diamond-strike-anywhere-greenlight-matches-300_35399_500.jpgThread: can you make priming compound?
Retrieved: 12/19/2014, 10/07/2016
Last Post: 10/05/2014
Ok so with everything reloading getting so #$%&*-@ expensive would anyone be willing to tell me how one can make some priming compound at home? In real SMALL batches!
nhrifle
02-01-2013
I am actually doing some reasearch on this now, with some testing when it warms up outside. I have been told repeatedly and read in many sources that you can use the white part of a "strike anywhere" match head to make priming compound as is. Apparently it is corrosive. I have also heard of people using cap gun caps, tho they are apparently corrosive too. The caps are going to be my first try since they are cheap and available at toy stores.
gunnerasch0
02-01-2013
As a chem major (and dropout) fifty YA, my feculent 68 YO memory is that the fulminates were he first priming compounds. M recollection is that mercury fulminate is made mixing nitric acid with metallic mercury but would suggest googling it. Mercuric primers have a reputation for ruining brass cartridge cases after firing as the mercury released amalgates with the copper in the brass case.
FWIW
Over on the Crufflers list there was an Iranian engineer named Mehdi that detaiied his efforts to reload berdan primed Makarov brass,
He used disks shaped like washers to resize the brass and reused the berdan primers by filling them with priming compound from shotgun shells. I haven't heard him for some years.
Skipper
02-01-2013
If you don't mind cleaning, the Frankford Arsenal mix uses Potassium Chlorate, Antimony Sulfide and sulphur. It leaves a corrisive residue
longbow
02-01-2013
As far as I understand it the chlorate primers preceded fulminates. Plain old potassium chlorate and sulphur mixed as powders will detonate with impact if the mix is right.
Willbird
02-01-2013
Quote Originally Posted by longbow
As far as I understand it the chlorate primers preceded fulminates. Plain
old potassium chlorate and sulphur mixed as powders will detonate with impact
if the mix is right.
That stuff made with KCLO3(potassium chlorate) is also known in the pyrotechnics circles as "death mix"....a pinch of it on a steel plate will detonate if you smack it with a hammer. Some safer mixes use KCL04 (potassium perchlorate) and sulfur and aluminum powder...but would not work in a primer. Another issue is that some sulfur is acidic (from what I read) and mixes made with it over time will break down and deflagrate(burn) on their own, not a good attribute to a priming mixture hehe.
From what I have read most primers are made with the mix wet, and they are then dried under controlled conditions before being ready to use.
Lighting off smokeless is tougher than black, so with a crude primer you might need to use a pinch of black powder back against the primer. Not sure if 209's would be easier to rebuild than boxers or not, they might be, there is more or less a berdan primer built in. The 12 gauge from hell guy says he uses 209's up to I think 35k psi with no issues ?
leftiye
02-01-2013
You can make potassium chlorate at home (might not be a good place?). It's a hydrolysis operation like breaking down water. Depending what you mix it in (vaseline is quite stable and provides fuel, other thangs are real scary), it can be properly sensitive. Might need something in the mix (believe it or not finely ground glass has been used in primers for this) to grind against and set it ff when crushed.
Desertbuck
02-01-2013
I have looked high and low for strike anywhere matches no luck. So I looked at the toy caps, it might work if you put a pinch of black powder on top of two disk's but there the Armstrong mixture, from what I understand is that it is very sensitive.
I plan on doing some simple test to see if a primer made from them can take the shock of re-priming a case, falling to the ground, recoil of firing, etc. before I use them.
But I would like to have a good old recipe that I can make in small batches at home preferably mixed WET with a marble pastel and mortar.
As for the ATF They can come to my door and see I making it for what it was meant for. The use in the manufacturing of my own personnel ammo only. I have nothing to hide!
oldred
02-01-2013
I think maybe the cap gun caps or match heads would be the safest route to go if they can be made to fire reliably, trying to play chemist and mixing our own compounds may create a mixture that fires too reliably! While thinking this over and researching how to make a priming mix I was naturally thinking more about creating a primer that would fire every time but it occurred to me that maybe a bigger concern would be primers firing when we don't want them too! If a batch of mixture is too sensitive the primer could conceivably fire from temperature change, light shock, in the magazine from recoil or just the shock from the gun firing or they might even just fire spontaneously. I am not saying we should not attempt to make our own priming mix but our main priority should be safety and that means our FIRST goal should be stability of the mix, stability is more important than a first strike ignition.
I'll Make Mine
02-02-2013
Here in North Carolina, you can get three boxes of strike anywhere matches bundled together in the barbecue area of the supermarket -- near the charcoal lighter fluid and briquettes, often close to paper plates and napkins. Might be different some other places.
Match heads are much safer to work with than paper cap mix, and even so should be loaded damp and dried in place. Match heads contain potassium chlorate, sulfur, and a tiny bit of phosphorus in the white striking tip, all stabilized with gelatin glue (the sulfur is present mainly to cover the stink of the gelatin burning). The white tip alone makes a viable primer mix, though it would ignite slow powders more reliably with some finely powdered aluminum or titanium mixed in; it might also ignite more reliably and quickly with a small percentage of ground glass as a friction enhancer.
If you don't mind getting on all the "government lists" that no one seems to want to be on, and being disowned by your insurance company if you blow yourself up, you can order potassium chlorate, antimony sulfide, and aluminum powder from chemical suppliers (Skylighter may still be in business; they specialized in pyrotechnic chemicals for fireworks, but I haven't looked for them in fifteen years or so). You can make suitable glue (binder and desensitizer) from Knox gelatin from the grocery store (there are recipes online for converting gelatin into glue). Once you have the chemicals and prepared primers (cups reformed and cups and anvils cleaned) you can reload a hundred primers in less than an hour with less than a teaspoon of mixture; the least amount of chemicals you can reasonably purchase will make tens of thousands of primers.
oldred
02-02-2013
Quote Originally Posted by I'll Make Mine
Match heads are much safer to work with than paper cap mix, and even so
should be loaded damp and dried in place.
Do you think maybe it would be possible to dissolve the match heads (just the tips) in a solution in order to make a paste that would be safer and easier to work with? I don't have a clue as to what one might use or even if it could be done but if a paste could be made that would retain the same properties as the match heads after it dried would that not be better than trying to use them dry or maybe just damp? I seem to remember that these matches did not ignite easily after getting wet even when thoroughly dried but I could be wrong about that.
I'll Make Mine
02-03-2013
Matches that have been damp (or especially genuinely wet) are hard or nearly impossible to light because some of the chlorate has been dissolved by the water and either carried off (hence lost from the mixture) or redeposited in a less uniform distribution. The heads are originally applied wet, the combination of chemicals and glue at a consistency approximately like pancake batter.
To dampen match head mix for loading into primer cups, you'd use the minimum amount of water that will make the powder stick together; it'll be no more than 10% water, at a guess, possibly as little as 3%, and you'll want a non- porous applicator (plastic toothpick, perhaps, rather than a matchstick or cotton bud) so it doesn't take away chlorate solution. That little water, left in the mix as it's applied and dried in place (warmth up to about 120º F with dry air), shouldn't affect ignition under primer conditions. You will want to dry the mix before reinstalling the anvil, if reloading Boxer primers.
perotter
02-03-2013
Quote Originally Posted by Dutchman
If there's any interest I can burn up a batch of CD of this:
$15 delivered U.S. only. Sold a bunch of these in this forum in 2008.
IMO, every member here should have a copy of this. While there are better formulas, these do work well. The guys that wrote this did in it in a very professional way, including pressure testing and that wasn't easy back then. There are 2 things that can be improved on what they did. One is if you use a binder with a wet mix the will work better. The other is their mixes aren't exactly perfect in the percentages. But, they did say that one may want to do more testing in this area. Today by using PEP software it was fast to be able to make them better.
I didn't test everyone of them for various reasons, but their mixes did last for 1 year when stored in a basement that had no dehumidifier.
Also, there DIY smokeless power works. I will work better if you add a catalysis to increase the burn rate. I was able to get this to work even in .38 special without having any booster charge of BP or NC power.
Thanks for offering this again Dutchman.
FWIW, this is just my personal experience with these mixes.
PS
These mixes are also safer, I my testing, to load dry than match heads or
paper caps. I've reloaded a lot of primers and have had both paper caps and
match heads go off. I wasn't able to get any of the A&O mixes I tried to go
off while reloading the cup even when I hammer on the packing rod. But they
still would fire in the rifle.
perotter
02-03-2013
If you can get or make red phosphorous, an easy non-corrosive can be made with it an barium nitrate. The US military used it for a while, but it has a short shelf life.
Also there is a chem you can get easily that will work for an easy non- corrosive, but it works only in Berdan primers. One maybe be able to use a 2 step cup reloading process that would work in Boxer cups.
Currently, I'm looking at a couple of different things for non-corrosives. One being sulfur nitride, as it can be made from what is available in any town USA. Grocery store and hardware store.
perotter
02-03-2013
Almost forgot. Get the book "Ammunition Making" by G. Frost. It was a NRA published book. It is out of print and copies are somewhat expensive. The last one I saw was $250( glad I bought 2 for $15 each in the 90's). But, there are online versions to download around. This book will give you the details of how to make what we buy now. A very well written book that is easy to understand.
I covers everything that one would need to know to run a commercial ammo factory. Like making cases, primer cups, primer anvils, shotgun shell cases, etc. It doesn't cover making powder or picking powder and only says to leave that to the powder companies. It was written to be the general tech manual for the ammo factory in the Philippines, whose name escapes me right now.
Skipper
02-05-2013
Can you explain more? I looked up sulfur nitride and got Polythiazyl. It says it used in LED lights, transistors, battery cathodes and solar cells.
Tetrasulfur tetranitride:
https://en.wikipedia.org/wiki/Tetrasulfur_tetranitride
http://energetic.proboards.com/index.cgi?board=lesserknown&action=display&thread=9
Desertbuck
02-05-2013
Making Red phosphorus and Potassium Chlorate looks to be more simply doable. Still toxic but not to that extreme. Good to know though.
John Boy
02-05-2013
I have only one purpose learning how to make primer formulas...
I reload and shoot 22 LR empty primed cases with black powder. Those of us that do call it 'Stepping Back into Time'
Many of my fellow BPR shooters want to follow suit but empty primed cases cannot be had anymore. So I can provide formulas that will allow them to use spent 22 brass and enjoy shooting 22 LR BP reloads
BTW - best shot string with no decrease in accuracy is 105 rounds, 50 and 100yds. Most efficient powder to use is Swiss Null-B. The bullets I and a few others use are from a custom David Mos mold that is the duplicate of the old UMC match bullet
ofitg
02-05-2013
This is one of the recipes from Tenney Davis's book, Chemistry of Powder & Explosives -
Potassium Chlorate..................................... 50.54%
Antimony Sulfide........................................ 26.31%
Sulfur .................................................. ..... 8.76%
Ground glass ............................................. 12.39%
Shellac .................................................. ... 2.00%
I've tried it, and it works. Mix it wet with alcohol, not water. The formula can be juggled to include one or two percent of Sodium Bicarbonate - this will extend the shelf life, especially in humid environments.
perotter
02-05-2013
I'd have to look it up, but I think that one is what was used by the US Army for the 30/40 Krag.
I'll try to check tonight. I also have 2 other ones that are easy. One is what was used for the 30/06 until some time during WW1.
perotter
02-05-2013
Quote Originally Posted by Desertbuck
Making Red phosphorus and Potassium Chlorate looks to be more simply doable.
Still toxic but not to that extreme.
That would still be corrosive. Also it is extremely dangerous to do. It is a contact explosive. If you can get RP, use barium nitrate(for example) instead of PC. To mix RP and PC is NEVER TO BE DONE dry. All the primers in the world are worthless to ones self, if they are dead or don't have hands to hold a gun.
RP and PC is also to sensitive to pass industry standard tests for sensitivity.
Desertbuck
02-05-2013
Finding Lead Nitrate, Antimony Sulfide is what I'm finding is the hardest chemicals to find. Lead Nitrate being the most difficult.
But the recipe Potassium Chlorate,Antimony Sulfide,Sulfur,Ground glass & Shellac look's to be one that I could make. I will give it a try AFTER I read and absorb sufficient information to do this safely as possible and confidently.
Desertbuck
02-05-2013
Sorry perotter I was working on my last post when you posted.
OH! no no I did not mean that I plan on mixing just the two as a %50 %50 mix HECK NO! Just there the easiest chemicals to make that's all. From what I'm finding I will never use RP & PC together in any of the mixes I make! I prefer to keep my feet in my shoes.
perotter
02-05-2013
No need to be sorry. I just don't want anyone to get hurt.
Source patent 2,194,480This is a non-corrosive. I've never tested it, but it is similar/same to the P4 primer that the US military used for a while in the 1940'sRed phosphorous 25 Barium Nitrate 58 Antimony Sulfide 17 RP 5-25 BN 40-70 AS 10-25
perotter
02-05-2013
FA-42This is primer that was used in the 30/06 until sometime during WW1. It works very well. The "in basement" test for dampness was over at 18 months, but that was because I had used all of that batch up. You might want to add 1% baking soda.Potassium chlorate 47.20% Antimony Sulfide 30.83% Sulfur 21.97%
perotter
02-05-2013
Tested Ron Brown's modified. This is more of hot spark primer. Should be a good all around.
Dry. Small pistol cup. Filled cup & pack(this is called 1/2 cup). Filled cup again & packed(this is called 3/4 cup). 1/2 cup did work each time. The amount of mix for 1/2 was 0.3 grains. The 3/4 did work each time. The amount of mix for 3/4 was 0.5 grains. When fired in the pistol, the flame from the end of the pistol was about the same as CCI small pistol.
Chem %weight by volume Potassium chlorate 46.6% 3 Sulfur 19.41% 2 Grit* 33.98% 1.5 Add 1% baking soda to this mix.* The grit I used was 4030 sandblasting sand. Just measured it out. I think this is to a little course. I also, think one could use less of it.
1. Measure out 2 volumes of sulfur and put it on a sheet of paper. Crush out any lumps.
2. Measure out 1 1/2 volumes of fine sand. Add this to the sulfur.
3. Pour the above back & forth between 2 sheets of paper 10 to 20 times.
4. Beside this pile of mix, measure out 3 volumes of potassium chlorate. Crush out any lumps.
5. Combine it all together.
6. Pour it back & forth between 2 sheets of paper until your very bored. 20 to 30 times for me. 7. Reload primers.
perotter
02-05-2013
Untested by me Ron Brown 'Homemade Guns and Homemade Ammo'
Chem %weight by volume
Potassium chlorate 52.73%--- 3
Sulfur 27.27%--- 2
Grit 20% --- 1.5
Add 1% baking soda to this mix.
The % by weight is close. Depends of what the grit is.
ofitg
02-06-2013
Quote Originally Posted by perotter
FA-42
Potassium chlorate 47.20%
Antimony Sulfide 30.83%
Sulfur 21.97%
This is primer that was used in the 30/06 until sometime during WW1. It works
very well. The "in basement" test for dampness was over at 18 months, but that
was because I had used all of that batch up. You might want to add 1% baking
soda.
I found this same formula in Hatcher's Notebook, he identifies it as "FH-42". I may have to try this one.
In case anybody has trouble obtaining Antimony Sulfide, it might be helpful to know that it occurs naturally as a mineral called "stibnite".
Desertbuck
02-06-2013
I found a place that has all the chemicals that is needed. And at a real good price!
http://www.hobbychemicalsupply.com/servlet/StoreFront
Potassium Chlorate (KClO3)
Price: $6.50 lb
Antimony Trisulphide (Sb2 S3) Chinese Needle
Price: $18.00 lb
Sulfur powder (S)
Price: $4.50 lb
Willbird
02-06-2013
Quote Originally Posted by oldred
I wonder if the feds will take interest in someone ordering what amounts to
be the ingredients for making explosives? Is it even legal for them for the
feds to watch us? Am I being paranoid? You bet!
There are a few "pyro" magazines out there, more of a black and white plain paper deal than a slick magazine, I subscribed to one for a year or so. They do talk about a lot of the chemicals involved and what ones raise suspicions. The oxidizers if bought in qty can raise suspicions, and combinations of things bought from the same company. You might innocently buy some aluminum powder to mix into acraglass, and some visco fuse for your black powder cannon from the same company, and arouse suspicions.
At one time I heard copper sulfate was on some list as a precursor for Meth, they sell the stuff in paper sacks at the farm store to put in ponds.
oldred
02-06-2013
This is getting really interesting and the info you have been providing is greatly appreciated but steps 6 and 7 have me a bit confused, "Pour it back & forth between 2 sheets of paper 20 to 30 times", then the next step is "Reload primers". What puzzles me is step 6 is obviously talking about a loose powder (or do I misunderstand) so does this mean the primers are reloaded with a loose powder? Does this mix form a kind of paste?
perotter
02-06-2013
This is for using the mix dry. Fill the cup level full and then press the mix down with a rod(I use steel) that is just a little smaller than the ID of the cup. This will leave you with a cup that is 1/2 full, allowing room for the anvil.
I drilled holes in a steel plate to hold the cups. A total of 25 holes. One for large primers and one for small.
Willbird
02-06-2013
Did you use a paper disk over the powder before seating the anvil ? I would think a dry powder would be likely to crumble if you carried the rounds around in your pocket, or in the gun, or the car glove box ?
You can buy stainless screens that work nice for powders, you just gently work the powder through the screen with a camel hair brush, it then falls onto your paper. There is also a blending agent called "cab-o-sil" that you can add to powders to make them mix nicer, I think it is chemically inert ?? I would keep batches very very small, and set off whatever batch size you propose in a safe manner remotely just to see what your up against if it were to go off while you were working it. A fireworks place in MI just south of the line blew up one year, killed two people, turned the building into an empty slab, then a month later another building same place, killed 1-2 more people.
KCLO3 (potassium chlorate) is sort of nasty stuff, bites even people who should know how to work with it safely now and then.
Desertbuck
02-06-2013
I don't know about the SS screen I would feel much safer with just paper and a plastic spoon to mix. And I would use my pestle and mortar to turn the chemicals into a powder individually before I mix them. Also dust with a screen would also be a concern for me.
Willbird
02-06-2013
I read of it somewhere in an article about making flash powder, it does work very nicely, a friend made me some frames about 2" tall with the screen on top, there is no dust the material just falls down on the paper. Any powders I have used were already ground, but sometimes lumps form in storage. The camel hair brush is very gentle.
Just for me I'm not putting KCLO3 in a mortar and pestle .
Desertbuck
02-06-2013
OW! I understand it's dangerous mixed with anything that will burn. But Potassium chlorate even by it self is shock sensitive and can exploded???? I'm going to have a look at an MSDS one more time
OK I found this MSDS for anyone that is new to this including myself, as to what the risks are with Potassium chlorate
Section 1 Identification Health: 2 Flammability 0 Reactivity 3 Hazard Rating: Least Slight Moderate High Extreme 0 1 2 3 4 NA = Not Applicable NE = Not Established Product Name: Potassium Chlorate Reagent, A.C.S., Crystal Trade/Chemical Synonyms Formula: KClO“ RTECS: FO0350000 C.A.S CAS# 3811-04-9 Section 2 Component Mixture Sara 313 Component CAS Number % Dim Exposure Limits: Potassium Chlorate CAS# 3811-04-9 100% W/W TXDS: unk-hmn LDLo:429mg/Kg,orl-rat LD•:1870mg/Kg Section 3 Hazard Identification (Also see section 11) Heat, shock, friction, or contact with other materials may cause fire or explosion. Harmful if swallowed. Avoid breathing vapor or dust. Use adequate ventilation. Avoid contact with eyes, skin or clothes. Wash thoroughly after handling. Keep closed. Section 4 First Aid Measures Heat, shock, friction, or contact with other materials may cause fire or explosion. Harmful if swallowed. Avoid breathing vapor or dust. Use adequate ventilation. Avoid contact with eyes, skin or clothes. Wash thoroughly after handling. Keep closed. FIRST AID: SKIN: Remove contaminated clothing. Wash exposed area with soap and water. If symptoms persist, seek medical attention EYES: Wash eyes with plenty of water for at least 15 minutes, lifting lids occasionally. Seek Medical Aid. INHALATION: Remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen INGESTION: If swallowed, induce vomiting immediately after giving two glasses of water. Never give anything by mouth to an unconcious person. Section 5 Fire Fighting Measures Fire Extinguisher Type: Water Only Fire/Explosion Hazards: Strong oxidizer. Contact with combustible materials may cause a fire. Fire Fighting Procedure: Wear self-contained breathing apparatus and protective clothing to prevent contact with skin and clothing. Section 6 Accidental Release Measures Evacuate area. Wear self-contained breathing apparatus and protective clothing. Eliminate all sources of ignition. Section 7 Handling and Storage Store in a cool dry well ventilated area. Keep away from heat and flame. Do not get in eyes, on skin, or on clothing. Section 8 Exposure Controls & Personal Protection Respiratory Protection:None required Ventilation: Mechanical: Hand Protection: Gloves to prevent exposure Local Exhaust: Eye Protection: Dust resistant goggles/face shield Other Protective Equipment: Wear appropriate clothing to prevent skin exposure Section 9 Physical and Chemical Properties Melting Point: 368° C Specific Gravity 2.32 Boiling Point: 400° C Percent Volatile by Volume: N/A Vapor Pressure: N/A Evaporation Rate: N/A Vapor Density: N/A Evaporation Standard: Solubility in Water: 7.1% Auto ignition Temperature: Not applicable Appearance and Odor: colorless, odorless, lustrous crystals Lower Flamm. Limit in Air: Not applicable Flash Point: N/A Upper Flamm. Limit in Air: Not applicable Section 10 Stability and Reactivity Information Stability: Stable Conditions to Avoid: Avoid contact with incompatible materials. Materials to Avoid: metals, organic compounds, acids. Hazardous Decomposition Products: Fumes of chlorine, oxides of potassium Hazardous Polymerization:Will Not Occur Condition to Avoid:None known Section 11 Additional Information Effects of overexposure. Acute and chronic:May cause irritation of eyes, skin. May damage respiratory and gastrointestinal tracts if ingested or inhaled. Ingestion may also cause nausea, vomiting and abdominal pain. Conditions aggravated/target organs: NonePersons with pre-existing eye, skin or respiratory conditions may be more susceptible. DOT Classification: Potassium Chlorate, 5.1, UN1485, PG II DOT regulations may change from time to time. Please consult the most recent version of the relevant regulations. Revision No:0 Date Entered: 9/1/2006 Approved by: WPF
Quoting from the book, Chemistry of Powder & Explosives -
"For mechanical reasons, the ingredients of primer composition ought not to be pulverized too finely."
perotter
02-06-2013
I didn't use a paper disk over any when dry loading. Paper is used for wet loading only so that no compound stays on the punch when it presses the compound into the cup. Spray the primers after the anvil is put in with hair spray, etc. If wet loading of course wait until it has dried. I mostly just test various compounds and don't often spray them.
Another tip for safety is to wash everything(tools, table, bread board, etc) with water when done for the day.
perotter
02-06-2013
If you buy PC from a pyro house, you can get it powdered fine enough for direct use. There maybe a few lumps to break up. If you have to grind some up, I was shown and told to use only wooden tools. A bread board and rolling pin/large dowel.
It is good that you are doing your research before jumping in. IMO, no point in reinventing the wheel.
perotter
02-06-2013
FWIW, normally for test batches I start with a 10 grain total weight batch. That is enough for 20 large rifle primers and , IMO, enough to get a feel for what is going on. After I make a new untested(by me) mix, I put about the amount that is in a toy cap on a steel plate and hit it with hammer.
oldred
02-07-2013
Ammonium Nitrate mixed with diesel fuel (commonly called ANFO when used for blasting) was and still is the most used explosive in mining. The mines where I worked loaded ANFO by the ton(s) from slurry trucks into drill holes in the area to be blasted, this was primed with a type of dynamite that was then detonated by the usual caps. I have many times seen literally whole mountain tops blasted apart in one huge "shot" that consisted of tons of ANFO and there are probably others here that have worked around surface mines that have seen the same thing. Timothy McVeigh used Ammonium Nitrate mixed with a gasoline/Nitro Methane mix for that horrendous terrorist attack.
n.h.schmidt
02-07-2013
I have something that my apply to this topic.
It's a small book called The Ultimate Do-It- Yourself Primer Cookbook. I just checked, Amazon has some for around $20. There is one formula that is interesting using citric acid ,hydrogen peroxide and Hexamine(Heat tablets like sterno). Personally I have rebuilt berdan primers using the toy cap method. They do work but, are dangerous to seat(they will go off if seated too deep). Many hangfires with this.
page 4
perotter
02-10-2013
I forgot about that book. I've have that one and think it is worth having. I was going to make a non-corrosive that I might be able to get to work using Olin duplex idea. But, I may just try the peroxide one first as it doesn't involve ordering anything. I do have what is need for the other one, the chem isn't normally available in most areas. It is use for electroless nickel plating.
Ron Brown's book "Homemade Guns and Homemade Ammo" is, IMO, a must have. His very easy primer compound works. I substituted sandblasting sand for the powdered glass. The mix worked and lasted for several months. Brown's book also has the details on make a chlorate generator with scrap materials.
perotter
02-10-2013
I forgot about that book. I've had it for years and haven't seen it for sale lately. IMO, it is a must have for those who are interested in this.
I was going to test a non-corrosive using the Olin duplex idea. It really is for 22 rimfire and Berdan primers, but not Boxer. But, the Olin idea may allow for its use in Boxer. It is very simple to make and get the raw materials, but the testing would take a while. I might just give the peroxide one a test first, as the need chems are easily available.
My experience with toy cap the last few years are the same as yours. I don't like the surprise I get when they go off when I'm working with them.
Bent Ramrod
02-12-2013
There was a giant explosion maybe 20 years ago in Henderson, Nevada when a fire broke out in the country's largest ammonium perchlorate manufacturing plant. Nobody actually thought the stuff would detonate by itself, but things that have been proven in laboratories sometimes change out in the real world.
perotter
02-24-2013
For a mix that should work with the Olin duplex idea. This is a non-corrosive mix.
Reloading-rimfire-cartridges/page2
Raven_Darkcloud
03-06-2013
Has anyone tried to make a a wet mix from the potassium chlorate / sulfur using alcohol? Watched a cci tour vid and it looks like a wet mix would be much easier to work with.
trapper9260
03-06-2013
you need to clean your gun after use but you can use the old cap gun caps in the roll and fine 4 fg black powder and you are good to go . you can get it at a dept store in the toy area .
jmorris
03-06-2013
The priming compound shown at 4:50 into this video would be the recipe I would want.
http://www.google.com/url?sa=t&rct=j...43287494,d.b2I
destrux
03-08-2013
I'd be really interested in that citric acid/peroxide/hexamine mix, what are the details to that recipe?
I tried extracting the primer out of some percussion caps the other night using some 50% rubbing alcohol, then I dried it on top of my furnace near the dehumidifier. It didn't work, but I suspect my mistake was replacing the anvil with the mix wet, it squished it out from the pinch point.
I'll Make Mine
03-09-2013
Quote Originally Posted by destrux
citric acid/peroxide/hexamine mix
Destrux, stay away. That stuff is a sensitive, detonating primary explosive (same class as mercury fulminate, but stronger), the high strength peroxide it requires is very hazardous to handle, and you need a Federal license to even possess the resulting compound (plus inspected and registered storage, same kind of place you'd store blasting caps).
perotter
03-10-2013
Quote Originally Posted by I'll Make Mine
Destrux, stay away. That stuff is a sensitive, detonating primary explosive
(same class as mercury fulminate, but stronger), the high strength peroxide it
requires is very hazardous to handle, and you need a Federal license to even
possess the resulting compound (plus inspected and registered storage, same
kind of place you'd store blasting caps).
You don't need a Federal license to possess this if you are going to use it for making your own ammo. Nor do you need an inspected and registered storage. We've been down this road a few times on this forum.
perotter
03-10-2013
Quote Originally Posted by destrux
I'd be really interested in that citric acid/peroxide/hexamine mix, what are
the details to that recipe?
I tried extracting the primer out of some percussion caps the other night using some 50% rubbing alcohol, then I dried it on top of my furnace near the dehumidifier. It didn't work, but I suspect my mistake was replacing the anvil with the mix wet, it squished it out from the pinch point.
http://www.martinfrost.ws/htmlfiles/june2007/imhv3.pdf
There are other thing in this FM that you may want to know. I think DuPont/Remington is who did the work on that section of the book.
