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Etanol
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Quote: Originally posted by Microtek  | The mother liquor was clear and not black the way it often gets in the patent method for NAP. This black colouring is, AFAIK, characteristic of AQ
decomposition under the influence of air. There are other decomposition modes of course. |
In the case of NAP, the black color is not a sign of the decomposition of aminoguanidine. This is really the color of the saturated solution of the
NAP. It is very dark red, so it looks almost black.
Thank you for trying to soften the atmosphere, but this comparison is inappropriate.
The ions of copper and silver are fundamentally different from nickel by the ability to quickly oxidize hydrazine and hydrazine compounds at room
temperature. This reaction does not require air.
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Microtek
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No, the black color I'm talking about is not the red of the NAP in solution. You can see it more clearly if you add prepared NAP to water. The water
is gradually colored black, and the NAP loses its effectiveness. If you do it with just a little NAP, the black color is quite dilute and you can
easily see through the water, bu it is still unmistakeably black, not red at all.
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ManyInterests
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Ok, so I need to report my latest attempt. It is currently drying, and there was a mishap.
The first thing I did was, in order to get to cool to 0C (or close to thereabouts) I used a saturated saline solution and put it in my freezer. There
was plenty of slush there, but no solid water, so it was good for my purposes. Secondly I did the ultrasonic treatment outdoors where it is close to
0C anyway.
I used 50ml of water in a 250ml beaker with a watchglass atop it to cover most of it, but still allow CO2 and water vapor to escape through the spout,
and I made sure it was boiling before putting in the reagents (1:0.86:0.43g proportions of the aminoguandine bicarbonate, ammonium perchlorate, and
nickel carbonate), and while I said I did want to let it boil for 25 minutes, the diminishing solution volume made me antsy as it was getting close to
35ml or 30ml and I was hearing some mild knocking sound. I wasn't sure what it was, but like I said, I got increasingly nervous, so I took it off the
heat after around 18 minutes of boiling.
There was next to no nickel carbonate left over. So much that I honestly did not think that decanting should not have been done... but I tried to do
it anyway, the stirbar fell out and I had to wipe my floor to make sure I didn't have any residue left. I needed to use a little more water in order
to wash the NAP that did stick to my beaker. I then started ultrasonication in the cold for 13 minutes. The glass I used wasn't heavy enough to sit at
the bottom and to prevent it from floating up and possibly tipping over, I had to hold it down by hand throughout the whole time.
And while adding more of the cold slush, I think I accidently had some fall in the beaker. I am hoping that this does not interfere with the end
product.
I noticed I have a lot more yield than the previous times which I did this, but I won't be calling it a success until I have some holes blown in
aluminum foil!
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pjig
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You could do a wash to remove chloride contaminants from the finished product , then again, some “accidents “ produce unbelievable results , or
changes in industry….
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ManyInterests
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Complete failure... it reacted no differently than the previous times. I am legitimately baffled as to what is going on. The only alternative I can
see is that this method is clearly not working for me, and I don't know why. I didn't even have that many problems with NHN synthesis.
I will not do any more attempts with the these three ingredients in a similar manner. I've had too many failures and nothing even remotely suggesting
that they would work another time. I will need to make in a different way. I will give one more attempt with iNAP (isopropyl alcohol), but I will have
to use my other ammonium perchlorate supply that may not be 100% pure.
I should mention that when I tried it, I put a coffee filter on a regular plastic funnel and I poured it in. Some some was so fine it seeped through,
I poured everything on a paper towel again and let it dry.
I am just not a very happy mad scientist right now.
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ManyInterests
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OK I decided to do the iNAP synthesis. I started with 75ml of 91% IPA and I boiled it, then added everything with strong stirring and kept the boil
for 14 minutes. The amount of solvent I used was starting to run dry, well below 50ml, so after 14 minutes I stopped the heating and immediately
poured out the stuff. I have a much larger 'yield' than last time I did it with iNAP. There was no nickel carbonate left undissolved, so the extended
heating and stirring did its job in that regard, but right now the final answer will be whether or not I will finally have a useable product.
To test, I put some on a thin sheet of aluminum foil and I use a cheap torch lighter beneath it to heat the foil.
Edit: I put a photo of what my stuff looks like.
[Edited on 19-1-2025 by ManyInterests]
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Laboratory of Liptakov
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The path to success is often lined with a trees. Trees of failures. However, in the case of NAP, the trees seems to have no end.
