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markx
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Excellent visual contrast between the different pH levels! Did you conduct the synthesis at room temperature? Judging from coloration of the product
(if the picture was taken shortly after drying was complete) it probably was done at room temperature or close to that.
Exact science is a figment of imagination.......
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PHILOU Zrealone
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My neutral one looks more like your acidic one, so I guess you did one or more mistakes during your synthesis:
-in too strong light (artificial or sun)
-you didn't exhaust the AgNO3 well with acetylen (the unreacted AgNO3 will darken your complex and make it more friction sensitive), this will also
lower the yield.
-you didn't wash your filter paper with demi water first (chlorides from bleaching are detrimental due to AgCl formation and reaction with light)
-you didn't wash the precipitate several times with demineralized water to take away all the uncomplexated AgNO3, this allows one to rerun acetylen
through the solution until completely exhausted --> increasing yield.
-you had some Ca(OH)2 from your acetylen generator that was taken by the acetylen into your AgNO3 solution....dark AgOH forms immediately and turns
into black Ag2O...this also sensitizes the salt.
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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Spirit of Niter
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Quote: Originally posted by markx  | | Excellent visual contrast between the different pH levels! Did you conduct the synthesis at room temperature? Judging from coloration of the product
(if the picture was taken shortly after drying was complete) it probably was done at room temperature or close to that. |
The syntheses was conducted outdoors under a carport in the shade. It was fairly warm out when I conducted the neutral synthesis and as for the other
two the synthesis were done at night. My final products were temporarily stored under a cardboard box in the shade until I did a few tests.
| Quote: Originally posted by PHILOU Zrealone |
My neutral one looks more like your acidic one, so I guess you did one or more mistakes during your synthesis:
-in too strong light (artificial or sun)
-you didn't exhaust the AgNO3 well with acetylen (the unreacted AgNO3 will darken your complex and make it more friction sensitive), this will also
lower the yield.
-you didn't wash your filter paper with demi water first (chlorides from bleaching are detrimental due to AgCl formation and reaction with light)
-you didn't wash the precipitate several times with demineralized water to take away all the uncomplexated AgNO3, this allows one to rerun acetylen
through the solution until completely exhausted --> increasing yield.
-you had some Ca(OH)2 from your acetylen generator that was taken by the acetylen into your AgNO3 solution....dark AgOH forms immediately and turns
into black Ag2O...this also sensitizes the salt. |
-My neutral synthesis was done in a shaded area during the day and the other two at night.
-I wondered if I was passing enough C2H2 through the solutions because I believe my yields could be a little higher.
- I was sure to rinse off the “bleached” filter paper with deionized water. I used deionized water in all three syntheses whenever called for,
i.e. the acetylene generator.
-As for your fourth point pleases elaborate a little bit more. Are you saying that I would have to wash the precipitate while still in the initial
solution? Followed by passing more acetylene through the solution to achieve a high yield? For the acid synthesis I filtered the precipitate and
washed three times; first with 150ml of NaHCO3N (0.15g)/ deionized H2O solution, next with 150ml of deionized H2O, and finally with 100ml of denatured
alcohol.
-I don’t doubt that my solutions received contaminants from the acetylene generator. I didn’t bother washing the gas. This was my first time
synthesizing Ag2C2 and its double salt. I was merely keeping the experiment simple. At least for now…
"If we knew what it was we were doing, it would not be called research, would it?" -Albert Einstein
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PHILOU Zrealone
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| Quote: Originally posted by Spirit of Niter |
| Quote: Originally posted by PHILOU Zrealone |
My neutral one looks more like your acidic one, so I guess you did one or more mistakes during your synthesis:
-in too strong light (artificial or sun)
-you didn't exhaust the AgNO3 well with acetylen (the unreacted AgNO3 will darken your complex and make it more friction sensitive), this will also
lower the yield.