It's at about page 48 or 49. This isn't a compound that you'll want to store for a long time in or out of primers.
deces
03-19-2013
Just curious, has anyone hurt themselves or had close calls yet? this thread died all the sudden. (no pun intended)
Azshooter2013
03-20-2013
well im not sure why the thread died, but with primers getting more expensive and harder to get, i have been doing some reloading of spent primers, i did not try all the chemical mixes from the thread, but here is what i have done. I loaded up several diferent coumpounds in some of my spent primers just ot see if they would work.
first i used 1 of the caps from the "roll cap" type caps, i trimed it with sissors to make it fit in the cup. pressed the anvil back in and loaded it in my gun (just the primed case), it did go off, so i loaded 10 rounds of my standard 380 load and went to shoot it. it sucked, the load was not even strong enough to cycle the slide. and one bullet even got stuck in the barrel.
strike 1 for the "roll caps"
next i loaded 1 "roll cap" and then filled the primer cup with a strike anywhere match counpound, then loaded it in to a case, i did not have any reloaded primers go off while repriming a case. i went out and shoot this mix of "roll cap" and match powder, all rounds fired and it felt just like my normal load, using new sp primers.
next i tried using 2 "roll caps" only in the primer cup, while setting the anvil some did go off. but after shooting the reloaded rounds it felt a bit lighter than normal but still worked properly.
next will be just a mix of match head powder only.
thats where im at right now.
Desertbuck
03-20-2013
Nope still here I'm still working on it. But I have been working on other projects. I did get the hand at making Potassium chlorate from Bleach. You don't get much from it but you can make it yourself with stuff you can get at the store. Next I need some sulfur that's going to be the easy one. I want some Antimony Trisulphide but I think I might have to settle for aluminum powder. I will take a picture of my first reloaded primer and post it as soon as I make it. I'm having fun learning.
Oreo
03-20-2013
I've been studying this too. The book / pdf from Dutchman has some very specific instructions on how to make a handfull of priming compounds and do it safely. All of those recipes are based on flash powders with some extra stuff added.
The author categorizes each chemical as Fuel, Oxidizer, Sensitizer, etc. Another book I read has some of the same chemicals categorized differently but in these particular formulas there are two ingredients that make up a binary flash powder that is shock sensitive. Then there is an oxidizer-fuel combo that is ignited by the flash powder for more heat and sustained ignition.
The author says that red phosphorus is a primary ingredient. Its the only ingredient I haven't been able to find available commercially in reasonable quantity or price. But that doesn't appear to be a major problem.
Most of the author's recipes use Potassium Chlorate which results in a corrosive primer. One non-corrosive recipe uses Barium Nitrate instead but also uses Red Phosphorus which is inconvenient. I have not been able to find any good reason why potassium chlorate can't be substituted by barium nitrate in the author's recipe 4 which does not call for red phosphorus. This would be a very good, non-corrosive primer made from cheap & easy chemicals. It would need to be tested for proper sensitivity of course.
ofitg
03-20-2013
Quote Originally Posted by Desertbuck
I did get the hand at making Potassium chlorate from Bleach.
Desertbuck, my hat is off to you! I tried to make KClO3 from bleach and I ended up just making a mess. I had better luck using an electrolysis rig to make KClO3 from potassium chloride.
Quote Originally Posted by Desertbuck I want some Antimony Trisulphide but I think I might have to settle for aluminum powder.
A lot of Stibnite crystals are offered on Ebay... or maybe you can find Stibnite specimens at a rock shop in your town... ?
Oreo
03-20-2013
Search ebay for antimony trisulFide. Same thing different name. There's one seller in GB selling it crushed by the pound for a way better price then having to buy the crystals, even after shipping across the pond.
ofitg
03-21-2013
In a different thread, "Drhall762" reported that he ordered all three chemicals - potassium chlorate, sulfur, antimony sulfide - from this supplier - http://pyrochemsource.ecrater.com/
uscra112
03-21-2013
The March 1943 issue of American Rifleman has some basics on how to make fulminate of mercury. I don't recommend anybody try it, based on what I saw. I enjoy the thought of a mass-market magazine giving details that would be relegated to the Anarchists Cookbook just 20 years later, and in wartime, too.
perotter
03-21-2013
http://www.hobbychemicalsupply.com
http://www.rollingthunderpyro.com/
I've bought from both of the last two. It is best to buy the fuels from someone different than who you buy the oxidizers from. For example, ordering both PC and aluminum powder is consider by the gov that you are going to make illegal fireworks and your order won't be processed. The gov seems to be very willing to shut down the supplier of these chemicals.
There are a few other chemical places to buy from also. I'll list a few more latter.
page 5
perotter
03-21-2013
Tin sulfide can be used instead of antimony sulfide. I'll post latter how to do it, as it simply melting the two together in the correct proportions. Or you can make antimony sulfide yourself, if you had to.
perotter
03-21-2013
Quote Originally Posted by deces
Just curious, has anyone hurt themselves or had close calls yet? this thread
died all the sudden. (no pun intended)
I've loaded a fair number of cups. But, I do small batches. The only thing that has happened wasn't an explosion. But, I did break 2 rules.
1. Poor 'house cleaning'.
2. Tried something at the spur of the moment.
I was walking out the door on the way to a school play when I got an idea. And thought I'd quickly test it. I didn't even take off my jacket. I finished the test and went to the play. I had gotten some oxidizer on the jacket. Either there was some grease/sugar on the jacket where the oxidizer also was or possibly someones cigarette started it. In the school lobby I smelled smoke and it seemed to be following me. Then I noticed that the jacket was burning without a flame. I put it out and went and watched the play.
wills
03-21-2013
Quote Originally Posted by Desertbuck
I have looked high and low for strike anywhere matches no luck. So I looked
at the toy caps, it might work if you put a pinch of black powder on top of
two disk's but there the Armstrong mixture, from what I understand is that it
is very sensitive.
I thought they were gone too, but our HEB has good ole fashioned Diamond, and it appears you can order them.
http://www.appoutdoors.com/liberty_m...FdSnPAod0z4Anw
perotter
03-21-2013
Quote Originally Posted by Oreo
If you use potassium chlorate it will be corrosive. As red phosphorus is on
the DEA list, it will be very hard to buy unless you are corporation. You'd be
better off making it than spending time trying to find it to buy on the legal
market.
I've test all the mixes from the AO book. They all work fine.
But I would load them wet and use a gum in the mix. Gum does make for a more consistent primer. One of my own created mixes would only fire on the first try about 95% of the time, but would then fire on the second try. I switched it to wet mix with gum and it would fire 100% of the time on the first try. IMO, it is hard to beat safer and better.
perotter
03-21-2013
Most ACE hardware stores carry strike anywhere matches. Forum member Delmar has a youtube video on how he does them. I use primer plates to hold the cups instead of how he does/did it.
FWIW, Delmar happened to get into guns at the same time as the last shortage and wasn't able to buy ammo for it. So in the spirit of can-do, he bought a Lee Loader, 100 primers(all he could get) and a pound of powder. Then had to start reloading primers to continue shooting.
perotter
03-23-2013
Quote Originally Posted by perotter
Tin sulfide can be used instead of antimony sulfide. I'll post latter how
to do it, as it simply melting the two together in the correct proportions. Or
you can make antimony sulfide yourself, if you had to.
Here is what I've got.
In a porcelain crucible put, by weight, 40% sulfur and 60% tin. Melt them together and mix well. Let it cool and grind into a powder.
I'll Make Mine
03-23-2013
Quote Originally Posted by perotter
In a porcelain crucible put, by weight, 40% sulfur and 60% tin. Melt them
together and mix well. Let it cool and grind into a powder.
I'd expect you'll want/need to keep a lid on the crucible during the hot part of the process to prevent sulfur loss -- sulfur ignites in air at not much above the melting point of tin. You'll probably also want to have the tin in the finest particle size obtainable, and the sulfur in powder, so you can mix them together as much as possible before starting the melt and avoid having to open the crucible to stir until most of the metal and sulfur have reacted.
ofitg
03-23-2013
IMM, thanks for mentioning that. I just looked up the sulfur's auto-ignition temperature.... that's shaving it pretty close... I wish there was some simple way to achieve precise control of the temperature...
perotter
03-24-2013
If one wants to just getter done this is how I'd say to do it.
If you are ok with using a corrosive primer, than just make the mix that the US military used back in the WW1 era. They spent a lot of money and time coming up with it and it works very well. And the chemicals are easily obtainable, cheap and is simple to do. No special equipment and it is faster and cheaper to reload with than using toy caps or cutting the heads off of strike anywhere matches. The cost would be about $0.60 per 1000 primers.
If you must have a non-corrosive primer, you have a few choices. But the simplest path to get a 100% result without doing a bunch of experimentation, is to make your own RP. It is pre-1600's tech making it and stone-age tech will work. Then buy barium nitrate and antimony sulfide to make the compound. Urine was first used to make it. Latter it was made from bones. The US military is currently working on replacing the current lead based primer mixes with a RP one. And in the past have used it.
If you don't want to make RP, than go the hypophosite route. Use Berdan primers, a booster charge or a duplex primer. It's simple, safe(relative to the topic) and currently you can just buy what you need.
After that, IMO, one moves from the "just getter done" into the more experimental world or you start spending a lot of time, money, work with very poisonous chemicals, etc. I somewhat like the experimentation and research that goes into the use of other things, but one should decide what their goal is before starting.
Stay safe. If in doubt, don't do it.
ofitg
03-24-2013
Good advice, Perotter. My primary goal is making caps for percussion revolvers, and the KClO3-based mix has worked very well for me. I'm still interested in developing backup sources for the chemicals, and the "tin sulfide" idea sounds intriguing.
Thanks for sharing your info - it's great to hear from others who are working in this area.
perotter
03-29-2013
I'm going to check the result of ammonium permanganate(non-corrosive). Currently the chemicals to make it are available everywhere in the US. And making doesn't require an equipment, special process or be expensive. This would be one that wouldn't have a real long life. Something like 6 months to a year. This could be a reason that it was never used for commercial ones.
Please keep in mind that testing this may not happen in a few days. Although it might go fast. It could be that it is to bulky.
Raven_Darkcloud
04-06-2013
I have been working with Diamond greenlight strike anywhere matches. They are potassium perchlorate, sulfur based. The first test was did it work. Now I am working on a slurry. The heads are water soluble and dissolving them off is the safest way. I have a batch dissolving now. The slurry should be ready in 24hrs with all the priming compound dissolved.
diamond-strike-anywhere-greenlight-matches-300_35399_500.jpg
The green looks odd but it lights well. In fact it lights a little too well when dry. That is why I wanted to do a wet mix. Plus dissolving is less time consuming then smashing them up. If this test works the next step is the potassium chloride, sulfur, grit mix. The wet mix is what will make it safer.
waksupi
04-07-2013
I use the green tip matches in my shop to light the stove. When the weather is cold, or damp, they do not light as well. Keep us updated.
The solid soft lead bullet is undoubtably the best and most satisfactory expanding bullet that has ever been designed. It invariably mushrooms perfectly, and never breaks up. With the metal base that is essential for velocities of 2000 f.s. and upwards to protect the naked base, these metal- based soft lead bullets are splendid.
John Taylor - "African Rifles and Cartridges"
Forget everything you know about loading jacketed bullets. This is a whole new ball game!
Raven_Darkcloud
04-07-2013
Now the trick is a consistent mix. Water by its self is slow drying, perhaps an alcohol to dissolve on the next test. They will light but the drying time is painful. I have about 28gr of mix in the slurry. A 24 to 36hr dry time is the slow down on this test. I think I will do a side test with IPA to make the wet mix. Hmm I wounder if a 10 min run at 100 in toaster oven will set it off? To the test cave Robbin!
Raven_Darkcloud
04-07-2013
Ok 6 matches in the toaster oven on low for 40 min and no ignition. I might be able to speed up the drying that way.
Yes I can buy it, but great pride can be taken when I make it myself!
Oreo
04-07-2013
I wonder if heat might cause degradation of the compound.
An alternative would be to build a vacuum chamber and place the wet primers in the vacuum.
Jon
04-08-2013
Oven drying is fine for match compound. Just remember that the dried mixture is somewhat sensitive.
page 6
Raven_Darkcloud
04-09-2013
A food dehydrator might be a safer way to do it, but For now it is a toaster oven on low. I had to mix the slurry for a few min and I think It will take 2 loads of the slurry per primer. This my work better with the KCL, sulfur mix as You can control the mix better. Also the alcohol to dissolve might be better.
Yes I can buy it, but great pride can be taken when I make it myself!
perotter
04-09-2013
When you make the PC/ sulfur mix as a paste you'll find it to work much better than a slurry. For both cost and convenience it is hard to beat the PC/sulfur mix. Safer too. Over the years I've had many matchhead and toy cap primers go off. And enough when priming the case to have decided, for me, that priming would be of the simplest method available.
Alcohol or acetone are both much faster to dry out. When they are compatible to what I'm using, I use one of those I just let them sit and air dry. Water based, I use a food dehydrator as you suggest.
Raven_Darkcloud
04-09-2013
Getting the mix consistent with the match heads is proving hard. 1 of 5 worked. I will have to get the pc and sulfur to test. The match heads are just too unstable.
Yes I can buy it, but great pride can be taken when I make it myself!
ofitg
04-10-2013
RD, I will second Perotter's recommendation. It takes me about 10 minutes to weigh out the dry ingredients and prepare the paste for loading percussion caps - within one hour, I'm finished.
As much time as you've expended, you could have tweaked a method for producing your own potassium chlorate...
victor3ranger
04-10-2013
Ok, I have a question. Where do you get the PC and sulfur to do this?? I am really wanting to learn how to do this just in case things get REALLY hard to buy in the future.
Oreo
04-10-2013
I wouldn't spend too much money on it at this point. Realize that storing these chemicals and making your own primer compound has its own risks. Money now is better spent on commercial primers. Build your stash and worry about making your own and sourcing components for such when that time comes that primers have been banned.
That's the conclusion I came to anyway.
perotter
04-10-2013
Oreo, I agree that one should spend only a reasonable amount. At this point learning how to do the details of the process and know what to expect is, IMO, most important.
victor3range
04-10-2013
That's my point, I want to have all the knowledge well before if or when they are either too expensive, too hard to find, or worse banned.
That way I will already have the knowledge on how to rebuild my spent primers.
ofitg
04-10-2013
Quote Originally Posted by victor3ranger
Ok, I have a question. Where do you get the PC and sulfur to do this?? I am
really wanting to learn how to do this just in case things get REALLY hard to
buy in the future.
Back on post #78 and post #80 of this thread, you'll find some links to retail sources of the chemicals. That's the simplest way to get started.
If you want to go a few steps further, you can make an electrolysis rig which converts potassium chloride (available at most hardware stores) into potassium chlorate.
Antimony Sulfide occurs naturally as a mineral called Stibnite.
Dusting sulfur is also available at most hardware/garden stores - it's about 90% pure sulfur - I haven't tried using it for primer mixes, but it works OK for DIY blackpowder.
Raven_Darkcloud
04-11-2013
Oreo, If I could find primers I would just buy them. That is my problem, I shoot up to 1k rounds in a trip to the range and only finding 1 or 2 hundred primers every 2 months will not work for me. I also want to know how to make it if it is needed.
Desertbuck
04-21-2013
I found two boxes of strike anywhere matches in my home town for $1.89. If you cant get it in the city go to a small town usa. They WILL have what a city wont. I have been experimenting with SAM compound havent shot boolits with them. But thay do go pop every time I tested them. Three matches a primer so a box of 300 will give you 100 primers. Not bad for $1.89. Im in the process of getting the chemicals for the WW1 mix I would rather use a compound that was intended to be used in a primer. But I do plan on giving the SAM compound a try in my Sharps 45-120 with black powder.
Desertbuck
04-28-2013
Update I got my chemicals on Friday. This morning I filed down four 22 long rifle cases for small custom measuring cups for each individual chemical and just super glued them to wooden handles.
20130428_153519.jpg
20130428_153504.jpg
sorry about the first picture being upside down.
Desertbuck
04-30-2013
okay so far I have made three batches sorry I didn't take any pictures. My first batch was to get my bearings and get a feel for it. Also I wanted to try primers packed with the mix dry and with some of the mix wet. I got two primers with the mix dry packed but I accidentally dumped way too much rubbing alcohol into the batch so I dumped the rest down the sink and forgot about the wet mix test at the time. I moved on to the test of the dry mix. I seated the two primers filled with the dry mix in some old empty 30/06 and proceeded to test them with my model 1917 the first one made a very good pop!!! The second one well wen't fizzle :-* But I attribute that to it getting a little wet from the spill somehow. My other two batches were to see if wet or dry was easier to use and all around which one was better. So far I can't tell the difference between a dry mix or wet mix pop and they do go pop! Just for fun I took an earplug placed in the case neck then setup a cardboard box and shot the earplug at it. And much to my delight the earplug hit the cardboard box with authority .
I do have one question though the residues that this mix leaves behind is kind of a reddish orange looks just like rust dust do I have to be concerned with this residue being abrasive ?
perotter
04-30-2013
I suppose one should always be concerned with anything in a barrel being abrasive, I've never been concerned with the reddish/orange residue being abrasive. It is most likely antimony chloride. or antimony pentasulfide or a combination of two. The amount of antimony sulfide in the FA-42 or FH-42 mix is about the same as is/was common in small pistol/rifle primers.
I have software that would normally tell me what all products of a mix would produce, but when I ran it tonite it failed because it didn't have a definition for antimony.
page 7
perotter
04-30-2013
Desertbuck, It sure is enjoyable when a new mix goes pop when you try it, isn't it? I think you picked the best mix to try first.
With the WW1 mix I think that a dry mix is fine and would be my first choice as one can just fill the cup and pack it. But I haven't tested it dry-vs-wet with a chronograph or pressure tester.
perotter
05-06-2013
I worked on making a simple non-corrosive(ammonium permanganate) this past weekend. I have to get a better yield before I'm going to consider this a viable option. At this point I'm not sure why the yield was so low, but I'm going to spend a little more time on it. I'm not yet sure it will work for Boxers.
Desertbuck
05-16-2013
Hay everyone. Sorry I have not been posting I have been real busy with work. But I did have some time to test my primers last week. I used my good old 91/30 in 7.62X54r. To keep the pressure on the low side I loaded 9 cases with HODGDON Triple Seven black powder substitute which I have been having some success with with a PP boolit in my 91/30. One was loaded with APP black powder substitute the most worthless BP sub I have ran into so I'm trying to fined a good use for it.
The primers worked GRATE! I now have a good feel for doing this and it is a lot of FUN to do I think I packed around 40 more primers this morning and they are now siting in my work room drying. I have been using my wife's hair spray to glue the priming mixture in the cup. I also want to share that I found an easy way to put a paper disk in the cup like the factory has in there's. A paper puncher makes nice little paper disks that fit nicely in the cup with room for the anvil. Some time shortly I hope I can get some pictures up for everyone.
I want to thank perotter for all his help and good tip's
I also want to thank Dutchman for the primer book CD It has helped me alot.
THANK YOU SO MUCH GUYS
Ps now I feel safe to say even IF primers and powder are no longer available I will still be able to enjoy my hobby it will just be a little smokier.
perotter
05-19-2013
Your welcome. I'm glad that what I've tried is useful to someone else. Thanks for posting the results of your work. I too like the peace of mind that I can go to the target range no matter what the store bought supply situation is.
FWIW, I'm sure that you saw the DIY smokeless powders in the A&O book that the Dutchman sells. I never got around to the paper one, but the other one does seem to work ok. But, most of it I added a burn rate cat to increase the burn rate. But, this is really off topic of primers.
Bert2368
05-21-2013
Oreo, a review of smokeless powder manufacture at a WWII level of technology is to be found in Tenney Davis' "Chemistry of Powder and Explosives" available for free download here:
http://www.sciencemadness.org/library/books/the_chemistry_of_powder_and_explosives.pdf
Pages 287 through 328.
Like a lot of other industrial chemistry, it doesn't really lend itself well to small batch processes in an amateur lab. You could almost certainly MAKE a smokeless propellant. But characterizing it well enough to use for reloading without losing guns/body parts? Unlikely with the experience, equipment and lab skill levels implied by the rest of this thread.
Not disparaging the members, I'd be scared to death to try it and I have synthesized or handled most of the chemicals involved in modern primer and propellant manufacture.
Bert2368
05-22-2013
Quote Originally Posted by perotter
But we do have Kmart, Walmart,supermarkets, etc. No need for old when you
can get new.
I am aware of what may be done with re-purposing commonly available materials.
Could you provide me with some concrete information on the Viet Cong or Afghani manufacture of reloading propellants you mentioned? Both countries were long term war zones with much UXO laying about, along with plentiful opportunities to acquire new ammo from neighboring countries- or the leavings by the opfor. Taking the time and effort to scratch make nitrocellulose/nitroglycerin and manufacture reloading propellants under those conditions seems needless.
Maybe this belongs in a whole new thread on improvised propellants, if someone cares to kick one off?
For the original topic, this may be of interest...
DON'T try this at home. An acceptable level of safety requires proper safety gear and a fume hood to work in along with practical knowledge of lab procedures and handling primary explosives. Toxic gasses, poisonous byproducts, dangerous, toxic, corrosive or flammable ingredients and a REALLY hazardous, takes your hand off kind of end product.
Under Federal law in the USA an unlicensed person can still do this legaly for their own use. But they can't store it improperly, distribute it to others or move it over a public road. As far as state and local laws are concerned, most municipalities and quite a few states would have a cow if they found you doing something like this.
Try dropping a pinch of starch , paraformaldehyde , or sodium nitrite into the reaction mixture to start the reaction.
5.4 g of red mercury oxide (HgO) was dissolved in 50 ml of room temperature 70% HNO3 in a 500 ml beaker, resulting in a clear solution with no visible fuming and only a mild warming.
50 ml of denatured ethanol was measured out, 25 ml of which was quickly added to the Mercury nitrate solution. After about 5 minutes, no visible reaction was noted. At this time, .25 g of Sodium nitrite (NaNo2) was added to the beaker. A mild effervescence and a change of the solution to a slightly yellowish color was noted after a few moments. The effervescence accelerated, with self heating and development of heavy white fumes. When the reaction seemed in need of moderation to prevent bubbling over, the remaining 25 ml of alcohol was added to the mix in several small portions. An additional 20 ml of alcohol was also added for purposes of reaction moderation after the initial 50 ml was expended, bringing the total to 70 ml.
About 30 minutes after the onset of effervescence, the reaction had subsided and a considerable amount of a light grayish precipitate had settled out. The contents of the beaker was added to about 200 ml of distilled water and the solids filtered out in a Buchner funnel. The retained solids were washed with several portions of water and then given a final wash with alcohol.
The first obtained solids weighed 5.1 g after drying, and were of a yellowish/grayish color and needle like crystal shape.
These solids were dissolved in 80 ml of 30% ammonia and the liquid filtered. The filtered liquid was carefully neutralized with glacial acetic acid, the resulting precipitate filtered out, washed with water and then alcohol and dried. The precipitate weighed 3.65 g after drying and was a dense sparkly white powder similar in appearance to fine table sugar consisting of small crystals, quite different in shape from the crystals of the initial product.
The product displayed the characteristics of mercury fulminate, deflagrating in small quantities in the open and detonating violently in larger quantities or if confined. The entire remaining batch was mixed in 80:20 ratio with Potassium chlorate and detonated, as dry storage seemed inadvisable and no use was anticipated for a primary explosive... "It made a jolly bang"
Just for referance, here is a link to download some litterature on Lead styphnate production methods and parameters for small arms primers.
http://www.sciencemadness.org/talk/files.php?pid=218392&aid=15556
Once again, DON'T try this at home.
perotter
05-23-2013
For making lead styphnate get G. Frost's book. He was one of guy's who helped perfect it for production by Winchester/Western. He goes into every detail. Including how to tell if the batch is suitable for primers or needs to be destroyed.
Bert2368
05-23-2013
quote
For making lead styphnate get G. Frost's book.
Title? Author's full name?
Personally, I'm fond of Tenney Davis' Chemistry of Powder and Explosives, but it is much more about synthesis than process engineering required for proper particle sizes and other details you really need to know for consistent effect.
Available here:
http://library.sciencemadness.org/library/books/the_chemistry_of_powder_and_explosives.pdf
Remove anvil from primer.
Remove firing pin dent.
Sulfur to your small mixing container I used a glass shot glass. I however do not think glass is the safest container to use for obvious reasons.But what I do like is that glass smooth surface will not allow the mix to stick to the sides of it.
Add Stibnite.
Add backing soda.
Mix well with ONLY the wight of a small long.
wood dowel
Next add your potassium chlorate mix well WITH ONLY THE WIGHT OF THE WOODEN DOWEL!
Use a small pistol primer for a very small...
...volumetric scoop.
Press the mix down with ether a nail or punch you DO NOT need the hammer for this.
At this point I found you should give the now repacked primers a small tap to settle any priming mix stuck to the wall's of the primer.
Give them a shot of hairspray and before they dry put them on a hairspray free plat or your going to end up sticking them to the plate.
you used to spray them on.
This is probable not necessary but I do put a disc of paper in my primers just in case some of the compound.
comes loose.
Now place the primer with the loose anvil in your primer ram seat then deprime the case. Your anvil should now be set firmly in place.
the now reloaded primers in your prevues empty primer trays.
Then reuse.
Oreo
5-24-2013
Thanks for all the pics. They all make perfect sense to me since I've probably read all the same source material.
It might be a good idea to find a pewter cup to do your mixing in though. Glass and even plastic can become shrapnal on the off chance a batch were to detonate while mixing.
perotter
05-25-2013
Thanks for the pictures. They are very good and IMO don't need any or few words to explain.
Short of making a set of primer plates, the only thing I'd suggest is a drill a hole in a piece of metal to hold the primer when removing the anvil. A quick look at a drill chart will show that the bit needed is very common and available at most local hardware stores.
I have a write up about primer plates, but no pictures. I may see if I can just do some copy and paste, as I have nothing new to offer that wasn't done decades ago in the industry. I should be able to do it this weekend. They really do make it faster and easier.
Nobade
05-25-2013
I would question the mixing of priming compound in anything. "Back in the day" I would mix it by rolling the powder on a sheet of paper, so that nothing touched the mix and if it did happen to ignite, no schrapnel produced but I might get burnt hands. Just wondering here...
Desertbuck
05-29-2013
Yeah the more I think about IF! The more I want to get away from glass OUCH!
I'm going to give the paper folding a try.
All I can say to anyone planing on doing this you had better DO THE RESEARCH! AND MORE RESEARCH! AND MORE RESEARCH!! AND MORE RESEARCH!!! Learn the history of the priming mixes you intend to use under stand how stable the chemicals are what can be mixed what CANNOT be mixed.
And understand it comes with risks just like reloading itself. If you are uncomfortable going it DON'T do it. But if you go into it with a clear understanding and want to learn have at it.
Bert2368
05-29-2013
Mixing priming or other very sensitive dry mixes is traditionally done by "diapering". Put the ingredients on a sheet of paper or other thin, flexible material. Alternately lift the corners of the sheet so the ingredients roll over each other, mixing with little chance for friction or grinding the mixture.
I have seen pictures of an old time factory where this operation was carried out remote from the operator behind a blast wall by pulling several strings attached to the sheet corners. A triangular thin rubber sheet was used, with the actuating strings run over pulleys above the mixing area and the operator observing through the blast wall via an armor glass view port.
Desertbuck
05-31-2013
Got my first duds today ,four in a row. I did not even bother to try more. The primers went off my pp boolit's came half way out of there case a good sign I made these primers way to underpowered. I came home a little bummed out but the 30bl of range lead I found cheered me up a little. Looks like I'm going to have to make them hotter.
perotter
06-01-2013
Desertbuck, Did you fill the cup full and then pack them to 1/2 full? I've never had a chlorate primer not work well when doing it that way. IMO, a wet mix is really the way to go and the mix you are using was done that way when it was the standard US Army mix.
FWIW, a wet mix that has a gum binder in it will give a better result than a dry mix. In both repeatability and reliability. I more or less proved this to my satisfaction when make a couple of different non-corrosive mixes. Going from dry to wet, reliability went from 80% to 90+%. Adding gun to the a wet mix took them to 100% reliability.
Also, with the board you drilled out for the cup can you use that to level a pile of mix into the cups? If so, then the cups will be full of dry mix and you'll have the same amount in each one. I've actually only ever done mixes that way and never using a scoop to fill the cups, so I can't really say that the scoop method isn't as good.
Bert2368
06-01-2013
Could you describe the types of gums used and quantity?
I have used a combination of gum Arabic as a binder with a small additional percentage of Guar gum to control the consistency of pyrotechnic wet mixtures. The Arabic provides cohesion, the guar makes the mix into a uniform pourable/paintable slurry without the tendency for the solids to settle out- kind of a waffle batter consistency. Using that much water without the guar and you end up with solids on the bottom and a layer of water on top.
ofitg
06-01-2013
Bert, the KClO3-based mix used in the old .30-40 Krag primers included 2% shellac.
Desertbuck
06-01-2013
I used the small pistol primer as the measuring scoop. So no they were being filled three quarters of the way maybe. The priming compound was doing its job there just wasn't enough of it. Thanks Perotter
Bert2368
06-01-2013
If they used shellac, did they pre-mix the chlorate prime with alcohol and dispense wet into the cups?
