Ag2C2.AGNO3 (DS)

Quote: Originally posted by PHILOU Zrealone

Sand will dry faster in a kind of tumble drier or into a fluidized bed (warm air from under through the sand that is lifted up (fluidized) a little and fall back down).

As I found out, much to my surprise, a heating cabinet and spreading out a thin layer of the stuff also does wonders


And yes....IT WERKS!!!


So I prepared a set of samples:



2* 50mg 100% SADS for baseline
1* 50mg 15% KClO3
1* 50mg 20% KClO3
1* 50mg 30% KCO3
2* 100mg 100% SADS for comparison

The cell was loaded with 40g of evaluation sand 250/100um fraction for all tests and then sieve analysis was performed with RETSCH AS200 apparatus on 100um sieve to get the fraction that passes the 100um limit as the assessment for brisance.
















The first results were as follows:

Baseline <100um for 50mg SADS 100% : 3,89g
Baseline <100um for 100mg SADS 100% : 5,82g

15% KClO3 <100mg fo 50mg : 4,42g
20% KClO3 <100mg fo 50mg : 4,09g ?? (probably an error in assessment)
30% KClO3 <100mg fo 50mg : 4,45g

This proves, although inconclusively, my previous assessment of the brisanse of these mixes based on the "match shattering" method. Seems that addition of KClO3 increases the power by quite a considerable amount compared to pure double salt.
As we can see from the baseline measurements ,the double charge of pure SADS caused about 49.6% increase in amount of <100um fraction. Where as the addition of 15% KClO3 caused about 13,6% increase in amount of <100um fraction. Derived from that, one could quite loosely estimate that the 15% KClO3 mix is about 27% more brisant than pure double salt. This applies only to this test under these particular circumstances and postulating that brisance increases linearily in relation to the amount of sand crushed. Which of course is not correct, but let's just assume for the sake of simplicity and just to make an example. All in all I'm very pleased with the performance of the cell and the first results. For further steps I will work with 100mg samples for better resolution and make more repetitions on all datapoints to get a more conclusive result and catch the most potent sweet point for the mix.
Oh yeah...I tried to set off the SADS KClO3 mix with friction and impact...no go, luckily it seems to be not too much more sensitive compared to pure double salt, but extreme caution is a must.

Nice side effect which can be seen in the last picture is that the top of the sample holder is covered in a shiny well adhered layer of metallic silver. It was deposited by the 100mg pure SADS baseline measurements. The 15% mix actually deposited a golden layer which looked even more pretty

As far as downsides of this perticular setup are concerned, then the fuse for initiation is best replaced by an electrical triggering system. The pyrotechnical route is messy, leaves ash and stinky byproducts if a BP fuse is used and must be set off outside....but it is simple and reliable.




[Edited on 1-2-2017 by markx]

Quote: Originally posted by quicksilver

GENERALLY; bottled industrial welding asses are fairly good

Teeheehee, welding asses

Great job and good lathe skills as wel! This would be a great tool to test small amounts of pirmary explosives for their brisance with the added benfit that it includes reasonably reinforced conditions, so also usable for less "hot" primaries so to say. As you said, one of the things that would be interesting to do is take several repetitions of exactly the same setup to get an idea of the variation inherent to the test. Assuming you want to be able to discern a specific effect size you can calculate how many repetitions would be needed to reach statistical significance, by the looks of it 4-5 may be enough for 10% difference.

Also, how does the packing densitty of the sand affect the test? Can imagine this depends on kernel shape and batch wise, maybe include a negative control (just unblasted sand) as well.

Did you design the setup after a commonly used one btw? If it does, would be interesting to compare your own data with those from literature. Very cool!

[Edited on 1-2-2017 by nitro-genes]

Quote: Originally posted by nitro-genes

Great job and good lathe skills as wel! This would be a great tool to test small amounts of pirmary explosives for their brisance with the added benfit that it includes reasonably reinforced conditions, so also usable for less "hot" primaries so to say. As you said, one of the things that would be interesting to do is take several repetitions of exactly the same setup to get an idea of the variation inherent to the test. Assuming you want to be able to discern a specific effect size you can calculate how many repetitions would be needed to reach statistical significance, by the looks of it 4-5 may be enough for 10% difference. Also, how does the packing densitty of the sand affect the test? Can imagine this depends on kernel shape and batch wise, maybe include a negative control (just unblasted sand) as well. Did you design the setup after a commonly used one btw? If it does, would be interesting to compare your own data with those from literature. Very cool! [Edited on 1-2-2017 by nitro-genes]

This testing device has not been benchmarked, at least not intentionally, against any particular device design of same function that is already out there and being used. So comparing results number by number is probably not going to be a trivial task, but that was not my intention to begin with. Rather I would depoly it in service of establishing a better understanding of the tendencies and relationships of the parameter known as "brisance" with regard to composition of energetic mix or substance. These tendencies have reasonably little regard towards the particularities of the testing device (which only sets the background system so to speak), so as long as a comparative set is tested within the same device, a comparable tendency should reveal itself.

The parameters of sand will most definately have a major effect on the outcome of the result, as the hardness, geometry, size, granulometry and packing density all affect the way in which energy is absorbed by the medium. I used soft limestone type to better capture the relatively small variations in brisance and prepared the sand fraction beforehand by carefully sieving and washing out everything above 250 microns and below 100 microns grain size. The unblasted sand shows close to 100% retention on 100 micron sieve....so anything passing through after test is the effect of the released energy. The sand surrounding the sample was not intentionally compacted (which would certainly increase the effect of crushing), but rather just poured over it and left as is. Either way will work and reveal the same tendencies as long as one keeps it consistent through the individual tests. So operator's adherence to preparative procedure and unbiased action is required...but that goes for all experiments

Quote: Originally posted by MineMan

Your results matched mine. I have found the addition of 20% Kclo3 to be best for both ignitability and brisance. This is important, as not only are we increasing the power, we are diluting it with a cheaper chemical. Above 20% it has trouble detonating in the open when exposed quickly to a flame. I have found also that it does not increase the sensitivity. SADS is really the most insensitive primary I think...

Nice.. could think of some comparitative test for some diazophenols. Would still be interesting to extrapolate results from taking some measurements from known primaries of course. Just hypothetically speaking (not really sure what this extra data would tell you), measuring the weight of several size fractions might also be interesting, starting with the smallest particle sizes and up, then looking at the distribution, maybe some correlations between total energy release and brisance would be apparent.

Regarding sand loading and packing by pouring, wouldn't round grains be optimal regarding density and consistency? Sharply edged sand grains take quite some tapping to get optimal packing probably. Maybe the total weight of the sand poured in can provide an idea of the most consistent loading procedure.