-you didn't wash your filter paper with demi water first (chlorides from bleaching are detrimental due to AgCl formation and reaction with light)
-you didn't wash the precipitate several times with demineralized water to take away all the uncomplexated AgNO3, this allows one to rerun acetylen
through the solution until completely exhausted --> increasing yield.
-you had some Ca(OH)2 from your acetylen generator that was taken by the acetylen into your AgNO3 solution....dark AgOH forms immediately and turns
into black Ag2O...this also sensitizes the salt. |
-My neutral synthesis was done in a shaded area during the day and the other two at night.
-I wondered if I was passing enough C2H2 through the solutions because I believe my yields could be a little higher.
- I was sure to rinse off the “bleached” filter paper with deionized water. I used deionized water in all three syntheses whenever called for,
i.e. the acetylene generator.
-As for your fourth point pleases elaborate a little bit more. Are you saying that I would have to wash the precipitate while still in the initial
solution? Followed by passing more acetylene through the solution to achieve a high yield? For the acid synthesis I filtered the precipitate and
washed three times; first with 150ml of NaHCO3N (0.15g)/ deionized H2O solution, next with 150ml of deionized H2O, and finally with 100ml of denatured
alcohol.
-I don’t doubt that my solutions received contaminants from the acetylene generator. I didn’t bother washing the gas. This was my first time
synthesizing Ag2C2 and its double salt. I was merely keeping the experiment simple. At least for now…
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So you did almost everything wel  .
To me your yield could be improved by passing several times acetylen into the solution with the permeate of the filter. Filtration each time between
acetylen session over the same already filtrated precipitate onto the filter.
The fourth point is that you have to wash the filter with the precipitate in it with demi water (a few 5ml) turn a little with a rod in the filter to
resuspend the precipitate...this will increase a bit the volume of solution for bubbling acetylen but this recycle all unused/unbound AgNO3 to the
complex.
The design is best with a vertical long tube and the bubble at the bottom...this allows a longer contact time (residence time) between acetylen and
AgNO3 solution..this also helps flocculation of the precipitate for easier recollection by filtration.
For your acid precipitate only the demi water wash is sufficient.
The basic wash with NaHCO3 will make Ag2CO3 if AgNO3 is still present in your precipitate and will eventually ruin the benefit of the complexated
HNO3, it will be neutralised as NaNO3 and leave the complex with your other washes.
The final denaturated ethanol wash is also useless because it introduces unknown denaturant into the equation...simply press between paper towels and
leave precipitate to dry in a mild warm and shadow area.
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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Spirit of Niter
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I appreciate the helpful tips. I’ll be sure to take note of them for next time. I think later sometime as I get more in depth with experimenting
with silver acetylide, I’ll synthesize it’s none explosives complex Ag2C2.6AgNO3.
"If we knew what it was we were doing, it would not be called research, would it?" -Albert Einstein
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MineMan
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More Infromation
Hello All,
I wanted to share some pages that I extracted from the book "Primary Explosives" about SADS. From what I gather the least sensitive product is made
from a hot acidic solution (30% nitric acid, or lots of silver nitrate compared to distilled water). I tried this and the product does indeed seem
less sensitive!
Attachment: Primary Explosives.oxps (5.4MB)
This file has been downloaded 1158 times
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markx
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| Quote: Originally posted by MineMan | Hello All,
I wanted to share some pages that I extracted from the book "Primary Explosives" about SADS. From what I gather the least sensitive product is made
from a hot acidic solution (30% nitric acid, or lots of silver nitrate compared to distilled water). I tried this and the product does indeed seem
less sensitive!
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Yes, hot acidic synthesis is the way to go. Product formed in these conditions was so numb towards mechanical stimuli that it did not go off in my
drop tester under a 2kg weight dropped from 60cm. Where as room temperature "neutral" synthesis product (discolored) could be set off with a light tap
of a hammer. Electrostatic sensitivity still remains, so care should be taken to handle the double salt at all times!
