Picric acid: different instructions

look in bag products, small , soil conditioners

Seek, and ye shall find

Not composition D but explosive D actually and you misuderstood/didnt read my post.Ammonium picrate was never suggested as a primary!!One must start with TNP/picric acid as my Idea developes
Add lead monoxide-methanol = lead picrate.lead picrate primay and TNP = very powerful composite cap.Explosive D or Ammonium picrate as a secondary can be cast as I am sometimes led to believe from ww1 arty reports? Ideal garage HE for shaped charges with a comparitively good VOD and insensitive to many lesser caps.All precautions to prevent various HE's from interacting with metal/each other.
But with all respect a composite cap with 4-5 grams pressed TNP at 7480 MPS with the same of granulated exp D in the det well should overcome any reluctance to fire .

However the appetite of exp.D for ammonia in its synthesis will likely put the end to that Idea$$
one of simplicity really.(very few OTC precursors needed)In additon bunker busters arent used industrially to my knowledge and as ammonium picrate has been used in HEAT SC it stands to reason military detonators or engineer special caps will suffice as military det wells are universal for hand carried charges.
Please excuse all the editing but a naval handbook I just came across compares comp A, 91%rdx-9%wax with EXP D sensitivity.



[Edited on 15-10-2008 by grndpndr]

[Edited on 15-10-2008 by grndpndr]

[Edited on 15-10-2008 by grndpndr]

My post suggesting granulated exp D in the det well should read the same 4-5 gr of picric acid next to the composite cap
inside the main charge of exp D again next to 5-10 gr. off granulated exp D as the explosive train.

Quote: Originally posted by User

How long and at wat temp. did you do the sulfonation/nitration?

TNP melts at a relatively low temp and deflagrates at a slightly higher temp.Recall it was used in ww1 arty shells loaded by melting the tnp.As I said it melts in a small teaspoon using just a cig lighter and shortly after decomposes by quick deflagration, small pop and a small amount of black soot.Combine that with the hammer impact test mentioned and there should be little doubt as to the product.Why your not getting there has to be inadequate time for sulofonation and or nitration.Perhaps the aspirin your purifying has a buffer that isnt being removed.Problem with your SA, Time allowed for sulfonation,temp etc.To rapid addition of the nitrate, inadequate /poor quality nitrates with additives.Poor synthesis instructions.Frankly I believe it to be a difficult synthesis to make fail!? Given the comparitive brisance to moderately high VOD HEs I have to assume what was made was always at least 80%TNP, likely far more than the 80%.

Zinc,ive never encountered anyone experiencing problems with used ,concentrated batt electrolyte salavaged from junk batterys which Im sure contained a great deal of lead.The very full of sediment (lead Oxide?) was simply removed by allowing the sediment to settle until electrolyte was clear and decanting the clear electrolyte.the used electyrolyte never required filtering and was absolutely clear after condensing by boiling w/o any filtering.

As far as purity of the TNP after recrystalizing from dist water no discoloration of the water or change in the color was noted,still retaining the distinctive bright canary yellow crystalls.
[Edited on 17-5-2009 by grndpndr]

[Edited on 17-5-2009 by grndpndr]

[Edited on 17-5-2009 by grndpndr]

[Edited on 17-5-2009 by grndpndr]

