otonel
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KNO3,P, charcoal mixture
What is your opinion about that mix, can be more safety for storage and use than KClO3, S ,P ?
I make some experiments with a mixture made from KNO3 65%,K 20% and charcoal15% to find the friction sensitive with good result, but I want to know a
chemistry specialist opinion about that mix, especially how safety is in usage
Thank you.
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Bot0nist
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Anything containing potassium chlorate and sulfur is a huge no no. It is prone to spontaneous ignition as well as extreme sensitivity. I think the
formation of small amounts of chloric acid is to blame. In the presence of atmospheric moisture I believe a small amount of H2SO4 can be formed in
sulfur containing mixes. Add potassium chlorate and I think a little HClO3 could form, which is bad.
So, a mix with KNO3, P, and C would be much more stable ( read: less sensitive) than a phos., sulfur, chlorate mix. I bet it will burn significantly
slower though. Also, is the C necessary? Wouldn't the P cover your fuel needs. Unless the C is just a cheap filler.
Be careful.
[Edited on 28-2-2011 by Bot0nist]
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Zinc
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Be careful when using any mixture containing P, they tend do be very sensitive.
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woelen
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@Bot0nist: You warn about the KClO3/S mixing, but what is MUCH MUCH worse is the KClO3/P mixing. The latter is insanely sensitive. Just a slight tap
with a little branch or a small wooden stick (e.g. a small stick as used in ice cream lollies) on a KClO3/P mix causes it to ignite. In many cases
even diapering a mix of KClO3/P causes spontaneous ignition. This stuff is MUCH more sensitive than KClO3/S.
I also did some experimenting with KNO3/P mixes. These are less sensitive and I never had spontaneous ignition of such mixes, but still, they are
rather sensitive. Igniting such a mix is very easy, just keeping it briefly near a flame causes a fast whoosh, while a KNO3/S mix really must be
ignited by keeping it in a flame for some time. A mix of KNO3/P also ignites spontaneously when a waft of chlorine gas goes over it. A static
discharge, even a small one, also ignites such a mix.
Personally I am inclined to advice against the use of mixes of P and oxidizers. I see no reason why you would want such a mix. Phosphorus is more
expensive and relatively hard to obtain, when compared to sulphur and carbon. And besides that, such mixes are much more sensitive than equivalent
mixes with sulphur, probably so much that there is a serious risk of spontaneous ignition. In modern fireworks you won't find any phosphorus, simply
because of safety concerns.
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otonel
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Sensitive mixture i search to obtain but not as sensitive and dangerous like armstrong mix.I know any mixture with red P is sensitive to friction but
what I want to obtain is a mixture more safe to use,with long storage period and reliable to ignition another pyrotechnic material
I use charcoal made from napkins in mixture because I think that will give good ignition and rise the temperature, another option is aluminum powder
but that wasn`t available for me
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SB15
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Quote: Originally posted by Bot0nist  | | I think the formation of small amounts of chloric acid is to blame. In the presence of atmospheric moisture I believe a small amount of H2SO4 can be
formed in sulfur containing mixes. Add potassium chlorate and I think a little HClO3 could form, which is bad. |
Oxidation of sulfur in air produces trace amounts of polythionic acids, which decompose to yield sulfuric acid and sulfur dioxide. Sulfur dioxide
reacts with the chlorate anion to produce chlorine dioxide gas, which spontaneously oxidizes sulfur at room temperature. The reaction is exothermic
and auto-catalytic, as it generates additional SO<sub>2</sub>, in turn driving the production of ClO<sub>2</sub> from
KClO<sub>3</sub>. If this reaction is allowed to proceed for an extended period of time, it can cause the composition to auto ignite.
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The WiZard is In
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| Quote: Originally posted by Bot0nist | | Anything containing potassium chlorate and sulfur is a huge no no. It is prone to spontaneous ignition as well as extreme sensitivity. I think the
formation of small amounts of chloric acid is to blame. In the presence of atmospheric moisture I believe a small amount of H2SO4 can be formed in
sulfur containing mixes. Add potassium chlorate and I think a little HClO3 could form, which is bad.] |
Herbert G. Tanner
Instability of Sulfur-Potassium Chlorate Mixture: A chemical view
Journal of Chemical Education Vol. 36 No. 2, February 1959
Numerous amateur rocket enthusiasts suffered serious casualties from
premature sulfur-chlorate explosions, according to C. Burns (1). This is most
regrettable. These accidents should challenge elementry, chemistry teachers,
textbook writers, and civic-minded chemists to do their utmost to teach safety to
tyro chemists. Chemistry without safety is too frequently fatal.