Alternately, could you fill and compress the dry mix and then put a drop of shellac solution into the cup on top.
Has anyone tried for centerfire primers the technique they use for eley rimfire ammo where the final reaction to produce the sensitizing primary only occurs after the mix is in position?
A closely guarded (and patented) secret, this new Eleyprime process had two huge consequences: It eliminated the risk of explosion from the preparation and dispensing of priming compounds, and it allowed the amount of priming material applied to each individual rimfire case to be very tightly controlled in a normal workshop environment using automatic equipment.
This last part is critical because it has long been known that case-to-case variation in the amount of priming material is the most important factor regarding variations in .22 LR rimfire performance. This is due to the fact that in small rimfire cartridges the primer is a significant portion of the actual propelling charge (much more so than in larger centerfire cartridges) and because conventional priming compound is too sensitive to be aggressively metered and applied.
The Eleyprime System allows exactly identical amounts of the inert powder to be put in each case. Then a round-tip rod is inserted down into the case to press the powder evenly into, and around, the rim, and a single, metered drop of water is added, which activates the compound over a several-hour period.
After drying, the cases can then be conventionally charged with precisely metered propellant (five rounds at a time on the TenEx loaders). Before Eleyprime, there was an average 31 to 39 milligram spread in the amount of priming material round-to-round in TenEx ammunition. With the Eleyprime System (EPS), the spread was reduced to only plus/minus 1.0 milligram. It was a stunning achievement, and in 1988 Eley received the prestigious Queen’s Award for Technological Achievement.
Nobade
06-01-2013
Is it better to use shellac flakes dry and then wet out the whole mixture with alcohol, or make up the mix and then wet it with prepared shellac? I tried the latter and got 100% misfires. The mix wouldn't even work by hitting it with a hammer. I assume I used way too much shellac.
perotter
06-01-2013
Quote Originally Posted by Bert2368
Could you describe the types of gums used and quantity?
In what I described, I used red gum and 1.5%. I know that this isn't what should be used, because is shortens the life of the primer. But it was what I had on hand that weekend. As I was testing a patentable compound that may have commercial use(it's green), I wanted to know if the mix needed changing, drop the project or buy more chemicals.
perotter
06-01-2013
Quote Originally Posted by Desertbuck
I used the small pistol primer as the measuring scoop. So no they were
being filled three quarters of the way maybe. The priming compound was doing
its job there just wasn't enough of it. Thanks Perotter
Your welcome.
If you weigh an empty cup on your powder scale, fill it with dry mix, pack it and then weigh it again you'll know how much mix was used. You'll very like find that the amount of mix you used matches what the military lists as to how much the mix should weigh. This seems to work with any mix there is.
If one goes to using a wet mix(for safety if nothing else), one really should(needs) do a weighing step when setting up. One can't fill the cup and then pack it down to 1/2 full. A wet mix has to be measured by volume. That is why using some type of matching primer plates are really needed for a wet mix. Sometime mix up a little batch of mix and then wet it. You'll see that your pile of mix seems to disappear. So the same volume can't be used. That will also show that the mix is more intimate and likely to work better.
Don't get me wrong. I'm not saying one needs to do wet mixing. Whatever shoe fits, is comfortable and works is fine. Assuming that we are all over the age of 10, each of us are capable of deciding these things for ourselves.
perotter
06-01-2013
Quote Originally Posted by Bert2368
Has anyone tried for centerfire primers the technique they use for eley
rimfire ammo where the final reaction to produce the sensitizing primary only
occurs after the mix is in position?
Eley has 2 different processes using different chemicals for this. One I've done and the other not. The one that did will work for Berdan primers(according of a Olin(?) patent) but not Boxer. While a Boxer primers did go bang for me, I never tried them with powder and a bullet. I just figured that Olin(?) knew what they were talking about. And I don't really go looking for problems. But, it may be doable if one does a duplex primer method. Look back in this thread where I wrote some about non-corrosives.
So the one I monkeyed with, but not really used, can be done. The chemicals are available and I think one could get it working well for one's own use. For the duplex primer, I think putting a barium nitrate, aluminum and/sulfur and antimony wet mix to fill the cup after the anvil is put in would work. I'd have to say that the extra mix would need to weigh about 0.25-0.35 grains to work for a large primer. If nobody else does it, I might test how much can be added this way to satisfy my curiosity.
Their other method, as far as I know, requires buying a license from them and buying pre-mix from them. This is their lead styphnate mix. So it isn't really something I can do. FWIW, I think the ammo made in Mexico uses this for all their priming.
ofitg
06-01-2013
Quote Originally Posted by Nobade
Is it better to use shellac flakes dry and then wet out the whole mixture
with alcohol, or make up the mix and then wet it with prepared shellac? I
tried the latter and got 100% misfires. The mix wouldn't even work by hitting
it with a hammer. I assume I used way too much shellac.
Nobade, my "recipe" for the Span-Am War mix -
I pre-mix the potassium chlorate with sodium bicarbonate in a 25:1 ratio - eg, 2.5 oz of potassium chlorate to 0.1 oz of sodium bicarbonate - add a few spoons of water to form a "ketchup" consistency, stir thoroughly, then dry.
Weigh out the following dry ingredients -
17 grains of the potassium chlorate/sodium bicarbonate powder
9 grains of antimony sulfide
3 grains of sulfur
4 grains of fine sand (passes through a 40-mesh screen)
These dry ingredients are then mixed - a safe way is to pour them back and forth between two pieces of paper.
Next I add 1/3 CC (the small LEE powder measure) of Zinsser "Bulls Eye" clear liquid shellac from the hardware store. This product is advertised to be 21% shellac solids by volume. This works out to almost one grain of shellac solids per 33 grains of dry ingredients - almost 3% concentration, but it works fine.
Next I add enough denatured alcohol to achieve a "toothpaste" consistency for loading... since I'm loading percussion caps instead of primers for metallic cartridges, the subsequent steps are not applicable to this thread.
perotter
06-01-2013
Here is some about making and using primer plates that is wrote up. This hasn't been proofed by anyone and there may be a few things wrong. Don't be shy about pointing anything that is questionable. If it is really bad, I'm not to proud to delete it. Also, there is better information about doing this than what I have here.
One can make this any size they want. One doesn't have to fill all the holes, just one row or something. I also have a none matched plate the has a total of six holes. Three are for large, three are for small and space about 1 inch apart. I use that for when I want to try just a couple of some mix.
Drill pattern for the plates.
A x B x x x x x C x x x x x D x x x x x E x x x x x F x x x x x G x1. Space 3/8 or 10mm between X's and edges. More distance doesn't hurt.
2. Drill at least 3 stacked plates at the same time.
A. One will be for holding the cup.
B. One is for wet primer mix.
C. One is for the anvils, as a guide for removing the dent left by the firing
pin and mix packer, and as paper punch.
3. Drill A and G first using a 1/8 drill. These are the index holes
4. Hold the 3 plates together with 1/8 rolled pin(spring pin).
5. Drill B, C, D, E, and F with a 1/8 drill.
6. Remove the rolled pin and seperate the plates.
7. Drill 1 plate to the correct diameter for the cup.
8. Drill 1 plate to the correct diameter for the wet primer mix.
9. Drill 1 plate to the correct diameter for the anvil.
Note:
If you don't want to have different full sets for LR, LP, SR and SP add a 4th
plate for the anvil. Then you only need a large primer and small primer set.
To use for dry mix:
1. Put primers in the cup plate.
2. Remove anvils.
3. Put guide plate on and remove the dents in the cups.
4. Remove the guide plate.
5. Put a generous quanity of mix on the cup plate.
6. Level the mix over the cups with a bussiness card(etc).
7. Place the guide/anvil plate over on the cup plate.
8. Pack the mix with your pack pin.
9. Put anvils in the guide/anvil plate.
10. Press the anvil into the cups.
11. Remove the guide/anvil plate.
12. Place a piece of heavy paper, card board, etc over the cup plate.
13. Turn the plate upside down.
14. Lift the cup plate.
15. Place a piece of heavy paper, card board, etc over the primers.
16. Turn the 2 over.
17. The primer anvils will now be facing up and ready for laquer to be applied.
ofitg
06-01-2013
Perotter, here's a photo of the can -
In May 2011 I loaded up a few dozen caps, using two variations on the "Span- Am" recipe. In one variation I pre-mixed the potassium chlorate with sodium bicarbonate, as described above.
In the other variation I pre-mixed the sulfur with sodium bicarbonate - 10 parts sulfur to one part sodium bicarbonate, add water, stir, dry.
Just last weekend I tested 12 of the two-year-old caps, no misfires, but I got the impression that the "potassium chlorate pre-mix" caps were more energetic than the "sulfur pre-mix" caps.
Shelf life seems satisfactory to me, but I live in the Phoenix area, so this wasn't really a humidity torture test.
Desertbuck
06-20-2013
I am now mixing the mix wet with 90% rubbing alcohol then let the mix dry for 45min, fill primer cup with the now mostly dry mix to the TOP of the primer cup then pack. I next take an eyedropper put one drop of the rubbing alcohol on the primers and let dry. This seems to me anyway to bind the mix ok.
After they have dried I seat the paper disc and anvil.
I loaded just 5rd with my primers but side by side with CCI #200 I could not tell a difference when fired. So they work like a primer should now.
Anyhow I have a question. Will shellac or any binders like the hairspray weaken the primer mix? Like dextran will to Black powder? Do I need a binder to keep the mix in place, or will the method I just described hold up to recoil of shootin and long term storage?
perotter
06-21-2013
The US government mix that was used for the 30/40 Krag had 2% shellac. Last night I didn't find what was used in the 30/06 primers for binder. I don't know about the long term shelf life, but Ofitg's 2 years is good enough for my.
I ran the PEP software for a mix similar to what you are using and added 1% binder. As for power there showed to be 2% reduction in flame temperature(4000 instead of 4100 degrees). There was no real change in the amount of gas or solids produced. What I do know for sure about using a binder, is that the reliability and primer-to-primer consistency is greatly increased. For myself, I'll put in binder if at all possible. Plus, the commercial manufactures aren't putting in a binder because the CEO's brother-in-law owns a gum company.
You might want to try adding shellac or polyvinyl alcohol in that last drop you add. That wouldn't force you to go using wet mix.
perotter
06-21-2013
I don't think you are really making it more complicated than it needs to be. You just want to have a good result, just like the rest of us. Somewhere I have what binder and how much was used in the 30/06 mix. It wasn't in the first 2 sources I checked. But when I do find it, I'll post it to this thread. I've bought, photocopied and download everything I've ever found on making primers since I was teen. And that was many years ago. So sometimes I can't lay my hands of the info I've real quick.
super6
07-22-2013
My guess Is Nitrocellulose lacquer. Ring a bell?
Bert2368
07-23-2013
A lot of solvents that dissolve NC will also dissolve such things as styphenates, TNT, tetryl & etc. that are used in priming mixes. Alcohol/shellac is a likely candidate for a binder, so are such things as water carried mixtures of gum Arabic & guar gum. The gum Arabic binds and sticks the pellet to the paper disc, the guar gum can be used to control the consistency of the mix, making it less runny for easier handling-
Desertbuck
07-25-2013
Quote Originally Posted by Janoosh
Will this recipe work with/for rimfire cases? I am asking as I have both a
32 and a 25 rimfire rifle. The size of these cases make it easy to remove the
firing pin mark. And to reload with Black powder would not strain these rifles
nor have ignition problems.
I dont see why it would not work. The mix works real good with my black powder loads. The only thing I can think you need to watchout for is how much mix you put in your case.
perotter
07-25-2013
Quote Originally Posted by Janoosh
Will this recipe work with/for rimfire cases? I am asking as I have both a
32 and a 25 rimfire rifle. The size of these cases make it easy to remove the
firing pin mark. And to reload with Black powder would not strain these rifles
nor have ignition problems.
The one for the 30/40 Krag might be better or one with even more ground glass in it like Ron Browns. As far as I know all rimfire mixes have about 20%+ ground glass in them.
If I was to reload a rimfire corrosive without knowing what was done years ago, I'd try this:
90 grains of the 30/06 mix
10 grains of ground glass(etc)
See if that didn't work well. If not:
85 grains of the 30/06 mix
15 grains of ground glass(etc)
See if that didn't work well. If not:
80 grains of the 30/06 mix
20 grains of ground glass(etc)
Maybe go in 2.5 grain changes. I've never really paid attention to what the old rimfire mix was. So I'm not sure that I have it anywhere.
page 10
Bert2368
07-25-2013
An effective rimfire mix can be made by gently removing and crushing the tips of "strike anywhere" matches, then adding a little hot water to make a slurry thin enough so that you can drip a bit into the bottom of the case, then spin the case on an appropriate sized dowel or drill rod to centrifuge the priming slurry out into the rim.
Both the settlers and Indians knew how to do this 100+ years ago... Lots of rimfire cases found on archaelogical digs in the West have 2, 3 or more firing pin marks on them. Even given that some of the early rimfire guns had double firing pins to increase reliability with the somewhat crude priming technology of the times, we KNOW they frequently reloaded these cases.
perotter
07-27-2013
While looking for something else I ran across an old rimfire primer compound that one could make with much fuss:
"At this time a typical .22" caliber rimfire primer composition was the United States Cartridge Company's "NRA" which was:
Potassium chlorate 41.43%
Antimony sulfide 9.53%
Copper thiocyanate 4.70%
Ground glass 44.23%"
http://www.bevfitchett.com/chemical-analysis-of-firearms/priming-compositions.html
It has more glass than I thought it would. There are things in the link that might be of interest besides that mix.
delmar
11-11-2013
Quote Originally Posted by rastus
Would pumice work in place of sand? just wondering.
Sand or ground glass works pretty interchangeably. pumice would be abrasive as well but would be a lot lighter, I think, so I doubt it would work as well. Besides I can get sand really cheap and broken glass for nothing.
T-Man
11-18-2013
I use Strike Anywhere Matches. Carefully scrape the end cap off, use a mortar and pestle to powder it fine. Mix with a dab of denatured alcohol to a medium paste consistency. Carefully pry out the inner cover of the used primer, use a nail flattened on the end to tap the cup flat on an anvil. Pack with paste, re-insert primer component and load as usual.
Minerat
02-09-2014
Try Murdoch's I just got 3 boxes there last month. You'll probably have to go to the store. The box says diamond Strike Anywhere Matches 250 count. There are no part numbers on the box but Jarden Home brands www.diamondbrands.com is.
They are truly strike anywhere. You can even pop (strike) them with your thumb nail, just like my Grandpa did 50 year ago. I keep them in my hunting pack and they will strike on most anything, as long as it is dry and rough.
perotter
03-18-2014
For a simple(?) non-corrosive mix.
I've known for some years that the French non-corrosive mix was based on lead azide instead of the German method and chems we use. It look me a few years to find the details of what they did. When I did read it I found they still used tetracene like all other NC primers. That was disappointing as it still wasn't a single primary based mix. But, a few days latter I got to thinking about using just tetracene. While looking into that I found that the French had a new patent that did use just tetracene. Over that last few months I've gotten the chems need to make it. I didn't start with the easiest method, but the one that would ensure availability of the chems. I hope to test primers based on this patent in the next few months.
The patent is US 8,052,813.
Bert2368
03-19-2014
Looking at the litterature, azide is susceptible to degradation from CO2 and water vapor. Lead styphnate is not- Does anything degrade tetracene? What kind of storage life would be expected from such mixes?
The new "green" mixes based on DDNP are not going to store quite as well as the styphnate mixes either, from what I gather.
Marshall
03-19-2014
I read through the French patent and they do not make any claims about the stability and longevity of the tetracene based mixtures. From a chemical standpoint, none of the ingredients look like they would degrade one another during storage since they are regularly used together in other common non- corrosive primer recipes. My opinion is that the French tetracene mixtures will be as stable to storage as the lead styphnate based mixtures.
I am looking forward to hearing about perotter's results after he completes his tests. In the meantime, I'm going to research the synthesis of tetracene and guanidine sulfate.
Bert2368
03-19-2014
Well, guanidine sulfate is dead easy from ingredients at Home Depot- See this link, it's the first step.
http://www.sciencemadness.org/talk/viewthread.php?tid=8911
perotter
03-19-2014
Thanks for the link on making guanidine sulfate. I have a few method that I've gotten from that sight on how to make basic chemicals needed. I'll have to look into this one more.
I have to agree with Marshall that a tetracene based compound would have as long of life as a lead styphnate one. Largely because a lead styphnate compound won't work very well without tetracene. One of the reasons I'm interested in the tetracene mix is because I can't find any practical DIY mixes that don't use a percentage of tetracene. I figure if one has to make it anyway, using it as the only primary makes for less work.
Marshall
03-21-2014
I just ordered the chemicals to make guanidine sulfate from Amazon:
5 lb 99%+ Urea, $9.99, free shipping
3 lb 99% Sulfamic Acid, $15.00, free shipping
I also checked Home Depot and their 1 lb can of sulfamic acid was $5.95 + tax
I was not able to find a good deal on the sodium nitrite at Amazon. The best value was 10 lb for $39 + shipping. This is way more than I need and the cost could be better. Most of the products for sale were pink colored and intended for curing meats. Perhaps the grocery store or drug store can do better. Anyone know of a better source of this chemical?
-=-=-=-
Update: Found an OK deal on NaNO2 at ebay
2 lb 99% Sodium Nitrite, $7.75, $10.55 shipping @#$$%%^&
-=-=-=-
I also checked into directly buying the guanidine sulfate. This chemical is on the expensive side. There were several folks selling guanidine hydrochloride for a better price ($28 for 100 gm), but I am not sure if that chemical could be substituted for the sulfate. I am guessing it would make the primer mixture corrosive since NaCl instead of Na2SO4 would be the likely by-product from reacting the guanidine salt with NaNO2. This assumes you are generating the tetracene in situ as described in the French patent.
Oreo
03-21-2014
We need to exercise a lot of caution in what we admit to buying and making here. I suggest making all statements in purely hypothetical terms. No one wants an early morning visit from the jackboots.
Bert2368
03-21-2014
FYI: BATFE "Orange Book" (Federal Explosives Laws & Regulations):
[LINK 404]
Because ignorance isn't an excuse-
I have never been treated poorly by an employee of BATFE. But I have the appropriate licenses for my work, and follow the applicable laws.
Assuming one doesn't commit an act of terrorism or other federal offense and is not found to be improperly storeing , selling, transporting or giving away any explosives, your problems are not likely to be with BATFE. However! State and local laws and attitudes are all over the map on this, you'd best know your local situation in that regard. Angering your neighbors is something you shouldn't do
While we should allways remember that communications on the Internet are every bit as private and difficult to connect to yourself as if, say, you were screaming them at the top of your lungs standing naked on main street- Short of obtaining large quantities of the more highly watched chemicals, buying obvious immediate precursor sets to make those forbidden chemicals, doing something to anger the neighbors or otherwise attract local law enforcement's attention- there just isn't enough time in the fed's day to bother with mere internet chatter. If you DO go and "wave your **** in their faces": Yes, you should expect to see your online history read to the jury by a DA. So don't.
As far as "ending up on a list"- There are now so many lists, so little discrimination on what triggers being entered on same, and so many types of surveillance on ALL communications... We are all on lists.
perotter
03-22-2014
Quote Originally Posted by Oreo
We need to exercise a lot of caution in what we admit to buying and making
here. I suggest making all statements in purely hypothetical terms. No one
wants an early morning visit from the jackboots.
We have been down this road a couple of times on this forum. I've posted the Federal laws on this site and it isn't illegal to make, have or use the - chemicals and final products for making ammunition primers or the the propellant for ammunition for ones own use. No Federal license is needed. But when I talk (verbally) about this topic in public and someone seems upset I do say that I have all the needed licenses to do this. A true statement because none are needed when dealing with these things in small quantities and use.
Also, when I do have a question about any legal issue about a chemical that is used for making primer compounds or propellants I call whatever Federal agency that is applicable about it to clear any concerns.
perotter
03-22-2014
Quote Originally Posted by Bert2368
As far as "ending up on a list"- There are now so many lists, so little
discrimination on what triggers being entered on same, and so many types of
surveillance on ALL communications... We are all on lists.
A couple of chemicals that are used for making primer compounds that I would both Google search about and look for on Ebay slowly (month or 6 weeks) quit showing up in the searches. To point that with Google I would almost think it didn't even exist as a chemical. One day I used public computer to do a Google search. There was no shortage of hits. Same with Ebay. Draw your own conclusion.
Also, I my case, companies that would sell me certain chemicals wouldn't any longer. Some just said they wouldn't sell to me and others stated very high prices. One that I'd bought from that had charged $100 for 500 grams wanted $8,000 for 500 grams. They said there was no problem selling to me for that price. I very truthfully said that as I needed it to finish up testing before filing for a patent, I'd pay that much. They then said that they wouldn't sell it to me. Again, draw your own conclusion.
I'm not trying to scare anyone nor making any claims here that the government/corporations are making effort to deny people freedom, etc. I'm just stating what I've experienced.
perotter
03-22-2014
Quote Originally Posted by Marshall
I also checked into directly buying the guanidine sulfate. This chemical is
on the expensive side. There were several folks selling guanidine
hydrochloride for a better price ($28 for 100 gm), but I am not sure if that
chemical could be substituted for the sulfate. I am guessing it would make the
primer mixture corrosive since NaCl instead of Na2SO4 would be the likely by-
product from reacting the guanidine salt with NaNO2. This assumes you are
generating the tetracene in situ as described in the French patent.
Is it guanidine sulfate or aminoguanidine sulfate that you are finding? I haven't yet found a method to convert guanidine sulfate to aminoguanidine sulfate. Do you know of one?
Marshall
03-22-2014
Perotter, you are indeed correct. It is actually aminoguanidine sulfate that is needed. The reference above from Bert2368 provides the first step. If you finish the synthesis to nitroguanidine, I found a reference that this material can be reduced to aminoguanidine sulfate using zinc dust. There probably are better ways, but I haven't yet completed an exhaustive search of the literature to find them.
I found where I was misled into thinking it was guanidine sulfate. The French patent refers to it as follows:
"According to a preferred alternative for obtaining a composition of the invention, a method is used whereby the tetrazene is formed in situ. According to this method, a dry mixture is prepared of a nitrite salt and a neutral guanidine salt, that is the reactants for preparing tetrazene, and the other components of the composition. An appropriate quantity of this dry mixture is then placed in the initiation cavity, the mixture is compressed and then humidified, this step causing the formation of the tetrazene, and the composition is finally dried. This process is suitable for all starting reactants for synthesizing tetrazene, in particular sodium nitrite and/or guanidine sulfate, and all components of a composition of the invention. This method is highly advantageous in that it combines handling safety with environmental safety."
The way "guanidine sulfate" is used in the next to the last sentence is what caused me to think that it was the precursor to tetracene. Further reading about tetracene cleared up that it was aminoguanidine that was really needed. In fact, the term aminoguanidine is not used in the patent at all. I guess those who are familiar with the state of the art would know this automatically. Well, I don't think I wasted my money since you can always use fertilizer and cleaning products around the house.
page 11
perotter
3-22-2014
I really should have given a warning about French patents and what they call chemicals. Even when it is in English they, for some reason, use different names than the rest of the world.
That was the reason I could never find their patents for non-corrosive lead azide primers. They call it lead nitride. A year or so ago I seen in an old German paper they had something like this: lead azide(lead nitride). I then was able to find some French primer patents that called it lead nitride in them. That lead to the patent of the current topic.
I think that the French just like to march to a different drum beat.
perotter
03-23-2014
I agree with you Marshall. Any patent(French or otherwise), IMO, is more a "What is possible" and it is a "Here is how to do it". Plus sometimes(usually?) a bit of exaggeration as to the benefits. I'm looking at this patent with the view that tetracene will work by as the only primary and about how much to use in combination with other chemicals. I'll also, at least at first, be looking at doing it by mixing the primer compound outside of the cup and not making the tetracene in the cup.
FWIW. The French powder company is the only one's I know of that still actively working on using ammonium nitrate as a propellant for ammunition. Or at least finding thing that can be patented.
wicket
04-06-2014
Excellent thread, lured me from lurking. I've seen a reference to iron sulfide as a substitute for antimony sulfide in chlorate priming mixtures, but can't remember where, anybody ever run across it?
Bert2368
04-06-2014
I have not seen anything related to priming compositions, but:
Iron 2 sulfide, FeS is pyrophoric- If you grind it finely enough, it will spontaneously catch fire!*I would prefer NOT to be the one mixing this into a batch of primer composition.*It's also one of those "indeterminate" compounds, the ratio of Iron to Sulfur in a batch is variable.
Iron disulfide, FeS2 is better known as Iron pyrite- Fool's Gold. It DOES have a history in firearms ignition- As the "flint" used in wheel lock firearms... It definitely does burn.
In mines where Pyrite is exposed to air, modern miners usually dust the mineral's surface regularly with ground limestone to prevent spontaneous combustion.
Iron pyrite in contact with air continuously decomposes into Iron and sulfate, there is a common bacteria that causes this.
http://en.m.wikipedia.org/wiki/Acidithiobacillus
The sulfate combines with any moisture (humidity!) to make sulfuric acid. Sulfuric or sulfurous acids DECOMPOSE CHLORATE.
Before the Lead chamber process, most sulfuric acid was made by leaving heaps of Iron pyrite out in the weather and collecting & concentrating the rainwater running off the heaps- So it's not a good choice with chlorate if you need your primers to be storage stable.
Isn't chemistry fun?
wicket
04-06-2014
Chemistry is indeed fun Bert. Back in the day making iron sulfide was one of the of the experiments in the manual that came with Gilbert chemistry sets, i remember being annoyed because Gilbert failed to mention that making the stuff cost you a test tube. Was entertaining making hydrogen sulfide from the iron sulfide though. The need for buffering the sulfur in chlorate mixtures already had my ears up, doesn't sound like iron sulfide improves matters, thanks for your input.
ofitg
04-06-2014
Wicket, if you don't want to mail-order antimony sulfide, it occurs naturally as a mineral called Stibnite.
You can do it the "old fashioned way" by getting a good Stibnite crystal from a rock shop (or eBay) and pulverizing it yourself.
Bert2368
04-06-2014
Quote Originally Posted by wch
Yes, you can make priming compound.
Now, can you grow new fingers and/or eyes?
I'm more worried about hands. Pshaw, fingers? Hell, you start with 10, who's gonna miss a couple? Explosives handler for 20+ years. Federal license to manufacture explosives for the last 12 years... All fingers & eyes in place. Possibly because I DON'T make priming compounds. I do answer safety related questions from others about the chemistry though.
I have "hands on" experience with lab scale synthesis of primary explosives used in some of the modern mixtures. And production batch sized experience with chlorate based pyrotechnic mixtures.
What is done to make reliable chlorate primer compositions is just about the perfect opposite of what is done to make a safe to handle chlorate fireworks star mixture- Sulfer. Sulfides. Thiocyanates. Ground glass/grit. I would need a REALLY strong reason to handle this type of mix, and even then it would be in very small quantities.
The single compound primaries are an interesting and very mixed bag as far as sensitivity and handling dangers when considered as individual chemicals, but they've got the same range of properties (SENSITIVE!) in their final condition as dry priming mixes, they have got to respond to the same stimuli.
I do like the several methods such as Ely prime patent method and the French method where the final reaction takes place only after loading. How I would do it if I HAD TO.
wicket
04-06-2014
Well gentlemen, it's like this: home-made caps are pretty much the final challenge to the self-sufficient black powder shooter, so i figured to take a run at them. Beyond making a couple of the more common fulminates years ago, i'm a babe in the woods regarding initiators. I have half an old bottle of Merck KClO3 kicking around, so figured to work from that. With the level of data mining going on out there in the real world and my own native paranoia, i'd just as soon try to do this with as little fanfare as possible given the joyless smothering embrace of the nanny state.
Bert2368
04-06-2014
Quote Originally Posted by wicket
Well gentlemen, it's like this: home-made caps are pretty much the final
challenge to the self-sufficient black powder shooter, so i figured to take a
run at them.
I understand completely-
Considering you should get around ?15-20? caps per gram of composition, you don't HAVE to work with quantities that will kill you. A couple of grams of a chlorate/Sulfer/Antimony tri sulfide composition not enclosed in a caseing isn't. Yes, eyes are at risk. If you add Mercury fulminate to the mix, it's snappy enough so fingers definitely are at risk, even with the mixture uncontained. An 80:20 mix of fulminate:chlorate was pretty standard blasting cap filler for a while before WWI.
Wear eye protection, keep amounts handled to a minimum, study carefully the historical information and safety literature. I don't choose to do this, but I'm certain you wouldn't want to do some things I routinely do either!
wicket
04-06-2014
Well Bert, i just took a crack at Forsythe's original mixture, and getting my Ohaus to weigh to .01 g is gonna involve potentially interesting levels of Kentucky windage. I used up all my store-bought HNO3 years ago, so fulminates are off the table, unless i get ambitious enough to make some acid. I probably don't need anything too snappy anyway, i use NC combustible cartridges and it doesn't take much to spark them to life.
