative nitrosation route.

Also, I edited the last post I made - the Sodium salt IS hygroscopic, or at least forms a type of hydrate from crystallizing in acetone.

I also don’t know how to post pics or videos in SM, if you could let me know how I’d be very grateful. Thanks

[Edited on 1-6-2023 by dettoo456]

[Edited on 1-6-2023 by dettoo456]

articneptune - 20-9-2023 at 01:02

Hello all,

I'm currently working on synthesis of hydroxylammonium nitrate HAN. I've got it setup as per the attachment but using 70% HNO3 instead of 65%.

I've had one attempt at it so far, but I couldn't keep the mixture cool enough and it started reacting quite violently. I'm going to give it another shot soon but with salt in the ice bath. I'm hoping this will keep it cool enough. Once I've got HAN I'm planning on adding some methanol and AN to make something like HAN269MEO (rocket monopropellant). If there's any left over I might just put it in the rotary evap and try get some HAN salt.

A question I have is how would you add the methanol and AN? Just measure it out and mix it in?

HAN synthesis.png - 21kB

Microtek - 21-9-2023 at 04:54

Yes, I would simply measure out AN and MeOH. Isn't this setup unnecessarily complicated? I would just add a slight excess of HNO3 and then neutralize the excess with a little ammonia. If you keep the mix well stirred and either add the acid very slowly (dropwise) or dilute it a little more, I doubt you will have any trouble with excessive exothermicity.

articneptune - 24-10-2023 at 02:18

Thanks for the reply

Quote: Originally posted by Microtek  
Isn't this setup unnecessarily complicated?


It may be yes but it's a procedure used in literature that I could reference if I ever need to. I've since managed to make a batch of HAN. I'm going to be mixing it with various things and putting it in a strand burner this week. Left over HAN is going to be concentrated to it's salt form and then ignited. I'll update if anything particularly interesting occurs.

dettoo456 - 20-11-2023 at 11:50

Anyone had experience with Silver 5-ATz complexes such as [(2Ag)5-ATz] NO3 or ClO4? The perchlorate is mentioned in engager’s tetrazole write up and a patent but there doesn’t seem to be much discussion on it. I tried to make the nitrate the other day according to klapotke’s procedure (https://pubmed.ncbi.nlm.nih.gov/19105192/) but it didn’t seem to yield anything that great. To start, 5-ATZ doesn’t dissolve that great in conc (anything higher than azeo %) Nitric Acid, and if you add too much water, the complexation time with AgNO3 can be ruined by just dumping out the Silver salt of 5-ATz. Too high conc of acid will form the 5-ATz nitrate salt instead which has low solubility as well and hinders complexation as well.

My product crashed out of the sol immediately on addition of AgNO3 to the 5-ATz/HNO3 mix as an off-white precipitate that started to yellow to a pastel yellow on air drying on a filter.

The product is supposed to detonate on flame contact and indirectly at 298C. For me, it does crackle faintly but I can’t seem to get it to dry. I would wager it’s like AgNTz in that it is a pain to detonate when wet but really goes when dry, but I can’t get this complex to dry to see anything amazing.

This salt could be a great alternative to LA, nitrotetrazoles, and such since it’s so seemingly easy to prepare, but I can’t get make it to match klapotke’s results. -My HNO3 and AgNO3 are pure and my 5-ATz is decently pure so idk.

B(a)P - 20-11-2023 at 19:04

Quote: Originally posted by dettoo456  
Anyone had experience with Silver 5-ATz complexes such as [(2Ag)5-ATz] NO3 or ClO4? The perchlorate is mentioned in engager’s tetrazole write up and a patent but there doesn’t seem to be much discussion on it. I tried to make the nitrate the other day according to klapotke’s procedure (https://pubmed.ncbi.nlm.nih.gov/19105192/) but it didn’t seem to yield anything that great. To start, 5-ATZ doesn’t dissolve that great in conc (anything higher than azeo %) Nitric Acid, and if you add too much water, the complexation time with AgNO3 can be ruined by just dumping out the Silver salt of 5-ATz. Too high conc of acid will form the 5-ATz nitrate salt instead which has low solubility as well and hinders complexation as well.