The following exposition of the chemistry of sulfur-mixture is presented-with the
hope that the information will be conveyed to secondary school chemistry
students as a lesson in safety. Safety is not a series of "'don'ts," but is a matter
of foresight, with avoidance of hazards. In the discussion of the chemistry of
sulfur-chlorate mixture, an example of how safety can be designed into an
experiment is included for the benefit of the chemists of tomorrow.
Sulfur, by itself, is not a particularly reactive element at ambient temperatures.
Even in the finely divided state it is difficult to ignite. Similarly, chlorate is a
relatively stable compound at ordinary temperature. It decomposes only when
heated (2) almost to its melting point of 368'C. It is much less reactive at room
temperature than is pure oxygen, for example. These facts would not incline one
to predict that a simple mixture of sulfur and chlorate might ignite spontaneously
after being stored in a warehouse many months, or detonate when a fuse is
being stuffed into a
rocket charge.
World accident records for the past, century show that sulfur-chlorate stability
is erratic and unpredictable. This fact indicates that the mixture might contain a
concealed chemical trigger. A close look, particularly at sulfur, discloses this
trigger and the manner in which it becomes cocked.
There are two basic grades of sulfur—crude and refined. Sulfur produced at the
mine is called crude sulfur (formerly “roll sulfur"). About half of the world of sulfur
is extracted from the ground in
Texas by the Frasch process. Traditionally, this raw product is called crude
sulfur, even though it has the amazing purity of 99.8 to 99.9% sulfur. The chief
impurities asphalt which is present in the dissolved state. This mere trace of
asphalt makes raw sulfur difficult to burn on a large scale. Air oxidation at
ordinary, temperature is detectable only after period of months. Moisture in the
air assists this slow “rusting” process.
Refined sulfur is produced by distillation. The purist is obtained conditions that
cause the sulfur to condense directly too the solid state, i.e., the sulfur is
sublimed. The product , called flowers of sulfur, when freshly prepared has an
average purity of 100.0% sulfur. Even when both grades of sulfur are pulverized
to the same degree of fineness, flowers of sulfur oxidize more rapidly because its
surface is cleaner.
Polythionic Acid, the "Trigger"
Air oxidation probably produces sulfurous acid on the surface of sulfur, but this
acid has not been detected (3) because, as H. Debus showed, sulfurous acid
reacts quickly with sulfur to form polythionic acids beginning with trithionic acid,
H2S306. The latter adds sulfur atoms successively to form tetra- and penta-
thionic acids. These acids, particularly pentathionic acid (5), are responsible for
the fungicidal value of dusting sulfurs. Aqueous polythionic acids accumulate
until the concentration reaches a limit (6) where evaporation or a temperature
rise will cause partial decomposition according to the equation:
H2S3O6 = H2SO4 + S02 + (n - 2) S
The reaction is irreversible, but loss of polythionic acids becomes repaired by air
oxidation of sulfur when the temperature subsides. Reaction (1) is significant in
that a sudden increase in temperature can, cause a significant amount of sulfur
dioxide to be formed, not by direct oxidation of sulfur, but by decomposition of a
concentrated solution of polythionic acids. This event, however, must await the
formation of a concentrated solution of these acids.
Reaction (1) is responsible also for the accumulation of sulfuric acid on sulfur.
The sulfuric acid, being hygroscopic, favors additional production of polythionic
acids. By capillary action, sulfuric acid coats the surface of chlorate and
produces chloric acid. Although dilute chloric acid at ambient temperature is a
very weak oxidizing agent, its presence has given rise to the theory that chloric
acid is the primary cause of sulfur chlorate instability.
Sulfur dioxide will react directly with moist chlorate to produce chlorine dioxide.