What's aggravating me at this point is finding a substitute for the antimony sulfide, and figuring out a way to get what's probably 10% bentonite out of my sulfur since i don't have much more than a couple ounces of USP sublimed sulfur left. What's the story on tin sulfide as a substitute?
perotter
04-06-2014
Also, for 2 reasons, use a wet mix to make primer. It's much safer and if a little binder is added, they are more consistent when used.
For using tin sulfide use the amount is about the same as antimony sulfide. I don't have much information on it's use and as far as I know only the French test or have used it.
perotter
04-06-2014
Quote Originally Posted by Bert256
but I'm certain you wouldn't want to do some things I routinely do
either!
Having an idea as to what you do, there is no way I'd want to do it. It would have to be a real emergency. I had a cousin who was a professional(licenses, insurance, etc) in your line of work. I didn't like to be around when he was working. It was interesting, but I preferred more of a lecture on the topic than a how to demo.
Bert2368
04-06-2014
Skylighter or Firefox have antimony tri sulfide and good quality (low acid) rubber maker's Sulfur.
http://www.skylighter.com/mall/chemicals.asp
http://www.firefox-fx.com/chemicals.htm
The 200 mesh "Chinese needle" Antimony tri sulfide is just ground Stibnite ore. I'm fairly sure the 325 mesh is the same material after being milled.
Garden store Sulfur with 10% anti cake is soluble in hot Toluene... And re- crystallizes when the Toluene cools to room temperature. If you're willing to filter a hot Toluene solution, this separation isn't too tough.
http://woelen.homescience.net/science/chem/exps/S+toluene/index.html
(edit) oops, wrong horribly smelly flammable solvent!
wicket
04-06-2014
Hot toluene's the solvent, but there's some debate about what's actually in paint store toluene these days, basement chemistry was a lot more fun before all the chemophobes got loose from their canvas jackets. Thanks for the suggestion though Bert, I'll try the solvent method with whatever Ace Hardware is selling and see how it goes.
Copy/pasted this from a chemistry forum : "Iron Sulfide might be a better substitution if you have no Antimony Trisulfide, prepare some by igniting Iron powder and Sulfur (about 56:32) in a crucible. It has about double the melting point which will make it less effective, Bismuth Trisulfide might be worth a try instead (81:19), or simply get elemental Antimony and prepare the Trisulfide from that (72:28). Using excess sulfur (e.g. 50:50 mixes) in these preparations and burning it off (outside!) is an simple and expedient production method." Not the reference i was looking for, but it's hopeful.
Bert2368
04-06-2014
Sorry about misremembering the solvent there. You CAN distill the **** sold at the paint store and just use the fraction coming over at the right temperature range- but we're getting further and further into the weeds here.
I've SMELTED Antimony tri sulfide into Antimony metal by roasting! (Antimony regulus, ask an old time printer or foundry hand) Never tried to MAKE the tri sulfide... The stuff comes out of the ground ready to use, sort Stibnite from the surrounding rock, crush and mill it to the right size.
I am totally spoiled. Just buying the chemicals ready to go leaves you a lot more time to use them.
I've not seen the Tin sulfide version of these primes. Bismuth sulfide? I've never even seen any. We use Bismuth trioxide for a few things.
Just in case anyone has some DO NOT USE ARSENIC SULFIDES. They make things too sensitive to handle when dry, think about those little pull string booby trap novelty fireworks.
wicket
04-07-2014
Interesting about the arsenic sulfide Bert, wish i knew more chemistry, be nice to understand the subtleties involving various metallic sulfides as additions to the mixture under discussion. I'll try the sulfides of iron and tin since i have the precursors, and then drop metallic sulfides. Perotter, i will work wet once i get a promising formula, even with a face shield and gloves i'm not too keen on messing with much more than a gram of this stuff at a time; i need to keep my oculars and appendages functioning to deal with machining some sort of die to stamp the copper into caps.
The experiment with Forsythe's original mixture was unimpressive. With and without ground glass it declined to respond to either friction or impact. Ignited with a flame it fizzed lazily like poorly made gunpowder, and left behind a residue of slag that would have clogged a fire hose, i doubt firing it in confinement would have improved matters significantly.
page 12
Oreo
04-07-2014
I don't understand the effort to find antimony trisulfide substitutes when the real stuff is easy to find.
I sure wish phosphorus was easier to come by though. All this chemistry stuff would be a non-issue and non-corrosive primer mix would be easy to make.
wicket
04-07-2014
Given the limited uses for antimony sulfide, i don't like raising my hand with an online purchase. Second point is that i can buy caps locally, same way i can buy powder, ball, and wads, but was curious how far i could push the envelope of self-sufficiency.
Even when i was a kid white phosphorus was tough to get, red you could find, but tweekers closed that door; probably saving some folks from the repercussions of playing around with Armstrong's mixture.
I agree that looking for substitutes or manufacturing necessary chemicals can be a pain in the neck Oreo, it's like being twelve again and lying to the pharmacist to buy KNO3, but it's a fact of life these days.
Bert2368
04-07-2014
(EDIT)
It's not an oversite that VERY dangerous to handle, insanely sensitive mixtures are given in these posts and links. The information is out there in many other places already. If you are foolish enough to make them, you WILL have an unintended ignition or explosion, the only question is when and how much it will cost you. Pee on the electric fence for yourself if you must-
------------------------------------
Let's COMPLETELY avoid the red Phosphorus/chlorate family of Armstron's mix and related... and the Arsenic sulfide/chlorate family of red explosive and relatives...
As far as things that are just too **** sensitive when mixed with chlorates, which I won't make and strongly recommend YOU all avoid:
Anything in here:
http://www.privatedata.com/byb/pyro/impactfirecrackers.pdf
And EVERYTHING in here:
Armstrong's deadly brew - My original article
Donald J Haarmann aka The WiZ
American Fireworks News #51 December 1985
A letter of some months past detailing a reader's experiences with nitrogen
tri-iodide, has occasioned this missive on its potentially lethal cousin,
Armstrong's mixture.
Dear WiZ,
"Quite some years ago (30?) I happened upon the following in the Popular
Science Book of Formulas: Recipes, Methods & Secret Processes. (1932) 'A
sensitive detonating mixture is made of potassium chlorate 10 parts, black
antimony sulphide 5 parts and red phosphorus 1 part. Mix without friction and
at some distance from the operator's face. It is quite sensitive to blows,
very unlike [?] the potassium chlorate sulphur mixture.'
"In those bygone days it was easy to obtain chemicals either from the local
druggist (who was probably amazed at the amount of potassium nitrate my mother
required for "preserving meat") or any chemical supply house. One local
chemical supply house would even give me a discount for being a student.
Therefore, obtaining the required reagents was not difficult.
"I started out by putting the mixture in 0000 gelatin capsules. Just throwing
them up into the air was sufficient to cause detonation upon impact with the
ground.
"One day a friend and I loaded quite a large amount into a cardboard tube that
BB's come in. We backed off quite a bit and fired upon it with a Daisy pump
action BB gun. The second or third pellet found the mark, resulting in a
tremendous blast which rocked us back on our heels and caused the propane gas
tanks next to the house to ring as though they had been struck by a hammer!
"This progressed to placing the material into a (you don't want to know).
Threw one off the roof of my friend's apartment house one night toward the
vacant lot directly behind. However, its errant trajectory caused it to
land/detonate on the fire escape of an adjacent building! Scared the S- out of
someone who was peacefully watching TV with the window open.
"For the ultimate and final folly, had taken to adding magnesium to increase
sensitivity! (Bet the second thing you did with your Chem Craft chemistry set
was to find all the fun things you could do with Magnesium!) At that time our
families both had country homes to which we adjoined each summer. In the
surrounding woods my friend and I had constructed a small shack. On this
fateful day while seated on the ground at the back, my friend was seated on a
stone wall directly in front mixing, when KABOOM! WHAT A BLAST!!! The smoke
blew away, and HE WAS GONE!!!! GOOD GRIEF, what am I going to tell his
mother???? He blew himself up and I can't even find the pieces?!?!
I am happy to report my grief was short lived, for these few seconds of no
little anguish were relieved by a plaintive cry of' Pssst -- Pssst I'm over
here, coming from some yards away. For as luck would have it, we (he) were
using a cardboard container, and "all" that happened was the bottom blew out,
resulting in numerous small holes in his blue jeans from the unreacted
phosphorus, and a not little-bit sore, blackened hand. There is, in
retrospect, no doubt in my mind that had mixing been completed and the whole
batch detonated, he would not have been able to play the piano. Regards,"
Name withheld under pain of having flaming arrows being sent in the WiZ's
direction while he is making flash and report.
Yes, indeed. I would add the following quote from the American Pyrotechnist
for March 1978. "[a PGI member] dry mixed about a teaspoon of potassium
chlorate and [red] phosphorous, put it in a plastic 35mm film container, and
it ignited or exploded violently just from the slight friction of snapping the
cap on! He says that he has learned his lesson, but the injuries to both hands
were so disabling that he will not be able to correspond with other members
for about 2 months."
Some time ago an outfit called Howell Laboratories, Folly Beach, SC, sold
through an advertisement in the Shotgun News information on a "frictional
impact explosive"
The information turned out to be 5 small photo reproduced pages on the
compounding of Armstrong's mixture, for use in "Security Bombs" (booby traps),
"Smoke Screen" (combined with ammonium chloride), "Impact Grenades" (gelatin
capsules), "Explosive Rodent Traps" ("It let's you know when a mouse or rat
has been caught."), and "Impact Detonator”, and "Explosive Paint" ("This
explosive paint lends itself well to practical jokes.") [Sure!] One half pages
were devoted to safety in compounding, with the admonishment that "A pencil
eraser sized piece will put the loudest fire cracker to shame, while a thimble
full will rival a stick of dynamite." Perhaps somewhat over stated, but not by
much.
An accident involving a substantial amount of Armstrong's mixture was reported
in Explosives and Their Power. Translated and Condensed from the French of M.
Berthelot. London 1892.
"The explosion which occurred in Paris, in the Rue Beranger, on May 14, 1878,
may also be mentioned, in a store containing amorces [caps] intended for
children's toys. These amorces were composed as follows:
One kind, called single, of a mixture of potassium chlorate (12 parts),
amorphous [red] phosphorus (6 parts), lead oxide (12 parts), and resin (1
part); the others, called double, consisted of a mixture of potassium chlorate
(9 parts), amorphous phosphorus (1 part), antimony sulphide (1 part), flowers
of sulphur (0.25 part), and nitre (0.25 part). The latter, more sensitive to
friction, averaged 0.01 grm. in weight. From six to eight millions of these
amorces pasted on paper slips, in lots of five each, were piled up in the
warehouse in boxes. A few of these having become ignited by an accident, the
origin of which was never clearly ascertained, caused the whole to explode.
One building suddenly gave way, the facade being blown out, and the stonework
hurled some distance. One stone, measuring a cubic metre, was thrown to a
distance of fifty two meters. A great part of the adjoining building was also
destroyed, fourteen persons were killed on the spot, and sixteen received
injuries.
"These terrible effects are explained when we consider that the weight of the
entire explosive matter contained in the amorces amounted to about 64 kgms.,
and that its force, owing to the composition of this matter, was equal to a
force of 226 kgms. of black powder. (These facts have been taken from the
report presented by the Committee of Inquiry.)
"It is essential that persons having explosive substances under their charge
should never lose sight of the conviction that, from the facts and general
truths which have just been stated, preventive measures should always be
prescribed on the hypothesis of an explosion." [Amen.]
I hope that these experiences point up the folly of working with combinations
such as Armstrong's mixture, its cousin the red explosive mixture, and other
less than safe and sane mixtures, i.e. potassium chlorate and sulphur, or
potassium chlorate and antimony sulphide, which, by by, was used during the
civil war in land mines! Further, although Armstrong's mixture and the "red
explosive" can be compounded "safely" when wettedwhat are you going to do with
them when they have dried out??
Although the word "detonation" is commonly used in connection with
pyrotechnics, the only comp that has been tested and found to produce true
detonation is potassium chlorate and sulphur. However, it is my firm belief
that if Armstrong's mixture were to be tested, it too would be found capable
of detonating.
Other than toy caps and such, the only modern use for Armstrong's mixture I
have been able to locate are three US Patents (4,372,210, 4,191,947,
4,130,082) describing intrusion alarm systems using the radiant output from
MAGICUBE flash lamps to initiate a quantity of Armstrong's mixture or SUPER
BANG CAPS (potassium chlorate, red phosphorus, manganese dioxide, sand and
glue) to produce an audible alarm.
Finally, A Thought for Today: There are old pyro's and there are bold pyro's,
but there are no old unlucky pyro's!
HELP WANTED
Even the WiZ does not know all (yet). Who, if any one, knows who Armstrong
was, and/or how his name came to be associated with the combination of
potassium chlorate and red phosphorous? WiZ
---------------------------------
HE DO NOW!
"Sir Williams Armstrong's explosive mixture for shells contains amorphous
phosphorus and chlorate of potash."
Rudolf Wagner - Handbook of Chemical Technology” D. Appleton and Company,
New York 1872.
Reprint by Lindsay Publications inc. pg. 546
Oreo
04-07-2014
Anyone know how to get phosphorus from phosphate? Phosphate is easy to come by.
perotter
4-07-2014
Quote Originally Posted by Bert2368
Have you previously handled red Phosphorus:chlorate mixtures?
You don't use a red phosphorus/chlorate mix to make non-corrosive primer. Beyond safety, it would still be corrosive.
You use a red phosphorus/barium nitrate mix for DIY. The US Army even officially adapted this for the 30/06 for a while after WW2. As soon as Remington's the patents ran out, the military dropped it's use. Mainly because it didn't have a long life. Now that most of the red phosphorus used in the US is coated, the DOD is spending millions to get ATK's P4 primer mix perfected.
PS
See post #38 in this thread for more information on the 1940's red phosphorus
mix. Also, the book Dutchman is selling has a couple of mixes in them also.
They are from the same era.
Bert2368
04-08-2014
De nada, I'd read it a couple of times.
For a pretty good overview of the matter, this is free online:
http://www.researchgate.net/profile/...dabf19270d.pdf
http://www.researchgate.net/profile/Jaime_Wisniak/publication/228647357_Phosphorus-From_Discovery_to_Commodity/file/60b7d515dabf19270d.pdf
perotter
04-08-2014
Here is a patent of ATKs for modern red phosphorous based primer mix. Some will find many other interesting patents by checking what other patents are reference or are referenced.
https://www.google.com/patents/US8540828
Here is the patent for coating red phosphorous with plastic. While the patent was for other reason, doing so for a primer mix greatly extends the live of primer.
https://docs.google.com/viewer?url=patentimages.storage.googleapis.com/pdfs/US4698215.pdf
perotter
04-09-2014
A non-corrosive primer can be made using phosphorus sesquisulfide. That is what I was looking a getting a patent on. It's commercial value would mainly be in getting a simple 'green primer' that might compete with ATKs. As I can no longer get enough phosphorus sesquisulfide to test it, I'll just put it out there. If some one can get it, it is worth using.
Phosphorus sesquisulfide has to coated also. Seems to only last a few day when mixed with most nitrates. With lead nitrate it lasts longer. I think if it was coated, it might last with other nitrates. The few 'green ones' I tried would only fire for 1 to 3 days after mixed and or put into a primer cup. Coating it should allow any nitrate to work.
I found that mixing it wet with a binder was needed to get it to fire 100% of the time.
FWIW: I wasn't able to 100% just substitute it for red phosphorus and have it work well.
Oreo
04-10-2014
Here's a link to a thread about how to make phosphorus. Its over 10yrs running and nearly 50pgs long but it really covers a lot of ground with a few successful, simple demonstrations of producing P in quantities up to several grams. The hard part seems to be providing enough heat for several hours of what is essentially a reduction and distillation process.
http://www.sciencemadness.org/talk/viewthread.php?tid=65
wicket
04-12-2014
The retorts based on black iron pipe looked practical, a decent burner and down-draft kiln purpose-built from insulating firebrick would probably fuse the silica and get the reaction going.
Jesse Early
04-19-2014
Look for an old Airbag from a car. The home made stuff is iffy at best. Armstrong mix is nasty nasty stuff. I think airbags have lead azide, we use the stuff in military blasting caps and i think some companies use it primers. I know some guys that will buy up airbags at junk yards for the explosives to build home made detonators.
This is what i would suggest, its called a hammer friction test
You place a small sample on a piece of steel, then use a regular hammer and place it on the explosives softly then gently push it flat and rub it back and forth increasing pressure. You are attempting to generate heat and friction. If it doesn't pop with this action then gently tap it hitting it harder and harder until it pops. Try and keep your impacts flat so you maximize shock and friction. This test is what we do in the military when we find home made explosives to test there sensitivity.
page 13
wicket
04-20-2014
That's useful information about the hammer test Jesse. Since my caps are intended for black powder I'm hoping to get away with a minimal charge of some sort of chlorate mixture. I tried Forsythe's original mixture of 70.6 parts of potassium chlorate, 1.8 parts charcoal, and 17.6 parts of sulfur and grit, but couldn't get it to spark hitting it with a hammer.
Now that I have some empty caps made I'll probably test right on the gun, I'm trying to find a composition that doesn't blow the petals off the caps but still lights the powder effectively.
wicket
04-23-2014
Have so far tried chlorate/ sulfur, chlorate/ iron sulfide, and chlorate/ tin sulfide, the mixture with tin sulfide burns cleanest, and goes off with a "poof" when a small pile is lit with a torch flame, it's also the only one of the three mixtures that doesn't blacken the copper caps when fired.
All three mixtures failed Jesse's hammer test and were dry pressed into the caps without any premature ignitions. The sulfides were ground to 60 mesh, the grit was 20 mesh crushed glass. The caps opened but didn't blow apart, and all three formulations had no difficulty igniting combustible cartridges.
Gun_nut83
05-31-2014
I got to about the fourth page and had to stop and quickly add this post to anyone trying to make the compound using the following chem:
potassium chlorate
sulfur
grit (ie. chalk, sand, baking soda et cet et cet)
and red phosphorus
This compound is commonly known as "Japanese or cap torpedoes" primers.
CAUTION: This compound MUST be mixed in TWO (2) parts!
One part the first three chems and they MUST be moistened to a porridge consistency, BEFORE beginning to mix them with a wood rod. In a separate container the red phos should be moistened too BEFORE adding to the first part of the compound. If you don't do it this way it will certainly explode in your face, proceed with caution! I can't stress this enough.
With all precautionary measures taken there is no reason THIS formula won't serve you well to reload your primers. It's simple and it's effective and reliable. The paper cap method while easy and safe isn't completely reliable. I've used both methods and have had misfires on the paper cap but not the cap torpedo primers. If you need more info I'd be very willing to give exact detail on the process and formula.
perotter
06-14-2014
If a person can get red phosphorus, it is better to use it in a non-chlorate based mix. If one uses a nitrate based mix, it is not only safer to make it is also non-corrosive.
Gun_nut83
06-14-2014
I won't say red phos is "EASY" to get, but I will say it is more available then one would believe if you want to do the work to get it. What chemical compound would you recommend in stead of potassium chlorate? Potassium nitrate?
perotter
06-14-2014
Barium nitrate is what the US Army used in the 1940's. Use: BN=80% with RP=20% or better use BN=56%, PR=25% and 17% antimony sulfide. Add 1% gum if you are mixing it wet and that is what I'd recommend. Depending on the powder you're using, you might want to substitute 3-5% aluminum powder for the same percent of antimony sulfide to give a quicker/stronger ignition to the powder.
perotter
06-14-2014
Quote Originally Posted by DeanWinchester
You fellers could always try some Nitrogen Tri-iodide. Ya wouldn't even
need a firing pin! LOL!
Iodine could be hard for some(most?) people in the US to get as it is on the DEA list. It is easy to get here in farm country though. Nice and easy to make. To bad it is to sensitive. There is one compound that will work, that is easy to make and every grocery store in the US has what is needed to do so. I'd use it in real pinch, but only if there would be a very big problem in a gun using a corrosive mix. Of course if you could get those thing in a grocery store, I'd have to think want was needed to make sulfur nitride would also be available.
perotter
06-14-2014
FWIW, potassium nitrate doesn't 'like' to give up it's oxygen as easy as some other nitrates. That is why a small amount of a some other primary is added with it when making primers. That way one can get 100% ignition and at a burn speed that is desired.
wicket
06-24-2014
I wouldn't make Armstrong's mixture or nitrogen tri-iodide in the first place but would select a somewhat more stable compound made from more readily obtained ingredients, and would prepare it in small batches as needed while wearing appropriate safety equipment. There are two ways around the current cap shortage: one is to make functional caps safely and efficiently in small quantities as needed, the other is to damage oneself physically to the point that caps are no longer needed.
Marshall
06-24-2014
I have made many small batches (~2 gr) of Frankford Arsenal H-48 primer composition for my primer reloading experiments. It has the perfect combination of stability during fabrication and handling, and firing reliability. When moistened with alcohol it is practically inert. I have found that H-48 compound is far less sensitive than working with toy caps. So far, I have reloaded in excess of 5,000 primers (mixture of SP, LP, 5mm Berdan, and 209 primers) without incident. All this talk about using materials (e.g. Armstrong's mixture, nitrogen triiodide... etc.) that are known to be too sensitive for use in primers is silly and indeed dangerous to those who do not understand their risks. Stick to the well known formulations that have been used by our military in the past and you will have success and safety.
Work with small amounts of primer compound (I make ~25 SP primers in a batch run that takes ~0.5 gr of compound), use non-sparking tools and wear the appropriate safety equipment and you will not get hurt.
Regarding reliability of H-48 primers, I have only had 2 FTF so far in my testing of 500+ H-48 primers and those were due to light primer strikes. Perfectly acceptable for practice ammunition. When I use my own cast lead bullets and homemade primers, my cost/round for .380 ammo is $0.008. Yes, 0.8 cents/round!
wicket
06-24-2014
Same experience here Marshall, but with FH 42, i diaper the mixture then load and press dry for percussion caps. It's interesting that word is starting to get around about employing the composition from toy caps (probably Armstrong's mixture) resulting in accidental detonation when the cap is placed on the percussion nipple. It's not generally a life/death issue with a percussion revolver since capping takes place before the chamber is aligned with the barrel, but with a rifle or single shot pistol the consequences can be lethal.
As you mention, the price can't be beat! My suspicion is that even when the uncertain supply problem goes away (assuming it does this time) that prices are going to remain substantially higher, so there's a considerable monetary incentive in learning how to produce safe effective primers.
bannor
06-24-2014
Only if your (skilled, at risk) time making primers is worth nothing. Sounds to me like you'd have to get 20c per primer if you sold them by the thousand, just to make minimum wage.
wicket
06-24-2014
Dunno bannor, i have a dual function press-operated die, am upgrading to a 24 cap loading tray, and don't have to drive 45 minutes each way to maybe get a tin of CCI # 11's. What kind of equipment are you using, and what's your reasoning behind making "lots" of primer in a bunch of small batches?
perotter
06-27-2014
Thanks for letting us know that the Frankford mix works in caps. I've wonder if the Frankford Arsenal mixes for rifles would work for percussion caps, but I've never owned a muzzleloader to try it.
perotter
06-27-2014
Quote Originally Posted by Marshall View Post ... Regarding reliability of H-48 primers, I have only had 2 FTF so far in my testing of 500+ H-48 primers and those were due to light primer strikes. Perfectly acceptable for practice ammunition. When I use my own cast lead bullets and homemade primers, my cost/round for .380 ammo is $0.008. Yes, 0.8 cents/round! Are you using any gum, shellac, etc as a binder? In part because of it having a chrome bore, much of my testing is done with a Type 99 that has a strong firing pin strike and I have little experience testing something that occasionally gives a light strike. I have tested binderless mix vs bindered and found that the use of a binder looks to be better and assume that the commercial manufactures add it for a reason. By the way, I'm happy to see that you stuck around Marshall and are able/willing to post about having good results to us and the low cost of your reloads.
Marshall
06-28-2014
Yes, I use an ~10% solution of shellac in ethanol as a binder. In my primer building method I dry pack the H-48 mixture, add a paper disk, pack again, completely moisten the packed pellet with a minimum amount of shellac solution, then press in the anvil while it is still moist. Allow to dry overnight and your primers are ready to go. I believe that the addition of the binder solution greatly enhances the reliability of the primer. I also add a few tenths of a grain of powdered aluminum (~60-80 mesh that I made in a coffee grinder) to each batch to help with slower powders. The most time intensive part for me is cleaning, removing anvils, removing dimples and sorting used primers. Rebuilding the primers is actually pretty fast. Working in small batches slows things down, but I can easily do 100/day in just a couple of hours.
I haven't given up on trying to find a feasible non-corrosive primer mixture, but it is not easy without doing some wet chemistry since you cannot directly buy most of what you need. I can't do it a work and I don't have the equipment/facilities to do it at home (yet). If you have some good ideas, please share them with me (by PM if you prefer).
Regarding staying around castboolits, I have recently started to cast my own and there is no better resource on the web. I have even been participating in several group buys of bullet molds. I already have bought a 32 cal Cramer style mold from Milhec that is a work of art (compared to a Lee mold at least).
page 14
perotter
06-28-2014
No new ideas(good or questionable) for a non-corrosive mix that would be easy. I'll certainly let you know if I do. For a local source of powdered aluminum you might look at using Silver Seal radiator sealer. It is 90% AL powder, 5% stearic acid, 2% silicon and 2% iron. I've never tried it and don't know if non-aluminum ingredients would cause a problem. I thought of using it years ago, but I use aluminum powder for an industrial casting process and always have 25-75 lbs of it around.
ofitg
06-29-2014
Marshall, I've been wondering, how finely ground/milled is your Antimony Sulfide?
According to an old 1922 book, the Army specified that the AS should pass through a 100-mesh screen, but no more than 50% should pass through a 200-mesh screen -
http://babel.hathitrust.org/cgi/pt?id=chi.087229635;view=1up;seq=64
nicholst55
06-29-2014
I would think that the Atomized Aluminum that Brownells sells for use when glass bedding would be more practical than using Silver Seal Radiator Sealer. Probably less expensive, as well.
Now, where can I find specifics on the Frankford Arsenal primer mixtures?
'I have a feeling we're not in Kansas any more, Toto!' Dorothy, in The Wizard
of Oz.
ofitg
06-29-2014
Nicholst55, here's a good summary -
http://www.northwestfirearms.com/threads/priming-mixtures.58110/
Marshall
06-30-2014
I have not sieved the antimony sulfide to know what its particle size would be. I am using the ground product as shipped from Pastime. My best guess would be ~100 mesh. All I can say is it works as is.
Marshall
07-03-2014
There is the theory and then there is the application. Here is a picture of a box of berdan primed (H-48 mixture) 45 ACP rounds that I made up last night.
DSC00402.jpg The loading used was one of my favorite 45 ACP loads:
230 gr FMJ / 5.4 gr W231 / 1.260 OAL / $0.17/round 18079 psi / 841 fps / 361 ft-lb / 99.6% Burn / 56.6% Fill So, a box of 45 ACP for $8.50 from casings that would have been thrown away. Not counting the time to make them, the primer cost was $0.00032/primer or $0.016 for the box of 50. BTW, these casings used 5mm berdan primers which are unavailable in the US. Therefore, the only way to reload them was to make my own primers. This size primer is also typically used in steel cased 380 and 9mm Luger ammunition. My local gun range happily gives me all the steel casings I want whenever I go there so I have a lot of them to play with.
In case you want to try this, I wet clean the deprimed steel casings in a rock tumbler with stainless steel pins and a squirt of dishwashing liquid. Only tumble for 15-20 minutes to avoid damaging or removing the polymer coating on the casings (yes I have done it). Resize as normal "without" your depriming pin. It helps if you use resizing lub, but it is not necessary with a carbide resizing die. The resizing effort is slightly more than brass when unlubed, and slightly less than brass when lubed.
So, what are you waiting for, there are berdan primed casings calling out to be reloaded instead of being scrapped.
perotter
07-03-2014
Besides free brass, another advantage of Berdan primers is there are several non-corrosive primer mixes that will work in them very well that won't work in Boxer primers. You might want to consider trying a lead nitrate/hypophosphite double salt mix. No special equipment needed and it's not explosive until after the completed primer is dry. I've tested a few and wasn't disappointed with the results.
Marshall
07-03-2014
Using one of the Eley Prime processes sounds like a great idea. I don't have the chemicals to make them, but they are on my future buy list. The cheapest source of Pb(NO3)2 that I have found is Elemental Scientific. If you know of a better supplier let me know. I'll also need some sodium hypophosphite solution from an electroless nickel plating kit, but it was kind of pricy the last time I checked. Looks like it Google search time again.
perotter
07-03-2014
Quote Originally Posted by Marshall View Post
@perotter, Using one of the Eley Prime processes sounds like a great idea. I don't have the chemicals to make them, but they are on my future buy list. The cheapest source of Pb(NO3)2 that I have found is Elemental Scientific. If you know of a better supplier let me know. I'll also need some sodium hypophosphite solution from an electroless nickel plating kit, but it was kind of pricy the last time I checked. Looks like it Google search time again.
