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grndpndr
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I understand your thinking i believe and while i assumed 3/16 there were actually 2 diameters of AL tubing used, 3/16-5/16 having no notes just
running on recollection had thought 3/16 but as there s no 5/16 left i know wonder as the old cotton? woven tar covered blasting fuse easily made a
slip fit into the tubing so more than likely the tubing was 5/16 or the cap likely would have been to long for the uses.
Only undeniable fact was the incredible power/brisance difference between simple FM cap
and the compound caps with 1-2gr TNP.The OD of the mil special cap is interestng at approx. 1/4 with the actual contents maybe 11/4 lenghth he 56.25%
wil fnd ts way into notes. Thanks.
PS; Is anyone aware of concave end blasting caps?Wouldnt be terribly difficult to duplicate except placing precisely focusing the jet to be centred in
the HE.
PS;closer inspecton revealed the tubing in queston to be 5/16 ,the cost of aging eyes..310 OD/.265 ID,more appropriate dia. for the cap in question?
[Edited on 25-5-2008 by grndpndr]
[Edited on 25-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr]
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grndpndr
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| Quote: | Originally posted by grndpndr
I understand your thinking i believe and while i assumed 3/16 there were actually 2 diameters of AL tubing used, 3/16-5/16 having no notes just
running on recollection had thought 3/16 but as there s no 5/16 left i know wonder as the old cotton? woven tar covered blasting fuse easily made a
slip fit into the tubing so more than likely the tubing was 5/16 or the cap likely would have been to long for the uses.
Only undeniable fact was the incredible power/brisance difference between simple FM cap
and the compound caps with 1-2gr TNP.The OD of the mil special cap is interestng at approx. 1/4 with the actual
contents maybe 11/4 lenghth he 56.25% wil fnd ts way into
notes. Thanks.
About purifying ASA,Ive used OTC HEET methanol based gasoline antifreeze slightly warmed at least a dozen times w /o any problems as described
w/acetone or isopropyl.With the crystals solidifying crystal clear.And finished TNP perfectly
nitrated and purified w/o a trace of impurities.
The pint bottles are adequate for up to 200x325mg tabsIIRC.
PS; Is anyone aware of concave end blasting caps?Wouldnt be terribly difficult to duplicate except placing precisely focusing the jet to be centred in
the HE.
PS;closer inspecton revealed the tubing in queston to be 5/16 ,the cost of aging eyes..310 OD/.265 ID,more appropriate dia. for the cap in question?
[Edited on 25-5-2008 by grndpndr]
[Edited on 25-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr]
[Edited on 26-5-2008 by grndpndr] |
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Sickman
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If I remember right, I remember Rosco Bodine mentioning that he got a descent yield of TNP using fertilizer grade sodium nitrate which had been
purified by a method that he didn't mention IIRC. There are several different brands of sodium nitrate, usually seen OTC as "nitrate of soda". I'm
wondering if someone or he may know what are the most common impurites in such sodium nitrate fertilizer and how best to purify it. Sodium nitrate is
not only useful for TNP nitrations, but also for several nitric esters, details of it's purification from the OTC fertilizer grade would be useful
info.
If I understand it right the usual impurities include several trace metals, along with some salts. Has anyone here found a method of purification that
boosts the purity of the NaNO3 to a level of purity acceptable for such nitrations that allow a pure product to precipitate without any significant
side reactions due to impurites found in the sodium nitrate?
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grndpndr
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Ace hardware;4lb sacks of nitrate of soda 15-0-0,nice white prills.IIRC the amount of sodium nitrate was reduced from 77
gr pott nitrate to 57gr sodium nitrate in a synthesis similar to the one mentioned previously.Ive used this fert.grade sodium nitrate w/o any problems
synthesising picric acid .In my experience( shadetree experimenter) its been a tough synthesis to mess up as long as adeqaute time and heat are
allowed to dissolve clumps + sulfonate ASA.The only failure was the first,self induced I washed the brilliant picric acid crystals with distilled
water until my yield was near gone not realizing the picric acid was dissolving down the drain.LOL no doubt that it and subsequent synthesis were
succesful when comparing the brisance to AN/NM 75/25 while impressive, the picric acid was far more effective against target plates and made a heck of
a composite detonator and suitable for SC as long as the TNPs density consistent and near optimum.