On more careful observation of my product form ASA after recrystalization it appears that my yeild has dimminished more than it should have for pure picric acid. I used about 300mL of boiling water to put my 20g in solution(should have been more patient with additions probably would have taken less H2O).My yeild after letting stand for 24 hoursin solution, then vaccum filtering and drying with moderate convection heat was only about 14g. I think this at least 2g more than I should have lost if fairly pure sample(I know losses can vary bassed on impurities but this seems excessive)
The hygroscopic nature of my product would indicate greater solubility than a non hygroscopic sample(I think). If it is the trinitro-phenol sulphonic acid then this would explain a lot as the solubility in the 40% H2SO4 solution after dilution at the end of nitration would not be as great as it would be in the water during purification(I think). The problems with losses due to nitro-sulpho-phenol are disscussed a little in a couple places in Urbanki book one section on manufacture of picric acid. A couple methods in that section report loses of from 20-30%(of theoretical)they partly attributed these losses to the inability to completely convert all of the nitro-sulpho-phenol to Picric Acid(oxidation losses also accounted for some,and lower nitro phenols). This was with very refined processes, and expert procurment and care of reactants. I believe lessons may be learned from this that can be used when dealing with the trinitro-phenol-sulphonic acid when going from ASA. Is this nitro-sulpho as easy to deal with as the phenol version? (I would also like to point out that if my 20g yeild did have much nitro-sulpho in it, due to bonded water in that molecule(as illustrated in link on last post), then my mass would have been reading artificialy high. For every mole there is 4 moles of water bound according to that.
Since I now have probably 60+g Picric + Sulpho (if correct), it could probably be nitrated further to nearly pure Picric Acid, if I could find or figure out a process. As purification seems impractical, unless I am just lacking techniques for purification. At some point, as pointed out by others purifications becomes difficult, and sometimes impractical.(good solid nitration should be primary goal,most economic way!)
There may be other routes to Picric Acid from ASA but I believe this to be the usual. But there is a lot I don' t know. Any insite appreciated.

7 hours later
note:I have been making kind of a mess of this, the ideas are there but there are inconsistencies and mistakes through the last page. I believe that I have solved my problems or at least figured out what they are. I have more information, but rather than hammer through with fuzzy thinking and mistakes, I am going to wait do some reading, experimenting and writting things down. Then I will have a better chance of writting something concise and to the point.
I think we may be able to get a good handle on the personality differences between the ASA and phenol routes(pros, cons, etc).

[Edited on 10-6-2009 by Hennig Brand]

[Edited on 10-6-2009 by Hennig Brand]