The Google search engine isn't the best one for chemical searches. In addition
to Google try a couple of the other ones.
bannor
07-03-2014
my reasoning is that I don't want to blow off some fingers, as has happened with people making more than 1/8 oz or so of this sort of thing at a time (and not using gloves, behind a wall of sandbags).
bannor
07-03-2014
8c sounds steep. You must be buying powder by the lb and primers by the 100 rd box. or paying for pure lead/tin. I know that quantity buying is not feasible for now, but when you get the chance, take a look at how much cheaper powder is by the 15 lb keg, and primers by the 100,000. as in half price, guys. When you KNOW that you're going to use it, why not save the money and buy plenty (and not worry about shortages)?
Marshall
07-04-2014
Your decimal point is off. The cost of the rounds with my homemade primers and cast bullets is $0.008/round or 0.8 cents/round. Buying 100,000 primers even at 1/2 price would still be $1,500 to $2,000. I don't have that kind of spare money laying around. There are only a few powders that I would consider buying more than 1 lb at a time (Bullseye, Unique, Power Pistol, W231/HP-38, Universal and Herco none of which are available in the current pistol powder shortage). Any others would probably not be used up in my lifetime. In 2 years of reloading, I have only emptied six 1 lb bottles of powder (of three of the above mentioned powders) and I have made a LOT of rounds.
Regarding your statement:
"my reasoning is that I don't want to blow off some fingers, as has happened with people making more than 1/8 oz or so of this sort of thing at a time (and not using gloves, behind a wall of sandbags)"
Risk is mitigated by knowing what you are doing and doing it the right way. If you don't know, then you shouldn't do it. If you don't want any risk, don't do it. However, if you learn how to do it safely, then it can be done safely and without having to work behind sandbags. No one here is proposing working on industrial scale batches. In small quantities (<2 grams) the worst that will happen while working out in the open (i.e. uncontained) is you might have to change your underwear after an unintended pop. After making and working with well over 50 small batches of H-48 mixture, I have yet to have any unexpected pops. In fact, the only unintended pops that have occurred at all were when I was pressing in a couple of reloaded berdan primers into casings. They were made from slightly flattened primer cups and didn't want to seat. I kept applying more and more pressure to force them in and eventually they popped. No harm done, adjusted primer inspection criteria to eliminate overly flattened primer cups, no more pops.
perotter
07-04-2014
Quote Originally Posted by bannor View Post my reasoning is that I don't want to blow off some fingers, as has happened with people making more than 1/8 oz or so of this sort of thing at a time (and not using gloves, behind a wall of sandbags). I almost always use a wet mix. I've never been able to get a chlorate based mix to go off until it has dried out.
perotter
07-04-2014
@Marshall At some point this weekend I'm going to look for a book I have about making lead nitrate. Over the years I'd read that lead nitrate is the only nitrate that can be made with just lead and ammonia, but had never seen how it was done. Last winter when looking thru an old chemistry book I came across how to do so. The equipment needed would be in most homes. No Apparently it didn't nor doesn't have a commercial application, but for amounts we use it may be of use. When I find it, I'll pm you the information so you can ponder if it might be worth trying.
Marshall
07-09-2014
I did some checking and lead nitrate can be made from copper nitrate and lead metal. The copper nitrate itself can be easily made from copper sulfate and potassium nitrate which are readily available from retail stores if you know what to ask for (hint: pond algae and stumps). In addition, lead nitrate is easily made directly from lead and nitric acid. I decided to just buy the lead nitrate directly for ~$20/lb from Elemental Scientific. As things stand, I am probably already on the DHS watch list from my previous primer chemical purchases, so I've stopped caring.
As an aside, I am trying to make my own aluminum powder using 1/2" steel balls and aluminum foil in a small plastic drink bottle on a tumbler. I saw a Youtube video where someone did this over a 3-4 day period. BTW, you cannot use a smooth wall bottle to do this (I tried) as the balls just gently roll around and do not beat on the aluminum. So, I am using an energy drink bottle that has deep designs molded into the sides. This causes the balls to rise and then fall back onto the foil. Still looks like it is going to be a slow (and noisy) process, but I'll be happy if it works. One other note, you will likely need to put a couple of rubber bands on the outside of the bottle so that it grips the tumbler rollers. Otherwise the smooth exterior of the plastic bottle slips on the rollers and barely spins.
Bert2368
07-09-2014
Could someone post links to the Eley prime type mixture formulations? I don't think I've seen those yet.
Aluminum flake powder via ball milling with large ball bearings takes a while and is hideously noisy, but it is possible- I have made ball mill jars from PVC pipe sections , with a glued on cap on one end and a reducer fitting with a rubber cap/worm drive clamp on the other end. I have screwed and glued "lifter bars" to the inside of the such mill jars, using countersunk screws from the outside of jar and a 2 part plastic welding glue sold in a double barrel syringe- I'll try to find one and post a picture, I started abuseing/re-purposeing my Sears & Roebuck "hobby rock polisher kit" a LONG time ago... Be aware that many pyrotechnic formulations call for SPHERICAL Aluminum, particle shapes (widely differing surface areas!) can matter a great deal in performance of pyrotechnic mixtures!
Lead salts thread:
MA HREF="http://www.sciencemadness.org/talk/viewthread.php?tid=5490"> http://www.sciencemadness.org/talk/viewthread.php?tid=5490
nicholst55
07-09-2014
Quote Originally Posted by perotterMbr< I put that out there because, for reasons all there own, some people don't like to buy primer chemicals online or mail order. The pryo houses have atomized aluminum for about 1/4 of what Brownells sells it for.
Yes, I see now where that's the case. I got to thinking afterwards that buying atomized aluminum from Brownells would doubtless yield a supply for several lifetimes!
'I have a feeling we're not in Kansas any more, Toto!' Dorothy, in The Wizard of Oz.
Marshall
07-09-2014
Find and review the following patents which discuss the Eley Prime process,
although sometimes its not the main focus of the patent:
US4432819
US4850259
US4336084
US5538569
GB1569874A
EP0047406A2, A3, and B1
EP0704415B1
Here is an extract from one of these patents for a rimfire formulation:
-=-=-=-
6) by reaction with styphnic acid:
A mixture was produced of the following materials in the stated proportions by weight:
a) styphnic acid 100 parts
b) white lead 100 parts
c) ground glass 50 parts
d) barium nitrate 50 parts
All of the materials were in dry powder form, and all powder particles passed through a 100 mesh (British Standard 410) sieve. When distributed between rimfire cartridge cases, the mixture was moistened with water and permitted to react in situ in the cases.
It was found that the resulting primed case could be made to explode satisfactorily with a substantial flame. The quantity of priming composition in each case was of the order of 14 to 15 mg.
The styphnate route is not limited to the production of lead compounds. Other heavy metal styphnates might be produced in a similar manner, and have previously been suggested for use in initiating compositions. Further, the acid reaction is not limited to the use of white lead (lead carbonate) or lead oxide (PbO). An alternative possibility is lead hydroxide. The use of lead oxide is particularly desirable, however, in that there are no resulting by- products, the lead oxide and styphnic acid combining exactly to produce lead styphnate. The use of lead hydroxide is also acceptable on this ground, however, since the only resulting by-product is water, which is in any event present as an ionising medium. A further possibility would be a reaction between lead acetate and styphnic acid. In this case, the expected by-product would be acetic acid, which would be volatile and could be driven off during the reaction. The by-product of white lead is CO2 which is driven off.
-=-=-=-
Bert2368
07-09-2014
I had found similar patent info with Sodium azide/Lead nitrate, producing Sodium nitrate as an additional oxidizer in the reacted prime mix. My personal experience with Sodium nitrate and humidity would not make that one my first choice-
perotter
07-13-2014
Quote Originally Posted by Marshall
I did some checking and lead nitrate can be made from copper nitrate and lead
metal. The copper nitrate itself can be easily made from copper sulfate and
potassium nitrate which are readily available from retail stores if you know
what to ask for (hint: pond algae and stumps). In addition, lead nitrate is
easily made directly from lead and nitric acid. I decided to just buy the lead
nitrate directly for ~$20/lb from Elemental Scientific.
The method I was looking for was making with just ammonia and lead, without any nitrate or acid. The book I thought it was in wasn't the one. I'll have to keep hunting for it, but it looks like it will take a while.
I have a fair amount of lead nitrate that I bought a few years ago. Enough that I use it increase the mass burn rate of ammonpulver.
perotter
07-13-2014
Quote Originally Posted by Bert2368
Question is, can you make it so it's reliable, ballistically uniform, and storage stable...
IMO, it being ballistically uniform at the same level as what we buy is the hardest for safe DIY.
Marshall
07-15-2014
Wow! I just snagged a couple of lbs of calcium hypophosphite off of eBay. Still not cheap, but I'll be able to make plenty of lead hypophosphite to try out the Eley prime process in berdan primers. You never know what you will find on eBay. Now, if I can just find some aminoguanidine at a reasonable price.
Marshall
07-15-2014
The closest reaction to your ammonia/lead idea that I can find uses ammonium nitrate plus lead oxide to make lead nitrate. I couldn't find any references to ammonia directly reacting with lead metal.
Marshall
07-17-2014
Do you have any ideas about why the lead hypophosphite/lead nitrate double salt eley prime mixture would work well in berdan primers, but not in boxer primers? Mechanically, they would seem similar enough to function the same. When I start my tests, I plan to make a few boxer primers as well to verify they will not work.
McMauser
07-21-2014
The reading of 15 pages of how to and/or how to not make primers has been quite educational for me and before I continue I would like to thank everyone for their experiences, knowledge of chemistry, experiments, recommendations and especially safety concerns.
My interest in self made priming mixture surfaced for at least two reasons; one being the scarcity of Berdan primers in the US, the other being the need to prime large bore rim fire cartridges.
I have thought about using the toy cap and match head method, but thought that this approach would be extra corrosive and erosive besides having to deal with the politically correct issues with the two products.
Long ago I read Hatcher's Notebook including priming mixtures and concluded that priming mixtures are dangerous to produce. I was excited when I learned about the safer to use Eley priming process, and finally came across some of the formulas.
I have several basic questions. One being, what should I pursue, the Eley prime, a Frankford Arsenal type or other. What I gathered so far is that potassium chlorate primers are reliable, dangerous to make if not done in small batches and using the wet method. As for Eley prime, I haven't read about chemical availability for home brewers.
If I have to use the match head tip method, what sort of solvent would be best, water or alcohol? I have thought of using shotgun primers, dismount the priming mixture from the cups and use a solvent to dislodge the mixture and transplant into the rim fire shells or Berdan type cups. Here again without experimentation I would like know what type of solvent to use.
Janoosh
07-21-2014
Shotgun primers are basically berdan primers. Just take a fired shotgun primer apart...primer cup, separate anvil, separate base....
Marshall
07-21-2014
I don't recommend digging around in commercial primers. However, the primer mixture was originally deposited into the cup as a paste made with water and then dried. If you can get the material completely wet (may be harder than you think) you could probably remove the primer compound for use in other cups. To me it sounds like more trouble than it is worth. I certainly wouldn't destroy perfectly good primers to use in other primers.
Regarding Eley Prime mixtures, if you have found the formulations and are knowledgeable in chemistry you know that some of the components cannot be bought but must be synthesized. Finding the needed starting materials is not easy (or cheap), and you still must do some wet chemistry. The Eley Prime process is safer than working with pre-made primer compound, but if it was easy to execute we would already be using it in this thread.
Don't shortchange the Frankford Arsenal formulas as they have been well proven in millions of military rounds. Other than their corrosive nature, they work just as well today as they did 100 years ago. Myself and several others in this thread have safely made primers using these primer compounds. Just this morning I made 15 SP boxer primers in about 15 minutes with H-48 compound. The best thing about these formulations is that the starting materials are easily and cheaply available on the Internet or can be made from common household chemicals (like bleach and salt substitute). This is valuable information you need to know for an uncertain future.
AlaskanGuy
07-22-2014
Wallace - Chemical Analysis of Firearms, Ammunition and Gunshot Residue (CRC, 2008).pdf LOCAL COPY
I would like to suggest reading and downloading this for reference... It is the book titled Chemical Analysis of firearms, am munitions and gun residue.
it has the recipe for most of the historic priming compounds...
McMauser
07-26-2014
Thanks for your input. The Eleyprime sounds great, but the chemistry is way beyond my capabilities. I think the Frankford Arsenal formulas would be workable for me. I think I will reread the data presented above in the 15 pages plus other references and come up with some guide lines, have the info commented on then make up my own procedure specification.
nhrifle
09-09-2014
I came across this site today, lots of good information http://www.powerlabs.org/chemlabs/styphnic.htm
Bert2368
09-09-2014
I would advise doing your own (careful!) research before home synthesizing Lead styphnate. Along with being shock & friction sensitive, it is one of the more static sensitive primary explosives.
Educate yourself about ESD and energetic materials handling before you go there, Learn how to make up a "stock solution" of Magnesium styphnate, and restrict quantities of dry Lead styphnate on hand to a gram or less. It is not a happy pleasant substance for blithe beginner explosive chemists.
See p. 440-
The-Chemistry-of-Powder-and-Explosives---Tenney-L.-Davis.pdf
Marshall
09-19-2014
I have finally obtained some aminoguanidine bicarbonate for testing of the Cheddite tetrazene primer process (US20090151825). In this method, tetrazene is formed in-situ from an aminoguanidine salt (sulfate, nitrate, bicarbonate) and sodium nitrite. While the overall primer formula is clearly presented in the patent, it does not provide any details on how to mix these two ingredients to generate the tetrazene in-situ. While I have some ideas on how to do this, I would appreciate some feedback from any chemists here to critique my plans.
Here is my proposed test plan:
1. Initially, the same molar ratio of aminoguanidine bicarbonate to sodium nitrite (1 : 1.6) that is used in several experimental methods to synthesize tetrazene in solution will be tried. The reaction probably does not need this much excess sodium nitrite since the reactants will be quite concentrated when the dry primer pellet is moistened with a minimum amount of water, but it seems to be a reasonable starting point. I can experiment with other molar ratios closer to the ideal 1 : 1 in the future.
2. The dry primer ingredients (aminoguanidine bicarbonate, sodium nitrite, barium nitrate, antimony sulfide, and aluminum powder) will either be ball milled or ground up in a mortar and pestle. This should be safe since the dry blend should essentially be inert. I am targeting a 10 gm (~150 gr) batch weight. I would definitely appreciate some feedback on the safety of this operation. If this is too risky, I can go back to mixing smaller batches on a sheet of paper. Alternatively, I could ball mill everything except for the aminoguanidine bicarbonate and blend it in with the other ingredients in a separate step.
3. I plan to make an ~5% aqueous binder solution of gum arabic and add a few drops of distilled vinegar to acidify the solution. Dilute acetic acid is used in all solution tetrazene synthesis methods I have seen, so I suspect it may be needed here as well. I'll make some tests without acetic acid, but I plan to start with an acidic solution. It is possible that the barium nitrate constituent is acidic enough to provide the proper environment for tetrazene formation.
4. After packing prepared primer cups with the dry primer powder and adding a paper foil, the compressed pellet will be moistened with the acidified binder solution.
5. For boxer primers the anvil will be installed while the pellet is still moist and then allowed to dry overnight at room temperature. If they still have any residual vinegar odor, the drying will be completed in a food dehydrator. For berdan primers, I am thinking about installing the moist primers into casings and after allowing a couple of hours for the tetrazene reaction to complete, then dry the casing/primer assembly in a food dehydrator. The reason for this is to allow the berdan anvil to mould the primer compound while it is still wet.
6. Test. Reformulate if necessary and test again. Some glass powder may be added to the primer mix if it needs to be more sensitive to percussion.
OK guys, what do you think?
Bert2368
09-19-2014
If you grind a nitrite, Barium nitrate, Aluminum powder, Antimony sulfide and an organic fuel, you might well have a problem! This is FLASH POWDER. Please cominuate the 2 oxidizers SEPARATELY from the rest of the mix...
It is common practice to add a very small % of a weak acid to any wet processed mixture containing Aluminum powder and a nitrate/nitrite oxidizer. The oxide coating of the Aluminum is attacked strongly under basic conditions, and a nitrate wet and in contact with Aluminum can generate AMMONIA- So the weak acid protects your Aluminum powder. Often, an additional 1% or so of Boric acid is milled with the oxidizer for this purpose in pyrotechnic manufacture.
More as I have time to think about the rest of the proposed process.
Marshall
09-19-2014
Thanks for the feedback. This is exactly the kind of information I need from folks who are experienced in pyrotechnics. It will be easy enough to grind the oxidizers separate from the fuels. So the following will be milled separately 1) sodium nitrite, barium nitrate, and 2) aminoguanidine, antimony sulfide, and aluminum powder. These two blends will then be gently mixed on a sheet of paper just before loading up a batch of primer cups. I'll also cut the final batch size back to ~2 gm to further reduce the risk. I don't have any boric acid, but I'll look for some at the drug store just in case I want to try it in a future test.
Oreo
09-19-2014
99.9% boric acid is just ant/roach powder found in the pesticide section of your local Lowes or Home Depot. I use it frequently, it does a good job controlling ants.
Marshall
09-20-2014
Thanks for the information. These types of alternative sources are essential information for the expedient chemist.
Marshall
09-22-2014
My first attempt to make the Cheddite primer formula has been a failure. I made up a batch of Cheddite tetrazene primer compound as described below and packed 5 SP, 5 LP, and 5 berdan primers.
Cheddite primer formulation (patent US20090151825)
Percent Gram grains
Tetrazene 20 2.000 30.9
Ba(NO3)2 48 4.800 74.1
Sb2S3 24 2.400 37.0
Aluminum 8 0.800 12.3
The 30.9 gr tetrazene above is formed in-situ from:
22.3 gr Aminoguandine bicarbonate (MW 136.11)
17.9 gr Sodium nitrite (MW 68.993, 1.6 molar ratio to aminoguanidine bicarbonate)
The primer ingredients were blended on a sheet of paper to form a dark gray mixture which had a clumpy and sticky nature rather than a clean free flowing powder. This powder was placed into the primer cups and then packed tightly using a wooden dowel.
After adding a paper foil and repacking, I moistened the pellets with acidified binder solution. I could tell with the first primer that the solution did not want to flow into the pellet. Therefore, I added a small amount of isopropyl alcohol to the acidified binder solution to cut the surface tension. That worked well and the modified binder solution easily flowed into the primer pellet. I then added the anvils to the SP and LP primers and let the moist primers sit for 6 hours at room temperature. I then placed the primers in a food dehydrator for ~1 hour to "complete" the drying.
It was found that the primer material did not dry under these conditions. Instead, the material in the primers retained a moist sticky playdough like consistency. As a test, a small amount of compound was prepared in a thin layer on a non-porous flat surface and allowed it to sit overnight in a well ventilated area. This material also did not dry. It is possible that the excess sodium nitrite is holding onto some of the water and prevents the mixture from completely drying. I may stick the primers back into the dehydrator overnight to see if that helps. However, I am concerned that the tetrazene will decompose under these hot moist conditions.
Plan B is to make the tetrazene in a separate step and directly use it in the Cheddite formulation. If that works, I'll start adjusting the AGB to sodium nitrite ratio to see if that helps dry out the primer mixture. I'll also see if the acetic acid is needed or not.
Oreo
09-22-2014
Got a vacuum pump?
Marshall
09-28-2014
Update on Cheddite non-corrosive primer tests
Well, I have some more failures to report and one partial success.
In my first trial, I used a 1 : 1.6 molar ratio of aminoguanidine bicarbonate : sodium nitrite in the primer mixture. I also used a slightly acidified aqueous solution of gum arabic to moisten the packed primer pellet. The end result was a play dough like material that never dried.
Test two used a 1 : 1 molar ratio of aminoguanidine bicarbonate : sodium nitrite and put the gum arabic powder in the dry mixture. In this test, I only used plain water to moisten the packed primer pellet. This combination dried to a solid pellet, but the dried material would not ignite under percussion, even striking with a hammer. I tried making this formulation both in a primer cup and mixed in a plastic weighing tray. Neither method gave a percussion sensitive material.
Test three used separately synthesized tetrazene in the primer mix. I also added 10% powdered glass, to give it a little more sensitivity. The formulation used is shown below:
Tetrazene........20%.........6.6 grains Ba(NO3)2........42.2%....13.9 grains Sb2S3.............20.6%......6.8 grains Aluminum.........7.2%......2.4 grains Ground Glass...10%.........3.3 grains .....................100.0%...33.0 grainsThis mixture looked quite different from the previous mixtures. It had a distinct yellow tint from the tetrazene. It was also much drier and less clumpy/sticky. A SP primer was loaded with this powder, the powder compressed, a paper foil added, and the pellet compressed a second time. In this test, the pellet was moistened with my standard dilute ethanol/shellac binder solution and allowed to dry for 24 hours.
The dried primer was installed into an empty 9mm brass casing and the casing fired in a Springfield Armory XDm pistol. Expecting another dud, I was surprised to hear a weak but clear pop. Removing and disassembling the primer showed that very little of the primer mixture appeared to be consumed. Interestingly, the unburnt residue in the cup was found to be insensitive to percussion with a hammer.
What I believe has happened is that the tetrazene in the mixture ignited and burned but did not transmit enough energy to the other primer components to initiate the desired redox reaction. This suggests that a more intimate mixture of the tetrazene with the other primer components is needed. The only safe ways I can think of to do this are: 1) to repeatedly brush the mixture through a fine sieve, and perhaps 2) wet milling/grinding. Perhaps someone knows of better ways to do this. Also, let me know if you think something else is the reason for this observation.
Finally, I still have not solved the problem of making the tetrazene in-situ. Let me know if you have any recommendations.
Marshall
10-01-2014
Another update of Cheddite tetrazene based primer experiments.
I wet ground (using 90% isopropanol solvent) a small amount of previously prepared tetrazene primer mixture to improve the dispersion/particle size of the primer ingredients. After drying, several SP and LP primers were loaded using my standard system: 1) fill the cups with the loose powder, 2) tightly pack the powder, 3) add a paper foil and repack, 4) moisten the packed pellet with dilute ethanol/shellac binder solution, 5) install the anvil, and 6) allow to dry for 24 hours.
The test primers were loaded into empty 9mm and 45 ACP casings and fired in Springfield Armory XDm pistols (I really like XDm service pistols and have 3 of them in 9mm, 40 S&W and 45 ACP calibers). The SP primer gave the same weak pop I obtained previously and very little of the primer compound was consumed during firing. On-the-other-hand, I was pleasantly surprised that the LP primers fired with a robust pop. Upon disassembly, the LP primer cups were found to be essentially empty, very clean and only had a trace amount of light gray residue inside. The casing and barrel also were coated with this light gray residue.
Based on this finding, it appears that there is a lower threshhold of primer material that must be present for the primer to fire correctly. In Cheddite's patent they were testing the primer mixture in shotgun primers which hold ~60 mg of compound. In contrast, a SP primer holds ~20 mg, and a LP primer holds ~35 mg of primer compound. Therefore, this approach is probably only useful for reloading LP, LR, and shotgun primers. With more experimentation, it might be possible to find a formulation that also works for SP and SR primers. However, much work would likely be needed to find a good formulation "if" one exists. While Cheddite claims their primer mixture can be used in "sporting arms" ammunition, I suspect that it would be limited to large primers.
In the meantime, my interest has shifted to a different approach. US patent 2175826 describes the use of hypophosphite double salts in primers. I already was planning to try the double salt method because it is mentioned as one of the Eley Prime processes (US patent 4432819). That patent describes making the primary explosive (Lead Nitrato Hypophosphite) in-situ from Lead Hypophosphite and Lead Nitrate. The 2175826 patent is similar, except it produces the above double salt along with calcium nitrato hypophosphite by wet mixing a paste of calcium hypophosphite and lead nitrate together for several minutes (same ingredients are used to synthesize lead hypophosphite in solution). After the formation of the double salts are complete, the other primer ingredients are blended in and the primer cups wet primed. I like this method since it is not necessary to make and isolate the lead hypophosphite intermediate. They claim that the calcium nitrato hypophosphite double salt is also explosive like the lead double salt so there does not appear be be a downside to leaving it in the mixture. Before trying this method, I want to get a non-porous mortar and pestle for making the double salts. I think either a glass mortar and pestle (cheap, $15) or an agate mortar and pestle (nice but more expensive, $35+) would do the job nicely.
I'll let you know how things turn out.
Marshall
10-03-2014
My latest tests on the non-corrosive calcium/lead nitrato hypophosphite approach were an unqualified success. The following formula and mixing technique were tested:
................%.......grains Ca(PO2H2)2......20.......6.6 Pb(NO3)2........40......13.2 Ba(NO3)2........16.......5.3 S................9.......3.0 Glass...........15.......5.0 ...............100......33.0The Ca(PO2H2)2 and Pb(NO3)2 were put into a small smooth round bottom glass bowl/dish. The mixture was ground to fine powder and blended well while dry. Enough water was then added to make a thick paste and the mixture was blended continuously for ~2-3 minutes. The remaining ingredients were added and enough additional water to maintain a paste consistency. The paste was blended for another 2-3 minutes and then allowed to dry in the glass bowl or placed onto a flat non-porous surface (i.e. glass plate) to dry. The dried paste was broken free from the bowl or plate using a plastic spoon and the mixture was gently ground into a fine powder using the back side of the plastic spoon.
Several prepared LP primer cups were loaded with the powder in the usual way described previously. The primers were air dried for about 8 hours and then dried in a food dehydrator for 1 hour. The primers were loaded into empty 45 ACP casings and fired in a Springfield Armory XDm pistol. The primers fired with a loud report that was equivalent to a commercial primer. Disassemblying the fired primers showed that the primer compound burned cleanly and completely. Only a very small amount of light gray residue was found inside the casing and barrel.
The next test will be with SP primers. If that is successful, then I'll load up some test rounds for my next trip to the range. I think we have a winner with this formulation.
Marshall
10-05-2014
I have completed my tests on SP boxer primers and 5 mm berdan primers. The latter are used in almost all steel Russian .380, 9 mm, and 223 ammo. Because new 5 mm primers are completely unavailable in the US, these casings were unusable without a way to reload the fired primers.
I am pleased to report that the SP and berdan primers robustly fired in 9 mm casings. I have also found that drying the primers for ~1 hour in a food dehydrator (max temperature attained was ~80C) greatly increases the reliability of these primers. Inspecting the disassembled fired primers showed a small amount of black residue (likely lead oxide) similar to that found in fired commercial primers. In summary, this primer mixture has been successful fired in SP boxer, 5 mm berdan, and LP boxer primers.
Based on these results, I believe I have found a relatively easy to make, non- corrosive primer compound. That does not mean it is optimized. It also does not mean that all the raw materials are easy to acquire. However, as I found and purchased the most difficult compound to obtain (Calcium hypophosphite) on eBay, it is certainly not impossible.
My final step to prove out these non-corrosive primers is to make up some test rounds and try them at the range. Stay tuned for a range report.
Oreo
10-05-2014
Good work Marshall! I have been following your progress and look forward to your continued reports.
Marshall
10-05-2014
The drying of the hypophosphite primers in a food dehydrator turns out to be more essential than I thought. The primers appear to pickup moisture over a ~10 hour period when sitting around under ambient conditions causing them to fizzle instead of pop. Putting the primers back into the dehydrator for an hour reactivated them nicely. I quickly built some 9 mm and 45 ACP rounds using the re-dried primers so hopefully they will work when I get to the range. I suspect that traces of residual calcium nitrate in the mix (which is known to be hygroscopic) is sucking up moisture and killing the primers. If this is the problem it can be solved by synthesizing the lead hypophosphite in solution which will separate the calcium salts by keeping them in solution as the lead hypophosphite is collected by filtration. The new formulation would look like this:
................%.......grains Pb(PO2H2)2......30......9.9 Pb(NO3)2.........30......9.9 Ba(NO3)2........16.......5.3 S................9.......3.0 Glass...........15.......5.0 ...............100......33.0Out of curiosity, I am also interested in getting some calcium nitrate and making pure calcium nitrato hypophosphite to see if it will work in the primer formula by itself. It would be nice to get rid of the hazardous lead compounds in the formula. That formula could look something like this:
................%.......grains Ca(PO2H2)2......30.......9.9 Ca(NO3)2........30.......9.9 Ba(NO3)2........16.......5.3 S................9.......3.0 Glass...........15.......5.0 ...............100......33.0
Marshal, as a test, after the primers are charged in a dry state, try spraying a coat of hair spray over them, and let dry. See if that doesn't block ambient moisture.