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12AX7
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| Quote: | Originally posted by grndpndr
Ace hardware;4lb sacks of nitrate of soda 15-0-0 |
Really? It certainly doesn't show up online..
http://www.acehardware.com/search/index.jsp?kwCatId=&kw=...
Only bicarbonate of soda, nothing else. Specific to your store?
Tim
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Rosco Bodine
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look in bag products, small , soil conditioners
Seek, and ye shall find
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grndpndr
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You should be able to order nitrate of Soda any time of year from ACE.If there not helpful google mastrgardening they have the same in 2x4lb sacks for
$21 shipped to the midwest.As to purifying it takes fire as easily as drug store Pott nitrate so purfying ive never found nescery for TNP at
least.They come as bright white prills w/o any apparent coating and 15-0-0 is the max for nitate of soda.Most Importntly Ive never encountered failure
with the stuff as is.
In fact my first failure w/TNP was recently using ACE crude oil black santeen H2S04 drain cleaner.What a mess,no color changes could be oserved
through the coal black sulfuric yes it was better than 95% no oxides on addittion of the nitrate just a chocolate brown foaming the few off yelow
crystals that were recovered were very large for TNP as well as having a yellow brown hue not the normal canary yellow.Its not the materials so much
as it was still a learning experience,#1 go back to batt electrolyte, cheaper and crystal clear after reducing to 95%-
98%. 2x 2.5l carboys are available through auto supply out here s well as a full 5gall 33.3% H2S04 resuting in crystal clear H2S04 of about
20-30wieght oil cheapr than drain cleaner.Also found very inexpensive ASA by the pound vetrinary pure which is good enough for human consumption
googling Vet supplys.Much better and cheapr than purifying $
drug store ASA.Mastergardning also carrys 4lb sacks of 45-0-0 Urea
but it could use purifying with water and filtering to rid it of dirt/other matter
Off topic but humor me if you would, Ammonium picrate came to mind as a family of primarys/ booster/ in dual comp caps but the cost of ammonia
required for ammoniun picrate econdarys put me off! Any alternate synthesis not so ruthless with ammonia consumption?
[Edited on 14-10-2008 by grndpndr]
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hashashan
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ammonium picrate as a primary/booster??????? it is unbelievebly inert
this is composition D and it is used industrially as the explosive of bunker busters, it is so inert that it is capable to withstand a close explosion
without detonation.
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grndpndr
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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]
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mormanman
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I don't want to sound like an idiot again but I've tried that synthesis and I just won't dry. Some will but only flakes. I burns very fast so I know
it works but I just won't dry.
What do you suggest?
Its TNP by the way.
[Edited on 2-12-2008 by mormanman]
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Leander
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You've probably forgot to wash or recrystallize your product properly. This way some sulfuric acid remains in your crystals, wich prevents drying.
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mormanman
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How do I was it then? I boiled it in the distilled water filter it. I'll read up on it. Thanks for telling me where I should start looking though.
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Leander
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Simply dissolve your TNP in a minimal ammount of boiling water, then cool to ~0oC, filter, dry. This method should get rid of the acid. Usually the
only method that yields TNP that doesn't dries at all, is when you filter it strait from the mixed acids and then dry without washing at all.
Unsufficient washing though, gives crystals that remain 'sticky' and form little lumps quite easily.
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grndpndr
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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.