Thank you for the information, the stuff in chemistry of powder and explosives is good stuff and I will keep it in mind. Actualy I was up till 2a.m. this morning doing another ASA go and I used only a two hour sulphonation, mostly out of lazyness, but after reading your post I am glad I did. I was also much more careful of the water, I verified that my H2SO4 was of at least 95% purity and I used a little less of my nitric acid(I thought originaly that by adding it in excess that I was doing the reaction a favor, but actualy once fully aware of water issue, I realized that by adding more than needed I was actualy adding more water to the mix. My nitric is measured at 90-92% by density, so that 8-10% water, but another thing it is kinda yellow cause I didn' t use vaccum or much gentle heat when distilling(in a rush). Dissolved nitrogen oxides can realy through off a density reading. e.g. in book 8 of encyclopedia of explosives and related items, I believe(same book that Picric Acid is in, n before p), it has some densities for different grades of nitric acid. White fumming 98% I believe is around 1.505 s.d., and the red fuming can be over1.59. Big difference, although I am unsure of all the implications. With practical knowledge a person could probably just look at the shade of the acid and tell a lot(I think). If my density was taken and used on white nitric tables what does that mean for my actual water content?
My yeild from my experiment was about 16g from 18g of ASA after recrystalization, which is a much better yield than last time. The reaction went totaly different. Color changes where very sharp. At first it was of course a purply, brown, blue or somthing then it went realy red, and after heating light again.(I think it went yellow but because of brown dye, (yellow plus brown does give a lighter brown I would think?) The product crystalized in beautiful large needles of a little darker yellow than my last experiment. It filtered and dried very easily(pure joy to work with)
When one adds Sodium Nitrate to H2SO4 there is no water produced (NANO3+H2SO4=NaHSO4+HNO3), to realy replace this one does need a nitric with no water( is this correct). I wonder if the power labs guy actualy tried his synthesis with 70% HNO3 and ASA? He did seem to try and compensate by useing a lot of the acid, but at 70% he is adding a lot of water to. In the future I am going to use HNO3 of strength and purity as good as I can produce. I haven' t gave a sample a whack yet because of torential rain storm all day, but the material looks good.
Rosco Bodine, I never realy known him to work with phenol when making Picric Acid(maybe he did and I didn' t see it). These reaction are not at all the same in their personality. There are similarites but that is as far as it goes. Phenol takes to nitration very easily and as a result water is not nearly as stiffling on the reaction. The end product seems to be quite different because of impurities, although if both went to absolute completion then they would of couse be the same,(pure TNP). Even with small yield the product from phenol seems better than a comparatively larger one from ASA(in my limited experience with phenol,(2 experiments)), however I have no doubt that some on this site can make a product from ASA that rivals any from phenol.
You are right about not letting it cool to much before nitration I believe(reaction seems to need a bit of momentum, several sources say to not let reaction temp dip below 100C during final stage, I presume to mantain this chemical momentum?
I get my pure aspirin very cheap as I have friends at the drug store, or they are at least friendly to my hobby(I am carful to always make my experimenting appear benign). A pound for 12-13$ canadian.
Ah the Monroe effect, I played around with that a bit a couple years ago when looking at home made claymore mines(just educational), cool stuff! I like shaped charges, but have never built one. I have played a little with different tampings and charge configurations though. I' ve made about half a dozen different nitric esters(ethers?) with very limited problems compared to these damn aromatic hydrocarbons.As well as peroxides (HMTD is the best in practise, regardless of what it says on paper, than AP) I also make a lot of my own chemicals(acids, bases, chlorates,metal powders, solvents, etc). I like improvising lab equipment as well, mills, stills, electrolisis cells,heating devices, modified vaccum for chemical use, magnetic stirrer, electronics and other.
I have seen those claims of super high yields with phenol as well, and while I don' t doubt they get it, I have also seen a lot of lab texts quoting yields not that disimilar from mine.
I would gladly tell you about the magnetic stirrer, even tell you how to obtain the parts. Maybe a picture and a discription should go somewhere?

What is PM?, do you mean just put in a post, or is it something else like email.(I don' t do a lot on computer other than look for info)
For starters though go to shroomery.org and look at the section on home made magnetic stirrers, thats where I got the basic idea. I don' t believe they had a speed control on theirs they just made it a slow managable speed by choice of power supply. A variable current or voltage power supply would be best, which is what I use(before chemistry I did a lot of home brew electronics). A small power supply from a model train set is variable output they usualy put out 16 volts or so which is over the 12volt specs on the fan motors, however as long as the output is not left wide open the current would not be enough to hurt the motor I wouldn' t think. Some small DC motors are tough as nails anyway, and this one has its very own worlds largest cooling fan! Distance from the fan motor to the attachment of the magnet will have to be determined through trial and error as the magnet strength and the distance will determine whether or not the magnetic field locks up the motor, or impeeds its function at low current(speed). Some sort of spacer will probably be in order. I used some PVC pipe the same size as the hub the blades of the fan attach to. The magnet could be held above the motor when running to see the effect on it at different distances and different speeds. The make spacer desired length. I ground a groove to seat the magnet in the top of the pipe, and hot melt glued it in place and also to the fan hub. A frame was made out of wood and small nails(as well as the casing piece the fan was attched to on the PS).The fan was taken off and put back on the opposite side so sides faced up, on yours it may be already right. The beaker with pill and some water can be held above the running fan/magnet at different speeds and heights to see what works best with your magnets. Remember as you get further away from a magnet the force becomes less, but also the lines of force change direction(my Dad told me this, he was a bit of a pyro in the fifties, I found some chems from the fifties, when he was a teenager, H2SO4, powdered metal). I got my magnet out of one of those perpetual flashlight, you know you shake like hell and get a little bit of light for a short time. Any way they are pretty cheap some times(full size name brand one for 7$ I think, 1/2 price). The magnet in them I believe is a rare earth magnet, strong, strong magnet. Probably too strong, but it is what I had. It is also not nearly as long as my pill(stir-bar), with gives me less torque, but the magnet is so strong I can hold the beaker away above and it works fine. To strong a magnet may cause extra pull and friction, but unless you are worried about burning out the motor or power supply, if for what-ever reason they are a little too weak, I wouldn' t worry about a little extra power consumtion.
I think it can be turned into a hot plate stirrer as well but I am still toying with it. I am looking at an old stainless electric skillet or something like that in my junk pile. Good stainless too, the kind a magnet don' t stick to! If the stirrer could be placed underneath this or something like this(maybe made of something else) and didn' t interfere with the magnetic field, I think it could work. The skillet/frying pan thing could be accuratly controlled with a big light dimmer, or something better and more professional if you wish.(something maybe with feed-back so you don' t have to be always adjusting temp a little?) Either water or oil would fill the pan, maybe evan sand depending on use. We will see how it goes.
I don 't know if all computer fans are DC but they must be. Avoid AC, it is very difficult to control unless the motor has brushes. Most times fancy power electronics are employed to change frequency of AC to moter(expensive). Some AC motors, like in some ceiling fans may be speed controlled with a light dimmer, but they are the anomoly, and are the appropriate power rating for the dimmer.
A DC speed controller can also be built, but most should not need to be reduced to that(unless they want).