Quote: Originally posted by nitro-genes

Nice.. could think of some comparitative test for some diazophenols. Would still be interesting to extrapolate results from taking some measurements from known primaries of course. Just hypothetically speaking (not really sure what this extra data would tell you), measuring the weight of several size fractions might also be interesting, starting with the smallest particle sizes and up, then looking at the distribution, maybe some correlations between total energy release and brisance would be apparent. Regarding sand loading and packing by pouring, wouldn't round grains be optimal regarding density and consistency? Sharply edged sand grains take quite some tapping to get optimal packing probably. Maybe the total weight of the sand poured in can provide an idea of the most consistent loading procedure.

Well yes...probably a synthetic media with closely controlled grain geometry, size and hardness would yield the most unbiased results, but I have to work with the tools that I have at hand right now
Performing fractional sieve analysis of the crushed portion of sand is no problem from technical point of view, but I'm not really sure how to model and interpret this data. I guess one could find out some things about the energetic as well as about the sand medium itself from these sieve curves. This seems like a really vast field of research on its own and a rather complicated one too....

Yes, there are endless options for research here and all of them are exciting to pursue, but I guess for starters I will probe the topic of SADS/KClO3 mixes in more depth Find out the effective limits for this particular mix from one end of dilution ratios to the other and seek out the most potent combination.
For next step I will investigate the properties of pure double salt with regard to synthesis temperature ranging from lets say 20C up to 90C with 10C steps and see what kind of plot reveals itself. From previous experience I can say with relative confidence that the sweet spot is near 65C, but it would be really great to see this result develop through the experimental data from brisance assessment. Perhaps there are several good spots in the temperature range or some other details reveal themselves....

I would also like to construct a compact impact sensitivity tester to be able to check for how near the the abyss I am playing. I do have a drop hammer device and it works like a charm, but it is bulky, noisy and uncomfortable to transport. Something spring operated with a relative scale of potential energy should do the trick...much like a gunlock in principle. Again this would be a DIY device without a benchmark and thus lacking the option for direct comparison of literature data. Even better if I could also come up with a compact design for friction sensitivity testing device. The combined results from these could really lay a solid foundation for any claims on the topic. But let's see...time will tell

SADS

SADS belongs nowadays between a best primary. Not poisoned, with relatively available precursors. Therefore is this research pretty interesting, because price silver is high always. Adding 20% KClO3 is price of course lower and power this mixture is even higher. Next questions is sensitivity this mixture and stability after for example half of year. I Estimate, that some EM can be initiated directly with this mixture, without secondary EM. Or secondary EM will require lower amount this mixture for full drive. Which is advantage again. Very interesting the research.
........LL.......

Quote: Originally posted by Laboratory of Liptakov

SADS belongs nowadays between a best primary. Not poisoned, with relatively available precursors. Therefore is this research pretty interesting, because price silver is high always. Adding 20% KClO3 is price of course lower and power this mixture is even higher. Next questions is sensitivity this mixture and stability after for example half of year. I Estimate, that some EM can be initiated directly with this mixture, without secondary EM. Or secondary EM will require lower amount this mixture for full drive. Which is advantage again. Very interesting the research. ........LL.......

I do concur to the opinion that SADS can be considered as one of the most reasonable choices of primaries in the amateur practice realm. When prepared under optimal conditions (elevated synthesis temperature and strongly acidic environment), it displays inherently passive behavoiur against impact...at least on par with heterocyclic nitramine secondaries. My drop test device was unable to initiate it at the maximum height of about 70 plus cenitmeters with a 2kg impact weight. In comparison an early sample that was prepared at room temperature in acidic environment was highly impact sensitive and could be set off with a slight tap of an hammer. The devil lives in details and so far friction and electrostatic branches are unexplored from my side...a serious shortcoming that I have to rectify.
As for the cost of materials viewed from the amateur practice side are quite negligible, so the dilution with chlorates mostly just serves to satisfy the scientific couriosity
Nevertheless an in depth investigation might unveil some details that might make it sustainable for industry practice in some "niche" applications, but given the high content of a precious metal and the cost involved makes the chances quite slim.

A slight update on generic developments regarding evaluation mediums seen below:






The left one is quartz sand fraction and the right side one is limestone sand. Both have reasonably same granulometry and have been washed, sieved and dried meticulosly to rid it of any <100um fines. Totally different animals though....and not just because of the coloration
As I suspected before, the quartz sand is too hard for testing of SADS and shows close to zero crushing effect after 50mg and 100mg samples being fired. So it can not be used to test this substance for brisance.....which is actually great, because it opens up a way of cancelling out the effect of the primary initiator stage when testing for secondaries and hence yields a very precise and unbiased result that is purely due to the secondary stage firing up. A very exciting discovery

On a more sad note I have run out of limestone sand fraction and can not continue to test for the series today. I managed to get enough sand for two test shots of 30% KClO3 dilution mix and surprisingly the results are quite exactly on par with the 20% dilution results. Both hover about 25-27% above baseline brisance. Quite neat if one third of the costly ingredient can be replaced with a virtually free component and still get a massive gain in output
I will have to hog a massive sample from next shipment of limestone filler and prepare a sizeable stock of testing media. Then a full run of repetitions can be made in one go and the results lined up on a nice graph.....can't wait to get working on it

[Edited on 3-2-2017 by markx]

SADS

Once again, I would sum up the principles for the preparation yield 450 mg SADS:
1) Solution, maximum pure all reagents: 8,7g H2O + 1,82g HNO3 65% + 700 mg AgNO3 in high cylinder glass is dissolved. Temperature go to on 65 - 70C - hold.
2) Generator acetylene : 40g pure H2O + 1,5g pure CaC2, start temperature 20 C.
3) tube (plast) for bubble with cigaret filter (or 2 filter series ?)
4) Start generator, waiting 30 second before insert pipe to solution 65 C.
5) cylinder glass cover against light
6) Bubble 4 minute, pipe out.
7) Separation on inert Buchners vacuum aparatus (cover light)
7.1) Separation on wet pure filter paper, from distilled washing (cover light )
8) Drying on this filter paper, thin layer 1 mm, dry air 25 C, (cover light)
9) waiting 12 hours on total dry EM, closing in plast container, cover light.