Exact science is a figment of imagination.......
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MineMan
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Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a
couple of decent hits!
I put some of my SADS in the way of a bbq pezio spark and it did not ignite... but I believe you.
It could be the "perfect" primary if we can reduce the static sensitivity... I only have a few ideas though...
-Adding 10-20% potassium perchlorate helps the oxygen deficiency and lessens the sensitivity without adversely affecting the power.
-Just use a humidifier while loading this into caps or devices, and then the caps should provide a faraday cage and there is nothing to worry
about... although an electric engineer told me once that static just needs a crack the size of a micron to enter.
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markx
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| Quote: Originally posted by MineMan | Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a
couple of decent hits!
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I've verified it on 5 batches of product (2-4g) synthesised according to the procedure that I described on this thread earlier. The sweet spot for
solution temperature during acetylene administration seems to be around 65C. I have started from metallic silver all the times and used metal from
only one batch of silver that I aquired for the purpose. It is not highly pure ( scraped leftover residues from the chamber of vaccum vapor deposition
process). It has a definitive copper impurity in it as can be seen from the characteristic blue hint of solution after nitric acid has dissolved the
metal. There may be other contaminants that are not visually detectable. So they may or may not have an effect on the final result, but so far it has
turned out very satisfactory. But these are just my observations and results that apply for the batches that I have syntesized so far. So please do
take them as exactly that and nothing else! I have no intention to suggest that you or anyone else using different materials is guaranteed to have the
same outcome. There may be numerous factors that influence the process, so always assume proper safety precautions. This is a very sensitive energetic
material and just because certain conditions allow it to be less responsive towards impact initiation does not take away the other hazards of heat,
flame and static discharge.
Exact science is a figment of imagination.......
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MineMan
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I am aware of this, thank you for your verification. My product was made at 70-75C and it cannot be set off by metal on metal friction even when the
sharp edge of one bar is used against a steel plate (1cm thick) and 30-40 pounds of pressure is administered. Just wish we could find a way to
reduce the static sensitivity... what about plasticizing this primary?
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PHILOU Zrealone
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| Quote: Originally posted by markx | | Quote: Originally posted by MineMan | Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a
couple of decent hits!
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I've verified it on 5 batches of product (2-4g) synthesised according to the procedure that I described on this thread earlier. The sweet spot for
solution temperature during acetylene administration seems to be around 65C. I have started from metallic silver all the times and used metal from
only one batch of silver that I aquired for the purpose. It is not highly pure ( scraped leftover residues from the chamber of vaccum vapor deposition
process). It has a definitive copper impurity in it as can be seen from the characteristic blue hint of solution after nitric acid has dissolved the
metal. There may be other contaminants that are not visually detectable. So they may or may not have an effect on the final result, but so far it has
turned out very satisfactory. But these are just my observations and results that apply for the batches that I have syntesized so far. So please do
take them as exactly that and nothing else! I have no intention to suggest that you or anyone else using different materials is guaranteed to have the
same outcome. There may be numerous factors that influence the process, so always assume proper safety precautions. This is a very sensitive energetic
material and just because certain conditions allow it to be less responsive towards impact initiation does not take away the other hazards of heat,
flame and static discharge. |
Copper into the mix may be a problem or not...depends on its interaction...
I suppose unsoluble CuC2 do form (copper II acetylide) what is not sensitive nor explosive to my experience (by opposition with Cu2C2 (copper I
acetylide) wich is sensitive and explosive).
You could have separated the Cu out of the Ag/Cu mix by cementing the nitric acid Ag/Cu mix with a piece of Cu pipe...all the Ag (and nobler metals)
would have precipited as a fine dust leaving a blue solution of Cu(NO3)2 and most of the Cu pipe.