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ManyInterests
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It is possible that my aminoguandine bicarbonate is no good. That is a possibility
With this case, it has a weak fizzle, but no pop. So it is a failure.
Edit: Does Aminoguandine bicarbonate degrade over time? Even if stored properly?
[Edited on 19-1-2025 by ManyInterests]
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Microtek
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My aminoguanidine*HCO3 is about 20 years old and my NAP works every time I make it. I think it's safe to say that it has a very long shelf life.
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Etanol
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This progresses very very slowly, much more than 10 years.
The color of your product indicates that you have received an aminoguanidine complex, but probably with a different anion.
Are you sure your NH4ClO4 is NH4ClO4? How did you prepare it?
Mix 1 gram of sugar powder and 3 grams of your powdered perchlorate. How does this mixture burn?
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pjig
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For the ammonium perchlorate you can tell if you burn it with hexamine or other fuels . It puts off hcl gas (burns nose ) . You can also introduce a
base like sodium hydroxide to release the gas to confirm your ammonium perchlorate. As for the aminoguanadine bicarbonate im sure one of the members
will have a simple spot test you cold perform to confirm your material and its condition.
[Edited on 20-1-2025 by pjig]
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ManyInterests
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Quote: Originally posted by pjig  | For the ammonium perchlorate you can tell if you burn it with hexamine or other fuels . It puts off hcl gas (burns nose ) . You can also introduce a
base like sodium hydroxide to release the gas to confirm your ammonium perchlorate. As for the aminoguanadine bicarbonate im sure one of the members
will have a simple spot test you cold perform to confirm your material and its condition.
[Edited on 20-1-2025 by pjig] |
Thank you for mentioning the hexamine test. Since I have two PbO2 (one bought, one made) anodes, I will be making more sodium perchlorate and from
there maybe perchloric acid.
I was advised against making perchloric acid since it is very dangerous. I want to try, but I will be as cautious as possible and gather as much
information before proceeding. Perchloric acid will allow me to make the purest ammonium perchlorate possible (by neutralizing it with an excess of
ammonium carbonate. Once it is nothing but perchlorate and water and carbonate, it can be boiled down to destroy the excess carbonate and leave
nothing but pure ammonium perchlorate), as well as making aminoguandine perchlorate. Since I put in an order for another 100g of aminoguanadine
bicarbonate, I will have enough to experiment with.
I really want to succeed at this. I want to make a packable, safe to load/lightly press NAP.
Quote: Originally posted by Etanol  |
This progresses very very slowly, much more than 10 years.
The color of your product indicates that you have received an aminoguanidine complex, but probably with a different anion.
Are you sure your NH4ClO4 is NH4ClO4? How did you prepare it?
Mix 1 gram of sugar powder and 3 grams of your powdered perchlorate. How does this mixture burn? |
My 'main' supply was made in 2022 or so when I made some sodium perchlorate (before my Pt anode died in the first attempt...) and I turned what I
could of it into ammonium perchlorate via a double displacement of ammonium chloride and sodium perchlorate.
I also tried to make some with a different method. Since I had some lithium perchlorate that I bought (and thus can safely assume is pure) I took 5
grams of it and mixed it with ammonium carbonate. I filtered out the lithium carbonate (which is mostly insoluble in water, and has reverse
solubility, too!) and slowly evaporated the water off the remainder, leaving me with 2.8 grams of pure ammonium perchlorate. I used an excess of
ammonium carbonate since even gentle heating destroys said carbonate fairly quickly.
This is the perchlorate I used in most of my tests since it is the purest I know I have.
This is why I am baffled as to why it isn't working. Maybe my other supply isn't pure enough, but the one I made from lithium perchlorate has to be
pure.
[Edited on 21-1-2025 by ManyInterests]
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Microtek
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How about your aminoguanidine, is that bought or home made?
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Laboratory of Liptakov
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He has purchased bicarbonate. He writes it on line 4. It seems it. Thus I estimate.
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Axt
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I'm with Etanol on this one, the chloride looks the same as the perchlorate but is of course, inert.
Try making the nitrate it'll also look exactly the same (perchlorate, chloride, nitrate, bromate all look the same) but will deflagrate somewhat like
chlorate/sugar without the white smoke. That way you'll know you are getting the complex, just not the perchlorate.
Here's the writeup for the bromate salt, nitrate is the same just don't add the sodium bromate.