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quicksilver
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If one is not working with TNP to begin with then there be problems associated with attempting to yield a detonation with a lower nitrated phenol (or
materials thereof). There is some extremely old literature* that had a very interesting test. Back in the day when MP tests were very inaccurate there
was a simple determination for whether the (PA) final product had a greater or lesser percentage of DNP in it. A high percentage TNP will detonate
from steel on steel impact: Dinitrophenol will not. Folding a few mg of one's final picric acid in a bit of aluminum foil & striking it upon a
heavy steel surface w/ a heavy steel hammer will result in a moderately loud detonation.
Majority of TNP has some DNP in the final product (that is what throws off the mp tests from those who have access to a fairly good one). But the
"hammer blow" test has yet to fail. If one's sample reacts to a blow of steel upon steel a good bet is that it has majority TNP. DNP can be very light
yellow & in all respects a useful material but will NOT respond as picric acid. Often due to the lengthy process & large level of fumes, the
proper level of nitration to reach TNP is not achieved. The resulting DNP/TNP material will not respond the way it should in other labs that demand
true PA.
* Weaver, Military Explosives, 1907
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grndpndr
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Thanks for the simple testing method!
As Ive never had any 'clumping' problems with the
sod /pott nitrates just the asa 'clumping' requiring time to sulfonate Ill stick with the inexpensive
sodium nitrate.Id prefer AN but as I can only find it online or in 2to4oz cold packs its far to expensive when the cheaper fertilizer grade nitrate of
soda is available.
"High Yield" man. nitrate of soda of 16/0/0 in 5lb sacks economically rather than ace 'mastergarden'/Bonide brand 15/0/0 4lb sacks.
More nitrate less fillers?LOL
[Edited on 12-3-2009 by grndpndr]
[Edited on 12-3-2009 by grndpndr]
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Zinc
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A few days ago I made some picric acid (at least I think). To 200 ml of conc. H2SO4 (boiled down battery acid) I added 25-30 g of ASA (extracted from
Aspirin pills) and started heating it in a water bath. The mixture than turned dark brown. When the ASA dissolved I added 70g of mixed ammonium and
sodium nitrate (don't know the proportions of NaNO3 and NH4NO3 in the mix) in several portions. Then the mix turned orange/red and then orange/yellow.
After that I continued to heat it on a water bath for around 30 min. Then I removed the heat and let it coll down. After it cooled down yellow
crystals and some hard yellow chunks precipitated from the solution. I then diluted the solution with water. The crystals floated and the yellow
chunks remained on the bottom. I then filtered only the crystals, dried them and recrystallized from water. They formed nice yellow needles. Then I
filtered them and let them dry and crushed them up (so they dry faster).
Now when the picric acid dried (over night) I tried to ignite a small amount with a torch. At first it melted and then burned but quite slowly and
weakly. I thought it should burn faster and without melting so is there anything wrong with it? Perhaps the ASA didn't fully nitrate?
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User
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Well my techgrade PA flashes with dark smoke upon ignition, alltough i have to say its not a real schoking deflagration.
How long and at wat temp. did you do the sulfonation/nitration?
This is very important for the full conversion to PA , working on a benzene ring takes some efford.
What a fine day for chemistry this is.
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grndpndr
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I tried several times with mine melting a small amt in a spoon then heating until melting then it would rapidly deflagrate with a small pop with a
resulting black soot airborne.I never encountered clumping but otherwise
sounds successful.Color,during and after synthesis, crystaline structure sounds OK.
MF always detonated comp. picric caps and the brisance seemed
far and away superior to 70/30 AN-NM. Follow the direction to recrystalize with dist water and you shouldnt have any problems with drying,its just the
acidic nature of the beast thats a pain.Also keep away from most metals.
Mine behaved very similarly to the above but i used aspirin
and OTC fert nitrates and SA drain cleaner,sometimes concentrated fresh electrolyte.
[Edited on 14-5-2009 by grndpndr]
[Edited on 14-5-2009 by grndpndr]
[Edited on 14-5-2009 by grndpndr]
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Zinc
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Then sulfonation/nitration lasted around 45-60 min, perhaps a little longer. The temp. never was over 100 C (heated it in a water bath), except for a
short time at the beginning of the reaction (I heated it a few minutes on an open flame so the ASA dissolves faster) and at the end of the reaction
(after all the nitrates were added and dissolved I also heated it a few minutes on an open flame).