Ag + Cu + HNO3 --> AgNO3 + Cu(NO3)2 + NxOy + H2O
2 Ag(+) + Cu(s) --> Ag(s) + Cu(2+) (as Cu(NO3)2)
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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PHILOU Zrealone
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| Quote: Originally posted by MineMan | | I am aware of this, thank you for your verification. My product was made at 70-75C and it cannot be set off by metal on metal friction even when the
sharp edge of one bar is used against a steel plate (1cm thick) and 30-40 pounds of pressure is administered. Just wish we could find a way to
reduce the static sensitivity... what about plasticizing this primary? |
BTW Thank you for the extraction work out of the book.
I wish I could read the rest of the book  .
I also dream of plasticizing SADS...but the plasticizer needs to be active (explosive) and stable towards SADS.
I hope being able to test some tested possibilities in a near future (by the end of the year)
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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markx
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| Quote: Originally posted by PHILOU Zrealone |
Copper into the mix may be a problem or not...depends on its interaction...
I suppose unsoluble CuC2 do form (copper II acetylide) what is not sensitive nor explosive to my experience (by opposition with Cu2C2 (copper I
acetylide) wich is sensitive and explosive).
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In fact it seems that most of the copper, if not all, remains in solution after the acetylene administration is complete...visually the solution's
blue hint is unaltered by the process. So I've not bothered with the purification techniques so far.
I've played around with some energetic mixes to "phlegmatize" SADS, but it seems that diluting this primary will quite sharply render it unresponsive
towards flame initiation. Then again out of fear of accident I've used very small amounts and the ratios were vaguely defined to be honest. Another
option would be to impregnate a pressed pellet of SADS with a solution of another energetic (of known concentration) to avoid the mixing and friction
of the process. Might be worth a shot...
Exact science is a figment of imagination.......
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Tricka90
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I tried SADS synthesis starting from pure silver metal. I obtained it by extracting silver via cementation from some tablespoons.
pH of my 8.5% w/w silver nitrate solution was slightly above 1 when I start reacting it with acetylene gas, from calcium carbide.
The solution was colorless, so no copper was present, noticeably.
I didn't warm up the solution, but ambient temperature was quite high considering it was a hot summer evening.
I used deionized water for both silver nitrate solution and acetylene gas production.
I washed the product many times with just deionized water, when dry it had a light grey color.
With that procedure I got a very stable product.
Hammer test was satisfying but nothing exceptional.
Friction test was outstanding: it had to put in so much effort to make it detonate by scratching it with an iron hammer on a not so smooth concrete
floor and I make it only once.
I didn't know SADS was also sensitive to static discharge. What does it mean exactly? Is there any way to test this kind of sensitivity?
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greenlight
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Here is an answer to your question taken from Introduction to the technology of explosives:
"Electrostatic sparks
There are no widespread standard tests yet for testing the electrostatic or spark sensitivity of explosives. A number of tests have been devised, and
perhaps a standard will someday be accepted. In general, secondary explosives are not particularly susceptible to this mode of ignition; however,
primary explosives and most pyrotechnics are susceptible. Initiation of an explosive materialby an electrostatic pulse is acheivef if sufficient
energy is delivered to the explosive material. Since most explosive materials are not good electrical conductors, the electrostatic pulse must have
sufficient potential to overcome the explosive material's low electrical conductivity.
Sandia National Laboratories has developed a uniform test specification for measuring the spark gap sensitivity of explosive-containing components. A
600-pF capacitor charged to 20kV is discharged through the component with 500 ohms in series with the discharge circuit. This test is considere to be
equivalent (or in excess) of the discharge that might be obtained from a static discharge from the human body.
In the loose powder test it is measured by discharging a 600-pF capacitor from a pointed electrode through a sample of loose powder (approx 0.2g) to a
ground plane.
the voltage is varied until one ignition in ten trials or the voltage limit of the testing equipment is reached."
Theres not much you can do at home to measure the exact sensitivity.