If is someplace error, please repair instantly from your experiences. Thanks..............LL

SADS

Still more question: Should be possible counting, how much pure Ag is added to 65 % HNO3 for preparation solution, which will directly used for prepare SADS. Without process separation, drying a weighing silver nitrate and after again dissolving in 28% solution HNO3. Thus so, that solution will content 28% concentration of HNO3 + silver nitrate before start of bubble gas C2H2. For example, in 10g HNO3 65% dissolved 500 mg Ag. And bubbe. Because any preparation and manipulation with silver nitrate Introduces impurities into the process. When we have only acid and Ag powder. Which is usual.........LL

Quote: Originally posted by Laboratory of Liptakov

Still more question: Should be possible counting, how much pure Ag is added to 65 % HNO3 for preparation solution, which will directly used for prepare SADS. Without process separation, drying a weighing silver nitrate and after again dissolving in 28% solution HNO3. Thus so, that solution will content 28% concentration of HNO3 + silver nitrate before start of bubble gas C2H2. For example, in 10g HNO3 65% dissolved 500 mg Ag. And bubbe. Because any preparation and manipulation with silver nitrate Introduces impurities into the process. When we have only acid and Ag powder. Which is usual.........LL

I use 4g metallic silver in 20ml 65% HNO3 which is diluted with 20ml of distilled H2O to speed up the reaction (silver does not dissolve in concentrated nitric acid too eagerly). After that another 20ml of water is added and temperature brought up and stabilised at 65C. Then bubble C2H2 for 10minutes under vigorous magnetic stirring and filter....wash filtrate with distilled water several times...rinse...store damp on the very same filter paper in a plastic trip baggy or let it dry in warm dark place. Very easy ratios to remember : 4/20/20/20/10
Might not be the most optimized numbers, but simple and fully functional.

SADS

Well..! This is flash and quality answer...Thanks, all main was say. The die is cast. . .............LL

Perhaps an illustrated synthesis run starting from metallic silver is also of value:



So let's weigh out a sample of Ag




And prepare the reactor with 20ml of water as the heel and apply PID heating on magnetic stirring




Warming up to setpoint....




Let's measure out 20ml of 65% HNO3





Dissolve the silver and filter the solution into a syringe to remove any persistent colloidal leftovers (with the help of a cigarette filter )



As one can see the solution has a characteristic blue coloration hinting to a copper contaminant in the metallic raw material....but no worries, as it turns out, most of this impurity shall remain in solution after the reaction and can be removed with washing and filltering of final product.





Let's inject all of the silver nitrate solution into the reactor and let it equilibritate to 65C according to the inner mercury termometer. This requires to overdrive the pid setpoint slightly.


The solution is ever so slightly murky....most likely the water contains some impurities that cause the silver to percipitate in various forms of insoluble salts...a minor inconvenience.




Let's get some calcium carbide ready to feed into the gas generator.....a horrible low tech garde....dirty as sin in the dark night of Instanbul



Let's fill some into the gas generator that has an ice cold ice/water filling and start the 10 minute bubbling of acetylene into the reactor under vigorous magnetic stirring....omit all filtering of acetylene gas!





Immediately a beautiful snow white double salt precipitate will begin to form...





After the ten minutes are up, the administration of gas is stopped and mixing is shut off, the product layer is thick and voluminous, filling practically all of the liquid phase. As can be noticed, the solution above the solid still retains the characteristic blue hint of a copper impurity. Seems that it mostly stays in solution and poses no hazard to contaminating the final product.














Spit, stir, filter, wash, squeeze, set a portion to dry.....and commence testing




[Edited on 7-2-2017 by markx]

SADS

Huhaha..!......white as the snow.. And in solution is absolute minimal blue. I mean, that nothing problem with copper. Nice preparation. I see pretty sofistick aparatus for heating during a stirring. Ice water for generator ? It is better for purity C2H2 ? Or only start of gas is slowly. Because during generate has water self heating. ..LL..

Look everybody on the shit on wikipedia.......





[Edited on 6-2-2017 by Laboratory of Liptakov]



[Edited on 6-2-2017 by Laboratory of Liptakov]

Quote: Originally posted by PHILOU Zrealone

Maybe that the tiny copper amount helps to get a super white product...this is observed when making mercury fulminate...usually gray because of metallic Hg...but white like snow when into the proces some Cu(2+) is present...

Whilst I am waiting for my limestone sand sample to arrive with the next shipment, I went forth and begun with the creation of a primordial secondary test cell....the "STAMMZELLE"






Round, face off and clean the main cell chamber.....














Fabricate the cell bottom and sample holder....






And the cell support stand is completed in another session of machining....fits like a glove.



Top of the cell is machined, complected, welded and the seams cleaned up on the lathe....





The top is centered on the main chamber and welded, supporting from the top end on the lathe with a live center, the seams are cleaned and the cell is polished up.

The details are assembled and the "STAMMZELLE" is complete.....ready for the generation of hard experimental data

[Edited on 8-2-2017 by markx]

Hopefully it is strong enough not to differentiate into another type of cell. Sure looks that way though, nice welding job btw, MIG or TIG?.

Performing the synthesis at high temperature was also one of the things that I noticed to help get a more white product. From what I remember long time ago, I used even higher temperatures with somewhat lower nitric concentrations, did you notice any difference in product there? I've also wondered if it is really the same product as doublesalts formed at lower temperatures, as acetylene can also react with nitric under certain conditions. Very interesting indeed, looking forward to the comparitative test!

[Edited on 8-2-2017 by nitro-genes]

That is really welding and turning master-piece.
Absolutely far from amateur work...really professional.

Stem cells?...gigantic blast(o) cells I would rather say ...with such a device you can go up to the gram (1000 mg) range maybe even more if there is some venting and if the primary is not too powerfull.

Quote: Originally posted by nitro-genes

Hopefully it is strong enough not to differentiate into another type of cell. Sure looks that way though, nice welding job btw, MIG or TIG?. Performing the synthesis at high temperature was also one of the things that I noticed to help get a more white product. From what I remember long time ago, I used even higher temperatures with somewhat lower nitric concentrations, did you notice any difference in product there? I've also wondered if it is really the same product as doublesalts formed at lower temperatures, as acetylene can also react with nitric under certain conditions. Very interesting indeed, looking forward to the comparitative test! [Edited on 8-2-2017 by nitro-genes]

Mitosis should not occur with this particular type of "stemcell"

The welding was done with MIG and actually is quite sloppy and unpalatable even by my standard, but since I was going to trim off the rugged edges then it makes little difference at the end.

As for going upwards of 65C I have noticed a quite distinct difference in the product properties already at around 70C.....it becomes more coagulated/agglomerated and seems coarser. Also the potency seems to drop, have not measured quantitatively yet (it is in the plan though), but "match shattering" results seem to indicate a downward spiral. I've gone as high as 90C and this resulted in a totally different product which was very coarse and dense, yet lacked a lot of potency and seemed to perform much like the most dilute mix that I made with 50% KClO₃. Also it darkened considerably during damp storing in the dark (the fridge), something that never happens to 65C product even over a period of 12 months. I think in the end I tossed the whole 90C batch as it seemed to posess a set of characteristics that I had no use for at the time.