[Edited on 12-6-2009 by Hennig Brand]

[Edited on 12-6-2009 by Hennig Brand]

I just wanted to say that I finaly have success with ASA route(although in small final yield). The last ASA experiment I did I told you I had 16g after one recrystalization, well after drying it seemed to melt well, burn well, look well, but it was still quite insensitive. It also seemed to not dry quite as well as it should(indicating presence of sulpho-phenol?). I did one more recrystalization and only collected the first 11g or so that came out of solution on cooling before it dropped much below 40C. I left the rest in the beaker and when it did come out, man what bad looking stuff(I believe floculant is the right word). Anyway this 11g of product dried in oven at 60-80C for hour or so and was tested and it seems to be about the quality of my sample from phenol(easily set of with quick snap of hammer on anvil, with satisfying crack). I need more work on my nitration obviously. As Grndpndr has said the product should probably almost be able to be set off right from the nitration. I think that if I can get a product that is decent after one recrystalization I would be happy though, which would also afford a better yeild. With more care to keep both acids strength at start of nitration up over 95%, the last stage of nitration would be much quicker, and would go more to completion before petering out. With even what I thought was a small amount of water the final stage of nitration goes on for hours, and even then never realy seems to complete. 11g from 18g of ASA, nothing to brag about, but I have a sample that is dry and a high concentration of TNP. For now I am happy.

Final note, when a nitration is such that it goes on for hours at 120C or near that, it is distilling of your precious nitric acid, leaving behind a mix with a higher concentration of water, and maybe even not enough HNO3 to do a complete job of final stage nitration.

Does anyone know if I could be damaging my Picric Acid in anyway by drying it in the oven at less than 80C? If still significantly damp when it goes in it may change the crystal density and stuff I think but I don' t know for sure. I don' t think it would change it chemicaly though(TNP is pretty tuff at those temperatures I think)
[Edited on 14-6-2009 by Hennig Brand]

[Edited on 14-6-2009 by Hennig Brand]

I'd also have to boil off the H2SO4 that was in there...but it does seem a little bit of a waste Ahh well.

This is more or less what I did right up until adding the ice when I found another member of the household had prepared a crushed ice smoothie . I will retry the synth at some point although I'm out of MeOH atm - my choice for removing the ASA from the tablets because it's cheap and easy to get hold of although a bit annoying because I had to evaporate it in a place devoid of any civilisation and in a good breeze. I could have used Meths but I wanted the colour changes to be as evident as possible, it being my first attempt at the synth and all, and the purple dye would have ruined that.