===================================================== ===================================================== ===================================================== 02-03-2015, 05:36 PM #312 otonel Originally Posted by vixny Lead styphnate is a VERY SENSITIVE explosive It is mild sensitive to impact and VERY SENSITIVE to electrostatic discharge so don`t wear synthetic clothes when work with this. What do you think about complex salt of basic lead picrate like monobasic lead picrate-lead nitrate-lead acetate, is powerful sensitive and is made from easy to find or synthesis chemicals. I was read this patent https://docs.google.com/viewer?url=p.../US3293091.pdf and tested a salt of lead picrate -lead nitrate lead acetate with some extra lead nitrate and aluminum For my tested I use a hammer and that mixture work good at first impression. 02-03-2015, 11:01 PM #314 perotter Originally Posted by vixny ..... Lead styphnate is a VERY SENSITIVE explosive and its synthesis should be performed only by professionals working under laboratory conditions ...... Or it can end up being very insensitive. Each batch should be tested. I too have long been of the opinion that it isn't the 1st thing one should make. And you didn't even mention that some of the equipment(containers) needed is expensive. 7-21-2015, 01:33 PM #316 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Texantothecore I love this place. I have been trying to use caps and the paper is jamming the nipple on my percussion gun. As soon as I can lay my hands on some chemicals I am going to try this. Probably will start with FA 42 and go from there. If FA42 doesn't quite live up to the task, add a little powdered aluminum to it. Start with about 1%. The powdered aluminum throws big hot sparks into the powder and the hot gases will be at a higher temperature. Reply Reply With Quote 07-21-2015, 02:05 PM #317 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 Perotter Can I substitute potassium perchlorate for potassium chlorate. And antimony trisulfide for antimony sulfide? Thanks Mike 07-21-2015, 08:44 PM #318 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Texantothecore Perotter Can I substitute potassium perchlorate for potassium chlorate. And antimony trisulfide for antimony sulfide? Thanks Mike I've never gotten that to work, but you can try it. Potassium chlorate is easy enough to get and I figure there is a reason they used it in the first place. Potassium chlorate is just plain more sensitive. Antimony trisulfide is what we mean when we say antimony sulfide. Reply Reply With Quote 07-22-2015, 04:06 PM #319 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 I should also state that potassium perchlorate produces hydrochloric acid when used and potassium chlorate doesn't. I don't know if that makes it any more corrosive than using potassium chlorate. 07-28-2015, 11:12 PM #323 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 I am trying to get a better grip on this chemical reaction. Can anyone comment on the contribution of antimony trisulfide to the chemical reaction? Reply Reply With Quote 07-30-2015, 01:22 PM #324 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Texantothecore, Antimony sulfide serves as both a fuel and a frictionator. Marshall Reply Reply With Quote 07-30-2015, 08:21 PM #325 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Marshall @Texantothecore, Antimony sulfide serves as both a fuel and a frictionator. Marshall Also as sensitizer as it reacts chemically easier than many other fuel/frictionizers. There is a chemical reason for this that can be used to show why it does. I don't really have a firm handle on it and have go the textbook examples to understand why metal tri-sulfides do that. I have substituted arsenic tri-sulfide for antimony tri-sulfide as that is known to work better by being a stronger sensitizer. I didn't get it to work enough better to do what I wanted. PS. Note that tin sulfide also can be used instead and a few guys here have posted here about them doing so. Tin sulfide is DIY. IMO, one the main reason antimony sulfide has normally been used is because of cost and it's worldwide availability in nature. Last edited by perotter; 07-30-2015 at 08:27 PM. Reply Reply With Quote 07-31-2015, 09:51 PM #326 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 Thanks Perroter and Marshall. I do know it is used in star displays and is probably a good sparking medium. Reply Reply With Quote 08-05-2015, 05:41 PM #328 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Texantothecore Did you test this ammonium permanganate mix? No I didn't. I let the fact that it has a limited self life overrule the Curious Carl I have in me. IMO if one wants make a non-corrosive primer mix and not spend a lot of time learning, buying/making equipment, have problems getting 'feed stock', and the result that Marshall got - I'd work with lead hypophosphite. FWIW. For myself, once I got corrosive primer mixes that work very well my personal need for a mix was over. After that it has been more of the Curious Carl, the challenge and having come up with a non-corrosive mix that was patentable. The one I came up with isn't practical for a widespread DIY one because of the feed stock needed(availability and current cost). 8-06-2015, 05:36 PM #330 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by footpetaljones Perotter, Would you know of a source for lead hypophosphite? I can find calcium hypophosphite on eBay as Marshall did, but avoiding the trouble of synthesizing the lead hypophosphite would be nice. One makes the lead hypophosphite themselves. It is very simple and fast to make as lead hypophosphite doesn't dissolve in water, but both calcium hypophosphite and lead nitrate do dissolve in water. One just dissolves the calcium hypophosphite in a container of water and dissolves the lead nitrate in a different container of water. Then the solution of lead nitrate is poured into the container of calcium hypophosphite. The lead hypophosphite immediately forms and settles to bottom of the now calcium nitrate solution. Then the calcium nitrate solution poured out of the container. Rinse the lead hypophosphite several times to remove any calcium nitrate. If there is any calcium nitrate in the lead hypophosphite, the double salt will form. I buy and use sodium hypophosphite that is already in solution instead of using dry calcium hypophosphite. All dry hypophosphites are on a DEA list as being their sale, import and export being controlled just like red phosphorous. But solutions of hypophosphite were removed a few years ago and my desire to not run afoul with the powers that be, I get the solution. As sodium hypophosphite solution is used for electro-less nickel plating it can be purchased easily. The widespread use of it created a lot of complains to the DEA and that is why the DEA removed solutions of hypophosphite from the list. This would only apply to buying, selling and import/export of hypophosphite in the US. That is the info on that and do as you think is best. Not likely one would get into trouble, but........ If you or anyone else wants to know how much calcium hypophosphite/water to use and how much lead nitrate/water to use, I'll go look it up in G. Frost's book if you haven't yet gotten a copy of that book. Like reloading ammo, I like looking things up when possible instead of going be what memory says is correct. Reply Reply With Quote 08-07-2015, 02:39 PM #331 Marshall Boolit Man Join Date Mar 2014 Posts 113 @footpetaljones, Here is a method for making a small amount (0.1 mole) of Pb(H2PO2)2. 1. Dissolve 33.1 gm Pb(NO3)2 into ~26 ml of hot water, 2. Dissolve 17.0 gm Ca(H2PO2)2 into ~136 ml of hot water, 3. Slowly add the Pb(NO3)2 solution to the Ca(H2PO2)2 solution with constant stirring, 4. After the addition is complete, cool the solution in an ice/salt bath to complete the precipitation of Pb(H2PO2)2, 5. Collect the Pb(H2PO2)2 by filtration and wash the precipitant well with cold water to remove any residual Ca(NO3)2, 6. Allow the Pb(H2PO2)2 to air dry, theoretical yield is 33.5 gm. This may not sound like much material but it is enough to make ~4,000 SP/Berdan primers using the Eley Prime method/formulation. Enjoy, Marshall Reply Reply With Quote 08-08-2015, 08:35 AM #332 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I made a batch of Pb(H2PO2)2 last night using the above method. Lead Hypophosphite.jpg I first dissolved the Ca(H2PO2)2 in boiling hot water in a 250 ml erlenmeyer flask. When using 26 ml of water, I had problems with crystals of Pb(NO3)2 forming on the surface of the boiling hot solution as it cooled. So I ended up having to add a little more hot water to keep it in solution. To control the addition rate, I used a syringe to add the Pb(NO3)2 solution to the Ca(H2PO2)2 solution. A coffee filter was used to collect the precipitant which allowed a small amount of the finer particles to pass through, but not enough to worry about. Anyway, I can verify that the method works well. Now to make some primer compound and start experimenting again. Marshall 08-10-2015, 07:50 AM #334 Marshall Boolit Man Join Date Mar 2014 Posts 113 @perotter, I am making good progress in the development of a non-corrosive primer mixture suitable for boxer primers. I just completed some initial tests of 2 primer mixtures in berdan primers. The first is based on the US4432819 patent mixture. Rimfire Formulation % gr Pb(NO3)2 40% 13.2 gr Pb(H2PO2)2 40% 13.2 gr Grit 20% 6.6 gr 100% It was prepared using the Eley Prime method where the cup was packed with dry powder and then a drop of 25 ethanol/75 water was added to initiate the double salt reaction. I used the alcohol/water blend to help reduce the surface tension and get the water to soak into the packed powder. This worked OK, but still needs improvement. Perhaps an acetone/water blend would work better. As an aside, I also packed this mixture into the rim of a fired 22 LR case for a test I am doing to reload 22 LR rounds. The second solution was a modified Eley Prime mixture where antimony sulfide and aluminum were added as fuels. It is hoped that this mixture would be better suited for boxer primers. Again the cups were packed with dry powder and then a drop of ethanol/water solution was added. Centerfire Formulation % gr Pb(PO2H2)2 35% 11.6 gr Pb(NO3)2 35% 11.6 gr Sb2S3 12% 4.0 gr Aluminum 3% 1.0 gr Glass 15% 5.0 gr 100% 33.0 gr After allowing the water to completely air dry at room temperature (24-36 hours), the berdan primers were loaded into 380 ACP casings and then fired. Both primers fired with a loud strong pop. Inspection of the fired primers and cases showed that the first mixture had burned extremely cleanly and left virtually no residue. The second mixture was not quite as clean, but is still much cleaner than regular primers. So, I consider this test to be a complete success. One other note: Using previously synthesized and isolated Pb(H2PO2)2 completely solves the hygroscopic problems noted in an earlier similar mixture where the lead nitratohypophosphite was formed directly from Ca(H2PO2)2 and Pb(NO3)2, and the Ca(NO3)2 side product was left in the primer mixture. This approach required drying the primers in a food dehydrator and immediately using them in ammunition to prevent adsorption of water from the air (which killed the primers). Based on these positive results, I have built 10 SP boxer primers with the second mixture and they are currently air drying. I'll let you know how these primers work in a day or two. I have also played around with wetting the mixture and packing the primer cups with the moist paste. This works OK, but is messy and leaves a lot of residue on your tools. Marshall 08-10-2015, 04:03 PM #336 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Thanks Marshall for doing the work, sharing what you've done and what you have planned to do. I do think it is good that you are doing the in cup process also. Safe is always good. I'll have to revisit making some double salt primers next weekend. But it will be winter before I can spend an amount of time on primer mixes and testing them. If when being used in live ammo there is any problem with the variation with modified mix, a small % more lead nitrate would provide more oxygen for the fuels. Everything I've read on the topic of the double salt is that any extra nitrate stays a nitrate and is still a normal oxidizer. Also from going by an old Winchester patent and from how artillery primers are made, for DIY boxer primers one could put mix on top of the anvil to give a better ignition of the powder if needed. That mix wouldn't need to a primer mix. Reply Reply With Quote 08-10-2015, 09:18 PM #337 Marshall Boolit Man Join Date Mar 2014 Posts 113 @perotter, I have thought about adding some Ba(NO3)2 as extra oxidizer (I want to save my Pb(NO3)2 for other uses). I'm just not sure how much is needed to balance the added fuel. Perhaps I can swap out about 1/2 of the Sb2S3 with oxidizer. The modified formula would look like this: Pb(PO2H2)2 35% 11.6 gr Pb(NO3)2 35% 11.6 gr Ba(NO3)2 6% 2.0 gr Sb2S3 6% 2.0 gr Aluminum 3% 1.0 gr Glass 15% 5.0 gr 100% 33.0 gr Any comments, ideas? Marshall Reply Reply With Quote 08-10-2015, 10:18 PM #338 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I can confirm that the boxer SP primers loaded with mix 2 (labeled as Centerfire Formulation above) work perfectly. Nice strong pop, almost no residue left behind in the fired primer. Folks, this looks like a winner! I will be making up some test rounds in 380 ACP with these primers to take to my next trip to the range. If these work well in ammo, except for some tweaking to tune the oxidizer/fuel ratio, I will consider the search for a feasible non-corrosive primer mix to be complete. Marshall Reply Reply With Quote 08-10-2015, 10:25 PM #339 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 @Marshall You'd end up with 2 double salts if you made it the same why you currently do. I don't know that the would be a bad thing and this type of thing has be tested by large companies and are in some patents. If memory serves, with what you list have both barium nitrate and lead nitrate available as oxidizers. I'm very short on time for the next few days and don't know if I'll be able to check more into this in the next few days as to how much nitrate to add or to come up with a mix that would be a starting point. For something to try one could use no lead nitrate in the primer mix and just try 41% barium nitrate. I too don't like to just use up a few pounds of lead nitrate I have. PS I'd use more barium nitrate to fuel than what you list and just the aluminum. Minimum 1-1. I really have to go now. Last edited by perotter; 08-10-2015 at 10:28 PM. Reason: ps Reply Reply With Quote 08-11-2015, 12:19 PM #340 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 @Marshall It looks like this weekend I should be able to try the your centerfire mix in sp and lr. Mainly in sp because I have both easy to ignite and harder to ignite powders. The lr because it allows me to do more detailed testing of ignition variation. It's not likely I'll be able to do much yet, beyond starting. I was thinking this morning that before maybe just more testing of what you have is all that is needed. The reason being no sense in doing work to solve a problem that doesn't exist. Reply Reply With Quote 08-11-2015, 12:48 PM #341 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Just got back from the range and the news is great! I made up and fired 6 berdan and 5 boxer primed 380 ACP rounds that used mix #2. All test rounds fired normally and felt identical to witness rounds made with standard CCI SP primers. The loading tested was: 100 gr FMJ / 3.2 gr Green Dot / 0.940 OAL 19391 psi / 976 fps / 211 ft-lb / 98.4% Burn / 85.9% Fill So, there you have it. A non-corrosive primer mix that is: 1. Relatively easy to make, 2. Raw materials are easy to obtain on-line and reasonably inexpensive, 3. Initial mixture is inert and safe to handle dry, 4. Mixture only becomes explosive after moistening with water and allowing to dry, 5. Reacted mixture is non-hygroscopic and as stable as commercial primer mixtures, 6. Mixture is suitable for use in both berdan and boxer primers, 7. Gives reliable consistent ignition, Material cost to make SP primers using current prices for raw materials: 1080 primers / $ if calcium hypophosphite is used to make lead hypophosphite 1250 primers / $ if sodium hypophosphite is used to make lead hypophosphite With this result, I feel I have reached my goals with this project. I may still pursue some of the safer priming mixtures that make lead styphnate in-situ, but that is a much lower priority and can stretch out to the indefinite future. It is time to pass the baton to others in this thread to refine the process and/or develop even better solutions. Enjoy and let us know how this approach works for you. Finally, I wish to give my personal thanks to the many creative folks who have contributed to this long and informative thread. The best part of all this work is that we no longer need to worry about or fear a shortage or cutoff of primers. Marshall Reply Reply With Quote 08-11-2015, 01:07 PM #342 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Thanks Marshall!!!! You've shown how to overcome the 2 things that stop most from DIY primers. Safety and being able to have a non-corrosive. 08-30-2015, 07:02 AM #345 Oreo Boolit Master Join Date Mar 2009 Posts 1,914 This was just posted on youtube. Now, keep in mind this guy isn't a "gun guy" really, he's a sciencey undergrad who's ambitious enough to try and fumble his way through all kinds of projects. This one just happens to be relevant: (I don't know how to embed) https://youtu.be/ONfeTsByKhM Reply Reply With Quote 08-31-2015, 12:49 PM #346 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Oreo, I was never interested in making mercury fulminate based primer formulations because it makes brass brittle. That kind of kills much of the reason for making your own primers. It is also one of the more poisonous compounds you can make and is on the sensitive side to work with. If you have to clean up your gun afterwards anyways, you might as well use a potassium chlorate based primer formula which have a long history of reliable use. Finally, all of the old dead primers that I have removed from black powder ammunition which failed to fire have been mercury fulminate based. To recap: 1. Makes brass brittle, 2. Poisonous to make, 3. Sensitive to handle, 4. Still corrosive, 5. Limited shelf life, Thanks, but no thanks. Marshall Reply Reply With Quote 08-31-2015, 01:05 PM #347 Oreo Boolit Master Join Date Mar 2009 Posts 1,914 I never said it was the best or even a good option. I merely presented a video of it actually being done in the real world by a real person "back yard" style. I wish we had this kind of video of all the formulations being made. Reply Reply With Quote 09-01-2015, 06:36 PM #348 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Oreo I never said it was the best or even a good option. I merely presented a video of it actually being done in the real world by a real person "back yard" style. I wish we had this kind of video of all the formulations being made. It would be an option for use in steel cases or shotgun shells. The main factor that limits it's live is humidity and temperature. That was why it was fine for military use in continental Europe, but not for the US or England. I also think that it is still used or very recently used in Russian mil spec ammo because of there desire for a primer that works in colder temps than what we think is needed, something like -60 vs -40. But I'd have to look that up. IMO. While I see no great need to use any non-corrosive mix other than the safe and effective one that Marshall has tested for now, there is nothing wrong with looking at a few other mixes that might be useful to someone. FWIW. I'm currently more interested in DIY smokeless powder now. But the 'fall rush' is on. So, outside of a very little thinking and reading I'm not currently actively doing a powder nor the couple of non-corrosive mixes that one can make for what is available in a local store. Reply Reply With Quote 09-01-2015, 08:04 PM #349 Rustyleee Boolit Master Join Date Apr 2008 Location Central Fla. Posts 456 Check this out... compound kit. http://22lrreloader.com/store/ Reply Reply With Quote 09-01-2015, 09:03 PM #350 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 Marshall, I'm still assembling materials for your mix and I was wondering what grit size you used as the primer mix is going to be used on Treso nipples. I am not sure whethet I should go large on the grit size or very small to pass through the .028 flash channel. Any ideas? 09-02-2015, 08:52 AM #352 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Texastothecore, Originally Posted by Texantothecore Marshall, I'm still assembling materials for your mix and I was wondering what grit size you used as the primer mix is going to be used on Treso nipples. I am not sure whether I should go large on the grit size or very small to pass through the .028 flash channel. Any ideas? While I have not measured the particle size of the glass powder I am using, it is about the fineness of flour (my guess is 100 mesh or smaller). I have used a little coarser material in past primer formulations and it works well, but I was worried about barrel abrasion. The finer powder should be more like a polishing agent than an abrasive. @Rustyleee, "Check this out... compound kit. http://22lrreloader.com/store/" Hey, I have that kit and have reloaded and tested about a dozen 22LR rounds so far. I have used the original Eley Prime mix to prime the cases since that was designed for rimfire cartridges. The combination bullet mold/crimp tool works OK but the quality is not stellar. I am looking at assembling an equivalent set of tools, but with higher quality components. For example: 1. CH-4D makes a superior 3 piece 22LR die set for ~$103, the shellholder is another $12, 2. Lyman gas check bullet mold 225438 will make a better bullet and has been used by several folks on castboolits for making black powder 22LR rounds. It costs ~$73, add $33 if you need a set of handles. 3. The most useful part of the kit to me is the small funnel. The exact same funnels are available from eBay, 20 for $10 (free shipping too). So for about the same cost, you can get much better tools to do this job. Finally, my tests at the range have been 100% successful so far. I used a loading of 1.5 gr Bullseye which seems to be a little hotter than standard target ammo, but not by much. @Oreo, I apologize if you thought I was criticizing you about mercury fulminate based primers. While I obviously am willing to take some risks in making primer compounds, this particular compound exceeds my risk threshhold. Anyone who makes and uses this compound needs to do a lot of reading beforehand and take all needed safety precautions to avoid getting seriously hurt. Marshall 09-12-2015, 03:59 PM #355 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 "While I have not measured the particle size of the glass powder I am using, it is about the fineness of flour (my guess is 100 mesh or smaller). I have used a little coarser material in past primer formulations and it works well, but I was worried about barrel abrasion. The finer powder should be more like a polishing agent than an abrasive." Marshall, Thanks for the reply. I have been thinking that the screen size probably doesn't matter but was curious what you used. I saw some 200 screen glass the other day and I will see how well that works. That would be less than a quarter of the size of the flash channel and it should pass through without any real problem. Reply Reply With Quote 09-14-2015, 10:41 AM #356 ofitg Boolit Master Join Date Feb 2013 Posts 701 TTTC, I believe that the U.S. Army switched from H-48 (which contained ground glass) to FH-42 (which did not contain ground glass) because they determined that the antimony sulfide crystals could serve as grit. In this excerpt (page 54) from the 1922 book, Microscopy of Small Arms Primers, the author includes the specifications for those particle sizes - https://books.google.com/books?id=ohkxAQAAMAAJ&pg=PA20&lpg=PA20&dq=microscopy+of+small+arms+primers&source=bl&ots=joDelyDWyk&sig=0kWs_jFgYHIY7hjGSo3Adkuw7Xw&hl=en&sa=X&ved=0CDsQ6AEwCGoVChMI8Nbr8-f2xwIVwtGACh02egW1#v=onepage&q=microscopy%20of%20small%20arms%20primers&f=false mp54_zpssomhpfr3.png 09-14-2015, 03:04 PM #357 Texantothecore Boolit Master I definitely am going to test a batch without the ground glass. The percussion nipples (treso) have much larger anvil and striker surfaces and I suspect that it might work with the antimony sulfide. The volume of powder being crushed and shifted is much greater than with a firing pin and it is good to know that in at least one formulation the glass was found to be redundant. Thanks for the info and the link. Reply Reply With Quote 09-14-2015, 07:54 PM #358 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I did a comparison of several variations on the mix 2 formula vs a S&B commercial primer. Here is a picture of several fired primers (fired in empty 380 ACP cases) after disassembly: 20150914_201302_001.jpg 1 = Mix 2, 2 = Mix 2 w/ 6% PbO2 and 6% Sb2S3, 3 = Mix 2 w/ 6% PbO2 & 3% CaSi2 ipo 3% Al, 4 = S&B SP Primer As a reminder mix 2 is: Pb(H2PO2)2 35.0% Pb(NO3)2 35.0% Sb2S3 12.0% Al powder 3.0% Glass powder 15.0% Therefore Mix 2 mod 1 changes the formula as follows: Sb2S3 6.0% PbO2 6.0% And Mix 2 mod 2 changes the formula as follows: Sb2S3 6.0% PbO2 6.0% CaSi2 3.0% ipo Al powder While all primers fired, and were more than energetic enough to set-off a cartridge, primers 1 - 3 were noticeably less powerful than the S&B commercial primer. Plus, as you can see, formulas 1 - 3 left a significant amount of residue in the primer cup after firing. This could be because there is not enough extra oxidizer to consume the Sb2S3 and Al/CaSi2 fuel. However, it could just be lead oxide residue since these formulations are mostly lead salts. It is also possible that the lead hypophosphite + lead nitrate reaction to form lead nitratohypophosphite did not go to completion. It looks like more experimentation/tinkering with the formula may be needed. On the positive side, it was nice to find out that you can successfully use PbO2 and CaSi2 in the formula. Any ideas on how to improve the formula would be welcome. Marshall Reply Reply With Quote 09-15-2015, 07:07 AM #359 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I did an additional test this morning out of curiosity. I had not yet tried the original Eley Prime (EP) rimfire formula in a SP primer. So, I made up a few and tested them the same way as my previous post in an empty 380 ACP case. I found that the primers fired without problems, but were clearly not as energetic as the modified EP formulas (I rechecked them at the same time to get a good comparison). The extra fuel and oxidizer appear to make a big difference in the energy of the primer. So, I think the modified formulas are the right direction to go. They just need the initiator to fuel to oxidizer ratios tuned to the optimal level. I am currently reviewing a number of published primer formulas to see if a pattern of initiator to oxidizer to fuel ratios can be identified. It may be possible to further reduce the lead nitratohypophosphite percentage and up the oxidizer/fuel percentage to increase the output energy of the primer. I'll let you know if I come across a better formula. Marshall 09-15-2015, 10:37 PM #361 Oreo Boolit Master Join Date Mar 2009 Posts 1,914 Indeed. I especially like that a good non-corrosive primer can be made without ground glass. Just the idea of sending ground glass down the bore is like nails on chalkboard to me. Reply Reply With Quote 09-17-2015, 11:47 AM #362 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, After doing some research on known commercial primer formulations, I found that they typically contained 20-40% oxidizer and 12-25% fuel. Many times the oxidizer and fuel content were balanced, but there were plenty of exceptions. The initiator content was normally in the 40-50% range. The original rimfire Eley Prime formula contained 80% initiator, 0% oxidizer and 0% fuel (perhaps a little misleading since lead nitratohypophosphite combines all 3 functions). My centerfire modifications reduced the initiator content to 70% and the glass content from 20 to 15% which allowed me to add in 15% of fuel for mod 1 and 6% oxidizer and 9% fuel for mods 2 and 3. It seemed clear that the oxidizer and fuel content needed to be boosted even more. Based on this information I mixed up 2 additional modified Eley Prime formulas to further explore the addition of more oxidizer and fuel. I will use the mod designations that I have in my records, so don't get confused about the numbering gaps. EP Mod 4, 60% initiator, 15% oxidizer, 15% fuel Pb(H2PO2)2 30% PB(NO3)2 30% PbO2 15% Sb2S3 12% Al 3% Glass 10% 100% Test firing SP primers made with mod 4 mixture in an empty 380 ACP case were successful. Energy was similar to mods 1, 2 and 3. The residue left behind in the fired primer was similar to that found in mods 1, 2 and 3. EP Mod 9, 50% initiator, 25% oxidizer, 25% fuel (no glass) Pb(H2PO2)2 25% PB(NO3)2 25% PbO2 25% Sb2S3 15% CaSi2 10% 100% Due to the high loading of Sb2S3 and CaSi2, which can function as frictionators as well as fuel, I decided to drop the glass powder from this formula. That should be a relief to folks who were concerned about the effect of the glass on their barrels. Test firing SP primers made with mod 9 mixture in an empty 380 ACP case were successful. Energy was higher that all previous mods and more importantly a large bright flash was seen at the muzzle. The residue left behind in the fired primer was about half that found in mods 1, 2, 3 and 4. In conclusion, EP mod 9 primer formula is the best one found so far. Its advantages over previous EP formulas are: 1. More energetic (due to more oxidizer and fuel), 2. Sb2S3 and CaSi2 replaces glass powder, and 3. Large bright flash (likely due to CaSi2). I have every reason to believe this formula should work well in all primer types (SP/LP/SR/LR/Berdan) since SP/SR primers are usually the most challenging for primer mixture functioning. Next steps: 1. See if the lead nitratohypophosphite loading can go as low as 40% or even 30%. 2. Should 40% or 30% not work, determine if 3% added tetracene makes a lower loading possible . 3. Determine whether aluminum powder or CaSi2 is best. 4. Determine if Ba(NO3)2 can replace PbO2 as an oxidizer**. 