Quote: Originally posted by PHILOU Zrealone

That is really welding and turning master-piece. Absolutely far from amateur work...really professional. Stem cells?...gigantic blast(o) cells I would rather say ...with such a device you can go up to the gram (1000 mg) range maybe even more if there is some venting and if the primary is not too powerfull.

Welds look far better than my TIG ones for sure, so yeah... should remain a monoblast with ease!

The almost linear dependence on temperature is interesting, maybe the amount of silver nitrate precipitated along with the carbide is sort of a continiuum instead of some fixed possibilities of x-carbide-y-nitrate combinations? With silver being able to maybe also bind other ligands along the way would be interesting to look at the precise composition of the stable product obtained.

[Edited on 8-2-2017 by nitro-genes]

SADS

Markx method preparation was tested, all working perfectly. For dissolving 4g Ag was use 20g H2O + 28g HNO3/65. Use pure silver very fine powder and process dissolving running only 30 second. In reactor by 66 C arises instantly white material after all time 10 min. Nothing problems with dirty Istambul night CaC2.... I estimate - recommend big amount water in generator. For example 500 - 1000ml. Maybe it working as partialy washing of gas. Only my opinion. Yield 4,8g SADS. Thanks Marks, Very scientific approach to things.........LL

Trying to make most of the Friday, I managed to shoot a series of samples in the "nr 36" cell to cover the dilution range of 0-40% KClO₃ in terms of limestone sand crushing ability.

The lot of 100mg samples:



My results of % dilution with KClO₃ vs sand crushed below 100um in grams:



Due to a rather hectic schedule I only managed to shoot one series instead of four repetitions for every point. I will do that tomorrow to back up the statistical aspect of the data, but since I carefully perpared all of the samples to have the same weight and also made sure the sand was homogenous then even the single point results should reflect a reasonably credible picture of the situation...at least I hope so





It seems that the sandstone from this shipment was a bit harder than the previous batch as the 100mg sample of pure SADS only crushed 4,16g below the 100 micron mark as opposed to 5,82g in my test with previous batch of sand. So already I have reached a situation where data from previous tests is not directly comparable to current one. This makes it quite apparent that when comparable data is to be obtained, then working with materials of the same batch throughout the whole series is absolutely mandatory. Luckily I have just enough of the sand stocked to complete this series with 4 repetition points for all dilution ratios and get a comparable set of data....also the SADS and KClO3 in all of the samples are from the same batch.

As for the relationship of brisance/sand crushing ability vs dilution ratio....seems that the sweet spot for this mix lingers with reasonable probability somewhere between 20-25% KClO₃ content. What is quite amazing is the fact that at 40% KClO₃ content we are still at about the level of pure double salt brisance or slightly higher (one datapoint is not enought to draw precise conclusions). Quite surprising, as I suspected a sharper drop, but well, the preliminary data suggests otherwise....

Very nice markx,

You should plot your first results and the new ones in the same graph. Can you do it please?

As expected the geometric factor plays a role...

About the maximum ("sweet spot") actually it can be also between 15 and 20%...since 20% is your maximum graphical point from 5% intervals...the true maximum can be right on it or on its right side or on its left side.




Also, once your process is mastered and reproductive...
I strongly invite you to make tinier intervals of 1%...
Once when working at Procter&Gamble, I was making a study of stiffeners to stop wrinkles of fabrics after laundry wash (post wash wrinkle resistance project)...so we were screening silicons and activated them by ironing the fabrics...then the rigidity of the fabric was analysed by its bending of a given lenght of rectangular calibrated piece of treated fabric.
My manager had chosen the % to analyse (1%, 3% ,5%, 10%)...normally you would expect an increase of rigidity of the fabric when increasing the amount of rigidifier...but the results were erratic no matter the type of rigidifier...so I asked to my manager if I could perform an extensiver study, he said OK but only during my free time...so I decided to perform a study on various product by 0.1% increments (thus instead of 4 point, I prepared, tested and measured 100 solutions per product)...result was very unexpected...the rigidity was following an amorted oscillating patern and in fact the use of 0.3% rigidifier was better than the use of 10%...so it had significant cost reduction impact.



[Edited on 11-2-2017 by PHILOU Zrealone]

Quote: Originally posted by PHILOU Zrealone

Very nice markx, You should plot your first results and the new ones in the same graph. Can you do it please? As expected the geometric factor plays a role... About the maximum ("sweet spot") actually it can be also between 15 and 20%...since 20% is your maximum graphical point from 5% intervals...the true maximum can be right on it or on its right side or on its left side. Also, once your process is mastered and reproductive... I strongly invite you to make tinier intervals of 1%... Once when working at Procter&Gamble, I was making a study of stiffeners to stop wrinkles of fabrics after laundry wash (post wash wrinkle resistance project)...so we were screening silicons and activated them by ironing the fabrics...then the rigidity of the fabric was analysed by its bending of a given lenght or rectangular calibrated piece of treated fabric. My manager had chosen the % to analyse (1%, 3% ,5%, 10%)...normally you would expect an increase of rigidity of the fabric when increasing the amount of rigidifier...but the results were erratic no matter the type of rigidifier...so I asked to my manager if I could perform an extensiver study, he said OK but only during my free time...so I decided to perform a study on various product by 0.1% increments (thus instead of 4 point, I prepared, tested and measured 100 solutions per product)...result was very unexpected...the rigidity was following an amorted oscillating patern and in fact the use of 0.3% rigidifier was better than the use of 10%...so it had significant cost reduction impact. [Edited on 10-2-2017 by PHILOU Zrealone]

Admirable persistence in executing a workload of an order of a magnitude greater than the initial plan and even more so outside of your required duties....I do hope your employer rewarded your efforts with more than a subtle "thank you" I myself have ventured on similar paths in service of similar employers in the past. Perhaps not so srikingly enourmous ones in terms of workload, but found to my not so great surprise that besides satisfying personal curiosity for the topic, it gains one little leeway in the upward direction of the rotten steps on the social ladder But I am digressing from the topic...

Sure I can and will include also the first results on a combined graph once I have completed the intended set of data. Perhaps displaying the results in % of gain in the amount of sand crushed compared to the initial baseline of pure double salt shall display a clearer picture of the relationships involved, as it offers a simple means to factor out the size of sample fired. The first results were obtained with 50mg energetic samples, but the latter ones with 100mg amounts. Of course the "cell constant" may be different with dissimilar mass of charge, but the overall realtionship displayed against the baseline in % difference between dilution ratios should be reasonably similar and comparable.
The "sweet point" proximity surely deserves a more enhanced resolution by smaller steps on the dilution range scale, but I would not venture on the path of covering the whole scale with say a 1% resolution.....I highly doubt there are any sudden bursts of performance that might get lost between the 5% resolution steps further away from the main peak area.

