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Bert
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Thank you for posting pictures, but they are not clear and well lit enough.
Re-take just the one showing BASE of cartridge, well lit and detailed enough to see any small scratches , marks, differences in curvature of primer's
edges.
Rapopart’s Rules for critical commentary:
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Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hennig Brand
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These should be a little better I think. The one on the right held the homemade propellant. There is a little bit of fresh brass exposed in one spot
on the casing which held the homemade propellant.
 
[Edited on 30-1-2015 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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franklyn
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@ Hennig Brand
" This morning I dug out a 30-06 Winchester rifle "
Now there's a good prepper 
" larger average particle size could have been the cause of lower performance "
Likely yes , you have not disclosed the milling methodology and subsequent sifting to achieve uniform grain size. This is
the most important step since very slight change in particle size will greatly affect the burn rate. Uniform granular consistency is your goal to
achieve consistent equivalent performance.
=> If you take any spectrum of granular material such as gravel inside a container and agitate it , the larger particles rise to the top and the
smaller settle to the bottom. This action with nonuniform propellant will cause wider erratic performance.
" there did also appear to be more dark colored fouling in the cartridge which held the homemade propellant "
larger than average particle size will result in leftovers.
You have produced a quality substitute for the commercial product as your testing concludes. What more can one want. Kudos !
@ Bert
" The test you described made my hair stand up "
Well , if you fire die cast zinc Saturday night specials it might.
" Did case head flow brass into the gun's extractor cut out "
Jeez Bert, 20 % less weight of lower bulk density propellant isn't anything close to a proof load.
as Hennig Brand states :
" Since the homemade propellant was 60-40 double base, flake propellant, it was decided that a lighter load should be tried first."
" Your uncoated grains are likely degressive burning "
What matters is that the burn rate is way up consistent with pistol type powder. The area under the time / pressure profile
determines the energy. Neglecting for the moment details like bullet seating depth and head spacing.
"Another factor in unburnt powder: A too large / non uniform grain size."
In that we can agree
.
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Hennig Brand
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I have been meaning to screen the flakes to separate them into different sizes. With the .22LR tests I did use a stainless steel kitchen sieve to
collect fines which were used for those tests. For the 30-06 test everything was used (no separation). The propellant was poured out on wax paper in a
thin layer (viscosity and layer thickness controlled by the amount of solvent/acetone used). Before the acetone had all evaporated (propellant about
the consistency of fruit leather) a multi blade rolling cutter was used to cut it into flakes. The degree of particle size reduction was determined by
eye and experience. Sieving the particles with a sieve stack would be a great way to separate the various particle sizes and greatly increase
uniformity. Using a set of adjustable rollers, as suggested by Bert, would be more ideal as well to regulate flake thickness.
Thanks for the compliments Franklyn and also to Dornier 335A who I forgot to thank earlier. The propellant is a bit crude but it does work amazingly
well. I was amazed at how close the muzzle velocities were, in the 30-06 test, considering the large difference in powder weights used.
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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Bert
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Franklyn- look for my PM.
Making a functional double base propellant AT ALL is more than most amateurs will ever achieve. Working to accurately characterize it (and reliably
replicate performance, batch to batch) is an order of magnitude beyond this.
I agree that the home made 60:40 powder is likely closer in performance to a fast burning pistol/shotgun powder than IMR 4895. Which is why up thread
I suggested a small volume case and a cast bullet, fired in a strong single shot rifle.
The total area under the pressure curve isn't what worries me.
The HEIGHT of that peak, worries me, especially right at the beginning, before inertia of projectile is overcome-
I have fast, 30% NG content powders on my shelf that will CERTAINLY flow brass at case head, can perforate a case/rupture a primer and may damage or
break a 30-06 rifle action (depending on type) with a 2 gram (31 grains!!!) charge under a 150 gr jacketed bullet. Total energy may be less than the
48 to 53 gr of 4895 I would probably use in such a rifle. BUT THAT DOESN'T MATTER.
Ironically, I also have slow burning powders that can damage a Garand with a heavy bullet by keeping the pressure curve up too long, and over
pressurizing the gas system.
We should know the make of rifle being used for this test. It matters.