5. Determine if Ba(NO3)2 can replace both Pb(NO3)2 and PbO2 in the mixture. ** This may or may not work since Ba(NO3)2 may compete with Pb(NO3)2 in forming a double salt. Enjoy, Marshall Reply Reply With Quote 09-18-2015, 08:33 PM #363 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 I spent a little time again looking for and finally found the heat of formation for lead nitrate. If I can find or at least estimate the heat of formation for Pb(H2PO2)2, it won't take long, a few hours, to figure out how much oxidizer is needed. My experience has been that when I've optimized that the primers are both more reliable and sensitive. @Marshall Are you using a gum or shellac? It would be interesting to see if there is any noticeable difference if you aren't. FWIW. While looking for that I came across something that is highly interesting in the area making primer compounds that I should have time to test in the next few days. If it looks like it has potential use, I'll post about it. Reply Reply With Quote 09-18-2015, 08:42 PM #364 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 @ Marshall I know I read a patent that when used other nitrates in addition to lead nitrate that worked. I think they are Remington ones. If I remember right, both double salts and triple salts are formed and how much of each directly dependent on the % of each nitrate used. As I'm now curious about it, I'll spend a little time looking for it. PS Was just looking and was reading Brun's patents. He states in 2239547 there that for lead styphnate primers "requires the addition of a small quantity of a substance which is more sensitive to percussion, such as tetrazene (guanylnitrosamilroguanyltetrazene), leadnitrato-hypophosphite, and the like." Then 8052813 used just 20% tetrazene so maybe a 20% leadnitrato-hypophosphite would work. In the French patent it was 20% tetrazene, 48% barium nitrate, 8% Al, 24% antimony sulfide. Maybe a primer with 20% leadnitrato-hypophosphite and the equivalent in lead nitrate to the 48% barium nitrate would work. That's about all I have time for today and don't even have time to figure the % of weight for the lead nitrate to provide that same oxygen as the 48% barium nitrate. Last edited by perotter; 09-18-2015 at 09:43 PM. Reason: PS Reply Reply With Quote 09-19-2015, 08:39 AM #365 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, More testing data: EP Mod 14 50% initiator, 25% oxidizer, 25% fuel (no glass) Pb(H2PO2)2 25% Ba(NO3)2 50% Sb2S3 15% CaSi2 10% 100% This does NOT work. I could tell when seating the anvil, that no double salt formation was taking place. The cup only contained a moist goo that easily squished around. So, this is a dead end. On-the-other-hand, the lack of reaction between Ba(NO3)2 and Pb(H2PO2)2 gave me hope that using Ba(NO3)2 in the place of PbO2 would work. EP Mod 13 50% initiator, 25% oxidizer, 25% fuel (no glass) Pb(H2PO2)2 25% Pb(NO3)2 25% Ba(NO3)2 25% Sb2S3 15% CaSi2 10% 100% This mixture works about the same as EP 9 which it was based on. I encountered one primer that would not fire and discovered a potential problem in my build method. It appears that the packed pellet sometimes does not completely moisten which limits how much reaction takes place. This was proven by scrapping out the unfired mixture for the failed primer, moistening the mixture outside the cup and repacking the moist mixture into the cup (with the dimple removed). After drying, the primer fired normally. I have probably been having this issue all along with all of my test primers. Therefore, I may have to go to wet packing until my tests are completed. @perotter, At the moment, I am not using any binder. I have been able to get away with this because the double salt reaction itself hardens and binds the pellet together as the lead nitratohypophosphite crystals form. As this happens during and after the anvil is seated, the resulting hardened pellet makes for a very reliable primer. That is partly why I prefer dry loading and then moistening the packed pellet. I have found that if you delay seating the anvil too long after moistening the mixture, it becomes difficult to seat them because of how hard the pellet becomes. Because of this, in my latest build method, I only moisten 5 primers at a time so I can quickly seat the anvils before the mixture becomes too hard. Regarding finding/calculating the optimal amount of oxidizer/fuel. I think I have enough guidance from published information on this topic. Experimentation will allow me to hone in on the best ratios to use. However, please share anything you find or calculate on this question. Marshall Reply Reply With Quote 09-19-2015, 05:45 PM #368 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by Desertbuck Wow! I can't believe how far this thread has come since it was started. Lots of good hard to come by information. And interesting ideas, keep them coming guys keep up the good work. Wish I had more to contribute but I have just been so satisfied with the Frankford Arsenal mix that I haven't pursued another. And truth be told primers are coming back so i haven't made any in awhile. Since 2009 I also have been satisfied with the FA mix and have firearms of all types that won't rust when using it. For me after that it is a more a hobby thing. Reply Reply With Quote 09-19-2015, 06:32 PM #369 perotter Boolit Master The advantage of using software to calculate to how the different amounts of oxidizer/fuel effect the compound is that in a few minutes one knows the both the amount of hot gas produced and temperature of it for a number of different percentages. After an initial run of using different percentages of what one thinks would work, one can quickly see the ranges that show the best potential. Then run again with much finer percentages(think 0.25% or less) to optimize the mix. By spending an hour or less with a computer and analyzing the output one can compare the experimental mix's amount and temperature of gases to known production mixes. But, even then there still needs to be enough make it and try it experimentation to occupy any time have available. Everyone should use the methods that make the them the happiest when working on a project of this nature. Reply Reply With Quote 09-23-2015, 05:54 AM #370 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, More testing data: EP Mod 10 40% initiator, 44% oxidizer, 16% fuel (no glass) Pb(H2PO2)2 20% Pb(NO3)2 20% Ba(NO3)2 39% CaSi2 11% PbO2 5% Sb2S3 5% 100% This mixture was based on a lead styphnate formula I found. Lead Styphnate 38% Ba(NO3)2 39% CaSi2 11% PbO2 5% Sb2S3 5% Tetracene 2% 100% So, basically the lead styphnate was exchanged for lead nitratohypophosphite. The tetracene sensitizer was dropped and its 2% loading was moved into lead nitratohypophosphite since it also functions as a sensitizer. This mixture worked well and gives good energy. Disassembling the primer shows about 1/2 the residue typically found in these primers. This formula shows that the lead nitratohypophosphite initiator loading can be reduced to 40% without problems. Next, I guess it is time to determine if a 30% loading will work. Marshall Reply Reply With Quote 09-23-2015, 02:25 PM #372 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Texastothecore Originally Posted by Texantothecore Marshall, did EP Mod 10 work? "So, basically the lead styphnate was exchanged for lead nitratohypophosphite. The tetracene sensitizer was dropped and its 2% loading was moved into lead nitratohypophosphite since it also functions as a sensitizer. This mixture worked well and gives good energy. Disassembling the primer shows about 1/2 the residue typically found in these primers. This formula shows that the lead nitratohypophosphite initiator loading can be reduced to 40% without problems." Yes it did. I only have two more items on my to do list from above: 1) go down to 30% lead nitratohypophosphite, and 2) compare aluminum powder and CaSi2 to see which is better. After that I am going to have to make another batch of lead hypophosphite in order to continue this work. Marshall Reply Reply With Quote 09-23-2015, 08:56 PM #373 TheDoctor Boolit Master Join Date Apr 2010 Location Needville, TX Posts 708 Anyone looked into Al-Bi2O3 yet? Reply Reply With Quote 09-24-2015, 08:33 AM #374 Marshall Boolit Man Join Date Mar 2014 Posts 113 @TheDoctor, Originally Posted by TheDoctor Anyone looked into Al-Bi2O3 yet? Do you have any references concerning this approach to making ammunition primers? I have seen several patents where a number of various metal oxides were used as oxidizers in primers (i.e. iron oxide, manganese dioxide, ...etc.). Let us know what you are thinking about. Marshall Reply Reply With Quote 09-24-2015, 09:43 PM #375 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Well I think I have found the lower limit of lead nitratohypophosphite loading. EP Mod 12 20% initiator, 48% oxidizer, 32% fuel (no glass) Pb(H2PO2)2 10.0% Pb(NO3)2 10.0% Ba(NO3)2 48.0% Sb2S3 24.0% Al 8.0% This formula is based on the Cheddite tetracene primer that was tested several pages back. Cheddite US8052813 Tetracene 20.0% Barium nitrate 48.0% Antimony sulfide 24.0% Al 8.0% After drying the primers in a food dehydrator for about 30 minutes they were tested as usual in a 380 ACP case. The primers fired, but were very weak. Disassembling the fired primers showed about twice the normal residue compared to previous successful primer formulas. I have concluded that 20% initiator is too low to get reliable ignition. It may be possible that replacing some or all of the aluminum with CaSi2 might help. In any case, I consider this formula a failure. So far, I like EP mods 9 and 13 the best. Marshall New information: I tried EP Mod 15 which is the same as EP Mod 12 except the Al was replaced with CaSi2. After drying I got the same result, only a weak pop and lots of residue left in the primer cup after firing. So, it doesn't seem possible to make a 20% initiator formula work. Last edited by Marshall; 09-25-2015 at 05:08 PM. Reply Reply With Quote 09-24-2015, 10:33 PM #376 TheDoctor Boolit Master Join Date Apr 2010 Location Needville, TX Posts 708 Can't get the link I want to copy. Google "Bi2O3 for priming". First link should be a pdf from dtic.mil. There are numerous references I'm looking at, but my research is in its infancy. I just got keyed onto the aluminum bismuth trioxide idea yesterday. Apparantly the NSWG has been doing a lot of research into this, and it seems that this will be the compound of the future. Last edited by TheDoctor; 09-24-2015 at 11:08 PM. Reply Reply With Quote 09-25-2015, 08:30 AM #377 TheDoctor Boolit Master Join Date Apr 2010 Location Needville, TX Posts 708 Ok, slam on the brakes for the Al-Bi2O3 idea. Further research reveals a fatal flaw to my plan. It seems that it's not just the addition of the aluminum, but the particle SIZE that's critical. Currently, and possibly forever, beyond my ability to make, and not economically feasible to purchase grades that fine. Talking nanometer scale.... Reply Reply With Quote 09-25-2015, 05:42 PM #378 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 Originally Posted by TheDoctor Ok, slam on the brakes for the Al-Bi2O3 idea. Further research reveals a fatal flaw to my plan. It seems that it's not just the addition of the aluminum, but the particle SIZE that's critical. Currently, and possibly forever, beyond my ability to make, and not economically feasible to purchase grades that fine. Talking nanometer scale.... A the nanometer size Teflon and aluminum work as primer compounds, but 4-5 years ago nano sized aluminum was over $160 a gram. Cheap enough to try, but too expensive for consider as a DIY primer. Reply Reply With Quote 09-25-2015, 05:53 PM #379 perotter Boolit Master Did you try a 20% mix with lead nitrate or lead dioxide instead of barium nitrate? But, I'm good with a 30-40% mix. Also, I'm thinking of use lead nitratohypophosphite as a sensitizer if a couple of simple non-corrosive mixes I made that didn't fire very often. I can't try them until after l get the fall getting ready for winter tasks done. Reply Reply With Quote 09-27-2015, 04:47 PM #380 Safeshot Boolit Master Join Date Mar 2005 Location Indiana, USA Posts 314 Cabela's has Large Rifle, Small Rifle & Small Pistol Primers "in stock" for $24.99 per 1000. Buy one of each, store in an ammo can, should "get you through" any period of "shortage" or "non supply". Purchase more when they are "on sale" and when Cabela's offers "free shipping". Just one approach. Reply Reply With Quote 09-28-2015, 08:44 AM #381 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Safeshot, You're missing the point. I bought over 10,000 primers from Cabela's when they had them on sale for $19.99/1000 a couple of months ago. When added to my existing stocks, I may not need to buy any primers for the rest of my life much less make them. We are doing this work for the knowledge it builds for the future. There will be shortages again one day, or worse yet, purchasing reloading components may be outlawed (illegally, but that doesn't seem to matter any more). This work proves that we can safely make reliable non-corrosive primers. To do this in the future may require the purchase of chemicals and materials that are easy to get today, but may not be later. Its your choice to make. After pressing in your last legally purchased primer what are you going to do? Personally, I'll be still shooting and hunting for many years after the last commercial primer is a distant memory. I also see it as a skill that could make you an invaluable asset to your friends and neighbors. Marshall 09-29-2015, 08:51 PM #383 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 FWIW. Some guanine nitrate arrived today that I'll be using to make both primer compound(two different ones) and for making powder. While there is no needed at this point to make a non-corrosive mix other than what Marshall is making, guanine nitrate can be made from easier to obtain(locally around here) chemicals if the need occurred. Also, I doubt the primer compounds will be as safe to use as his method. I won't be doing much work on either of these until the snow flies. Reply Reply With Quote 10-06-2015, 09:02 AM #384 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I have improved/fixed my build method for making EP primers. I traced my earlier problems to the water/alcohol mixture pooling on top of the paper foil instead of flowing into the primer mixture. The new method wets the packed primer compound "before" installing the paper foil (see below). ep primer build method.jpg First, the primer cup is filled with loose dry powder. After lightly (not tightly!) packing the primer mixture into a pellet, small drops of water/alcohol are added to one spot at the edge of the primer and the solution allowed to flow into the powder. As additional drops are added, you can see the moistened area grow larger. Look for the surface of the pellet to develop a sheen once it is completely moistened. No additional water is needed after that point. A paper foil is added and pressed into place, and then the anvil is mounted. If done quickly (i.e. within 1 minute) the mixture should easily flow around the anvil. If you delay too long, the pellet hardens and it will be difficult to get the anvil seated. Anyway, this is my new method and it works well. To avoid problems seating the anvils, I limit the number of primers I moisten at one time to 5. One other tidbit, I have determined that the perfect diameter for the paper foil in SP/SR primers is 4mm (or 5/32"). I have only been able to find 1 hand held paper punch in existence that makes this size hole and the only supplier is in England. There are plenty of leather punches in this size and even a metal punch, but not hand held punches. Marshall Reply Reply With Quote 10-06-2015, 02:09 PM #385 Oreo Boolit Master Join Date Mar 2009 Posts 1,914 Mind saying who? Or where to buy said punch? Reply Reply With Quote 10-07-2015, 06:25 AM #386 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Oreo, Hand Held Round or Ticket Punch - 4mm Hole http://www.amazon.com/gp/product/B00...ilpage_o00_s00 http://www.amazon.com/gp/product/B00M0NS0LG?psc=1&redirect=true&ref_=oh_aui_detailpage_o00_s00 4mmhandheldticketpunch.jpg It is <$10 with shipping from England. I have also seen this exact same paper punch from the same supplier on eBay, but for some reason it was more expensive there. Marshall *New Info* The 4mm punch has arrived and works great. The brand name is Rayher and it was made in Germany by Rayher Hobby GmbH (www.rayher-hobby.de). This information may open up other sources of the punch. I have also found out they are made in 1.5, 3, 4, 5, and 6mm sizes. I think the 5mm size might work well for punching out foils for LP primers. Last edited by Marshall; 10-10-2015 at 05:24 AM. Reply Reply With Quote 10-10-2015, 06:19 AM #387 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 FWIW. The only reason for the paper that is in a primer cup is to keep primer compound from sticking to the punch that is used when wet loading. If one is dry loading, there is no need for the paper. Also if you are setting up to reload primers, you really should make matched primer plates. For wet loading make one set that indexes over the cup plate. Between these 2 place a properly sized piece of paper. Then you when press down the punch it will both cut the paper and put it into the cup. Reply Reply With Quote 10-15-2015, 12:27 PM #388 Marshall Boolit Man Join Date Mar 2014 Posts 113 @perotter, Originally Posted by perotter Did you try a 20% mix with lead nitrate or lead dioxide instead of barium nitrate? But, I'm good with a 30-40% mix. Also, I'm thinking of use lead nitratohypophosphite as a sensitizer if a couple of simple non-corrosive mixes I made that didn't fire very often. I can't try them until after l get the fall getting ready for winter tasks done. I just finished testing EP Mod 16 % Pb(H2PO2)2 10.0 Pb(NO3)2 34.0 PbO2 24.0 Sb2S3 24.0 CaSi2 8.0 This mixture is similar to EP Mod 15, but replaces the 48% Ba(NO3)2 with +24% Pb(NO3)2 and 24% PbO2. This Mod fired weakly and left lots of residue in the primer cup. At this point, I have concluded that 20% lead nitratohypophosphite initiator is insufficient to properly set off the main redox reactions. I have not yet made a 30% lead nitratohypophosphite mixture, but it is planned in the near future. Here is the formula I have written for that test EP Mod 11: % Pb(H2PO2)2 15.0 Pb(NO3)2 15.0 Ba(NO3)2 35.0 Sb2S3 15.0 PbO2 10.0 CaSi2 10.0 I should have results on this mixture within a week. Marshall Reply Reply With Quote 10-18-2015, 05:32 AM #389 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, The results on EP Mod 11 are in and they are mixed. I had 2 out of 5 test primers give a strong pop while the rest gave only a weak pop. Disassembly of the fired primers showed that the ones with the strong pop contained little residue. The ones with a weak pop contained a lot of residue, some of which appears to be unburned. I plan to repeat this test to find out what happened. It could simply be we are in the intermediate zone between the amount of initiator that gives a consistently strong pop (40%) and that which gives a consistently weak pop (20%). Alternatively, it could be that the primers needed more drying time. Anyway, at this point I am not recommending going this low in lead nitratohypophosphite initiator. I'll report on the second EP Mod 11 test in a few days. Marshall Reply Reply With Quote 10-19-2015, 09:54 PM #390 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, The repeat test of EP Mod 11 gave better results, but were still mixed. 4 out of 5 primers gave a strong pop when fired and had very little residue in the cup after firing. On-the-other-hand, 1 primer completely failed to fire. The reason is unclear since all 5 were assembled at the same time using the same technique. I don't feel confident in this mix and don't recommend it for use. My preferred formulas are EP Mod 9, EP Mod 10 and EP Mod 13. Based on this information, I am thinking about revisiting the tetrazene based primers. If you recall, these primers used 20% tetrazene and did not work well in SP primers. I am thinking about bumping the tetrazene up to 30 or 40% of the mix to see if that will work better. Here is one possible formula: % Tetrazene 40.0 Ba(NO3)2 32.0 Sb2S3 20.0 CaSi2 8.0 The tetrazene formulas are especially attractive since they are lead free. I''l let you know how it works out. Marshall Reply Reply With Quote 10-21-2015, 05:54 AM #391 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Great news on the tetrazene based primer formula EPT 3 (see previous post for formula). SP primers made with this mixture fired strongly. My opinion is that these are the strongest primers I have made so far. Plus, there was NO residue other than fragments of the paper foil left inside the fired primer cups. ept3 test primers2.jpg Unlike the lead nitratohypophosphite formulas, EPT 3 was "wet" mixed in 90% isopropyl alcohol to safely breakdown and disperse the tetrazene. The result after air drying and gently crushing back into a powder was a light gray powder with a yellowish tint. Because all the ingredients are already mixed, more precautions should be exercised than the standard Eley Prime formulas we have been experimenting with lately as this mixture is complete and will be sensitive to handling. Primer buildup involved loading the primer cups with loose powder, packing tightly with a wood skewer, adding a paper foil, repacking tightly, moistening the pellet with dilute shellac/alcohol binder solution, and seating the anvil. Finally, the alcohol was allowed to completely dry. (Updated info: primers can be made without the binder solution, but with a higher risk of accidentally causing it to pop-off during anvil seating. However, based on testing, firing is unaffected by leaving out the binder.) According to the Cheddite patent, it is supposed to be possible to make the tetrazene in-situ which would improve the safety of this mix. My previous tests with this process presented earlier in this thread were a failure. If anyone has some ideas on how to make the reaction between aminoguanidine and sodium nitrite work in a neutral water medium I would be interested to hear them. (Updated info: I found some early (1928) synthesis methods for making tetrazene that used a neutral water medium for the reaction, so just plain water should work after all.) In conclusion, this approach with a higher loading of tetrazene was very successful in SP primers although with a higher safety risk during primer assembly. Marshall Last edited by Marshall; 10-22-2015 at 03:38 PM. Reply Reply With Quote 10-22-2015, 06:25 PM #392 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 One of the pro's of tetrazene is that what is needed to make it can be made easier than the ones for lead nitratohypophosphite. Of course at this point it this isn't a major concern, but who knows what the future holds. Thanks again Marshall for sharing your important work in this area. FWIW. Now that Marshal has shown how to make 2 different primers that are good for long term storage, I'm going to go back try a couple that are useful as short term use. The only advantage being the ease of getting what is needed to make them. I'll be starting the first on this week end, as I have Saturday night free and have the base chemicals, etc here. Reply Reply With Quote 10-24-2015, 06:14 AM #393 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, One of the reasons progress has been slow in testing Eley Prime process formulations is the amount of time it takes to completely dry the water out of the assembled primer. While I have put primers in a food dehydrator several times to speed up drying, the lack of temperature control on my dehydrator concerned me since the temperature would reach ~80C. After thinking about the problem, I imagined having a thermostatically controlled heated aluminum block to set the primers on that could be kept around 50C. While searching for something like that I stumbled across the perfect solution. Biologists have used temperature controlled heating blocks to incubate things in test tubes. Sure enough, eBay is full of used ones at reasonable prices. So, I picked up the one shown below for $19.99 + shipping and am now using it to dry primers. equathermprimers.jpg I flipped the test tube holder block upside-down so that the flat bottom was exposed. The unit keeps the aluminum block at a uniform constant 50C. There are other ways to do this job, but this approach is almost ideal. Marshall Reply Reply With Quote 11-06-2015, 10:34 AM #394 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Several miscellaneous recent activities. 1. Based on how remarkably clean the tetrazene based EPT 3 formula fired, I decided to make an analogous lead nitratohypophosphite formula to see if it would burn as cleanly. EPH 19 % Pb(H2PO2)2 20 Pb(NO3)2 20 Ba(NO3)2 32 Sb2S3 20 CaSi2 8 100 The test primers were found to fire strongly. However, they were not as clean as the EPT 3 primers. A small amount of residue, similar to that in EPH 13 primers, was found in the cup after firing. Either the optimal oxidizer to fuel loading is different for lead nitratohypophosphite based primers, or these primers just inherently produce some residue on firing. Perhaps perotter can run some theoretical calculations for me to help identify the best oxidizer to fuel loadings. BTW, the new Equatherm block heater was used to dry these primers and they were ready for testing after only 1 hour of drying at 50C (instead of two days at normal ambient conditions). It has been raining, drizzling and humid here for the past 5 days, so the block heater really helped speed things up. 2. I had the recent opportunity to test a number of .380 ACP reloads using a combination of steel berdan primed cases and standard boxer primed brass cases. All primers were made using EPH 13 compound. I am pleased to report 100% success with these test rounds. The testing confirms that EPH 13 when combined with my latest build methods provides a reliable, consistent primer. 3. Just before the above shooting session, I was showing someone how I made primers using the EPT 3 formula. I mentioned that the percussion sensitivity of primer compounds could be tested by striking a small pile (about the amount that goes in a SP primer) with a hammer. So, I decided to give a demonstration and was quite surprised at the results. I was UNABLE to get the EPT 3 formula to explode by striking the pile of compound with a hammer. Frankly, I am both astounded and relieved that the same formula that works so well packed inside a SP primer cup is so insensitive to repeated hammer blows. This behavior suggests that working with the EPT 3 formula is not as risky as was initially believed. This finding does not imply that we need to drop reasonable precautions in working with EPT 3 (i.e. goggles, small batch size, non-sparking tools, avoidance of unnecessary friction, ...etc.) but does suggest a lower risk of accidental ignition while working with it. I would love to know if anyone can offer up a good explanation for this difference in behavior to percussion. 4. Finally, I have been so impressed with the power and cleanliness of the EPT 3 primers that I am seriously thinking about making and using them in most of my pistol practice ammunition. That would preserve my stock of commercial primers and also allow me to make a large scale evaluation of the reliability of these primers. I have already made up ~250 SP primers over the past month. I have also made up 100 9mm steel cased berdan primed rounds. The reloading of these steel cased rounds is especially pleasing since I am literally turning trash into treasure. One of the local ranges is more than happy to give me all the steel cases I want when I visit. So, I have plenty of steel cases to work with. Next steps 1. Synthesis some barium hypophosphite and use it in a double exchange reaction with lead nitrate to make both lead nitratohypophosphite and barium nitrate in one step. The formula for making the equivalent of EPH 13 would become as follows: EPH 17 % Ba(H2PO2)2 25.0 Pb(NO3)2 50.0 Sb2S3 15.0 CaSi2 10.0 100 End is result is the same as EPH 13, EPH 13 % Pb(H2PO2)2 25.0 Pb(NO3)2 25.0 Ba(NO3)2 25.0 Sb2S3 15.0 CaSi2 10.0 100 Whats the advantage? None really, except making barium hypophosphite is less hazardous than making lead hypophosphite. Plus, it is just plain clever to do it this way! 2. Synthesize some styphnic acid and use it to make Eley Prime process lead styphnate based primers. I have everything I need to do this, I just need ~1/2 a day to dedicate to the synthesis and purification of styphnic acid. I don't need much material to prove out the method. For me this is the ultimate conclusion of this work, to safely make primers that use the same compounds as commercial primers. I plan to do this for both rimfire and centerfire cartridges. I have NO plans to ever make, isolate and directly use lead styphnate. Here is my planned rimfire formulation: EPS 0 % Styphnic Acid 21.5 PbO 20.0 Ba(NO3)2 20.0 Tetrazene 3.5 Glass 35.0 100 and here is my planned centerfire formulation: EPS 5 % Styphnic Acid 20.0 PbO 18.0 Ba(NO3)2 39.0 CaSi2 11.0 PbO2 5.0 Sb2S3 5.0 Tetracene 2 100 That's all that is happening at the moment, but ideas are always coming on interesting things to try out. Marshall Last edited by Marshall; 11-06-2015 at 10:40 AM. 12-08-2015, 07:07 AM #396 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, The final step has been taken in making a "modern" non-corrosive primer compound. I synthesized some styphnic acid last weekend using a method that generated nitric acid in-situ from ammonium nitrate and conc. sulfuric acid. Be warned that in solution, styphnic acid is a highly staining, bright yellow chemical. It was found to be possible to remove spills/drips/spots of the material from undesired places with baking soda (and it will find its way to undesired places!) This even works for your hands/skin, so keep some handy if you ever work with this chemical. With the styphnic acid in hand, I prepared the following Eley Prime type centerfire formula: EPS 5 % Styphnic acid 20 Lead oxide 18 Barium nitrate 39 Lead Dioxide 5 Cacium silicide 11 Antimony sulfide 5 Tetrazene 2 After dry mixing the above ingredients a light brown powder was obtained. This mixture was dry packed into prepared SP primer cups and lightly moistened with a water/alcohol mixture. A paper foil was added and the anvil was seated while the mixture was still moist (note: the end of my bamboo skewer was heavily stained yellow during the addition of the paper foil, so be very careful as to what the moist mixture touches). The completed primers were placed on my test tube block heater at 45C for about 1 hour to complete the reaction between styphnic acid and lead oxide, and to dry the primers. The EPS 5 primers were tested in an empty 9mm casing and they worked perfectly. The firing was very strong and there was a bright flash at the muzzle. There was very little residue left in the cups after firing (mostly paper fragments from the foil). These primers seem to have exactly the same power and flash as witness commercial primers I have tested in the same way. In conclusion, the Eley Prime process works for safely making a modern lead styphnate based primer compound. The only other place to go from here is to make some of the recent non-lead/non-toxic compounds. Lots of wet synthesis will be needed to make the precursor chemicals for these formulations (e.g. PETN, DDNP, KDNBF). I am not sure that I am up to this task without a well equipped wet lab. These things are hard to do on your picnic table out back. Who knows what the future may hold. Anyway, I am very pleased with the results on the EPS 5 formula and will happily stay with it for awhile. Reply Reply With Quote 01-02-2016, 08:50 AM #397 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, During our family's traditional target shooting on Christmas day (to try out those new guns some of us received that morning) I tried some 9mm test rounds made with the EPS 5 primers. As expected, the rounds fired identically to those made with commercial primers. This is the final confirmation that the primers work as intended and with 100% success. I continue to make and stockpile between 10-20 EPS 5 primers each day. Once I have enough saved, I'll start routinely making my practice ammunition with them. I am also thinking about making indoor practice ammo that uses just the primer to propel a glue bullet. This works great with commercial primers, but I have always been reluctant to use up my hard earned purchased primers in this way. Using EPS 5 primers will solve this dilemma and give the same fun without the pain. I don't expect everyone to want to make their own primers, but as long as there are people in power that keep the drumbeat of gun/ammunition control going, we need to be prepared for the worse. At a minimum, I highly recommend that folks keep a good stockpile of components for making all of their important ammunition. Get it now while you can. That is what I am doing myself. I still need to get my stockpiles of 40 and 45 projectiles up to an acceptable level. I also need a few more bullet molds to be able to cast for everything I shoot. Time is not our friend in this struggle for freedom. Marshall Reply Reply With Quote 02-22-2016, 08:36 PM #400 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Its a red letter day! I just finished making and storing my 1,000th EPS 5 SP primer. It took about 3 months to complete this task (its a labor of love not economics). These primers were made in batches of 10-25 at a time and used multiple preparations of EPS 5 compound. Every new batch of EPS 5 compound was tested as it was introduced to make sure it worked properly. And every batch made so far has worked perfectly. As this number of primers meets my threshold for storage, future batches will now be used in reloading ammunition. When these primers are combined with my cast bullets, the cost per round essentially drops to just the powder cost. One interesting aside, while cleaning up previously fired primers for use in my reloading experiments, I ran across a couple of dozen of old primers that used 2 legged anvils. This type of primer has probably not been made since the 1960's or 1970's. It was fun to think that these antiques could be resurrected and reused instead of thrown in the scrap bin. You might could even think of this as being "green" @Dean Weingarten, Thanks for the support. Those of us who are committed to this work have endured much derision for doing something with an element of danger. Thank goodness, the Internet was not around to discourage the first astronauts that strapped themselves on top of a large tube packed with high energy compounds. We persevered, and we were successful. Marshall 02-26-2016, 09:53 AM #401 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 Marshall, my understanding is that producing styphnic acid releases obnoxious vapors. How do you handle the vapors? Reply Reply With Quote 02-26-2016, 01:51 PM #402 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Texantothecore, The noxious gas that is produced during the nitration reaction is reddish-brown colored NO2. The only safe way to do this reaction inside is in a chemical fume hood with good ventilation. Instead, I ran the reaction outside on the picnic table and stayed upwind of any fumes. To help reduce the amount of fumes emitted, I placed a small inverted plastic condiment cup over the mouth of the flask. It did not seal the flask so any pressure could easily be relieved, but it did drastically reduce the amount of fumes released. I periodically manually stirred the mixture using a glass rod, but would have greatly preferred using a magnetic stirrer. Be sure to use nitrile gloves to keep from staining your hands bright yellow. You really need a vacuum filtration setup to quickly separate the precipitated styphnic acid from the reaction mixture and efficiently wash out the residual mineral acids and salts from the filter cake. I decided to not recrystallize the styphnic acid as the crude product is plenty pure enough for making primer compound. It certainly has worked flawlessly in the EPS 5 formulation. I hope this helps. 