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Rosco Bodine
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The thought I was describing above about a possible alternative synthesis approach could result in a coprecipitation or possible double salt of nickel
hydrazine nitrate and nickel hydrazine azide described on the preceding page by Mr.Greenix
http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...
I don't know if this has ever been tried before or proposed as an experiment
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PHILOU Zrealone
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@Rosco and LL,
If I remember correctly (IIRC) LL has made a comparative study of various copper detonators diameters with NiHN against witness plate... 4, 6, 8 mm
that indeed showed that too low a diameter resulted in unefficient detonation...
Correct?
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Rosco Bodine
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There was a patent GB821586 I posted early in the thread that claimed IIRC the diameter had to be above a certain range for the DDT of the NiHN to be
assured.
http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...
Adding some silver nitrate and sodium nitrite with the nickel nitrate being added to the hydrazine nitrate could result in silver azide being produced
concurrently and copreciptated in the NiHN .....and that could be interesting too if it works
[Edited on 6/22/2016 by Rosco Bodine]
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MineMan
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LL and Rosco,
ETN has proved to be very impact sensitive from my experiments... just a light hammer tap (8oz hammer) while NiHN is 80cm drop with a 2kg weight.
Both of you already know this, but my point is aren't we going backwards if we use ETN as a base, or a mix? Certainly it is better than HMTD and
AP... but that is not saying much.
LL I don't have any NIHN so could you try a experiment for me for a NEPD?
Mix 1 gram of:
.8-NiHN
.15-Potassium Perchlorate
.05-Mg Power (preferably 1000mesh or below)
Then take .2grams of this mixture and place it in the center of a 4cm x 4cm piece of aluminum foil and insert a fuse in the center of the mixture and
fold the corners of the foil square around the fuse and twist around the fuse and compress with the fingers.
After this, take 6cm x 6cm piece of Al foil and place .5 to .8grams of the above mixture in the center, then place the above made initiator inside of
this and fold the corners around the fuse and twist (like above) and compact with the fingers. The resultant should be the shape of an over sized
raindrop/teardrop, with the tail being the fuse. Then wrap 1 or 2 more pieces of Al foil around this and compact with the fingers, then wrap some
electrical tape around it for further confinement.
I am hoping this will produce a completely safe NEPD which forces the mixture (in the outer layer) to go from DDT because of the resulting pressure
from the inner mixture
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MineMan
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Right after I typed the above I decided to go into the garage and perform some more sensitivity test with ETN to "prove" my conviction that ETN should
still be avoided.
Oftentimes a flick of the wrist with a hammer (8oz) will set a few milligrams off when folded in Al foil and set on another hammer, sometimes fully,
sometimes partially. And sometimes it will not set it off...but that still bothers me... maybe it is an OCD thing but I would like to avoid ETN
altogether.
LL I hope you are willing to perform the above experiment for me, and even more so, I hope it works...!
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PHILOU Zrealone
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Quote: Originally posted by MineMan  | Right after I typed the above I decided to go into the garage and perform some more sensitivity test with ETN to "prove" my conviction that ETN should
still be avoided.
Oftentimes a flick of the wrist with a hammer (8oz) will set a few milligrams off when folded in Al foil and set on another hammer, sometimes fully,
sometimes partially. And sometimes it will not set it off...but that still bothers me... maybe it is an OCD thing but I would like to avoid ETN
altogether.
LL I hope you are willing to perform the above experiment for me, and even more so, I hope it works...! |
Hand hammer testing is not reliable since:
-you get a mix of shock and friction (slight twisting from the wrist)
-the speed of the hammer and the strenght you apply on it is hard to evaluate
-multiple hits heats the substrate that becomes more sensitive (usually when the first strike doesn't work, people hit several times)
-the effective surface contact of the hammer and angle of percussion is hard to evaluate and to repeat precisely...often hammer surface is curved by
use so if the sample is perfectly centered it will get more energy (pressure per surface) than a little asside
For all those reasons it is better to use a machine for the testing following the recommandations of international testing normalisation.