Preparation: Two solutions are made, for the first 1.49g (0.02mol) of nickel oxide is dissolved into 20mL of boiling 68% nitric acid and allowed to
boil dry on a 200 degree hotplate. The remaining nickel nitrate in the form of a yellowish green plate is redissolved into 50mL of water. 6.04g
(0.04mol) of sodium bromate is now added and dissolved.
For the second solution 5.45g (0.04mol) of aminoguanidine bicarbonate in 50mL of water is dissolved by the addition of 3.70g (0.04mol) of 68% nitric
acid with the release of carbon dioxide gas. This solution is then freebased by the addition of 1.60g of sodium hydroxide in 10mL of water, solution
turns from yellow to orange.
The first solution is rapidly stirred as the second solution is slowly poured in, the mixture quickly turns dark bluish purple and within 10 seconds a
brick red precipitate fills the liquid. This was left to stir for 15 min then filtered and dried, yield 7.70g (83% to bromate, 116% to nitrate).
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ManyInterests
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Just to point it out, the nickel carbonate is purchased from a chemical supplier (onyxmet), so I assume it is lab grade and not pottery grade.
Quote: | Here's the writeup for the bromate salt, nitrate is the same just don't add the sodium bromate.
Preparation: Two solutions are made, for the first 1.49g (0.02mol) of nickel oxide is dissolved into 20mL of boiling 68% nitric acid and allowed to
boil dry on a 200 degree hotplate. The remaining nickel nitrate in the form of a yellowish green plate is redissolved into 50mL of water. 6.04g
(0.04mol) of sodium bromate is now added and dissolved.
For the second solution 5.45g (0.04mol) of aminoguanidine bicarbonate in 50mL of water is dissolved by the addition of 3.70g (0.04mol) of 68% nitric
acid with the release of carbon dioxide gas. This solution is then freebased by the addition of 1.60g of sodium hydroxide in 10mL of water, solution
turns from yellow to orange.
The first solution is rapidly stirred as the second solution is slowly poured in, the mixture quickly turns dark bluish purple and within 10 seconds a
brick red precipitate fills the liquid. This was left to stir for 15 min then filtered and dried, yield 7.70g (83% to bromate, 116% to nitrate).
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That sounds like an interesting experiment. But I cannot do the bromate since I have no sodium bromate and it isn't something I thought about making
or getting. Your first step I assume is making nickel nitrate. I already have some available, so I don't need to make any... unless an excess of For
the second step I will have to make some nitric acid since I don't keep that around. But I was planning on making lots of nitric acid anyway, so it
isn't an issue (I aim for WFNA, but that can be diluted with distilled water to 68%).
It'll take a bit for that to happen since I will be a bit busy with other projects. I had made some detonators with NAP in mind, but since this has
been taking so long, I used an ETN:NHN filler. I hope it is enough to set off some of my overpacked RDX caps!
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Nemo_Tenetur
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My experience with NAP
Now I want to share my two cents concerning the different synthetic pathways and results.
The promising power and ease of synthesis draw my attention to this thread for more than one year and I´ve decided to give it a chance.
As I have no problems to get (almost) all precursors from commercial lab suppliers, I´ve bought perchloric acid, aminoguanidine bicarbonate and
nickel acetate. I could also buy directly nickel perchlorate, but the price was a ripoff (several hundred Euro for a half kilogram). In such cases,
I´m a cheapskate and I´ve bought commercially available nickel acetate, added the appropriate amount of 72 percent perchloric acid and evaporated
it in the vacuum to dryness.
The much stronger and less volatile perchloric acid liberate the much weaker and more volatile acetic acid, conversion and yield close to 100% - for a
fraction of the called ripoff-price.
The commercially available nickel carbonate isn´t pure nickel carbonate, it´s always a mixture with nickel hydroxide, in most cases not further
specified. This makes stoichiometric calculations more difficult.
Anyway, I got the cheapskate nickel perchlorate and the aminoguanidine perchlorate in the same way (aminoguanidine bicarbonate and perchloric acid, no
vacuum necessary).
Then I combined the appropriate amounts of concentrated solutions, boiled it for several minutes, cooled it down and the result was NOTHING.
Sad. No reaction, no orange crystals, just a dark green but clear solution.
Where was the mistake? I´ve repeated it twice, with more and less concentrated solutions, more and less heat and stored it even in the fridge for
weeks.