[Edited on 7-9-2016 by greenlight]
Be good, otherwise be good at it
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MineMan
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I have my doubts about SADS being as static sensitive as everyone says...
When made properly right temperature, right PH, and the right ratio of Silver Nitrate to to solution it is nearly immune to friction as Tricka stated,
infact, if he had heated the solution and made sure that the solution contained 25% nitric acid, the hammer test would have been more impressive.
Several times this product has failed to detonate when compressed with a visco fuse also. I have placed small amounts of this product between a
pizoelectric spark from a blow torch with no detonation (flash powder had the same results).
What I do know is that the same SADS that refuses to go off with the hardest of hammer blows on steel, will go off with a light tap when placed on a
rough hard rock... so perhaps a small static spark can... the sucky thing is, we just don't know... even with spraying everything with static
gaurd... static electricity seems impossible to predict... so I am afraid of a false sense of comfort.
SADS works great still with 10-15% potassium perchlorate, maybe this would help reduce it some....?
I believe Bert has a story of his SADS going off unexpectedly just from peeling a label off the container it was kept in. But I don't know how his
product was made, if it had been exposed to sunlight and the such.
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markx
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| Quote: Originally posted by MineMan | I have my doubts about SADS being as static sensitive as everyone says...
so perhaps a small static spark can... the sucky thing is, we just don't know... even with spraying everything with static gaurd... static
electricity seems impossible to predict... so I am afraid of a false sense of comfort.
SADS works great still with 10-15% potassium perchlorate, maybe this would help reduce it some....?
I believe Bert has a story of his SADS going off unexpectedly just from peeling a label off the container it was kept in. But I don't know how his
product was made, if it had been exposed to sunlight and the such. |
That is exactly the point....static is very deceptive as one can not see, feel or predict its presence with reasonable means. Most excessive
mechanical factors can be avoided or alleviated with proper procedures, but static remains the devil in disguise. So all false comfort is to be
avoided at all cost in our field of practice
As for testing the static sensitivity in home laboratory...in fact a lot can be done if one has a little electronical inclination and the will to use
it. To devise a small power supply that charges a high voltage capacitance to a preset voltage through feedback is not too complicated of a task. This
needs to be coupled with a small test chamber that has a means to decrease the standoff between electrodes (either manually or electromechanically
triggered) to initiate the discharge of the capacitance through a tiny sample of the compound to be tested. The voltage on the cap can be displayed on
a low volt digital voltmeter through a suitable voltage divider bridge. The same can be done for setpoint voltage. There are halfbridge driver ICs
with error amp inputs available for pennies and these can govern the whole process.....got my gears turning actually
Exact science is a figment of imagination.......
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Tricka90
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Yes, static discharge seems like a real pain in the ass due to the fact that it's almost unpredictable.
I think one of the best thing we can do to handle SADS a bit more safely is avoiding the use of materials which can easily accumulate electrostatic
charge.
In the following link there's a list of materials which tend to get charged. Paper, cotton, steel and wood seems to be the safest, so I would use
those materials to handle, store, let dry and transport SADS. According to the list, the most dangerous thing we can do is touching SADS with bare dry
hands or leather gloves while it lies on a Teflon surface...
http://www.school-for-champions.com/science/static_materials...
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Tricka90
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Hello everyone.
I would like to ask you what quantity of unconfined SADS can, in your opinion, cause serious damage if detonated in the very proximity of one's hand.
I think a 20 mg dose is not so dangerous, but what about 100 - 200 mg? Or even a few grams?
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MineMan
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Tricka90, I am disappointed with your question, from your previous posts it seemed like you were learning quite rapidly....
A few grams! 10mg causes a hole in a soda can, 20mg causes shrapnel from that hole to pierce the other side!
I think it would be best if you made a small quantity and experimented with small amounts and then told us what you think.
20mg could/would probably take flesh off the fingers to expose bone, 50mg definitely would. 100-200mg hmmm, ouch. A few grams, I am still
flabbergast that you asked this.