I have done the graph...
I have done the normalization... and the % increased performance graph too :-)

Was ready for posting two days ago, but the forum was unaccessible for me during two days (between 11/02 after midnight up to now) with a weird message "Forbidden 403" and that I had no permission to acces it...this did also happened on 8/02 for a day long.

Here it is:

To continue the topic, below are my results from repetitive test of the same series under same conditions and with the same batches of materials:




As one can without doubt see, there is noticeable and systematic dissonance between the first test series and the following ones regarding the range past 15% chlorate content and upwards. The reason for it I have despite my sincerest efforts not discovered yet. But as it seems Philou was correct in assuming that the maximum might be in either direction towards 15% as well as towards 20%. As the repetitive test shows it seems to be around 15% chlorate content according to current results, despite my previous assumption that it might be more towards the 20% range. The devil lives in repetitions, as one might say

But to make things even more complicated I repeated the series of five datapoints per dilution ratio for both 15% and 20% chlorate content last weekend to find out if the trendline is correct. To my great dissapointment I had again run out of testing medium and reused the sand that I had kept from previous tests. To my surprise I received results that were below all of the previous ones in terms of sand crushing ability by as much as 1g per datapoint for all shots fired. The trendline still revealed the maximum being near 15% though.
Either the previous testing knocked softer particles out of the testing medium and harder ones remained to show lesser brisance in retesting or the double salt degraded during the week. The latter one is less probable and I think the dog is buried in the testing medium's altered properties. One can not reuse it reliably and compare results (only if a full series is retested with the shot sand and calculated as % gain against a new setpoint). Sigh....I ordered a new batch of filler with larger average particle size to be able to sieve out more of the useable 250/100um fraction.

I guess more testing around the "sweet spot" with the new fresh sand are on the way

On a different note I also tried the "Stammzelle" function with 150 and 200mg ETN samples that were initiated by the 100mg SADS/KClO3 primary in quartz sand medium. A satisfactory sharp "ping" note arose from the successful initiations and recoil launched the cell off the holder by about 15cm. After sieve analysis it was concluded that 150mg sample had crushed 11,8g and 200mg sample 12,8g of quartz sand below the 100um mark. A satisfactory result in terms of the cell function, but no more at the moment...

[Edited on 20-2-2017 by markx]

Very nice and surprizing...

To get a special view of the problem I have redone the graph...the normalization... and the % increased performance too :-)

From this one can see that results are not reproductible despite inside the same cell , with the same straws, fuses, geometry and the same batch of SADS...this is obvious from the large distribution of the first points (pure SADS 100 mg) so the discrepancy must come from:
-the sand (and obviously his previous history)
-the pressure/compaction of the charge
-precision of the charge weighting (although if your scale is into the range of 1 mg...it must be 2% variation)



What is also stricking is the fact the "curve" is not a beautiful smooth Bell one but suffer from oscillating moves with shoulders...we may be into the same kind of case scenario as the one I exposed earlier about my study at P&G

I think that the first thing to do is to harmonize the sand batch...and to get more reliable results from pure SADS...
Maybe that the use of your special sand is not the best because not composed at 100% of silice...so the proportion of other softer ingredients may vary (like CaCO3, clay micro-nuggets, ...) from batch to batch or even by simple segregation into the bag itself.

I will try to make a blastcell on my own...
Could you please give the dimensions of your two blast cells...external dimensions and internal chamber dimensions?
Since I don't have the same welding abilities as you and not the same material I will use plumbing pipes 4/4, 3/4 or 1/2...but I need to be close to your system.

[Edited on 20-2-2017 by PHILOU Zrealone]

Yes....the dissonance between the individual test results from experience this far has been much higher than I could anticipate in the beginning. Exact reason for this remains a mystery and the nature of the drifting seems to be systematic througout the series. It is as if the scale would shift every time I decide to shoot a series.....the first one was way up through the whole range...the second attempt of repetitions fell lower....and the third attempt on 15% and 20% even more so.
The third one I can account for the recycled sand, but the shift between the first and second testing is unaccounted for as I really tried to keep the conditions as close as I possibly could and the time between testing runs was only 24h, so any degradation of the energetic is not really possible on that scale in this timeframe.
I do think that most of the wrinkles in the results are realted to the limestone sand and self seggregation of it in the storage vessel....plus the altered average hardness of the used sand in third testing run.
The apparent occillations on the edges of the curve are perhaps more realted to the model of trendline approximation than the real nature of the performance itself, although I dare not to oppose that position severly. Further testing will tell...
As for the cell dimensions I will give exact numbers tomorrow once I measure them properly, but the primary "36 cell" is very close to standard 1" pipe in its main chamber, so using a threaded section and two end caps shall make a rather good copy of it for comparative testing.
As for using silica (quartz) sand for this material....probably not going to work out good. At least in my attempts the crushing action of sads mixtures on silica sand was close to zero. Perhaps you may find a softer version, but the relative errors in measuring these small amounts of crushed material may distort the results very significantly.
One option to enhance the crushing effect upon testing media and getting better resolution is to use bigger test samples of say 200-300mg each if one does not mind the cost and has a plentiful supply of silver available.

All in all, despite the shifting between the series we still have a rather clear trendline through the dilution range, so I think something has been revealed and the problems of data distortion can be fixed by correcting the testing procedure and parameters...I'm quite happy with the results and the challenges that have been put in front of us

Excuse my fugly techical handdrawing....but that was the quickest and most effortless way of getting the dimensions visualised for making a close replica:




The smaller "36 cell" holds 40g of sand and "Stammzelle" exactly 200g....was not intending to copy literature value, this is pure coincidence. I must say that this sample holder design is not really suitable for testing of high brisance secondaries and there needs to be some cm of clearance between the sample holder and the actual high brisance sample. Even with the relatively "tiny" 150mg and 200mg ETN samples I can see that the sample holder has been deformed and crushed in on itself. Measuring with caliper reveals that the top end of the sample stem has become 0,2mm wider than the bottom only after 2 test shots with minimal energetic content. The holder has been fabricated from a rather strong 10,9 strength class bolt and it is tough as a coffin nail, but no match to the direct pressure wave from ETN and with this rate of degradation it is not going to last even one testing series.