S02 + 2KC103 = 2CIO2 + K2SO4 (2)
Chlorine dioxide immediately attacks, sulfur, the chief reaction being,
2CIO2 + 4S = 2SO2. + S2Cl2 (3)
Expressing reactions (2.) and (3) as one reaction.
S02 + 2KClO3 + 4S = 2SO2 + S2Cl2 + K2S04 (4)
Reaction (4) is a chain reaction because more sulfur dioxide is produced than is
consumed. Initiation of reaction (4) requires an extraneous source of sulfur
dioxide. This trigger is cocked by the growth of polythionic acids on the sulfur,
and is “pulled" when the heat from friction, impact, sunshine, the like is sufficient
to release a threshold amount of sulfur dioxide from the "reservoir" of polythionic
acids. Heat from reaction (4) quickly ignites a portion of the mixture, and, if the
gases produced cannot escape readily, the mixture will explode.
Popular formulas for preparing sulfur-chlorate mixtures generally specify more
sulfur than can be oxidized by the chlorate to sulfur trioxide. The reasons for this
are not pertinent to this subject, but it is important to note that the excess sulfur
increases the instability of the mixture by favoring formation of a greater amount
of polythionic acids.
This “trigger" theory was capable of explaining some previously baffling industrial
accident conditions, but it needed experimental confirmation. It predicted that a
chlorate mixture prepared with an oxidation resistant crude sulfur would be more
stable than one prepared with flowers of sulfur. Comparative tests were made
using ignition temperature as an index of stability.
Experiment A: 2 g of flowers of sulfur, 4 g of reagent grade chlorate, and 4 g of
cleaned and dried sand were intermingled on unglazed paper with a metal
spatula; 1 ml of water was added dropwise, and the mixing was continued. The
product was pressed lightly into a thin open-ended cardboard tube made from a
paper match-cover after the striker strip had been cut off. The tube was laid on
an asbestos board in an empty ventilated hood and was heated at approximately
1oC temperature rise per minute by a heat lamp suspended above the tube. The
temperature was measured with a thermocouple inserted to the center' of the
mixture. Ignition temperatures on repeat experiments ranged from 82 to 91oC,
and averaged 85oC.
Safety precautions that were designed into the above experiment include mixing
the powders with a metal spatula and the use of unglazed paper to reduce
accumulation of static charges. The powder was dampened primarily to give it
sufficient cohesion to remain in the cardboard tube, but the dampness no doubt
helped to suppress static charges. The striker strip was removed from the
match-cover because it contains a sulfide of phosphorus which might ignite the
mixture prematurely by contact with stray chlorate. Porosity, contributed by sand,
and the short open-ended tube all owed easy escape of gases, thereby reducing
the probability of an explosion. Both ends of the tube were left open to reduce
fire hazard by canceling rocket effects when the mixture ignited. Fire hazard was
further reduced by the asbestos board and by the emptiness of the hood.
Experiment B: Mixtures similar to those in Experiment A were prepared with
crude sulfur that had been pulverized until the particles had a mass median
diameter of 44 microns, thereby approximating the particle size of flowers of
sulfur. These mixtures ignited ,sharply at 124oC. This temperature is above the
melting point sulfur and indicates that ignition may have been initiated by sulfur
dioxide produced by air oxidation of hot sulfur vapor.
Experiments A and B definitely demonstrated the predicated greater stability of
the crude sulfur mix. However, the chloric acid theory could predict that the
greater sulfuric acid content of the flowers of sulfur, instead of the polythionic
acids, would cause the lower ignition temperature. As a matter of fact, the
flowers of sulfur contained 0.02% "acidity" calculated as sulfuric acid. The
acidity of the crude sulfur was detectable but was too small to titrate.
As a test of the "chloric acid" theory, Experiment A was repeated using flowers of
sulfur dampened with sufficient 0.2 N H2SO4 to give it an acidity value of 0.50%.
When this highly acidified sulfur was mixed with chlorate, an abnormal amount of
chloric acid must have been formed. In spite of this excess, the ignition
temperatures averaged only 87oC in close agreement with Experiment A. These
results dismiss the "chloric acid" theory as a primary explanation of instability.