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KesterDraconis
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| Quote: Originally posted by Tricka90 | Hello everyone.
I would like to ask you what quantity of unconfined SADS can, in your opinion, cause serious damage if detonated in the very proximity of one's hand.
I think a 20 mg dose is not so dangerous, but what about 100 - 200 mg? Or even a few grams? |
Depends on your definition of serious damage. Removing skin and flesh is easy, it won't take many milligrams to do that. Breaking bones (potentially
irreparably) would be in the 250mg to 500mg range I think. After that, you are most definitely losing fingers if not the hand.
It also depends on what type of confinement you mean. Even a quarter of a gram if held in your fist and set off is going to basically take your hand.
So, the question is really relative. Best advice is to make small batches (about 0.5 grams), keep it far from your hands when you can, and use
precaution about flame, heat, impact, friction, static, etc.
[Edited on 10-9-2016 by KesterDraconis]
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Tricka90
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Thank you for your quick and informative replys.
I'm sorry, I think I didn't make myself clear with my last question: when I asked about detonation "in the very proximity" of one's
hand I was intending the explosive to be very near the hand (less than 10 cm) not in direct contact of it, for God's sake 
Of course even a few tens of mg can be extremely harmful if exploding right in contact with the bare hand, as you said, but I think (and hope!) nobody
would handle a primary this way!
So, do you think those quantities can provoke permanent damage even when detonating at a 5 to 10 cm distance from the hand? I would say 100mg can
cause irreparable injuries even at such distances, am I guessing right?
As for a few grams...I asked but I'm frightened to know the answer!
p.s.
I never manufactured (nor I'm planning to) more than a 100mg SADS batch: I think it would be unjustifiably dangerous since that quantity is more than
sufficient for conducting the major sensitivity tests and for detonation purposes within certain ranges.
[Edited on 11-9-2016 by Tricka90]
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KesterDraconis
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| Quote: Originally posted by Tricka90 | Thank you for your quick and informative replys.
I'm sorry, I think I didn't make myself clear with my last question: when I asked about detonation "in the very proximity" of one's
hand I was intending the explosive to be very near the hand (less than 10 cm) not in direct contact of it, for God's sake
Of course even a few tens of mg can be extremely harmful if exploding right in contact with the bare hand, as you said, but I think (and hope!) nobody
would handle a primary this way!
So, do you think those quantities can provoke permanent damage even when detonating at a 5 to 10 cm distance from the hand? I would say 100mg can
cause irreparable injuries even at such distances, am I guessing right?
As for a few grams...I asked but I'm frightened to know the answer!
p.s.
I never manufactured (nor I'm planning to) more than a 100mg SADS batch: I think it would be unjustifiably dangerous since that quantity is more than
sufficient for conducting the major sensitivity tests and for detonation purposes within certain ranges.
[Edited on 11-9-2016 by Tricka90] |
Yeah, I don't know if its smart, but I don't know it it is smart, but I use soft pieces of straw to scoop or handle primaries, this way, there is
little risk of friction or shock, and my hands stay a good 5cm-7cm away at all times. (though frankly, I don't like dealing with primaries, and I've
only ever synthesized three, and never actually used one to set off a secondary charge).
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Tricka90
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Yes, I think it definitely is a good idea.
I read that when making SADS, 10% HNO3 (by weight) should be added to the AgNO3 solution.
So if I have 9ml water should I add 1ml of 65% HNO3 or 1ml of 99% HNO3?
Or maybe the weight of AgNO3 salt itself also has to be consider in the calculations?
[Edited on 18-9-2016 by Tricka90]
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Metacelsus
International Hazard
Posts: 2539
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
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If you want a 10% w/w solution, you'll need a total of 9 grams of water and 1 gram of nitric acid. You can calculate the volume amounts using the
density and the concentration of your nitric acid.
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