Ok....more surprising nuances that I just discovered. I built an electrical ignition system for the "nr 36" cell, based on a small high voltage "tazer like" module that creates an electrical discharge on the surface of SADS sample between two electrodes. And I mean a nasty bright, loud, fat arc discharge that burns through paper with ease and chars it. Something that by the sound and looks of it will really make one feel the shock if it should contact your system. Loaded it all into the cell under the sand and pushed the button......one can hear the arc from under the sand going at about 50Hz discharge rate and NO INITIATION!! I let it crackle for about 5 seconds straight....and nada, nothing, no bump, no bang, no ping.
I dissassembled the cell and pulled the sample out, totally intact. Imagine that, the surface was scarred black and also the walls of the plastic straw were covered in black deposit.....so there was no doubt that the arc touched the sample and decomposed the surface layer, but it did not ignite the primary. So I sprinkled some loose SADS on top of the pressed sample and reassembled the system so that the electrode tips were immersed in the loose acetylide. This time the sample went off straight away, so I repeated the test with another sample, but this time I added a bit less loose SADS on top. Not a complete layer, but chunks around the electrodes with a bit free space inbetween them.....and got no ignition! Upon dissassembly I again found that the surface was scorched and also the loose bits were dark colored, but no go nevertheless.
It seems that the much talked about sensitivity of this compound towards electrical discharge might be a bit overstated. Only if the discharge is forced directly through the loose layer of SADS an ignition might occur.





Notice the black goop on the inside of the sample tube.....that was caused by the arc burning on the surface.

Unfortunately Liptakov is right about cost being the main driving feature behind commercial applications. But that does not mean that a discovery is unusable just because of higher cost, there are fields of application where cost is not imperitive, but rather the fact that a function is fulfilled or a specific property of a substance is present. Like aerospace, military or some other niche applications.
Taking a patent application is easy, but before that, one has to be rather sure that there is a viable practical interest behind it all. Otherwise it is just a rather big hole in your wallet caused by that document that nonone wants to buy in the end. And it is quite a cost to cover really just for applying for and keeping patent protection over a particular application. I know because I have several patent references in the electochemical energy storage field and went through the whole process.
For now I'm just happy to have a reasonably usable solution for hobbyist experimentation purposes....as much as what we engage in can be called reasonable after all

About the electrical sensitivity testing....well yeah, I do need to construct a device that can store a variable predetermined amount of electrical energy and then release it through the sample under testing to get a quantitative result. It involves quite a bit of mechanical and electronical work, but it is doable. Zapping samples with piezo discharge or the kind of zap box that I used and making statements about the sensitivity or nonsensitivity of the sample is not going to hold water in any way. So again I must remind that my results are at the monent singular, preliminary and by no means should
they be translated as a green light to handle DS without concern to electrostatic dangers.

Quote: Originally posted by PHILOU Zrealone

@Mineman, LL and markx, Not only the price is important but also: -the efficiency of reliable D2D (from shock, flame or electric spark) and -the initiating ability...for example how much Lead azide is required to set off TNT vs SADS?

Of course....I was speaking on a generic level assuming comparable performance of a device/solution.

BTW Philou, how are your attempts on the sand crush test going? Any luck of seeing comparative data on the SADS mixtures? It would be really interesting to compare the results

My new coarser samples of limestone sand also arrived this week, but the granulometry is different at the upper end of grain size distribution. I guess I will try a whole repetition of the series with a single batch of the new sand to limit the uncertainty factor and see what comes out of it.

SADS

Quote: Originally posted by MineMan

As being part of the blasting industry I disagree. Not long ago I was on a loaded blast pattern when an excavator almost (less than 1" away) ran over a surface cap that was connected to all of the holes. They already pay $30 a cap... I don't think .1g of silver per cap would change that much... safety is king with the mining culture... they pride themselves in it... on mine I worked at one could not enter a pickup bed truck without fall protection. Remember, they only use 120mg of this stuff to fire PETN... we as armatures can make that amount for nearly 10 cents. Accidents and investigations cost a lot... If a company like orica announced a switch to a infallible primary explosive, because of the strong safety culture in the industry their stock would go up, and all competitors would have to follow. [Edited on 4-3-2017 by MineMan]

Quote: Originally posted by MineMan

They already pay $30 a cap... I don't think .1g of silver per cap would change that much... safety is king with the mining culture... they pride themselves in it... on mine I worked at one could not enter a pickup bed truck without fall protection. Remember, they only use 120mg of this stuff to fire PETN... we as armatures can make that amount for nearly 10 cents. Accidents and investigations cost a lot... If a company like orica announced a switch to a infallible primary explosive, because of the strong safety culture in the industry their stock would go up, and all competitors would have to follow. [Edited on 4-3-2017 by MineMan]

Quote: Originally posted by markx

Quote: Originally posted by PHILOU Zrealone   @Mineman, LL and markx, Not only the price is important but also: -the efficiency of reliable D2D (from shock, flame or electric spark) and -the initiating ability...for example how much Lead azide is required to set off TNT vs SADS? Of course....I was speaking on a generic level assuming comparable performance of a device/solution. BTW Philou, how are your attempts on the sand crush test going? Any luck of seeing comparative data on the SADS mixtures? It would be really interesting to compare the results My new coarser samples of limestone sand also arrived this week, but the granulometry is different at the upper end of grain size distribution. I guess I will try a whole repetition of the series with a single batch of the new sand to limit the uncertainty factor and see what comes out of it.

I have bought a lot of material...
1°) I have to build my cells...
I can build 2 or 3 different size from 4/4 piping...but I also found an interesting possibility from modulable iron steel pieces to make support structure or to make kinder playground...see pictures below.
2°) I have to have acces to my 0.001 mg scale into my appartement (must wait that my ex-grilfriend is leaving (maybe at the end of the month?))
3°) I have to make SADS the way you did it (warm at 80°C)...so eather I have to make AgNO3 from Ag jewellery and HNO3 or eather I need to have acces to my old SADS stock and to my AgNO3 stock (into my appartement)...also need acces to my NaClO3 and KClO3.
4°) I have to cut all the pipes I have bought (Al, Cu, bronze) from various diameters at given various lenght with a pipe cutter, and drinking straws (also various diameters and lenght)
5°) I have to build a screening plate (I have a thick grid with medium holes) and to test aquarium sand/gravels screening with it. The sand is apparently some kind of silice (2-3mm diameter) with a dark glassy shine (garnet, glass?) anyway it is commercially available from AVEVE shops and sold by 10kg (8L), I also have a finer white version (0,2-0,5 mm diameter) also 10kg.

Then I will be ready...for testing and reporting.