Thanks man, I would like to watch now but alas I am way out in the country and technology hasn' t found it' s way here yet. My dial-up is even slow for dial-up! Probably time to break for that satellite internet connection, it has come down in price a lot in the last few years. I will definately check it out when at my girlfriends, as she lives in the city and has the benifit of high speed. Maybe just let it download when computer not in use. Thanks and have a nice day

Quote: Originally posted by Hennig Brand

If one did have problems with oxidation would it be obvious at the end? Would there be just a mysterious loss of yield, or would it be very clear with insoluble products. In reading posts on the subject I have seen many times people talk of red,dark yellow, maybe some almost black resinous material which was very insoluble. I just wonder if maybe oxidation could acount for a loss or partial loss of yield and still maybe not be an obvious cause visualy?

I would refer you back to Rosco's experiments & his deductions on the subject. The "where, when" of oxidized product appears to shift. His conclusions of ASA as superior may, in fact have more to do with the starting medium (liquid) & it's responses to temperature in a magnetic stirrer (or without).
However it may also be a property of the oil of wintergreen itself & surrounding (additional) materials such as alcohol depending on where obtained. Such a thing may exist with ASA. Large Boluses for cattle have minimal binder of a easily extractable nature. Adulterants will ruin an experiment quicker than poor equipment.

ASA may be obtained in a known purity level and as a solid, it may have more consistency when exposed to a given temperature (the oil of wintergreen may separate out for a period during sulfonation).
I have seen successes vary with wool, horn, & indigo & the simple concept of their density may be a contributing factor in their usage (as a precursor).
Obviously the horn must be ground fine, the wool must also be of a powdered property, & so on. Or the black sludge of oxidation will be apparent sooner with higher temp than lower. But will exist more so than most any pure ASA. Frankly some of the finest light white-yellow TNP I have seen was an ASA lab.
{.....Which "popped" consistently with impact at a multi-milligram level.}
The whole issue of an powdered alkali nitrate used to obtain nitrogen, etc is a separate bedevilment... Those that may add greater nitrogen my not be the best for evolving a solution with H2SO4....

[Edited on 17-6-2009 by quicksilver]

Magnetic stirrers are a fine thing - that's for sure.
Occasionally, ammonium nitrate is just the thing for making a sold nitrate/mixed acid because it appears to "mix" well in your H2SO4 unlike sodium nitrate, etc.
So lets say you only source is "cold packs" (that are expensive); you can still get a good mixed acid from such a thing.
IF you can only lay your hands on KNO3, use something to drop the particulate to a very fine level (600mesh or 40um). You'll get a much better mix & a much better final product. This is where your $19.99 coffee grinder outshines the mortar & pestle.

There ARE some threads on making a magnetic stirring device but must people find that a mechanical stirring device (non-magnetic) can be rigged up to do the job as there are some stainless steel devices for mixing paint that, with a bit of fine tuning, will suffice. If you have a real one from a lab; treat it like a baby. Replacements cost at least $100+.

Agitation with air is feasible: I have seen it done with an aquarium pump and a vortex design for the insertion tubing.

Quote: Originally posted by Hennig Brand

I wasn' t really trying to be critical of the video and to be truthful I have only seen the first bit.