Again, nothing. Sad.
Then I found a comment here from a fellow member that I should add aqueous 25% ammonia.
I decided to give it a last try and BINGO, almost immediately orange crystals appeared and settled down to the bottom of the erlenmeyer flask.
The quantity of ammonia seems not decisive, two drops with a pipette were enough. Therefore I think (just my speculation) that a catalytic amount is
enough.
I´ve repeated the synthesis without boiling, just a warm water bath, and got a copious amount NAP.
No ultrasonication, no boiling necessary.
Then I started sensitivity testing. Some told here that it is less sensitive, but I could initiate it with a hammer hit out of my wrist. Is this less
sensitive? Maybe less sensitive than lead or silver azide, but with a moderate hammer strike it goes off, no excessive force necessary.
The response to a flame seems difficult to predict. From my experience, small quantities (up to a matchhead) deflagrates in most cases. Sometimes it
makes a sharp "whomp", but no bang.
The slightest confinement, however, produce a powerful and sharp bang. See the mpeg "NAP clamp", a quantity less than a matchhead partially covered
between the tip of a clamp gave such a powerful explosion that the gas flame was blown off, whereas a larger quantity at the tip of a knife gave an
intense "whomp!" but no bang - and the gas flame was not blown off.
After the first flame tests of unconfined samples (just deflagration, no detonation observed) I´ve decided to destroy the residual NAP soaked in the
filter paper - the residual quantity was so small that I couldn´t scratch it off with a knife or spatula, thickness much less than a millimeter -
and hold the filter paper in the flame.
To my surprise, I got an ear-ringing detonation! My assumption is that the very weak confinement in the porous filter paper was enough to promote
ddt.
As a side note: the gaseous explosion by-products are very unpleasant and irritating to lungs and/or mucous membranes, even in tiny amounts.
To sum it up: yes, it´s an interesting and very powerful primary, easy to synthesize once you´ve found the way.
But there are some serious drawbacks. Nickel and its salts are always problematic, although maybe less problematic than lead or even mercury. The
strongly irritating fumes after a minuscule explosion are a red flag for me.
Also there are still not fully evalutated stability issues (water sensitivity) and some other data/values are also not investigated (for example,
compatibility with aluminum, copper and plastic, with secondaries, and - very important - it´s sensitivity against electrostatic discharge), unknown
or at least not published.
Feedback and comments to my results are welcome.


Attachment: NAP clamp.mp4 (615kB) This file has been downloaded 58 times
Attachment: NAP hammer.mp4 (1.2MB) This file has been downloaded 47 times
Attachment: NAP knifetip.mp4 (759kB) This file has been downloaded 44 times
Attachment: NAP spatula.mp4 (3.1MB) This file has been downloaded 47 times
[Edited on 23-1-2025 by Nemo_Tenetur]
[Edited on 23-1-2025 by Nemo_Tenetur]
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Microtek
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Yes, the products of the explosion, whether it is nickelcarbonyl or just atomized nickel, and the potential (probable) health effects are the reason
I'm searching for alternatives based on iron, copper or cobalt. If you're interested in that, I'm writing some of my findings in the "complex salts"
thread.
Regarding the sensitivity, it does indeed seem there is some variation. In my own experiments, with quantitative tests, NAP produced by either the
ultrasonication method or the rapid stirring method shows a little less sensitivity towards abrasive impact (rigid hammer pendulum oblique impact onto
180 grit sand paper backed by steel) than PETN. Your pictures seem to indicate that your crystals are quite small, so maybe something other than grain
size is at play.
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Laboratory of Liptakov
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I'm also looking for copper ion alternatives to basically anything that bangs. Similar to Microtec. I observe nickel compounds including NAP thread
through the user interface. For sure.....
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Nemo_Tenetur
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Copper and iron, yes. But cobalt is - as far as I know - as problematic as nickel. Many cobalt salts are classified as SVHC according to EU
legislation. And, from a commercial point of view, it´s more expensive.
The "jack of all trades" primary is still not found.
For small detonators indoor, I prefer silver azide even if it´s expensive. Atomized silver isn´t poisonous in such quantities. The preparation
according to the pacific scientific energetic materials company performs well, an almost granular product and good pourability.
For big detonators outdoor, NHN is still my choice. It´s safe to handle, the synthesis is also safe, easy and high-yielding. I´ve gotten enough
hydrazine hydrate (from industrial water boiler treatment, a really good deal by the way ...) that I don´t need to bother with it´s synthesis.