Final confirmation that sulfur dioxide triggers the ignition was obtained by
repeating Experiment A, but. instead of heating the mixture, a long capillary
glass tube containing sulfur dioxide flowing at the rate of 0.3 cc per second was
thrust into the mixture. Ignition occurred almost as quickly as though the flame of
match had been applied.
Sulfur--chlorate typifies many fuel-chlorate mixtures. Metallic sulfides and
polysufides behave qualitatively like sulfur. Phosphorus cannot yield sulfur
dioxide, but at room temperature it evolves reducing vapors of phosphorus oxide
and possibly some elemental phosphorus which react so energetically with
chlorate that an explosion usually occurs before mixing can be accomplished.
Carbon disulfide, rosin, turpentine, thiocyanates, aldehydes, sugars, tannin, and
numerous other materials that form volatile reducing agents on heating,
contribute instability to chlorate mixtures. Powdered metals such as oily
aluminum, zinc, and magnesium are sometimes used with or without other fuels
in chlorate mixture. These metals are corroded by chlorate. Their chlorates are
hygroscopic and decompose at relatively low temperatures. The high heats of
oxidation of these metals could cause local temperatures sufficiently high to
ignite the mixture. No wonder such concoctions are unpredictable in stability.
Much of the unsavory reputation assigned to chlorate should be reassigned to
those who have selected the fuels. Apparently availability and cheapness,
instead of chemistry, have dictated the choice of fuels. Any fuel that is subject to
air oxidation at ordinary temperature, or forms an unstable chlorate, or produces
an easily oxidizable vapor below 100oC, or reacts with chlorate below 150oC
should be excluded. Starch (7) is a fuel that survives these requirements.
Literature Cited
(1) BURNS, C., J. CHEM. EDUC., 33, 308 (1956).
(2) BROWN, F. E., AND WHITE, W. C. 0., Proc. Iowa .Acad Sci., 31,291(1924).
(3) MELLOR, J. W., "Comprehensive Treatise on Inorganic and Physical
Chemistry," Longmans, Green &, Co., Inc., London, 1947, Vol. 10, pg. S8.
(4) DEBS. H., Ann.. 244, 76 (1888),
(5) YOUNG, H.C. AND WILLIAMS ROBERT, Science, 67, 19 (1928)
(6) MELLOR, J.W. "Modern Inorganic Chemistry," Longmans, Green & Co., Inc.,
London, 1916, p. 458; EPHRAIM, FRITZ, "Inorganic, Chemistry," Gurney and
Jackson, London, 1926, p, 463.
(7) TANNER, H.G. U.S Patnet 1,966,652 (1934)
----
See also —
Chapman & et al
Studies on the Thermal Stability and Sensitiveness of Sulfur/Chlorate Mixtures
Part 1 Introduction. Journal of Pyrotechnics 6:30-35. Winter 1997
Part 2 Stoichiometric Mixtures. Journal of Pyrotechnics 7:51-57. Summer 1998.
Part 3 The Effects of Stoichiometry, Particle Size and Added Materials. Journal of Pyrotechnics 11:16-24 Summer 2000
Part 4 Fireworks Compositions and Investigation of the Sulfur/Chlorate Initiation Reaction. Journal of Pyrotechnics 12:43-51 Winter 2000
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Bot0nist
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Thank you so much SB15 and The Wizard. I am jumping into that literature first thing, and I apologize for speaking on a subject that I was not
knowledgeable on. I knew chlorate + Sulfur was bad, just not why.
On another note, I love this place! I have learned more than I ever thought possible in the last week just by lurking in the forums. I admit that a
gross amount is over my head though. I really like the "we know our shit" atmosphere, and the fact that you all don't suffer the k3wl_ kids or the
shit cooks here anymore.
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metalresearcher
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Just tried the following mixtures (1-2 grams):
- KNO3 + S : needed a Bunsen burner to ignite: VERY slow.
- KNO3 + S +C (black powder) : hardly lit by lighter but self sustaining
- KNO3 + sugar: can only be lit with bunsen burner and not self sustaining and very smoky
- KClO3 + S (mixed slowly within fumehood because of possible spontaneous ignition) : lit by lighter , rather slow but faster than KNO3, blue flames
- KClO3 + sugar : very fast burns with purple flame, filled the fumehood with smoke
Fortunately I have no P
So KClO3 is a much better (and more dangerous !) oxidizer , NEVER mix with P and NEVER use it for firecrackers.