My product crashed out of the sol immediately on addition of AgNO3 to the 5-ATz/HNO3 mix as an off-white precipitate that started to yellow to a pastel yellow on air drying on a filter.

The product is supposed to detonate on flame contact and indirectly at 298C. For me, it does crackle faintly but I can’t seem to get it to dry. I would wager it’s like AgNTz in that it is a pain to detonate when wet but really goes when dry, but I can’t get this complex to dry to see anything amazing.

This salt could be a great alternative to LA, nitrotetrazoles, and such since it’s so seemingly easy to prepare, but I can’t get make it to match klapotke’s results. -My HNO3 and AgNO3 are pure and my 5-ATz is decently pure so idk.


I have previously made a complexes with 5ATZ and nickel perchlorate as well as copper chlorate. The nickel perchlorate complex is not too friction or impact sensitive and detonates from flame in the smallest amount. I have not done any real tests on it though. The copper chlorate complex was somewhat sensitive to impact, but not friction and also detonated from flame in small amounts. The copper chlorate complex decomposed on standing for about a week. I have a bunch of similar complexes that I would also like to test including silver, so interesting to hear your observation.

Microtek - 21-11-2023 at 04:33

I have experimented with the silver 5-ATz perchlorate some years ago. IIRC, it worked fine, and was quite responsive to flame (no issues getting it dry). It did discolour over time, though that may have been due to residual silver nitrate rather than decomposition of the complex itself. I didn't see anything to prefer it over some of the other high performance primaries though.

dettoo456 - 21-11-2023 at 11:37

Thanks for input. I’d agree that it might not be the best compared to even more accessible Ni and Co salts, but I figured it’d be a better alternative to the NTz’s since you wouldn’t need to go through the NaNTz prep. I’ll have to try the Ni salt sometime.

AgNTz has always been consistently good for anything I need out of it.

Microtek - 22-11-2023 at 02:56

I didn't mean to imply that there isn't a use case for silver 5-ATz perchlorate, just that when I experimented with it I also had numerous nitrotetrazoles, NAP and others. So compared to the others, it didn't arouse my interest.

dettoo456 - 27-11-2023 at 09:47

Oh ok, I understand what you mean. I did manage to dry the SAN (I’ll just use that acronym to make it easy) and it does seem to perform the way Klapotke described it to; flame sensitive to complete detonation with a pretty powerful effect. The friction, impact, & shock sensitivity all seem low though - hammer on hardened steel doesn’t do anything and putting a dried chunk between the contacts of a blasting machine (2J @ 225V) doesn’t do anything. Also, its flame sensitivity seems mild compared to AgNTz. I am able to wave a flame in front of it without setting it off but if I hold for about 1/2 second, it’ll detonate.

I am going to try storing it underwater and in dry-contact with HDPE, Al, brass, and Cu to get an idea of storage stability.

[Edited on 27-11-2023 by dettoo456]

[Edited on 27-11-2023 by dettoo456]

MineMan - 28-11-2023 at 23:52

Quote: Originally posted by dettoo456  
Oh ok, I understand what you mean. I did manage to dry the SAN (I’ll just use that acronym to make it easy) and it does seem to perform the way Klapotke described it to; flame sensitive to complete detonation with a pretty powerful effect. The friction, impact, & shock sensitivity all seem low though - hammer on hardened steel doesn’t do anything and putting a dried chunk between the contacts of a blasting machine (2J @ 225V) doesn’t do anything. Also, its flame sensitivity seems mild compared to AgNTz. I am able to wave a flame in front of it without setting it off but if I hold for about 1/2 second, it’ll detonate.

I am going to try storing it underwater and in dry-contact with HDPE, Al, brass, and Cu to get an idea of storage stability.

[Edited on 27-11-2023 by dettoo456]

[Edited on 27-11-2023 by dettoo456]


What compound is this? How does it compare to NAP?

dettoo456 - 29-11-2023 at 13:30

Disilver salt of 5-aminotetrazolium nitrate. Literature stated properties are only related to sensitivity and include: ESD sensitive, impact sens of 15J, friction sens of 18N, Tdecomp @ 298C, and a fast ddt (detonates on flame contact). My own findings generally match those in the literature. The energetic properties most likely match or exceed those of NAP simply due to the coordination of Ag and the BDEs in 5-ATz.