Also impact sensitivity testing is a mather of statistics...usually defined as the 50% out of 10 trials that crackled, took fire, deflagrated or
detonated after impact...
So for example if IS is 20cm for 2kg weight (roughly 20 N for 0.2m or 4 Nm); this means that:
-5 trials out of 10 where positive by using 2kg weight falling from 20 cm
-increasing the weight or the height will increase the chances of positive result ...
For example
at 21 cm 6+/10 trials,
at 22 cm 8+/10 trials
and at 23 cm 99+/100 trials
-decreasing the weight or the height will reduce the chances of firing...
For example
at 19 cm 3/10,
at 18 cm 1/10,
at 17 cm 1/100,
and at 16 cm 1/1000.
[Edited on 29-6-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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MineMan
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PH Z,
you make some great points and I agree with them all. But I don't have an apparatus to test as such, and I think the hammer test still gives a good
indication of whether a EM is:
-Will never go off through impact (ANFO)
- Extraordinarily stable (TNT, ANAl)
-Stable (RDX)
-Sensitive (PETN)
-More sensitive (ETN,SADS)
-Very Sensative (Lead Azide)
-Then substances such as HMTD and AP
I would love to see some official numbers for ETN and SADS though...
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PHILOU Zrealone
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| Quote: Originally posted by MineMan | PH Z,
you make some great points and I agree with them all. But I don't have an apparatus to test as such, and I think the hammer test still gives a good
indication of whether a EM is:
-Will never go off through impact (ANFO)
- Extraordinarily stable (TNT, ANAl)
-Stable (RDX)
-Sensitive (PETN)
-More sensitive (ETN,SADS)
-Very Sensative (Lead Azide)
-Then substances such as HMTD and AP
I would love to see some official numbers for ETN and SADS though... |
Some forum members have made nice devices...search for the tread.
When I will have time (after my ex-girlfriend has left home) I will for sure build one such device...imperative if you want to test energetic
materials qualitatively.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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MineMan
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PH Z,
I look forward to seeing the results, please share with us all!
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Σldritch
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Iron (III) Acetate Oxide Persulfate Trihydrate (?)
I tried to prepare the compound in the title and i think i have suceeded.
The name is kind of crazy so i will just say it is the persulfate salt of basic iron (III) acetate, also im not even sure about the name of the title
but thats my best guess.
Anyway it was prepared from basic iron (III) acetate dissolved in water wich was mixed with sodium persulfate solution and then diluted with denatured
alcohol. The resulting precipitate was filtered off and dried.
It is obviously not very energetic considering the poor oxygen balance, the water, carboxyl groups and iron but it fizzles when a burning match is
held above it. It also gives an ocasional pop but it just melts itself too a yellow-ish goop.
Anyway ill try making the nitrate but i think i read somewhere it is very unstable but i can not find the document.
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PHILOU Zrealone
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| Quote: Originally posted by Σldritch | I tried to prepare the compound in the title and i think i have suceeded.
The name is kind of crazy so i will just say it is the persulfate salt of basic iron (III) acetate, also im not even sure about the name of the title
but thats my best guess.
Anyway it was prepared from basic iron (III) acetate dissolved in water wich was mixed with sodium persulfate solution and then diluted with denatured
alcohol. The resulting precipitate was filtered off and dried.
It is obviously not very energetic considering the poor oxygen balance, the water, carboxyl groups and iron but it fizzles when a burning match is
held above it. It also gives an ocasional pop but it just melts itself too a yellow-ish goop.
Anyway ill try making the nitrate but i think i read somewhere it is very unstable but i can not find the document. |
The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...
Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.
[Edited on 30-7-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Σldritch
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| Quote: Originally posted by PHILOU Zrealone |
The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...
Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.
|
I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex
exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.
Replacing the water with ammonia might be doable but i dont think it would make much of a diffrence when the oxygen balance is so bad anyway.
I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with
perchlorate
would probely improve it the most IMO
EDIT: Think i found the document http://scholarsmine.mst.edu/cgi/viewcontent.cgi?article=8134&context=masters_theses.