Making you own firecrackers is a bad idea anyway, lots of prople lost some fingers or even eyes.
I use this only in small quantities for reaction speed and flame color tests.
[Edited on 2011-2-28 by metalresearcher]
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otonel
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Is very good to know about how dangerous is potassium chlorate mix, but if that stuff is very dangerous like in that description why matches don`t
self ignite and potassium chlorate sulfur mixture was used in priming mixture for a long period with good result. The secrets in my opinion is anti
acid used is mixture like chalk or gelatin glue used in manufacture process and waterproof container.
Anyway I open that topic to talk about KNO3/ P mixture more safe than KCO3/ P , and about potassium chlorate was a lot of topic with discussion.
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otonel
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| Quote: Originally posted by metalresearcher | Just tried the following mixtures (1-2 grams):
- KNO3 + S : needed a Bunsen burner to ignite: VERY slow.
- KNO3 + S +C (black powder) : hardly lit by lighter but self sustaining
- KNO3 + sugar: can only be lit with bunsen burner and not self sustaining and very smoky
- KClO3 + S (mixed slowly within fumehood because of possible spontaneous ignition) : lit by lighter , rather slow but faster than KNO3, blue flames
- KClO3 + sugar : very fast burns with purple flame, filled the fumehood with smoke
Fortunately I have no P
So KClO3 is a much better (and more dangerous !) oxidizer , NEVER mix with P and NEVER use it for firecrackers.
Making you own firecrackers is a bad idea anyway, lots of prople lost some fingers or even eyes.
I use this only in small quantities for reaction speed and flame color tests.
[Edited on 2011-2-28 by metalresearcher] |
You can find some red P in strip of matchbox and with some acetone you can scrape some RP which is stabilized red P for use in experiments
KNO3 + P burns quickly with smoke, and if you strike mixture with hammer blow
My new experiment was :KNO3 40%, PbO2 20% P20% Al 20% which is more sensitive than KNO3/P and is was I search a sensitive mixture for percussion rod
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Bot0nist
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I have always found that KNO3, C, S mixes(BP) only preform well when ball milled for a bit. I have had great luck without a ball mill by using a
mortar & pedestal for a long time (hours while watching TV). I had lots of fun making mini-rockets by casting it wet, and it even works great for
bursting shells. Though it doesn't really throw the stars well unless you coat it on some broken bits of hay or granulate it with a screen.
If you don't mind me asking, why the phosphorous anyway? Just to experiment on sensitivity? It's expensive (or a pain in the ass to obtain), its
apparently sensitive, and i think its toxic. I've had luck with a lot of other fuels combined with potassium nitrate. Like powdered sugar. Just add
sulfur to decrease the ignition temperature. Use a little stoichiometry and controlled experiments to get the perfect ratio. You can even add some 300
or so mesh silicon (Si) to the mix to increase the heat emitted and broadcast little drops of red-hot molten glass, which greatly enhances the
composition's ability to be used as initiating device. I have even successfully ignited thermite mixes using similar blends. Had to mix a bit with
some of the thermite, of course.
[Edited on 1-3-2011 by Bot0nist]
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gregxy
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Otonel,
I don't think you will find out much here that you could
not get from the chapter on primers in Davis.
Many of the "safety" rules (like never mix chlorate+sulphur)
were developed for handling large quantities where rough
handling or internal heat buildup could set them off.
For your application tiny amounts are needed so this is
much less of an issue. Unfortunately a percussion prime
needs to be very sensitive so an "unsafe" mixture
is needed... Since you can wet mix there is not much
danger during the preparation phase.
At least chlorate mixes are safe when wet
mixed. Azides, fulminates etc remain sensitive when wet.
KNO3 + red P + charcoal sounds like a good composition.
Since the starting materials that you have are limited and
of unknown purity your best bet is to experiment.
The main danger is a cap could go off
when you press it on the nipple. I suggest you test for
this by leaving the BP out of the cylinder, placing the cap
on the nipple and vigrously twisting it while pressing with
a wood dowel. You can then reduce the sensitivity by
reducing the red P if needed.