The drawbacks (confinement and large quantities necessary) are not decisive for me.
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Etanol
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Don't worry. Nickelcarbonyl is not there. High temperature and enough oxygen do not allow this to form.
An irritating smoke consists of NiCl2 and HCl. This is unpleasant, but it is much safer than carcinogenic Co or Pb or Hg or even Zn.
Copper is as toxic as nickel.
Is the oxidation of Fe(II) noticeable the complex to Fe(III) during storage?
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Microtek
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Not so far, but it has only been a few weeks. I'm not convinced that nickelcarbonyl cannot be formed. Varying amounts of CO is produced in most
explosions, and the detonation products cool quickly. You are probably correct that equilibrium concentrations of the compound will be very low, but
transient concentrations may be another matter.
Regarding Co, as far as I was able to find with just a little searching, cobalt is a probable carcinogen when it is bonded to tungsten carbide
(cutting tools such as end mills), but only a possible carcinogen in other contexts.
"Based on chronic toxicity data in animals [Patty 1963], the original IDLH for cobalt metal dust and fume (20 mg Co/m3) is not being revised at this
time. This may be a conservative value due to the lack of relevant acute toxicity data for workers." From https://www.cdc.gov/niosh/idlh/7440484.html
"Overall, these results show that repeated exposure to copper compounds results in an acute cellular response with no associated pathology and which
fully resolved after the cessation of exposure." From https://www.sciencedirect.com/science/article/pii/S0300483X2...
"The revised IDLH for copper fume is 100 mg Cu/m3 based on an analogy to copper dusts and mists which have a revised IDLH of 100 mg Cu/m3. This may be
a conservative value due to the lack of relevant acute toxicity data for workers exposed to concentrations above 100 mg Cu/m3" From https://www.cdc.gov/niosh/idlh/1317380.html
"The revised IDLH for nickel compounds is 10 mg Ni/m3 based on acute inhalation toxicity data in animals [NDRC 1943]. This may be a conservative value
due to the lack of relevant acute inhalation toxicity data for workers. [Note: NIOSH recommends as part of its carcinogen policy that the “most
protective” respirators be worn for nickel compounds at concentrations above 0.015 mg Ni/m3.]"
From https://www.cdc.gov/niosh/idlh/7440020.html
"The available toxicological data contain no evidence that an acute exposure to a high concentration of iron oxide dust and fume would impede escape
or cause any irreversible health effects within 30 minutes. However, the revised IDLH for iron oxide dust and fume is 2,500 mg Fe/m3 based on being
500 times the NIOSH REL of 5 mg Fe/m3 (500 is an assigned protection factor for respirators and was used arbitrarily during the Standards Completion
Program for deciding when the “most protective” respirators should be used for particulates)."
Thus it seems that nickel is ten times as toxic as copper but only two times as bad as cobalt. Iron is expectedly non-toxic (but ideally nothing other
than air should be inhaled).
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Laboratory of Liptakov
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The whole breathing is based on the oxidation of iron. So a little extra dust won't hurt anyone. If we could create a primary substance with iron
ions, it would be revolutionary. After all, Fe2O3 is a reliable fire accelerator.....
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pdb
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Be my guest !
In 2007, I planned to try Na[Fe(NT)₃(H₂O)₃] from NT and FeCl₂·4H₂O (example 2 of the patent), but I didn’t for some forgotten reason.
That same year, Engager conducted an extensive investigation into NT synthesis and M-NT compounds, with no clear conclusion IIRC (see https://www.sciencemadness.org/whisper/viewthread.php?tid=81... and the following pages).
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Etanol
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Quote: Originally posted by Microtek  |
Thus it seems that nickel is ten times as toxic as copper but only two times as bad as cobalt. Iron is expectedly non-toxic (but ideally nothing other
than air should be inhaled). |
Hm. You are right. It seems inhalation toxicity is different from the oral. I focused on the values for salts:
FeCl2 LD50=450mg/kg (oral,rat)
CuCl2 LD50=140mg/kg (oral,rat)
NiCl2 LD50=105mg/kg (oral,rat)
CoCl2 (hexahydrate?) LD50=80mg/kg (oral,rat)
It would be ideal to create a non-gigroscopic, poorly soluble, waterfree Fe(III) complex with fast DDT.
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