But NAP is cheaper and more easily sourced, plus its amateur reporting is far wider in scope.

Microtek - 30-11-2023 at 00:07

Hmm, I only experimented with the perchlorate variant but those numbers look enticing. Maybe I will give it a shot to see if the product is also sufficiently stable. In indoor testing, the HCl fumes from perchlorate salts have to be taken into account; nitrates do not have this problem. As far as I know, silver also has low toxicity.

B(a)P - 30-11-2023 at 02:40

Quote: Originally posted by dettoo456  
Disilver salt of 5-aminotetrazolium nitrate. Literature stated properties are only related to sensitivity and include: ESD sensitive, impact sens of 15J, friction sens of 18N, Tdecomp @ 298C, and a fast ddt (detonates on flame contact). My own findings generally match those in the literature. The energetic properties most likely match or exceed those of NAP simply due to the coordination of Ag and the BDEs in 5-ATz.

But NAP is cheaper and more easily sourced, plus its amateur reporting is far wider in scope.


Do you mind sharing the full pdf of the paper you referenced or more detail on the procedure that you used? I am curious to give this a go also.

EF2000 - 30-11-2023 at 05:33

Quote: Originally posted by B(a)P  

Do you mind sharing the full pdf of the paper you referenced or more detail on the procedure that you used? I am curious to give this a go also.

Here's the paper

Attachment: konstantin-karaghiosoff-energetic-silver-salts-with-5.pdf (742kB)
This file has been downloaded 216 times

dettoo456 - 30-11-2023 at 08:24

A word of warning though to those trying anything with AgNTz or this silver complex; the AgNTz (and probably the compex) ARE NOT COMPATIBLE with Aluminum metal or materials like Tetrazene & MTX-1. The 5-AgNTz is compatible with cyclic nitramines, copper, and brass.

‘New’ primaries such as NAP and the silver salts described can carry serious dangers if not handled properly. Even milligram amounts can and will mame through microshrapnel if they go off prematurely. Please keep surfaces grounded and wear googles/faceshield.

B(a)P - 30-11-2023 at 12:01

Thanks very much for the paper EF2000. Also thank you dettoo456 for the word of warning regarding various compatibilities. I have done quite a bit of testing for the compatibility of NAP with various metals and am yet to find one that it does not appear to be compatible with. My results are however inconclusive, because some of my NAP decomposed due to what I believe to be improper synthesis (having the final product in water for too long). I will report back when/if I find otherwise.

Quote: Originally posted by dettoo456  
To start, 5-ATZ doesn’t dissolve that great in conc (anything higher than azeo %) Nitric Acid, and if you add too much water, the complexation time with AgNO3 can be ruined by just dumping out the Silver salt of 5-ATz. Too high conc of acid will form the 5-ATz nitrate salt instead which has low solubility as well and hinders complexation as well.

This salt could be a great alternative to LA, nitrotetrazoles, and such since it’s so seemingly easy to prepare, but I can’t get make it to match klapotke’s results. -My HNO3 and AgNO3 are pure and my 5-ATz is decently pure so idk.


They don't report and difficulty in their method in the paper, are these your own personal observations? I will try to make time to perform some similar experiments this weekend and report back on what I find.

dettoo456 - 1-12-2023 at 14:50

Those are the issues I had. I will try to re-synth the complex when I get time as well.

B(a)P - 1-12-2023 at 23:42

Unfortunately my weekend has become filled with domestic tasks, so it will be at least a few days before I try. I will keep your observations in mind and see if I can replicate the issue and find a way around them.

MineMan - 3-12-2023 at 23:27

Quote: Originally posted by EF2000  
Quote: Originally posted by B(a)P  

Do you mind sharing the full pdf of the paper you referenced or more detail on the procedure that you used? I am curious to give this a go also.

Here's the paper



Those sensitivities are impressive. The copper version of NAP is 2J impact but 20N friction if I remember. I regard friction as more important. There are primaries that are immune to friction. This does look like a complex snyth tho. Wish the friction was less sensitive

MineMan - 3-12-2023 at 23:29

Quote: Originally posted by dettoo456  
A word of warning though to those trying anything with AgNTz or this silver complex; the AgNTz (and probably the compex) ARE NOT COMPATIBLE with Aluminum metal or materials like Tetrazene & MTX-1. The 5-AgNTz is compatible with cyclic nitramines, copper, and brass.