EDIT 2: Forgot to mention that nitrosyl metal complexes might make good explosives or add extra oxidizer too compounds with bad balance. Maybe
something like Copper (II) Butyndiolate Nitrosyl?
[Edited on 30-7-2016 by Σldritch]
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PHILOU Zrealone
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| Quote: Originally posted by Σldritch | | Quote: Originally posted by PHILOU Zrealone |
The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...
Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.
|
I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex
exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.
I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with
perchlorate
would probely improve it the most IMO
|
Fe(III) and formate anion are stable together except under heating...
Formic acid is relatively stable with H2O2 as long as you don't heat it.
The oxygen balance will be better for most of the proposed compounds vs acetic acid...don't forget that most are diacids not monoacids like acetic:
Monoacids: (multiplied by 2 to get valid comparison with diacids)
2 HO2C-CH3 = C4H8O4 needs 8 O to completely burn
2 HO2C-C#C-H = C6H4O4 needs 10 O to completely burn
2 HCO2H = C2H4O4 needs 2 O to completely burn
Diacids:
HO2C-CH=CH-CO2H = C4H4O4 needs 6 O to completely burn
HO2C-CHOH-CHOH-CO2H = C4H6O6 needs 5 O to completely burn
HO2C-C#C-CO2H = C4H2O4 needs 5 O to completely burn
One may even consider oxalic acid...
HO2C-CO2H = C2H2O4 needs 1 O to completely burn
****************
Adding Nitrosyl ligand might indeed be interesting for OB.
The use of perchlorate anion would of course make a big difference even if the mix doesn't form a complex ... the binary stoechiometrically balanced
mix of iron III perchlorate and any iron III organic acid fuel salt would be energetic and cocrystalization will make a molecular level intimate mix
prone to D2D from heating or shock.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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kratomiter
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| Quote: Originally posted by Σldritch | | Quote: Originally posted by PHILOU Zrealone |
The water content is also to blame...it will temper seriously any exothermic oxydoredox reaction.
Maybe change the acetate for the formate or the tartrate to improve OB...
Probably even better for OB:
-fumaric acid/maleic acid
-butyndioic acid
-propynoic acid
The last two would be much better since the alcynic triple link is explosophoric.
|
I think formate would be oxidized by the persulfate or maybe even the iron (III) and i dont know how you would prepare the tartarate if the complex
exist because it is likely insoluble. The other carboxylic acids might be intresting but sadly they would make the oxygen balance even worse.
Replacing the water with ammonia might be doable but i dont think it would make much of a diffrence when the oxygen balance is so bad anyway.
I think it still a pretty intresting compound considering iron oxides ability too catalyse burning (Like in R-candy). Replacing the persulfate with
perchlorate
would probely improve it the most IMO
EDIT: Think i found the document http://scholarsmine.mst.edu/cgi/viewcontent.cgi?article=8134&context=masters_theses.
EDIT 2: Forgot to mention that nitrosyl metal complexes might make good explosives or add extra oxidizer too compounds with bad balance. Maybe
something like Copper (II) Butyndiolate Nitrosyl?
[Edited on 30-7-2016 by Σldritch] |
You can replace water with DMSO. Lots of metal perchlorates and nitrates form high explosives that way (patent). Mixing it with AN or AP improve the OB.
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symboom
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Amine complex with cobalt and nickel
Trying to synthesize tetramine cobalt nitrate
Materials
Cobalt nitrate
Ammonium nitrate
Ammonium hydroxide
Ethanol
Tetramine cobalt nitrate
Is what color im getting a brown powder
I can't tell if I keep getting the hydroxide
No crystals??