Recommend you see all of it, then be the critic. Alice cannot describe wonderland before traversing the rabbit hole fulget crucis mysterium

There are ways to make stir bars,procedures can be found in old lab texts. The one I have seen a couple times is to put something ferrous or magnetic in a piece of glass tubing and seal the ends by melting process. The teflon is probably the best but a substitute can be improvised or so it says in the books.
With regards to the stainless, I took one of those cocktail battery powered stirring devices(hand held), and replaced the cheap plastic stirring arms with stainless steel welding rods(tig rods). The cromium I believe or something else made a huge mess and produced this big fluffy precipitate that filled my beaker. And to make matters worse I couldn' t seem to get the beaker clean enough to keep the same thing happening even without the stirrer(it looked clean but wasn' t). I eventualy did get it clean and never looked back, now using only glass and teflon. It is good to point out though that there are many different types of stainless steel and some are probably very suitable for nitrations(I believe industry uses stainless in a lot of these sorts of situation). I just don 't know enough about the different metals, and was not sure that it would be cost effective, and would maybe raise some eyebrows if I order some exotic stainless. There may be some common stainless that I overlooked though, that would be suitable) . I have since rounded up some large chunks of teflon in the form of runners for snowmobiles(people do a lot of that around here) which could be cut/shapped into a paddle or something for the cocktail stirrrer. The batteries could be replaced with a small cheap (wall wort) power supply of suitable voltage, and speed could be controlled simply by using variable resistance between power supply and motor(remote control via cord). One of the main reasons I abandoned the regular motor stirrer, for the magnetic stirrer was abviously because the stirring contraption had to be used with something large enough to except the stirring apparatus and still give space to work while doing experiment. The rising acid vapors also were damaging to the stirrer(plastic, exposed metal, motor?), I could tell it would be an isue in the not to distant future(probably destroy the stirrer), I am sure there are ways of doing it though, and protecting it from acid vapors. The cocktail stirrer was only $5, so no big loss and it was a valuable learning experience. The magnetic stirrers seem much more versatile, useful and user friendly. And in my limited experience easy to improvise a descent diy model.
Coffee grinders are awesome, I use them all the time and have several for different uses. The last two I bought were about $10 each and were simple yet tough and practical. I always did powder my KNO3 for TNP nitration but a lot of the problems seemed to be in relations to the characteristics of the chemical itself and its products during and dealing with them after nitration, rather than with the partical size of the chemical when adding. I guess that could be a problem to, but I don' t know as I always powdered my nitrate as per Rosco' s instuction in his posts.

Note: when I was researching teflon I believe I found that it was at decomp temperature at about the same temp as melting, but that layers or pieces could be made to fuse without decomp at a significantly lower temp. This might prove useful(I experimented a bit but didn' t put much in and didn' t get great results). It is done however in industry routenly I think, whether or not teflon tape would work well I don' t know. Also there is much thicker teflon tape that can be bought, one example is the stuff used for gas lines instead of regular plumming(it is much thicker, good around stills too).

[Edited on 20-6-2009 by Hennig Brand]

[Edited on 20-6-2009 by Hennig Brand]

Quote: Originally posted by Rosco Bodine

But the purpose of it all being for the glorification on earth of a God who cannot be seen or measured with instruments, but is a matter for the heart to discern, is a concept which gives atheists indigestion, so they deride and ridicule the church.

IF we are just talking about yield levels then phenol is your choice. If such is not available ASA is fine. But any route than direct nitration will not get you what you may expect. This was the whole issue with R-Salt & RDX; the problem there being the precursors (acidic anhydride) being too tough to obtain for the synthesis of choice.
Plant-level synths are MUCH more efficient than anything one can do in a lab. The recycling of acids being a major issue. That's why items like CL-20 are so expensive.....they can't be plant produced via the re-cycle of their expensive precursors. The military STILL pays top dollar for CL-20. IF we were to deal with plant-level TNP one could even start with benzene. Plant-level TNT is so inexpensive that costs are ridiculous. That's why we still use it today.

Most fellows interested in energetic materials skip the reading about plant production, thinking they could never emulate it or compose a lab that would function in that medium. But actually, it can be done on a lab-dedicated level. It's a great hassle, yes. But IF the idea is to have enough TNP to make sand castles with - it could be done. Most folks could experiment till boredom with a few ounces.