‘New’ primaries such as NAP and the silver salts described can carry serious dangers if not handled properly. Even milligram amounts can and will mame through microshrapnel if they go off prematurely. Please keep surfaces grounded and wear googles/faceshield.


Grounding electronic mats? Yes they have thin steel spectra gloves that don’t take any dexterity away.

MineMan - 3-12-2023 at 23:38

Quote: Originally posted by EF2000  
Quote: Originally posted by B(a)P  

Do you mind sharing the full pdf of the paper you referenced or more detail on the procedure that you used? I am curious to give this a go also.

Here's the paper



Those sensitivities are impressive. The copper version of NAP is 2J impact but 20N friction if I remember. I regard friction as more important. There are primaries that are immune to friction. This does look like a complex snyth tho. Wish the friction was less sensitive

Microtek - 4-12-2023 at 04:27

I wouldn't say that the synthesis is particularly complex; you are simply adding silver nitrate soln to a suspension of aminotetrazole in nitric acid. The problem is that the synthesis seems to be quite sensitive to small variations in the experimental parameters.

I tried it the other day, and the product I got was energetic, but not imressively so. On flame contact it puffs off with evolution of distinctly yellowish smoke and when wrapped in Al-foil it explodes with moderate violence. However, 40 mg fuse initiated in a plastic pipe only burns.
It is possible that my nitric isn't quite concentrated enough - it has been a while since last I titrated it.

[Edited on 4-12-2023 by Microtek]

dettoo456 - 4-12-2023 at 10:09

I’ve had the same issues when confining the compex in a brass shell and trying to initiate with bickford fuse; it finds a way to burn/puff out without shattering the metal tube. Also, when dry and in contact with flame to detonate, it does detonate but clearly doesn’t have the same power as other salts. It’s subjective since it isn’t feasible to determine VOD and brisance from just sight and hearing, but NaNTz, for example, is noticeably more violent than the SAN.

I will try to confine the SAN with some nitrocellulose next to the bickford fuse and see if that gets it going. I have a feeling the high tDecomp is causing it to be too insensitive to flame/sparks from something like common cannon fuse.

Also, my SAN has fully discolored at this point (about 2 weeks storage) to a pastel yellow. I don’t think that’d affect performance but who knows. Yellow chemistry has never been detrimental to me, only an aesthetic nuisance.

B(a)P - 5-12-2023 at 20:16

Quote: Originally posted by Microtek  
I wouldn't say that the synthesis is particularly complex; you are simply adding silver nitrate soln to a suspension of aminotetrazole in nitric acid. The problem is that the synthesis seems to be quite sensitive to small variations in the experimental parameters.

I tried it the other day, and the product I got was energetic, but not imressively so. On flame contact it puffs off with evolution of distinctly yellowish smoke and when wrapped in Al-foil it explodes with moderate violence. However, 40 mg fuse initiated in a plastic pipe only burns.
It is possible that my nitric isn't quite concentrated enough - it has been a while since last I titrated it.

[Edited on 4-12-2023 by Microtek]


I tried this earlier in the week and got the same result. I generally followed the procedure in the referenced paper, except that I added a heating step following completion of the addition of silver nitrate. I had no issue with getting the product dry.

DPPE-1 synthesis and some testing

Nemo_Tenetur - 20-12-2023 at 11:28

Inspired by the recent publication in nature communications, I´ve decided to synthesize this brand new primary.

Due to the largely unknown properties is protection equipment a must:

Protection.jpg - 135kB

My lab scale is not precise enough to weigh out milligram quantities. So I used the ten-fold quantity (3,7 gram DABCO-dihydrochloride and 0,55 gram ammonium chloride in 50 ml H20 for solution A and 12,8 gram sodium periodate in 80 ml H2O for solution B:

Solutions.jpg - 125kB

The first attempt was performed with 2,5 ml solution A and 4 ml solution B. The expected yield is about 500 mg. This should be enough for several tests, but not too much to avoid serious damage with remote handling.

To reduce friction and minimize the damage (avoid glass shrapnel) in the case of an unexpected explosion I used hdpe-plastic reaction vessel and hdpe pipette for stirring. Aqueous solutions at room temperature is really a benefit.