Attempting amine nickel complex
Maybe better results
Also nitro complexes should be interesting
Like ammonium hexnitrocobaltate
And ammonium hexnitronickelate
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symboom
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Attempted ammonium based complex salts
Tetramine nickel perchlorate is very easy to synthesize
No ethanol to help it percipitate
Hexamine nickel sulfate is added to ammonium perchlorate
A purple percipitate forms after the addition of ammonium perchlorate
Tetramine copper perchlorate
Ethanol is needed for the percipitation
Copper sulfate is not used due to that also being insoluble in ethanol also the tetramine copper sulfate is also insoluble
So copper oxide is added to ammonium hydroxide
With ammonium perchlorate after a day the solution goes from black fine percipitate to tge tetramine complex blue color
Solution is deep blue once it is added to ethanol purple precipitate forms
Next step to add hexamine to tetramine copper perchlorate
In ammonia solution
To hopefully form copper hexamine perchlorate
[Edited on 11-3-2017 by symboom]
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DraconicAcid
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Tetramine nickel? Surely it's the hexamine- nickel is usually octahedral, unless you've got bulky ligands (to make it tetrahedral) or strongly
splitting ligands like cyanide (to make it square planar). And the perchlorates are crappy ligands, unlikely to displace ammonia.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Laboratory of Liptakov
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CHP
Copper hexamine perchlorate is good material. His VoD is 7590 m/s ( at 1,91g/cc) and pressure 260 000 Bar. Therefore his preparation was reported and
delete admin from my youtube channel.......... .....Dr.
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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symboom
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| Quote: Originally posted by Laboratory of Liptakov | | Copper hexamine perchlorate is good material. His VoD is 7590 m/s ( at 1,91g/cc) and pressure 260 000 Bar. Therefore his preparation was reported and
delete admin from my youtube channel...............Dr.
|
That is the procedure im following is Laboratory of Liptakov
Great work also is your vaccum funnel homemade? I hope it isnt deleted :-(
And for cerealkiffer
For the synthesis of hexamine nickel perchlorate
Complex salts are very interesting
Such as
Chromium
Cobalt
Nickel
Copper
Zinc
Videodemolitions also is another interesting youtube channel
Diamine zinc perchlorate?
[Edited on 12-3-2017 by symboom]
[Edited on 12-3-2017 by symboom]
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Laboratory of Liptakov
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TACP NH4ClO4
Next interest is it, that in Liptakov converter for preparation double salt (especially TACP) is possible preparation TACP directly from NaClO4 +
NH4Cl + Cu wire + NH3 water. Yield is basically quantitative on NaClO4 (strategic salt). Basic charge for attempt are :
NaClO4 monohydrate 22g + NH4Cl (dry) 20g + Cu wire 8g + NH3 100g water 24%. Dissolving salts by 30C, insert to Liptakov converter. After 150 minute
at 20 - 25 C running temperature we have in glass (after drying) 18,5g dry TACP (non hydrate) Crystals from this reaction is pretty big, about cca 1
mm. All others is dissolved in solution: NaCl, residuum NH4Cl and NaClO4 + Cu wire 1g. Reaction requires better counting ratios between NaClO4 xH2O +
NH4Cl for better yields. However I recommend use small overlap NH4Cl, because is cheap and free available. 100g ammonia water is minimum, on edge for
dissolving.
Next:
This method is possible use for preparation NH4CLO4 and not for TACP. Copper respectively his ligand bonding on NH4. Arises crystals, in relatively
high purity. When you need NH4ClO4, simply dissolved TACP in distill water and separe fine CuO powder. After boiling and evaporate all water we have
NH4ClO4. Advantage this method is it, that we not need use crystallization process between different solubility salts NaClO4 (as residuum) + NH4Cl (as
residuum) + NaCl (production from reaction) + NH4ClO4 (product) which are all in one solution. Copper coordinate ligand helping get out NH4ClO4 in
pure form, without multiple recrystallization. All is try again and again, confirmed.
Dr.........:-)
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NeonPulse
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I could find only a little information on cesium picrate and was not even sure it could be made.
so i decided to find out for myself. i simply took a boiling hot solution of picric acid maybe a gram and neutralized it with Aq CsOH added dropwise.
it got to the point of being neutralized and i accidentally added an extra drop so the solution was slightly basic PH 7.5 -8 oops. it did not seem to
affect the product though and it crystallized gradually in tiny orange needle shaped crystals. these were separated via gravity filtration and rinsed
with ice water and set out to dry.