Anhydrous acid is not needed for TNP. Use of solid nitrates is not just a hobbiest expedient method. Some solid nitrates have a greater nitrating effect than nitric acid, in anybody's lab. Urbanski charts the nitrating activity of various nitrates and it is not a fixed rule but can vary also with the thing being nitrated.

There is further I should share concerning the general "search for truth" by science or philosophy or religion with regards to intellectual honesty. It has been observed by me that there is a measure of agnosticism found in the humility of honest religious people, honest scientists, and honest philosophers, which is an intellectual honesty about the unknown, including things honestly recognized as probably being not knowable.
As an experienced observer who is familiar with analysis, mathematical proof, logical deduction, and reasonable conclusions, which are required for valid thinking, I personally know that a measure of agnosticism must
be present to keep ones feet on solid ground with respect to the ethic of intellectual honesty. The pseudo-certainty which emboldens atheists to proselytize a falsehood that science and religion are somehow at odds, venturing the false "belief" and proposition of atheism that science has exclusive claim to reason and rational perception and other noble virtues, while religion does not or cannot, and is only "superstition" has always been observed by me as lacking that reserve of agnosticism found to be always present with those who are intellectually honest. The certainty of "belief" of atheists about something which no mortal could be certain, even to an extreme of their venturing to redefine history which may not fit their belief so that history becomes more politically correct with regards to their biased view, is an indulgence not even allowable to science. Ironically, for their lacking the humility of agnosticism
any atheist has a bias which is intellectually dishonest and
provides that false confidence of youth which emboldens their ridicule of their elders (and their betters) for being
superstitious. Scientifically speaking, how do any of us know
that the entire realm of things which we know is not itself a
"science experiment" on a cosmic scale in which we are
unwitting participants ? If there can be no certain and definitive answer to that question, then what intellectual superiority could actually exist for anyone having the audacity to presume their own unproven knowledge or belief about any "meaning of life" kind of stuff is somehow an ignorance which gives them license to chastise people of faith as being "superstitious" or "unscientific". There is an inherent non-sequitur there which must be denied by all
irrational fanatics whether they are religious fanatics or
atheist fanatics or anything intermediate. Whether this same
rule also applies to any extra-terrestrial fanatics or extra-dimensional fanatics not covered by the preceding limits
would of course be pure speculation

Science and philosophy and science and religion are inextricably linked in the purpose of seeking greater knowledge and if that fact doesn't reside comfortably
with some individuals belief preferences, then they lack maturity. There is simply no honest intellectual basis
for bias and ridicule there concerning "superstition" than
there is for racial or gender bias. Men from earth in a spacecraft orbiting the moon were overwhelmed by the experience of what they were seeing and it was near Christmas as I recall many years ago when they got on their radio and began transmitting back to earth what they felt
compelled to be reading ......from Genesis. My family was
directly involved in that Apollo mission so I have a special
insight concerning the linkage between science and religion.



[Edited on 23-6-2009 by Rosco Bodine]

I applaud your perspicacity for recognizing that there are those among us who would push other peoples buttons
for sheer amusment, as if they were the walking incarnation of the left hand of an accordion player,
and the world was their polka

And your posts did not bore me, I just don't have time
right now to research the old posts or I would be more helpful.

Quote: Originally posted by quicksilver

ADVANCED PRACTICAL ORGANIC CHEMISTRY, J. Leonard, Lygo, & Proctor (especially CH 16 "What To Do When Things Don't Work) - saved my efforts many a time... It's inexpensive & many folks here have read it. I still have mine & that was a 1st edition. I go back to it every so often as it answer things like this so concretely & gives examples of how to set up an example for the use within a common lab. It's a paperback (cardboard back) & inexpensive. You'd love it; as it doesn't start off with useless material.

Appreciate both replys gents.497 HMTD was suggested as he has all the precursors for both the fulminate and the HMTD
which I wasnt aware of.The more i looked at HMTD the more I was impressed ,particularly the lack of that nasty ass Mercury.