Here are the pictures of the pipes and metallic pièces for cell confection: (The AA battery is there for visual scaling purpose)

The conventional galva piping 4/4 is 2,7 cm internal diameter and 2,5mm wall thickness (thus external diameter 3,2 cm).
The larger "Flex Fit" pièces I have found (I have looked onto internet or into the provider website...but brand is nowhere to find???(*))
It is composed of 5mm wall thickness and 4,5 cm internal diameter...you can stick a pipe of suited lenght into it (4,5 cm external and 4,2 internal)...thus the total wall thickness would be 8mm for a cell of 4,2 internal diameter...easy to assemble and dissassemble with a simple hexagonal screew (seen on the pictures) I just need to figure a way to close the ends with circular iron plates to put inside and perfectly fits the hole (I think I will have to make it on my own and make it as thick as I want eventually by using multiple layers...in a way the minimum internal height of the cell will be 18 cm... for a nominal testing cell volume of at least 210 cm³

[Edited on 7-3-2017 by PHILOU Zrealone]
(*) I have found references by internet by using the code engraved onto the metallic pieces:
JM 131-C42 (A27)
Interclamp products
Raccords tubulaires
JM 149-C42 (C42 or D48)
Raccord tubulaire


[Edited on 7-3-2017 by PHILOU Zrealone]

The cell project seems to be coming along nicely, Philou! Hope you get everything sorted out without too much trouble and can start experimenting....

In the meantime I took one step further (or rather sideways) and made some experiments with SADS/ETN composite. This mix really packs some serious sand crushing power. I figured that since ETN has a positive oxygen balance, then it should suit well for the purpose of boosting double salt performance without rendering it too insensitive towards flame initiation. I did not have to dissapointed...first brisance results with 100mg samples place the mix well above any previous KClO3 based results:



Calculating for the same amount of additional oxygen as with 15% KClO3 the mix came up with a 1/1 ratio of DS/ETN, which in practice turned out to be passive towards flame initiation and could not be initiated with a fuse. Coming down with ETN content it was found that at about the ratio of 65/35 DS/ETN the mix became sensitive towards flame initiation in slightly compacted state, but was dead pressed very easily and after that became passive again. At a composition of 77DS/23ETN the mix remained reasonably sensitive to flame also in the pressed state and exibited highly increased brisance. The limestone sand was compacted so strongly by the test that it formed a thick solid layer on the walls of the cell and it had to be scraped off with a metal spoon to perform sieve analysis.

P.S. The nitroester mixes were prepared by dissolving ETN with a few drops of acetone and then mixing into the DS in wet state to avoid too much agitation.

[Edited on 7-3-2017 by markx]

It are perfect results... My reason was identical, but fear was bigger than making experiment. OK. If I read good, is possible under acetone making mix 65 DS + 35 ETN. As output segment can be use pure ETN, for example 0,25g and as DDT segment described mix 65/35 with low -lower density, pressed only on 3 Kg in cavity 6 mm, w. 0,25g. And insert Bickford fuse. It seems , that semi - NPED will be.......LL

Quote: Originally posted by Laboratory of Liptakov

It are perfect results... My reason was identical, but fear was bigger than making experiment. OK. If I read good, is possible under acetone making mix 65 DS + 35 ETN. As output segment can be use pure ETN, for example 0,25g and as DDT segment described mix 65/35 with low -lower density, pressed only on 3 Kg in cavity 6 mm, w. 0,25g. And insert Bickford fuse. It seems , that semi - NPED will be.......LL

Silver acetylide double salt common plasicsizer

SADS/ETN

Of course, plasticizer exist. Here is entire video : https://www.youtube.com/watch?v=dqUzKELQUM4
I mean, that is possible add ETN. According markx 80DS/20ETN and mix all together. Estimate + 8% plasticizer. However, is necessary try it very carefully.
.........LL

Quote: Originally posted by symboom

are these good Polyisobutylene sources the video that LL has that tape is been replaced mainly with silicone he is lucky off to figure out other sources such as bike innertubes would work but they are halogenated polyisobutylene as I read on wikipedia I could be wrong. bladders from basket ball or other sport balls and waterproof electrical tape wikipedia also states chewing gum now that would be an interesting source Any ideas [Edited on 31-3-2017 by symboom]

Quote: Originally posted by agent_entropy

Has anyone here experimented with, or is anyone aware of reported accounts, of adding acetone to the silver nitrate solution to increase the solubility of acetylene? Since acetylene is often stored as a solution in acetone, this seems go me like a logical iteration of the experiments concerning this substance. Of course a nitric acidified solution would have to be dilute to avoid oxidizing the acetone.

Quote: Originally posted by agent_entropy

With the acetone... If silver isn't reduced to its metallic form it might (?) result in some new practically worthwhile morphological variants. If the nonvolatile acetone oxidation products are included or occluded into the SADS it could help with the gas production problem.

I tested some SADS with KClO3 and found it less than impressive (perhaps I should have mixed them more intimately using a few drops of water, then dry).

I also tested some of the above mentioned SADS:ETN (80:20) and was absolutely shocked by the massive increase in apparent power as indicated on the witness plates pictured below. I don't have a fancy sand-crushing cell, but the experiment below seems to demonstrate the relative brisance handily.

Small aluminum foil balls full of the stuff were prepared using approximately 0.17 g of aluminum foil each and each charge was provided with a length of visco fuse. The test charges were then scotch taped to the center of a 15 oz food-can lid to prevent the spit of the fuse from propelling it off center. Each test was rested gently atop some grass of length approximately 8cm and ignited. In the picture below, from right to left: A test charge taped to its witness plate / 0.50g SADS / 0.25g SADS:ETN (80:20) / 0.50g SADS:ETN (80:20).

@ Agent_entropy,
Nice visual comparative testing

Quote: Originally posted by Bert

Silver acetylide has quite high sensitivity to static electricity, perhaps this might help address this?

Quote: Originally posted by agent_entropy

Quote: Originally posted by Bert   Silver acetylide has quite high sensitivity to static electricity, perhaps this might help address this? From what I can tell by handling it, the SADS:ETN (80:20) is indeed somewhat less sensitive to static electricity than pure SADS. I'm not sure how to quantify it though. Bonus tip: I realized that I could add some methanol or isopropanol to the water in the calcium carbide acetylene generator, in order to help control the foaming.

Nice idea to use alcohols as a foam killer...suds depressant.