Here is my experiment in forming this picrate: https://www.youtube.com/watch?v=MtUXoU_sjVg
Formed in much the same way as one would prepare potassium picrate, with the resulting product looking much the same, perhaps a little more orange.
upon heating the salt on foil over an alcohol burner it first melted then deflagrated in a nice puff of bright blueish violet light and black smoke.
i did attempt to set it off via friction and impact but these failed.
it did detonate with an oK report at first so i used several more layers of foil and gently pressed the foil hard which in turn increased the density
of the picrate.
the reports from these little amounts -50-100mg in the pressed foil was much more satisfying and actually quite loud and spread glittery foil
particles all over the place.
Once i can get to retrieving my stash of styphnic acid i really would like to see if i can form cesium styphnate to see how this performs
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PHILOU Zrealone
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| Quote: Originally posted by NeonPulse | I could find only a little information on cesium picrate and was not even sure it could be made.
so i decided to find out for myself. i simply took a boiling hot solution of picric acid maybe a gram and neutralized it with Aq CsOH added dropwise.
it got to the point of being neutralized and i accidentally added an extra drop so the solution was slightly basic PH 7.5 -8 oops. it did not seem to
affect the product though and it crystallized gradually in tiny orange needle shaped crystals. these were separated via gravity filtration and rinsed
with ice water and set out to dry.
Here is my experiment in forming this picrate: https://www.youtube.com/watch?v=MtUXoU_sjVg
Formed in much the same way as one would prepare potassium picrate, with the resulting product looking much the same, perhaps a little more orange.
upon heating the salt on foil over an alcohol burner it first melted then deflagrated in a nice puff of bright blueish violet light and black smoke.
i did attempt to set it off via friction and impact but these failed.
it did detonate with an oK report at first so i used several more layers of foil and gently pressed the foil hard which in turn increased the density
of the picrate.
the reports from these little amounts -50-100mg in the pressed foil was much more satisfying and actually quite loud and spread glittery foil
particles all over the place.
Once i can get to retrieving my stash of styphnic acid i really would like to see if i can form cesium styphnate to see how this performs
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Very nice work NeonPulse...
Now I imagine Lithium picrate (more soluble) --> red flash
What would be the deflagrating colour and properties of Rubidium picrate?
For your health safety don't play with Francium picrate would stil be theorically
interesting because probably more unsoluble and more sensitive.
Now you can also play with Calcium, Strontium and Baryum picrate to get colorized flame from deflagro-detonating stuffs.
Ca --> pink orange
Sr --> deep red
Ba --> green
Remain the copper --> blue/green?
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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greenlight
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Excellent work Neonpulse, I can't find any information on Cesium picrate at all except for what you have provided.
I have made potassium picrate from picric acid and potassium carbonate before so surely carbonates of Strontium, Barium and copper could be used.
Very interesting.
Be good, otherwise be good at it 
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James Ikanov
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I was under the impression metal picrates were "too dangerous" (I recall stories of people booby trapping old munitions in a low tech way by smearing
picric acid on exposed metal threads of UXO and just waiting for metallic salts to form after it was threaded back in) but it seems there's some
consensus that that danger was overstated?
“To do good work one must eat well, be well housed, have one's fling from time to time, smoke one's pipe, and drink one's coffee in peace” -
Vincent Van Gogh
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PHILOU Zrealone
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| Quote: Originally posted by James Ikanov | | I was under the impression metal picrates were "too dangerous" (I recall stories of people booby trapping old munitions in a low tech way by smearing
picric acid on exposed metal threads of UXO and just waiting for metallic salts to form after it was threaded back in) but it seems there's some
consensus that that danger was overstated? |
Depends strongly of the "metallic" cation involved...
Some are less sensitive others are more sensitive...copper and calcium may be amongst the worst IIRC.
Also there is a difference between heat sensitivity, shock sensitivity and friction sensitivity...for picrate the 3 are not always wel correlated...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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18
19
20
..
27 |
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