I handle explosives for a living. I teach and direct new employees to do the same. And I've been reloading ammunition since 1978. A conservative
approach, with minimum exposure of your body to results of testing is strongly indicated. Luck doesn't last, only good technique gets you through.
A chronograph is a good start. A piezo strain gauge is indicated as well, unless a barrel can be drilled for a crusher mechanism or other such older
technology pressure measuring equipment
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Hennig Brand
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I think that good consistency from batch to batch, in terms of NC & NG strength and purity, could easily be achieved. The next step would be to
carefully control particle size and shape, which admittedly I haven't done yet, but it could definitely be done much better than I have done up until
now without much trouble. Storage stability is a big one with smokeless propellants also, but I think we may have that under control as well with the
easily purified MCNC and probably a stabilizer such as diphenylamine.
The propellant used in the test above is definitely not ideal for a 30-06 rifle, but it is serviceable. The rifle used is a bolt action 30-06.
[Edited on 30-1-2015 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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Bert
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If I were going to make a rifle propellant, I would likely use something like this:
I own one. It is made of plated brass. The roller section is finely adjustable for thickness, and the cutter heads come in several widths- from angel
hair pasta (square cordite?) to fettuccini (cross cut the strands into squares for "Poudre B"?)
Rapopart’s Rules for critical commentary:
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Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hennig Brand
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I have been making propellant in 10g, or less, sized batches for testing. For practical sized batches I think you are on the right track. I should get
one.
Bert, I do understand what you and Franklyn were talking about with faster burn rate/quicker rise in pressure and understand that flake propellants
are not ideal for a 30-06 rifle. I also understand that a 30-06 is still at the end of the spectrum where it very much falls into the category of
small arms. A 30-06 is much closer to a .22LR than it is to a lot of the guns that smokeless propellants are used in. From the bit I have read it also
seems that the faster initial burn/quicker pressure rise can be compensated for quite a bit by using a smaller powder load often at the expense of
some muzzle velocity. These faster burning powders, especially if double based and if overloaded, can be harder on barrels though, often stripping
rifling from the breech end of the barrel at an accelerated rate.
Here is a very successful and famous cartridge that used flake propellant, though it was single base:
German 7.9x57mm cartridge, also known as the 8mm Mauser
The webpage can be found here:
http://www.cruffler.com/Features/JUL-01/trivia-July01.html
I made a pdf of the page also, which is attached, but the formatting is not perfect by any means.
Attachment: History and Development of the 7.9X57mm Cartridge.pdf (307kB)
This file has been downloaded 1059 times
Calculating Propellant Load Requirements using the Kinetic Energy Equation
Here is a simple method for determining the approximate amount of a given powder to use, using known values from an earlier test (bullet &
propellant mass and muzzle velocity). This assumes equal burn efficiencies and equal frictional losses, etc. This simple comparison does not give peak
pressures, but it is a very simple and effective way to get into the ballpark of what is an acceptable powder load.
Using the kinetic energy equation:
K.E. = 1/2 * m * V^2
It can be seen that kinetic energy is proportional to mass and to the square of velocity.
Comparing the results from the earlier .22LR test and later 30-06 test:
.22LR Bullet mass: 40gr
.22LR Muzzle Velocity: 1166fps
.22LR Powder load: 0.10g (1.54gr)
30-06 Bullet mass: 150gr
30-06 Bullet velocity: 2631fps
30-06 Powder load: 2.0g (30.8gr)
Powder load for 30-06 based on what was used for .22LR assuming equal efficiencies = (150gr/40gr) * (2631fps/1166fps)^2 * 1.54gr of propellant
Powder load for 30-06 = 29.40gr
Very, very close to what was actually used!
Once again, this doesn't give us the maximum barrel pressure, but it can at least give us a very good approximation of the appropriate amount of
energy/powder to use.
[Edited on 31-1-2015 by Hennig Brand]
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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Hennig Brand
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Of course I meant the proportion of losses due to friction and other sources were assumed equal for the above calculation.
Just read an interesting section from, "Chemistry of High-Energy Materials" by Klapötke.