A layer of organic oïl on top (0,5-1cm) or of benzine/ether/petroleum ether will do aswel

[Edited on 31-10-2017 by PHILOU Zrealone]

Quote: Originally posted by Rocinante

CHP seems like nonsense since the starting perchlorate is quite sensitive primary and you won't (likely) be making small mg size batches like with SA.DS plus the amount of handling during CHP synthesis is quite large. That's similair to the situation with NHN, where some hail it as a work of god, yet they fail to remind that NHN is among the most static sensitive primaries or that un-dextrinated lead azide is more sensitive to friction than HMTD and faar faar more sensitive to friction than TATP/DADP. It's like dangerous boasting about ones ability to get the right chemicals (being a grown up with tons of NaN3 in the chems room). In the end of the day you still need remote handling, large pieces of paper with small amounts of said primary, blast mitigation devices, cotton wrapped sticks and many layers of body protection. Would it be possible to use another acid instead of HNO3 to create the needed acidic conditions? I mean, would a few drops of sulphuric acid be enough? It (the sulphate) should be possible to wash it from the filter. [Edited on 14-11-2017 by Rocinante]

Quote: Originally posted by Rocinante

I was talking about Dr. Liptakov synthesis on Vimeo, where he uses 10 g of TACP to synthetise CHP - I was pointing out that this TACP is quite sensitive and handling 10 g of it is simly too big of a risk (even though you might handle it in its not completely dry state). The fact that CHP is quite unsensitive should not lure anybody to directly handle/store 10 g of TACP. It requires somewhat more of a work than making SA.DS or lead azide, so a person is tempted to go into the gram scale, rather than to quickly make 400 mg of SA.DS or LA for use in blasting caps. If you use another route, without the TCAP step and in small quantitiy, than yes .. it is indeed a workable solution. SA.DS - I understand that the nitric acid should be ideal due to the common ion effect, making the precipitation of SA.DS easier, but would it be possible to avoid the use of HNO3 and use something else instead .. like a few drops of sulphuric acid, has this been tried out? [Edited on 17-11-2017 by Rocinante] [Edited on 17-11-2017 by Rocinante]

I have handled much much more than 10Grams of TACP at a time, but have not stored it of course. The point it, it is not a primary explosive, it can be treated like PETN. Look, CHP is the best around, unless you can come up with another DDT system. Of course, there are main charges that are safe and can DDT from just a blackpowder cap... but those are kind of a secret of mine, but now you know, they are out there! Also, there are several AN mixtures that 2grams of flash (even confined in plastic) will bring to full orde Report back to us, but trust me, you don't even need a primary . I can say this because I have invented a complete binary system... including the det

[Edited on 21-11-2017 by MineMan]

Quote: Originally posted by DrManhattan

Im having touble with my SADS. I made a batch about 6 months ago and have been using the primary from this batch to fire my charges. All worked well at the start with 5 continuous charges going off without a hitch. Now using the same batch i get 100% misfires. My cap has always been 700mg pressed etn - 300 loose etn - 200mg SADS, set off with an E Match. E match always went off but even though it was in direct contact with the SADS it didn't ignite it. The product was an off white - pale brown color at the start but it turned blackish so i thought id make a new batch. still get problems with this fresh new batch. It seems as though either none of the primary goes off or only a fraction of it does. I took a misfired cap apart and poured out the primary and put a blow torch to it and it crackles as apposed to all going off in one bang. Any idea on whats going on?

Ratios i used were - 8.7ml H2O
- 1.3ml 68%HNO3
- 700mg silver nitrate

Acetylene is from a gas bottle and passed through a solution of copper sulfate. Silver nitrate solution was kept between 65-70 degrees Celsius during the reaction. Passed gas through the solution for 3 minutes. SADS is then filtered and neutralized to get rid of the acid. The end product is certainly SADS or at the very least silver acetylide. Makes a nice bang even in the smallest amounts but after putting it into a cap it just seems to go dud. No change was made to the original successful batch. I have even tried alternates to the E match including nichrome wire in direct contact with the primary and even smokeless powder + e match. Smokeless powder ignited but didnt even set the primary off, very unusual indeed. I even had a cap where at least a small amount of the primary detonated as the cap was shattered (i use 10mm plastic test tubes as the housing for the cap) but i recovered some silver acetylide after sifting though the remains.

I attached 3 images. I use an ear plug as a plug to keep everything together. Green plug was the failed cap with partial detonation of primary. Orange plug cap was a successful cap. Only difference to the green was a larger 2 gram base charge of etn. SADS of both came from the same batch.

Quote: Originally posted by DrManhattan

SADS is then filtered and neutralized to get rid of the acid. The end product is certainly SADS or at the very least silver acetylide.

Quote: Originally posted by markx

What did you use to neutralize the end product...something caustic? In fact I would suspect that this step might be the culprit here. Omit the neutralization step, just wash with coupious amounts (within reason) of distilled water and store damp if you dare not dry bigger amounts. You mentioned that the product darkened upon storage....how long did it take for that to happen and was it stored in dark or in open light?

Quote: Originally posted by DrManhattan

I used sodium bicarbonate to neutralize the end product. Took about a month for it to turn black. Stored under acetone in a storage box in complete darkness. It was still reliable after 2-3 months of storage, only as of late has it been troublesome. I have been thinking of trying Mercury Fulminate if i cant get my silver acetylide to work reliably.

Quote: Originally posted by markx

Your acetylene comes from a gas cylinder? A welding grade product I presume? They usually have acetone mixed into the gas tank to lower the sensitivity of compressed acetylene in storage (I'm not totally sure it is still practiced, but I know that it was done)....perhaps the acetone vapours also have an effect on the synthesis? If you can access some calcium carbide, then it would be useful to try the synthesis with the generated gas and compare results. Generated acetylene purity seems not to have a profound effect upon final product, so thorough filtration and washing of the gas is not required. At least I've never bothered and have had no issues.

Quote: Originally posted by markx

So try it without the bicarb and in simple water damp storage....compare the results. If still problems arise, make sure your thermometer is not "crooked" and the 65-70C range is really true. Also you may try to slightly increase the acid content in the synthesis stage if all else fails, it should not worsen the odds of getting superior product. I've had weak product from higher as well as lower temperature ranges that showed high sensitivity towards light and also mechanical factors, as well as a weak performance. Your acetylene comes from a gas cylinder? A welding grade product I presume? They usually have acetone mixed into the gas tank to lower the sensitivity of compressed acetylene in storage (I'm not totally sure it is still practiced, but I know that it was done)....perhaps the acetone vapours also have an effect on the synthesis? If you can access some calcium carbide, then it would be useful to try the synthesis with the generated gas and compare results. Generated acetylene purity seems not to have a profound effect upon final product, so thorough filtration and washing of the gas is not required. At least I've never bothered and have had no issues. MF is by far more uncomfortable, poisonous and probably also more sensitive than double salt. I trust it would be wiser to work carefully towards perfecting the double salt synthesis than engaging in the mercury route.... Hope this helps and be safe in your practices!