I forgot to say that the H2SO4 had a small amount of I believe lead particles floating in it (only a small amount). So probably some lead was also
dissolved in it. Could that cause a problem?
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User
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Well it could lead to the formation of leadpicrate, which makes your product unpredictable.
But still i cant really imagine it ruining the product.
My lab notes recall something like leaving de ASA in the nitrating mixture till the next morning.
I do these things rather late and tend to go to bed afterwards.
I think your product just isnt fully nitrated.
If the sulfonation isnt fully finished the nitration also takes longer, I cant find the data backing that up.
What a fine day for chemistry this is.
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quicksilver
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[Please see my previous post]
I would only re-iterate that impact testing was of value during the turn of the 19/20th century to determine the very rough level of true TNP from DNP
back before MP testing was exacting enough to determine levels of nitration. While DNP will form lead picrate just as TNP, it is only TNP that will
detonate at the milligram level via weight drop testing (or a tiny amount enclosed in foil, struck w/ a hammer against a steel anvil)
If one does not have access to a quality MP test apparatus; striking a "match head" level amount will detonate - should the product be of great
percentage - TNP.
DNP just won't perform in detonation via impact at that level of material. The problem of both DNP/TNP existing in the same nitration is quite common
& both will perform in making picrate salts as well as secondary detonation from sufficient primary initiation. However this is a test of such
crude measurement, one may have a combination of DNP/TNP to as high as 20% DNP.
I have found no late 19th century testing that would yield a conclusive result of "pure batch TNP". The problem of melting point testing without a
quality lab-level machine is that to achieve conclusive temp measurement with something like a thermometer, the volume/weight level would need to be
too dangerously high. I have seen very small weights of TNP detonate vigorously when struck with a steel hammer on steel anvil consistently &
questionable samples did NOT respond to this stimulus. Yet those same questionable samples yielded lead picrate; indicating the presence of nitrated
phenols....
I did a short search of old literature, hoping to find some other method but I couldn't find any that would put the lab at a realistic purity level of
above 80+%
[Edited on 14-5-2009 by quicksilver]
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grndpndr
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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]
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quicksilver
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I remember back in '06 that a gentleman here made it from Oil of Wintergreen; I've seen it made from Indigo - & successfully.
I totally agree, it's hard NOT to make TNP. It may be one of the more "flexible" higher nitrations. To purify the aspirin easily, make a paste from
the materiel [the solvent] at or above 80C prior to a slow filtration (again at such or higher temperature) so that the binders are removed to a
greater degree.
However if one is using a solid nitrate to create a mixed acid, make sure that material has been brought to complete solution & maintain control
of a sulfonation [that is thorough]. When someone has trouble with TNP often it comes back to a sulfonation that is incomplete.
If I didn't care about the stench, quite honestly I think I could even make horn or wool function because once you get the little indicators correct
it's kitchen chemistry.
It's an interesting question however that of using a battery electrolyte with lead material exposed therein. Just my opinion; but I would need to make
that decision depending upon the condition of the material and how much lead is actually broken down within the salvaged material. It could be a real
mess that has time & condition enough to go into solution. Is drain cleaner that difficult to get?
However on that note I would think over using a material (unintentionally) that brought lead into that lab. It's all too easy to loose sight of what
the material is & can do. {Very bad pun; sorry.} A possible mistake here is no joke.
The introduction of lead could definably be a very serious hazard. It has been the major source of factory travesties in the distant past.
[Edited on 17-5-2009 by quicksilver]
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grndpndr
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Used battery electrolye is probably a bad Idea.New 35% electrolyte can be ordered at most parts stores relatively inexpensively.I believe another
advantage to a clear H2SO4 is you can observe the progress of the synthesis through color changes maybe an equally important indicator than time/temp
alone?
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