"While single-base propellant charges (NC) are used in weapons from pistols to artillery weapons, the higher performance double-base propellant
charges (NC + NG) are used predominantly in pistols and mortars. The disadvantage of the double-base powder is the strong erosion of the gun barrel
(see below), resulting from the significantly higher combustion temperatures as well as the appearance of a muzzle flash because of the explosion of
some of the combustion gases upon contact with air. To prevent erosion and the muzzle flash, a triple-base powder (NC + NG + NQ) with an NQ content
of up to 50% is used, particularly in large calibre tank and NAVY weapons. However, the performance of triple-base powders is lower than that of
double-base powders (Tab. 2.4). In a triple-base powder, particularly in large tank and NAVY cannons, NQ is replaced by RDX in order to increase the
performance. However, the barrels suffer increased erosion problems again due to the significantly higher combustion temperatures.
The erosion problems in guns are generally caused by the formation of iron carbide (Fe from the gun barrel, C from CO) at high temperatures. Modern
research on propellant charges is therefore focused on the development of powders which burn at lowest possible temperatures, but show good
performance (see Ch. 4.2.3). Moreover, the N2/CO ratio, which lies at approximately 0.5 for conventional propellant charges, should be increased as
much as possible. The formation of N2 instead of CO should also strongly reduce the amount of erosion, since iron nitride has a higher melting point
than iron carbide (Fe3C) and furthermore, it forms a solid protective layer on the inside of the gun barrel. New studies have shown that the
introduction of propellant charges which are based on nitrogen-rich compounds such as e.g. triaminoguanidiniumazotetrazolate (TAGzT) result in a
considerably better N2/CO ratio and the life-span of high calibre NAVY cannons can be increased by up-to a factor of 4 [11]."
Double base propellants have a lot going for them, but they are, apparently, often much harder on barrels. Some powder companies are now advertising
that their double based propellants cause no more erosion than their single based propellants, because of special additives, but I am skeptical of
such claims at this point.
"A risk-free world is a very dull world, one from which we are apt to learn little of consequence." -Geerat Vermeij
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Bert
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Nitroguanidine- One of the first adjuncts to lower flame temp without sacrificing too much in performance, and still a good choice.
The history of cordite reformulations is representative of the early attempts to balance good propellant performance against acceptable barrel life.
History of cordite production
The first formulation @ 58% NG burned so hot, .303 barrels lost accuracy in under 1,000 rounds- The second formulation @ 30% was about as high as any
common rifle propellant made since.
Cordite fell from use mostly due to performance and cartridge manufacturing limitations imposed by the grain (strand!) shape.
You could not blend different lots to standardize performance- This is typically done by tumbling different batches of grained powders together
through a tall "blending tower", can't do that with cordite.
In manufacturing cartridges, the cordite was inserted into the case and then the shoulder and neck of the cartridge was formed. It is desirable to
have the neck of a cartridge case annealed fairly soft, so as to allow expansion and a good seal against the chamber walls without cracking-
Obviously, it was not safe to anneal the cartridge necks with the cordite already loaded.
If there were attempts to modify burning profile by coating cordite, I have not heard of it. For pistol rounds and some gas generator uses, it could
be chopped into short pieces. The shorter the cut, the faster the propellant.
Additionally, they never did get cordite to be as temperature insensitive as might be desired- Cordite rounds had to be loaded to a fairly low
pressure, if they were used at tropical temperatures (or allowed to "cook" in a hot chamber), pressures rose markedly. Similarly, at arctic
temperatures the burn rate went low- I have seen old cordite rounds leave many thin remnants of the strands littering the snow when fired in winter.
But it was easy to make, easy to meter in loading- and evaded Nobel's Balistite patent...