I have a BP revolver and it kind of worries me when I put
the caps on the nipples that one could go off, and I have
commercial caps. Alway point your gun in a safe direction
while loading.
To test for stability put a cap in a plastic jar with a couple
drops of water an bake it in the oven at 150F overnight
then see if the cap still works. Stability problems in primers
typically result in misfires.
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The WiZard is In
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| Quote: Originally posted by Bot0nist | Thank you so much SB15 and The Wizard. I am jumping into that literature first thing, and I apologize for speaking on a subject that I was not
knowledgeable on. I knew chlorate + Sulfur was bad, just not why.
On another note, I love this place! I have learned more than I ever thought possible in the last week just by lurking in the forums. I admit that a
gross amount is over my head though. I really like the "we know our shit" atmosphere, and the fact that you all don't suffer the k3wl_ kids or the
shit cooks here anymore. |
The French chemist Fourcroy described potassium chlorate
as a compound seeming to contain the elements
of the thunderbolt in its molecules, and in one in
which nature seems to have concentrated all her
power of detonation, fulmination, and inflammation.
djh
----
Accidents in Thawing Dynamite, One killed.
Cartridge left in pocket of trousers which were
hung before a fire to dry.
Courtenay De Kalb
Manual of Explosives : A Brief Guide for the use of Miners and Quarrymen.
Ontario Bureau of Mines 1900
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otonel
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My try to make priming mixture is based on reading some invention patents where oxidizing agent is barium nitrate but I don`t have that chemical and I
replace with potassium nitrate
I search for that documents and attach
Attachment: priming mixture patent .pdf (222kB)
This file has been downloaded 1318 times
Attachment: Frankford arsenal research.pdf (384kB)
This file has been downloaded 651 times
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Bot0nist
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You could synthesis some Ba(NO<sub>3</sub><sub>2</sub> if
you get some barium chloride. I imagine its pretty cheap. A pretty simply metathesis that would precipitate barium nitrate and leave potassium
chloride in the solution might work. NaNO<sub>3</sub> may be better than KNO<sub>3</sub> for this though.
<a href="http://www.skylighter.com/mall/chemicals.asp?Sort=B" target="_blank" > Cheap Barium Chloride and Nitrate</a>
<a href="http://unitednuclear.com/index.php?main_page=product_info&cPath=16_17_69&products_id=616" target="_blank" >Cheap Barium
Nitrate</a>
These are probably only applicable in the states, I'm afraid.
[Edited on 2-3-2011 by Bot0nist]
(Please use one post for cont. information. Moderator)
[Edited on 2-3-2011 by quicksilver]
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bearcreek
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otonel,
Your has encouraged me to join after a few years of lurking. Gun propellants & primers are my 2 areas of work with energetic materials. I've tried
dozens of different primer compounds. Wish I could easily buy red phosphorus.
Your KNO3, P & C mix would be somewhat insensitive & not the best for use with many modern powders. While it does produce good amount of gas
the temp is very low.
Temp 1338K
NUMBER MOLS GAS AND CONDENSED= 1.7069 0.2380
Your KNO3, PbO2, P, Al is better & would be more sensitive.
Temp 2473K
NUMBER MOLS GAS AND CONDENSED= 1.0849 0.3707
One version of the new P4 primer that the US Army is testing(the patent you attached) is:
KNO3 64.8%,P 25%, Al 5%, TNT 5%
Temp 2005K
NUMBER MOLS GAS AND CONDENSED= 1.4697 0.0927
or
KNO3 64.8%,P 25%, Al 5%, PETN 5%
Temp 1963K
NUMBER MOLS GAS AND CONDENSED= 1.4082 0.1126
Also, you are going to want to add a little binder(gun or dextrin) to them to get them. That makes them more sensitive & reliable. To test for
sensitivity a steel ball of a certain size is dropped onto a loaded primer. At a certain height 0% should fire & at a certain height 100% should
fire. If you want info on testing I will try to help.
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otonel
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Thank you bearcreek, you help me with a lot of information, which help me in my research.
I try to find barium nitrate to buy but what I find was barium sulfate and I need some help to easy make barium nitrate from barium sulfate, I think
best option is to make first barium chlorine
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Bot0nist
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You mean barium chloride? Can you place online orders? Its pretty easy to find.
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