Quote: Originally posted by 497

My suggestion would be HMTD. It seems to be far superior to AP in almost all aspects, especially initiating ability (not just in my experience, many others have said the same). Of course it is still very dangerous stuff, but no more so than AP or MF. I would imaging less the 0.5g would do the trick for TNP. I have found HMTD is best initiated by a small amount of pyrotechnic material coating a nichrome wire, rather than direct nichrome. Sometimes with a power source that is too weak or nichrome that is too thick, it can fail to DDT. Never had it fail by initiating with a "Solar Flare" igniter (used to start model rocket engines.) I'm sure a visco fuse would do just as well, but I don't trust them for large scale stuff. [Edited on 24-6-2009 by 497]

Federoff would have to be citing data for a reenforced cap and it will require a whole lot more to do the job.

Lead Azide or the azo-clathrate will work better. Picric Acid is relatively insensitive and not easily initiated, as is true for many nitrated aromatic compounds, being only slightly more sensitive than TNT to initiation. Styphnic acid is a bit easier to initiate and almost as powerful as TNP, probably on par with TNT, but more easily nitrated, synthesized. Initiation of these relatively insensitive materials is a task for an "unequivocal primary" especially in an unreenforced cap, and HMTD isn't one of those.

On a humorous note, cleverness can lead to a smile
of self-satisfaction which is similar to a cat that ate the canary scenario, however one should be watchful ....
as that may not be the end of the matter

http://www.youtube.com/watch?v=DkLwFfAwbts&feature=relat... Bill The Cat

[Edited on 24-6-2009 by Rosco Bodine]

Even a relatively thin steel tube has much greater strength than just about any common aluminum one, doesn' t it? Just how reinforced do you mean? Or is this way just not very practical? There really is just no comparison between aluminum and steel, as with the primaries I haven' t had a chance to play with the better ones yet. Time to dig up some azide! That stuff on clathrates looks nice, powerful and staight forward.
Thanks for the links and info in the last half dozen posts or so, it is very helpful to me.

Quote: Originally posted by Rosco Bodine

Federoff would have to be citing data for a reenforced cap and it will require a whole lot more to do the job.

Oddly enough, 0.05g reinforced cap, 0.06 unreinforced. For a non-unequivocal primary this seems wrong. (Page H84 )

Also interesting is the sand crush data, 42.5g for HMTD vs 16.5 for Hg fulminate

Perhaps it is an under-appreciated primary?

Still go with one of the unequivocal ones, and to add to rosco's suggestions: silver nitrotetrazolate.

[Edited on 25-6-09 by The_Davster]

Quote: Originally posted by 497

So maybe the instability issue is a little overblown?

There is a quite lengthy thread at E&W where I posted a bunch of historical patent references
http://www.roguesci.org/theforum/showthread.php?t=367&hi...
I never explored solvent recrystallization for purification to see what may be helpful there but that is a possibility
for experiment, as well as possible double salt formations which are sometimes a means of stabilizing an otherwise unstable material.

I try very hard not to do bad science nor report bad data,
and when I speculate or propose unknowns I generally try to identify that sort of qualified information for what it is as intuitive or hypothetical. The instability of HMTD is a fact for every sample I ever made and there have been quite a few.

The thread which Axt started about 2,3,5,6-Tetraazidobenzoquinone which evolved into chloranil and nitranilic acid related discussion could lead to some interesting experiments. I keep having to go back and take another look there so maybe I have an idea brewing subconsciously

The lead azo-clathrates definitely still bear further investigation and in my opinion are actually the most intriguing thing to arise, of lesser technical challenge than the energetic tetrazoles which are of course top of the heap. I pretty much said this same thing many years ago and so far anyway, it still holds true in my estimation.

The hydrazine nitranilate or some of the possible nitranilate complexes in possible mixture with lead nitranilate or other materials also has an interesting potential for experiments.

[Edited on 25-6-2009 by Rosco Bodine]