Exactly as described, a few seconds after the combination of the solutions a white crystalline precipitate appear at the bottom of the vessel:


Precipitate.jpg - 115kB

The filtration performs well and the filter was washed three times with several ml cold distilled water. Then the filter paper was transferred together with the still wet crystalline product into a flat plastic bowl. The still wet batch was remotely divided in four almost equal-sized parts, to reduce damage in the case of an unexpected explosion.


Filtration.jpg - 106kB

After drying over-night it looks macroscopically like table-salt, it is free-flowing.

Product.jpg - 98kB

A matchhead-quantity was wrapped in a layer of thin aluminum foil. The explosion occured after a second exposure to a blue gas flame of a bunsen burner, the aluminum foil was shattered:

Aluminum foil test.jpg - 124kB


The wet product, however, ist not so sensitive to the flame. Some weak plop-plop, but no real explosion. After a few seconds in the flame, the sound becomes somewhat stronger:

Attachment: DPPE-1 wet.mp4 (771kB)
This file has been downloaded 176 times


The completely dry product detonates immediately without confinement even in matchhead-quantites:


Attachment: DPPE-1 dry.mp4 (166kB)
This file has been downloaded 153 times


A large orange-brown cloud is evolved immediately after detonation, visible in slow-motion:


Attachment: DPPE-1 dry slow-motion.mp4 (254kB)
This file has been downloaded 181 times

The dry product is quite sensitive to friction and impact. A matchhead quantity placed on concrete floor hit with the top of a pliers set it off (no excessive force necessary, just a slap out of my wrist).

dettoo456 - 20-12-2023 at 20:25

Great work, your product looks to be exactly what the literature described. Tuning might be possible through use of cheaper and more accessible ClO4- instead of IO4- (the perchlorate should also be more stable), as well as maybe modifying the diamine by introducing more carbon. Though, I doubt something like hexamine would form a complex in the same way the DABCO and piperazine could.

Nemo_Tenetur - 20-12-2023 at 23:24

Well, perchlorate is much cheaper than periodate. I´ve paid 330 Euro for one kilogram sodium periodate, this is more than enough for the rest of my life. Potassium perchlorate availability for the general public is highly restricted in the European Union (EU-regulation 2019/1148):

https://www.legislation.gov.uk/eur/2019/1148/data.pdf

In Germany, the mere possession of sodium and potassium perchlorate is a crime and can be punished with incarceration up to three years:

https://www.gesetze-im-internet.de/ausgstg/__13.html

The law has some loopholes (i.e. sodium and potassium perchlorate is restricted, but not perchloric acid itself), but I guess this is just a matter of time to get closed.

Microtek - 22-12-2023 at 08:41


Quote:

A matchhead quantity placed on concrete floor hit with the top of a pliers set it off (no excessive force necessary, just a slap out of my wrist).



This sounds as if it is much more sensitive than NAP, NiCP and related compounds. They require hammer blows that are powerful enough to break bones.

Nemo_Tenetur - 22-12-2023 at 10:44

Yes, I think it´s too sensitive for a broad application (apart from the relatively low thermal stability) and I doubt that the reported IS value 3,5 Joule is in accordance with my sample. It is also conceivable that slight changes in the manufacturing process (temperature, concentration, stirring velocity, impurities etc.) are of great influence for the properties of the final product.

Yesterday I´ve tried to set up an improvised "BAM-Fallhammerapparat" to measure the impact sensitivity of my sample, but after several trials I gave it up. This is nothing you can do with "ghetto style" equipment and expect reliable results. An internet search revealed that it is really a challenge to get an exact and reproducible value. Even the BAM federal agency in Germany (with state of the art equipment) emphasize the trouble and problems in this area ("Herausforderung für die Qualitätssicherung"):

https://opus4.kobv.de/opus4-bam/frontdoor/index/index/docId/...

My original intention was to test this primary for squibs. Squibs are hard to get and very expensive here. Unfortunately, even small quantities produce a visible orange-brown cloud.

Maybe this is usable as a kind of "reactive target" for airguns? Like matchtape, with a spot primary below adhesive strips? It should be initiated from a low velocity airgun pellet, if I estimate the impact sensitivity correct.

 Pages:  1  ..  4    6