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Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Hennig Brand
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Interesting post, Bert, I think for rifle I will take the hints and move towards using cooler propellants with less NG (20-30% NG perhaps). I took
another shot from the .22LR and the 30-06 using the same propellant. This time I used a small kitchen sieve to separate the fines from the coarse
flakes. Some of the fine flake (0.102g) was used to load the .22LR cartridge and some of the coarse flake (2.004g) was used to load the 30-06. I am at
the end of or in between snow storms, with high wind and blowing snow, so it was difficult to get good chronograph readings (at least outside) and
impossible to get pictures of the readings. The chronograph would show the reading and then within a few seconds a gust of blowing snow would go
through and the chronograph would give an error message before I could get my camera out to take a picture. The difference between actual measured
results and theoretical results obtained using the kinetic energy equation were different by 12% this time, which is more than I was hoping for. I
hoped that using more accurate scales would result in closer agreement between theoretical and experimental results. I expect that the greatest
difference this time is due to the fact that the fines were removed from the 30-06 propellant. Flake size appears to have a major effect on muzzle
velocity from the .22LR and 30-06 tests done up until now (some earlier .22LR testing was not reported here). Regarding 30-06 chamber pressure, to be
completely truthful this time the bolt did come up easier after firing than it did the last time after firing with the fines included (indicating
lower chamber pressure with fines removed). This time the bolt could be lifted with just my little finger. A bit of fresh brass was exposed again on
the end of the cartridge casing and I have determined that it is occurring while loading the shell. The reason for the exposed brass is that the
shells are going in harder, which is happening as the result of an expanded and/or bent casing neck caused by the crude method used to pull the
bullets.
Measured Quantities:
.22LR
Bullet Weight: 2.548g
Propellant Weight: 0.102g (flake, all passed through ~30 mesh SS wire kitchen sieve)
Muzzle Velocity: 1193fps
30-06
Bullet Weight: 9.671g
Propellant Weight: 2.004g (flake, none passed through ~30 mesh SS wire kitchen sieve)
Muzzle Velocity: 2543fps
Theoretical Propellant Load based on .22LR Results (assuming equal efficiencies) = (9.671g/2.548g) * (2543fps/1193fps)^2 * 0.102g = 1.759g
% Difference = (2.004 - 1.759) / 2.004 * 100% = 12%
Versus 4.5% difference last time
The fines were removed from the propellant used in the 30-06 this time and more accurate scales were used this time as well which could both have
effected the results.
 
 
[Edited on 2-2-2015 by Hennig Brand]
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Bert
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Optical comparator- Harbor freight, ebay or wherever cheap... Good way to characterize grain size, if you don't own a set of assay screens.
http://www.amazon.com/gp/aw/d/B0000WTZM2/ref=mp_s_a_1_10?qid...
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Hennig Brand
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Here is a microscope shot, at 40X magnification, of a fairly representative sample of the homemade flake propellant that was retained on the 30 mesh
SS kitchen sieve and used for the last 30-06 test. The second shot, at 40X magnification, is the mm scale on a plastic ruler. Because of the thickness
of the plastic ruler used, both the propellant and ruler could not be in focus at the same time.
 
And here is a 40X microscope picture of the flake which passed the 30 mesh sieve and was used for the last .22LR test.
[Edited on 2-2-2015 by Hennig Brand]
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Hennig Brand
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Here is a chapter from a text with a lot of good general information about nitrocellulose. Many interesting facts, for instance, according to this
text single base propellants are made with ca. 80% gun cotton (13.4%N) and ca. 20%, 12.5%N NC.
The pdf was taken from the following university's website:
Universita' degli Studi di Napoli Federico II
Attachment: Cellulose Nitrate.pdf (272kB)
This file has been downloaded 1688 times
[Edited on 3-2-2015 by Hennig Brand]
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Bert
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Sub thread on high N adjuncts, removed from "quick questions, short answers" & merged with "bullet propellants"
Has anyone considered (or tried!) azodicarconamide as an additive to a high NG content double base propellant? High Nitrogen content, should be
completely gaseous output, might speed burn rate as it does in some composite rocket fuels- While perhaps providing a cooler flame and maintaining
high gas output similar to nitroguanidine?
World wide, used as a blowing agent for thermoplastics. In USA, it's a legal food additive! The only shipping restriction is as a flammable solid
above a certain quantity. Seems to be rather easier to come by than "picrite" (nitroguanidine).
http://en.m.wikipedia.org/wiki/Azodicarbonamide
http://en.m.wikipedia.org/wiki/Nitroguanidine
[Edited on 5-2-2015 by Bert]
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Bert
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Ah, might just have re-invented the wheel. AGAIN..
Tons of referances, but for airbags, seat belt tensioners with ammonium nitrate, rocket fuels with double based propellants- Can't find anything yet
on small arms propellants, cannon powders etc.
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DubaiAmateurRocketry
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what about NH2-NH-CO-N=N-CO-NH-NH2 ?
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Pasrules
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@Bert
I was doing some work in a PVC manufacturing plant in Australia when someone placed a cardboard box of azodicarbonamide underneath the mezzanine I
welding on.
All I can say was it was lucky we had special class fire extinguishers.
Atropine, Bicarb, Calcium.
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Bert
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I have not had enough coffee yet today- Common name or IUPAC of that?
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Bert
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Quote: Originally posted by Pasrules  | @Bert
I was doing some work in a PVC manufacturing plant in Australia when someone placed a cardboard box of azodicarbonamide underneath the mezzanine I
welding on.
All I can say was it was lucky we had special class fire extinguishers. |
Welding and HazMat- What EVER could go wrong...
A while back, someone here in the USA at a freight forwarding facility told a welder to go put up some metal signs in the freight dock that handled
hazardous materials. Right over where a shipment of FIREWORKS STARS, packed in cardboard boxes were stacked up, waiting for loading.
Dead welder, wrecked facility. And the hazmat rules in USA were changed. But rules don't help people who can't or won't read placards & THINK!
The PEPCON explosion started when a maintenance welder ignited building materials contaminated with ammonium perchlorate residue. Welder + management
not thinking clearly = a couple of kiloton range explosions.
http://youtu.be/_KuGizBjDXo
http://nsc.nasa.gov/SFCS/SystemFailureCaseStudyFile/Download...
[Edited on 3-2-2015 by Bert]
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Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Dornier 335A
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Does azodicarbonamide burn that vigorously? The fire diamond on Wikipedia doesn't give it more than a "1" on flammability.
Bert, I can't find the structure anywhere but the name would be azodicarbohydrazide if I'm not mistaken. Googling that name gives no
results what so ever though.
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Bert
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Azodicarbamide produces flammable gasses on decomposition, Carbon monoxide and ammonia. The transport regulations have some extra packaging
requirements related to the ability of bulk shipments to explode strong containment in a fire.
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that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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DubaiAmateurRocketry
National Hazard
Posts: 841
Registered: 10-5-2013
Location: LA, CA, USA
Member Is Offline
Mood: In research
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is it possible to use the azo group connect other energetic guanides and similar groups?
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deltaH
Dangerous source of unreferenced speculation
Posts: 1663
Registered: 30-9-2013
Location: South Africa
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Mood: Heavily protonated
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Aminoguanidine is also being researched for this:
From the wiki article:
| Quote: | | Aminoguanidines and their derivatives are also being developed for energetic material applications. Thorough combustion of aminoguanidines can produce
voluminous non-toxic gases, at moderate temperatures, with a minimum of smoke or dust.[13] This characteristic favors application to explosive gas
generators for automotive airbags, and solid-rocket propellants that generate high thrust per kilogram, while emitting minimal visible smoke or
infrared radiation (useful militarily as well as to reduce environmental impact). Aminoguanidines can also be used as precursors for the synthesis of
tetrazole-based energetic materials and drugs. |
, though the oxidised form:
is another interesting potential... don't know if it's possible though.
[Edited on 4-2-2015 by deltaH]
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Bert
Super Administrator
Posts: 2821
Registered: 12-3-2004
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Mood: " I think we are all going to die. I think that love is an illusion. We are flawed, my darling".
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Yay! More candidates-
Propellant engineering and optimization with double base + high N adjuncts (now including these various non traditional & non energetic ones)
would be a rather large project, if one followed all the paths. Perhaps we should do some engineering on paper before we start mixing chemicals...
What Tesla said about Edison?
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“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he
found the object of his search. I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per
cent of his labor.”
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Hennig replicated ca. 1900 state of the art in a very short time, kudos for that. The next couple of steps will be more challenging, can we figure out
how to work smart instead of hard?
And should the posts in this series get merged with the gun propellant thread? I do not think there's a quick answer to the short question coming.
[Edited on 4-2-2015 by Bert]
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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