02-26-2016, 11:31 PM #404 Dean Weingarten Boolit Mold Join Date Feb 2016 Location Arizona Posts 6 Congratulations on the 1,000 EPS 5 primers. Quite an achievement. I look forward to further reports. It seems you have found the EPS 5 method superior to EPT 3. Doesn't the EPS 5 require the synthesis of both stypnic acic and tetrazene? Are there advantages in the EPT 3 method, and was that the method explained in post 334 on this thread? Could you explain the advantages on one of the above methods over the other? Sorry if I am being a bit dense, but the thread is a little confusing in the nomenclature. Reply Reply With Quote 03-01-2016, 11:23 AM #405 Marshall Boolit Man Join Date Mar 2014 Posts 113 Dean, There is a method to my madness. The "EP" in the name stands for "Eley Prime" which is the method for safely producing the primary explosive in situ. The last letter represents the primer technology used. Here is a complete list: H = Hypophosphite, T = Tetrazene, S = Styphnic acid, P = Picric acid (unpublished results), N = Non-toxic (unpublished results), Be aware that there are not any true EPT formulations since despite a valiant effort, I was unable to synthesize tetrazene in situ. So, despite the EP name, these formulations use previously synthesized tetrazene and no reactions occur in the primer cup. The advantage of the EPS 5 primers vs EPT 3 primers are mainly due to the greater power and hotter sparks of the EPS formulation. As you note, both styphnic acid and tetrazene must be synthesized in order to make the EPS 5 formula. The only formulation that matches the power and flame of the EPS formulas are the H-48 corrosive primers. Post 334 describes several lead nitratohypophosphite formulations, so they are of the EPH class. The main advantage of EPT primers is that they are lead free and non-toxic (but so are the H-48 based primers). Also, if you can get the precursor chemical to tetrazene (aminoguanidine bicarbonate) the synthesis of tetrazene in high yield is trivially easy. I hope that helps. Marshall Reply Reply With Quote 03-01-2016, 09:11 PM #406 Dean Weingarten Boolit Mold Join Date Feb 2016 Location Arizona Posts 6 Thank you very much. It helps quite a bit. Very useful and intiguing information. Have you given advise on depriming steel cased berdan cases? I tried a hydralic method on a steel .223 case. My first attempts did not work, and it seems that I expanded the neck so that I needed to use a different tool for a pressure ram. Pointers would be appreciated. Reply Reply With Quote 03-02-2016, 08:24 AM #407 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Dean, I have successfully hydraulically deprimed berdan 223 steel cases using a bolt that was laboriously ground down with a file while spinning it in a drill. However, 99% of the berdan cases I deprime are done with a drill bit that has ~1/2" of the end ground down small enough that it will fit inside the tiny flash holes. I then slowly tap out the primer while alternating between flash holes. Sometimes, I'll put some WD-40 around the primers and let it soak in a few minutes to help break them free. You occasionally lose a stubborn primer when the end of the drill bit pierces the primer while trying to walk it out. It sounds tedious, but when I am on a roll, it only takes about 10 seconds/case to remove a berdan primer. I'll see if I can take a picture of my "depriming tool" when I get home and post it later. Small numbers of primer cups are easily cleaned ultrasonically in water using a drop of dish detergent and a pinch of citric acid. BTW, virtually all of the berdan primed steel .380 ACP, 9mm, 45 ACP, and 223 Rem cases use 5mm diameter primers. While some berdan primers are available in the US (mainly for 7.62x39 and 7.62x51 NATO), nobody seems to carry this particular size. So, the only way to reload these cases is to reload the primers. Reloading the primers is basically the same as for boxer primers until the paper foil has been added. At that point, either the primers are dried and stored for future use, or they are loaded into cases while still wet and then dried. The latter method is what I have been doing lately. Once a berdan case is primed and dry, the rest of the reloading steps are identical to boxer primed cases. As an interesting aside, the aluminum berdan primed cases that are sold under the Blazer name, use standard size SP and LP primers but without the anvils. So, if you wanted to reload one of the cases (e.g. to use them with glue bullets) you could just pop out the anvil from a standard SP/LP primer and press it in. Finally, the new Winchester steel cased 9mm ammunition uses standard SP boxer primers and is easily reloaded. Some might ask, why go through the trouble of reloading berdan cased ammunition? One reason is that cases are plentiful and free. One range I practice at gives me all the steel cases I want just to take them off their hands. Second, in a crisis situation, steel cases may be the only cases you can get. Third, steel cased ammunition is great when you are shooting in areas where there is no hope of recovering your cases (i.e. shooting over water, in high weeds, at some shooting ranges that keep all brass). Fourth, its something that many people do not believe can be done. So, it blows their minds to see someone doing it. Lastly, it is turning trash into treasure. Marshall Reply Reply With Quote 03-03-2016, 06:30 AM #408 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Here are some pictures on how I deprime almost all berdan primed cases: 20160302_201643.jpg Here is my setup and a .308 Win steel case. 20160302_201631.jpg The drill bit is in a flash hole and after a few taps it is switched to the other flash hole. With experience, you can feel the primer move as it slowly backs out. 20160302_201820.jpg Success! Primer is out and undamaged. After cleaning it up and removing the firing pin dimple, it will be ready to reload with new priming compound and reinstall into the case. So, that is how I do it. If the primer cannot be successfully removed, the case is thrown into my scrap steel bucket without regrets. Marshall Reply Reply With Quote 03-03-2016, 08:37 PM #409 Dean Weingarten Boolit Mold Join Date Feb 2016 Location Arizona Posts 6 I wonder if anyone is making a two pronged depriming tool. I seem to recall them from a few decades ago, when I was reading about reloading berdan cases. I would think the spacing for 5mm berdan flash holes would be fairly uniform; but I know some berdan cases use three flash holes. I suspect the larger primers have different hole spacing. I read on an India forum that Afghans made primer cups from brass head gasket material. I suspect that primer cups would be a fairly simple 1 or 2 step process. Reply Reply With Quote 03-04-2016, 06:49 AM #410 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Dean, The main problem with making custom tooling is finding a machinist who is interested in working on what may be a one off project. My attempts to interest Lee Precision in making me a couple of custom items have been invariably turned down (latest was a collet crimp die for 22 LR). I have talked to a couple of local machinists as well and I was unable to interest any of them in my projects. Regarding depriming berdan cases, I ran across a few custom tools on eBay that hydraulically removed them, but without using a tight fitting piston. Instead, the case was sealed at the bottom, the tube filled with water, and the piston fit the tube rather than the case. Same effect, but with no danger of swelling or distorting the case as the piston pressurizes the tube interior. It would be a slower method, but I could envision a bayonet style connector on the bottom that could quickly be put on and taken off. This is probably the only way to remove crimped in berdan primers. I have swelled several brass 223 Rem cases using the piston inside the case method. It looked like a balloon just below the case neck. My ground down drill rod tool was worthless as well with the primers invariably being pierced. The quick, clean, undamaged removal of berdan primers is definitely an operation that needs some good solutions. 03-05-2016, 12:49 PM #415 Texantothecore Boolit Master Join Date May 2011 Location Jersey Village, Tx Posts 1,340 22 rimfire has the dimple removed by putting the round, half full of water, into a short length of 22 barrel inserting a small closely fit rod and hitting it with a hammer. It was commonly done during the great depression and it did keep the case from swelling. So you might try that technique. 03-05-2016, 05:36 PM #420 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Texastothecore, Yes I am familiar with the RCBS tool. Unfortunately, it destructively removes the primer. Because 5mm berdan primers are unavailable in the US, the primers need to be removed in such a way that they are reusable. Marshall Reply Reply With Quote 03-05-2016, 08:17 PM #421 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 One could maybe get Pat Marlin to make up the tooling to make 5mm berdan primer cups. It wouldn't be different than one of his gas check maker, just a different size. I think he is still a forum vendor here and one can contact him thru this sight. FWIW. I have made a few boxer sized cups with aluminum and tried them in .38 Special rounds. They worked. My neighbor had a punch that worked for making the blank. I bolted 2 pieces of metal together and drilled an 1/8 hole. Then took them a part. In one I drilled a hole to make the cup, in the other I drilled a hole to center the blank and bolted them back together. I tapped the blank though the cup forming hole with a piece of rod and hammer. They weren't pretty and it was slow, but they worked. It satisfied my curiosity as to if it could be done without any special tools, knowledge, etc. I used anvils from commercial primers. It was 20+ years ago and don't remember the thickness's or any other measurements. PS Somewhere(gas check section?) here on the forum there is a down-loadable pdf on how to make a proper one pass die for making cups. One would want to have a lathe available to do this. One would have to figure out the sizes, as only the sizes for gas checks are in it. Also, G. Frosts book goes into plenty of detail on making the tooling for primer cups. I check and I do have it downloaded and can email it to them as it isn't very large. Last edited by perotter; 03-05-2016 at 08:28 PM. Reason: ps Reply Reply With Quote 05-09-2016, 07:20 PM #422 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I just received an interesting result on SP primers made with toy caps. My son-in-law recently fired a box of 50 9mm rounds I made in June 2013 using toy cap primers (see design below). Homemade Primer.gif Each primer uses 2 cap blisters with a dash of fine gunpowder between the caps. After carefully mounting the anvil, they are ready to load. The particular rounds fired used 4.4 gr of Bullseye and a 115 gr FMJ bullet. Results were: 100% normal firing! So, reliability was 100% after ~3 years of storage under typical household temperature and humidity conditions. Cap primers are not strong enough for reliable ignition in all applications, but in this particular round they work very well. So, although corrosive, this simple primer solution has a valid place. Plus, caps are cheap and do not (yet) draw any unusual attention when purchased. Toy caps are another useful item that can be purchased and saved for a rainy day. Marshall Reply Reply With Quote 05-10-2016, 08:43 AM #423 GONRA Boolit Master Join Date Jan 2016 Posts 205 GONRA noted comments on hydraulic decapping. This was pretty successful on a batch of 14.5x114 Soviet "brass" (Chicom lacquered coated steel cases) years ago. Got about 100 cases out of initial batch of <150 "fired cases". (Some weren't fired, so didn't mess with 'em.) Making the 9mm Berdan primers (2 grains Donnard's 1959 patent mix: lead styphnate 37%, tetracene 3%, barium nitrate 30%, lead dioxide 5%, PETN 5%, antimony sulfide 15%, zirconium 5%) using cups formed on CH Swag-O-Matics with my own tooling was a Whole New Hobby...... Last edited by GONRA; 05-11-2016 at 04:10 PM. Reply Reply With Quote 07-01-2016, 07:06 PM #424 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I have not been completely idle since my last post. I have been acquiring some additional lab equipment and chemicals to make some of the lead free primer formulations. Yesterday I snagged a used but nice Corning PC-351 hotplate stirrer for only $43 on eBay to help with the required syntheses. While waiting for all this stuff to come in, I have been reloading some 22LR rounds using EPS2 formula: Rimfire Formulation EPS 2 % gr Styphnic Acid 24.9 8.2 PbO 23.0 7.6 Ba(NO3)2 22.5 7.4 Glass 25.0 8.3 Tetrazene 4.6 1.5 Here is a photo of how these rounds are made: 20160701_060712.jpg After wet tumble cleaning some fired 22 LR cases with SS pins and drying, the cases were resized, and the rim area scraped clean of old primer residue. The mouth is lightly flared to receive a bullet (best done BEFORE priming the case) and a scoop made from a SP primer of EPS2 compound was added to each case. Enough water was added to make a moist slurry of primer compound and it was stirred with a small metal rod to make sure the compound was well mixed and flowed into the rim area. The slurry was allowed to air dry for several days at room temperature at which point they were ready to reload. 1.5 gr of Bullseye was added and a 40 gr cast lead heeled bullet popped into the case. The bullet was crimped using an Old West Bullet Moulds collet crimp die. Finally, I lubed the bullets using Blue Bear Lube Cold and they were finished. So far, all of the 22 LR rounds I have made and tested have fired normally in both a bolt action rifle and a Ruger SR-22 semi-auto. Waste of time? Perhaps. I recently bought a couple of 325 round bricks of Federal Champion Match ammo, so I am not hurting for 22 ammo at the moment. But, it just feels good to know that you could roll your own if you needed to. Once the cases are primed, the rest of the process is really quite trivial. Marshall Reply Reply With Quote 07-03-2016, 07:04 PM #427 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, See this link for a copy of a training course I did for making homemade primers: Homemade Primer Course Update.pdf While it does not cover all the work I have done, it covers all the basics of the various ways primers can be reloaded. I'll expand the section on lead free non-corrosive primer formulations after I have done some experiments. Share this document with anyone you think might be interested. We need a knowledgeable army of folks who would not be affected by a government crackdown on ammunition and reloading components. The more we know, the less likely it will affect us, and ultimately the less likely it would be that the government would try it. This is my end goal, to share knowledge now so we can give would be tyrants the finger in the future. 07-17-2016, 07:13 PM #431 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Due to a recent unpleasant accident, I am now recommending that ~1% gum arabic be added to the EPS2 formula. I knocked over a small plastic condiment cup that contained about 80 primed 22 LR cases and it fell ~24" onto a carpeted floor. The primer compound in around 1/3 of the cases fell out or turned into a loose powder after this very mild fall. Sadly a small amount of the powder spilled onto the carpet, !@#$%^&*. Fortunately, I managed to vacuum it up without incident (risky, but I got away with it this time.) If that small spot ever gets wet in the future, its probably going to turn into a yellow mess . Anyway, I went back and added gum arabic binder solution to all the cases to make sure the pellets stay together after drying (again). I'll let you know if I encounter anymore problems with these fixed cases. BTW, this is not a problem with EPH0 primer compound since it is self binding. The lead nitratohypophosphite crystals make an interlocking network as they form creating a strong solid pellet. Also in its favor is that the lead nitrate/lead hypophosphite/glass powder mixture is a white non-staining powder . Still is not good if you spill some on the floor because of the lead salts, but at least it doesn't make a stained mess. Some things you learn the hard way . 09-08-2016, 05:43 PM #433 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, Well its time for something a little different. Many folks have noticed that it is not always easy to obtain some of the raw materials needed to make non-corrosive primers (e.g. resorcinol which is needed to make styphnic acid). So I decided to work on a series of formulations that start with a raw material that anyone can make starting with common off the shelf materials, namely picric acid (aka 2,4,6-trinitrophenol). Picric acid can be easily synthesized starting with 1) aspirin, 2) Rooto Drain Cleaner (i.e. conc H2SO4), and 3) Spectracide Stump Remover (i.e. KNO3). I won't waste time detailing the synthesis since there are plenty of Internet links explaining the procedure. Using one of these procedures, I recently made a small batch of picric acid in high yield (>90%). picric acid crystals.jpg Picric acid is chemically similar to styphnic acid and forms percussion sensitive lead salts. Also like styphnic acid, the lead salts of picric acid can be made in 2 chemically distinct forms: 1) "normal" lead picrate and 2) "basic" lead picrate. However, while both the normal and basic forms of lead styphnate can be used in primers, only the basic form of lead picrate is sensitive and energetic enough to be used in primers. Another drawback of picric acid is that it's reaction with lead oxide is more difficult and slow compared to styphnic acid. In addition, the direct reaction of picric acid and lead oxide produces the "normal" version of lead picrate instead of the desired "basic" version. Basic lead picrate is typically made by reacting an alkali metal picrate salt with lead nitrate. None-the-less, I was curious what would happen if I attempted the Eley prime process using picric acid and lead oxide. The first formulation tried is an adaptation of a known "basic" lead picrate formula in patent US1900157. US1900157 % Lead Picrate 25.0 Pb(NO3)2 55.0 CaSi2 8.0 Sb2S3 10.0 Tetracene 2.0 EPP5 % Picric Acid 13.0 PbO 12.0 Ba(NO3)2 55.0 CaSi2 8.0 Sb2S3 10.0 Tetracene 2.0 After moistening the mixture, I could immediately tell that picric acid was less reactive than styphnic acid with lead oxide as no perceivable reaction occurred. Primers dried overnight at room temperature only gave a weak fizzle instead of a pop upon firing and contained a lot of unburned residue. The remaining primers were remoistened and redried to see if more lead picrate could be formed assuming the problem was caused by a poor/slow conversion of picric acid and lead oxide into lead picrate. The remoistened and dried primers also failed with identical results. Another batch of primers were made and dried at 50C to see if a higher temperature would improve the conversion to lead picrate. These also failed, with only a weak fizzle being obtained. So, either the reaction to make lead picrate in situ doesn't generate enough lead picrate to initiate the primer and/or the "normal" form of lead picrate just doesn't have enough sensitivity/energy to work. Before abandoning this approach, another try was made on an EPS5 analogue. The styphnic acid in EPS5 was directly replaced with an equivalent amount of picric acid. This formulation was designed to test whether an increase in lead picrate loading would improve firing energy. EPP7 % Picric Acid 20.0 PbO 18.0 Ba(NO3)2 39.0 CaSi2 11.0 PbO2 5.0 Sb2S3 5.0 Tetracene 2.0 Unfortunately, the results were identical to the EPP5 formulation and only a weak fizzle was obtained. At this point it looks like if you want to make a lead picrate based primer, it will be necessary to synthesize "basic" lead picrate in a separate reaction. Although lead picrate is less sensitive to shock and ESD than lead styphnate a significant risk remains of accidental ignition. I came across one story where a careless home chemist destroyed his kitchen oven while drying ~2 grams of lead picrate. So, this approach will have significantly reduced safety. I'll post again and let everyone know if I decide to directly synthesize and test basic lead picrate (or you might read about it in the national news . One Eley Prime type approach to make basic lead picrate that might work is to react potassium picrate and lead nitrate in situ. While it can be detonated, potassium picrate is much less shock sensitive than lead picrate (Ref: According to Urbanski**, Potassium picrate detonated 10% of the time when struck by a mass of 2kg dropped from the height of 21cm. By comparison, the more sensitive anhydrous lead picrate detonated 10% of the time when struck by the same mass dropped from the height of 2cm.) EPP8 % K Picrate 25.0 Pb(NO3)2 55.0 CaSi2 8.0 Sb2S3 10.0 Tetracene 2.0 Any lead nitrate in excess of what is needed to react with the potassium picrate will function as an oxidizer. The side reaction product will be potassium nitrate which will also serve as an oxidizer. This approach is interesting and may have some promise since it is similar to the reaction that produces basic lead picrate. The main problem I anticipate is that the initial reaction of potassium (or sodium) picrate with lead nitrate produces basic lead picrate monohydrate. The percussion sensitive form of basic lead picrate is anhydrous which is formed during continued heating (at ~80C) in the standard prep procedure. In this case, it may be necessary to dry the primers with heat to get the dehydration step to occur. Here is an additional formulation that is adapted from one in the Frankford Arsenal Ordnance Laboratory Report AD0223114 dated 1932: AD0223114 % Lead Picrate 38.0 Ba(NO3)2 38.0 CaSi2 11.0 PbO2 5.0 Sb2S3 5.0 Tetracene 3.0 Eley prime version EPP9 % K Picrate 23.0 Pb(NO3)2 28.0 Ba(NO3)2 25.0 CaSi2 11.0 PbO2 5.0 Sb2S3 5.0 Tetracene 3.0 So much to do and so little time. I'll get back with some more results on these new formulations once they have been completed. Marshall ** Urbanski, Tadeusz (1964), Chemistry and Technology of Explosives, Volume 1, New York: Pergamon Press. Reply Reply With Quote 09-11-2016, 02:00 PM #436 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, I synthesized some potassium picrate yesterday to use in the EPP8 and EPP9 formulations. Potassium Picrate.jpg I then made up and tested a batch of the EPP9 formulation: EPP9 % K Picrate 23.0 Pb(NO3)2 28.0 Ba(NO3)2 25.0 CaSi2 11.0 PbO2 5.0 Sb2S3 5.0 Tetracene 3.0 Primers were prepared using the normal Eley Prime build-up method. They were then dried at 50C for 6 hours. This was longer than planned (ok, I forgot to turn them off) and shorter/milder drying times need to be tried. The dried primers were tested in an empty 9mm case and they fired as strongly as my EPS5 primers. Very little residue was left in the fired primers. So, this modified procedure appears to have successfully made basic lead picrate. Drying at lower temperatures and for shorter times will tried later to determine if dehydration of the basic lead picrate occurs during heating operation and whether or not it is required. I haven't made any of the EPP8 formulation yet, but have no reason to believe that it will not function just as well as EPP9. In any case, we have another useful approach to making non-corrosive primers. Marshall Reply Reply With Quote 09-12-2016, 05:49 PM #437 Marshall Boolit Man Join Date Mar 2014 Posts 113 @All, The good news just keeps on coming. EPP9 primers that were air dried at room temperature for 24 hr fired strongly and exactly the same as the ones dried at 50C for 6 hr. In addition, the primers do not appear to be hygroscopic. I retested some of the original primers I made after sitting out in the open for 24 hr. All fired strongly. This approach seems to be wrapped up now. Another viable Eley Prime method to safely make non-corrosive primers. I haven't stopped working on non-toxic / lead free formulations and have in fact received all of the needed chemicals to make KDNBF and DDNP. It make take another month or two, but I will eventually finish this work. Admittedly, there is not a lot of urgency since so many good solutions exist. Marshall 09-17-2016, 07:37 AM #440 Marshall Boolit Man Join Date Mar 2014 Posts 113 Range Report on EPP9 primers Although my test firings of EPP9 primers in an empty 9mm casing have been successful, the ultimate test of a new primer formulation is in ammunition. Therefore, I made up 2 sets of 9mm test rounds, 10 using SP boxer primers in brass cases, and 10 using 5mm berdan primers in steel cases. These were compared against reference rounds made with Sellier and Bellot SP primers in brass cases. The loading of all rounds was: 115 gr FMJ / 4.4 gr Bullseye / 1.150 OAL 26647 psi / 1154 fps / 340 ft-lb / 97.8% burn / 80.8% fill The test results were very good with 100% firing of all test rounds. In addition, based on perceived recoil and bullet placement on the target the test rounds performed exactly like the reference rounds. In conclusion, SP boxer and 5mm berdan primers made with EPP9 compound perform equivalent to commercial primers in 9mm rounds. 09-17-2016, 07:53 AM #441 Marshall Boolit Man Join Date Mar 2014 Posts 113 NOE resizing die for 5mm berdan primers @All, I have wanted a resizing die to repair mushroomed 5mm berdan primers for some time. I typically have to reject ~50% of all primers removed from berdan cases due to slight mushrooming of the head of the primer: 5mm Berdan Primer Resizer.png This mushrooming makes it difficult to seat the reloaded primers back into a case. If the mushrooming is minor, the primer will squeeze down enough to seat (i.e. the primer resizes in the primer pocket). On-the-other-hand, primers with more severe mushrooming have popped off while trying to "force" them into place. I envisioned a custom 5mm resizing die to remove the mushrooming from these primers so they can be reused instead of scrapped. After discussions with NOE Bullet Mold company, they have made me a custom 5mm (0.19685") bullet resizing die. It was not a simple request since they did not have tooling to made a die this small. Instead of telling me to buzz off (like Lee Precision did) they discussed it with their machinists and eventually figured out a way to make this die. Thanks NOE! You have my eternal gratitude! NOE 5mm Resizing Die.jpg Although these dies are made for resizing bullets, the 5mm die is plenty robust for fixing these distorted 5mm berdan primers. The mushroomed primers are coated with a little Lee case lube and then forced through the resizing die head first. I can confirm that primers fixed this way do seat normally. Some of these fixed primer cups were recently used to make test EPP9 primers for the recent range test of 9mm rounds. The only improvement I need for this die is a modified end on the pushrod that supports the inside of the cup as it is forced through the die. This will true up the inside of the cup and better support the cup as it is resized. It might even restore the rounded edge of the cup for slightly flattened cups. Ram Modification.png I tried to talk NOE into making this modification, but they didn't bite on this one. However, this is a fairly simple mod that I may be able to make myself using a drill press and a file. Anyway, I am thrilled to finally get this new die and look forward to being able to reload a lot more berdan primed cases in the future. Marshall 10-05-2016, 10:43 AM #444 EDG Boolit Master Join Date Mar 2005 Posts 2,552 If you want to safely make a priming mix you might think about the handling processes and the equipment design that will keep you safe. I used to work for the largest semi-conductor capital equipment manufacturer on the planet. It was founded by a chemical engineer who wanted to supply chemicals to the semiconductor manufacturers which was an emerging industry at the time. A couple of his chemicals were silane and arsine. Both are pyphoric and burn on contact with the air. His potential customers were very impressed by the design of his lab equipment which was designed to handle these materials safely. Instead of buying his chemicals they wanted to buy his equipment so they too could safely handle these guaranteed to kill you materials. Safety can include lock out tag out. Fail safe valves. Redundant controls and back up systems. The designs included a cabinet (box) built around the stick of gas mixing valves. If any of the 6 to 12 gas lines and valves had a leak the cabinet exhaust system would transport the gas out of the factory. All transformer cabinets had locked access doors. Inside were clear lexan safety shields locking out the ordinary employees. Only qualified service electricians could open the clear shields. During the design of this equipment one of the last things done was to check the fit of the shields for "Darwin Holes". A Darwin Hole was any gap in the shields that would permit an employee to reach the energized circuits with a screw driver. Helium though inert can suffocate you in an enclosed space so you have to be careful with it. The factory's helium purge gas is used to flush the atmosphere and remaining process gases out of a chamber before starting the next process. The helium keeps the inside of the chamber dry and clean. An example of how you can screw up was one of our designs that had many gas line junctions in a common area. One of our set up employees crossed 2 sets of lines. The helium line was supposed to be connected to a normally closed valve. Instead it was connected to the chamber which was connected to the factory exhaust system. The employee went home and $500,000 of helium was vented to the atmosphere over the week end. This shut down the factory until a new supply of helium was delivered. My employer paid the cost of the helium and the shut down. In this case the design engineering group was held responsible. The gas lines were redesigned so none of the connections could be crossed up. 10-05-2016, 11:43 AM #445 Traffer Boolit Master Join Date Feb 2016 Location Central Wisconisn Posts 418 While the processes involved are very different, it is good to have ample warning about dangers. I have read many of the stories on the internet of accidents involving Armstrong mix. Indeed I have had it send me to the hospital. Armstrong mix was the common primer of the past. It was even manufactures on a large scale. A manufacturer in London had an accident in which stone blocks over a ton were thrown hundreds of yards and many people were killed. Many people have been killed or maimed by it through the years. When I work with it now, I never work with it unless it is wet. And then only in batches of less than 5 grains. The last time I used it I had about a third of a grain ignite on me...EVEN THOUGH IT WAS WET. Certainly that much did not harm me but startled me where my pulse definitely went up a lot. So thanks for the further warning. Can never be too safe handling dangerous material. 10-05-2016, 09:34 PM #446 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Traffer, Can you provide a reference of Armstrong mixture ever being used as a primer? In all my reading and research on primers, I have never come across any reference to this mixture being used in this way. It is possible that this mixture might have been used as a primer in cap form since they are made from Armstrong mixture. So, I guess the use of roll caps in some pre-percussion cap muzzle loaders, or in homemade percussion caps from aluminum cans, or in primers reloaded with toy caps, or to reprime fired 22 LR cases could be considered to be primed with Armstrong's mixture. However, I think as a general rule, Armstrong mixture is way too sensitive and unpredictable for normal use in standard ammunition primers to the point of being very dangerous. It looks like your experience with this mixture bears that out. I would like to warn folks considering Armstrong mixture for reloading primers to be aware of the extreme danger of making and handling this material. Before trying this idea, you would be well served to do a lot of upfront research. Plus, you still end up with a corrosive primer. So, they would have no advantage over H-48 mixture which has an excellent balance of sensitivity and stability when used in ammunition primers. Be safe folks! Yesterday, 12:18 PM #447 Traffer Boolit Master As I was not a chemist when starting to use this material, I was not aware of it's historical uses. I started using it after reading that it was being used as a primer in 22lr by the Sharpshooter company that produces a kit for reloading 22lr. At that time I researched it in the internet and found a good deal of reference to it concerning it's potential hazards. I also had first hand experience with the danger of it as I had a mishap as a child making fireworks. I checked again on the internet when writing my last post, a couple of days ago. I was rather amazed and disappointed to find that the information appears to be gone. I couldn't find any of the references to accidents with Armstrong mix in the past. Indeed even the word Armstrong Mix seems to have been purged from the normal search channels. Eventually I gave up looking. Why would Google or the powers of the internet purge Armstrong Mix? I don't like this development. As far as citing instances of it being used as primer, I only know of the recent use of it that is documented on the internet. It was a surprise to me to hear you say that it was not used in the past. I wonder what they were using it for back then. There certainly were factorys producing it in volume. I am not a chemist. I am not advancing a new chemical or compound for a new use. I am one of many people who has learned that Armstrong Mix (in the form of toy roll caps) can be used for the explosive in primers. Indeed I would not even be using it now if I hadn't bought so much of it when first starting. I am anxious to move away form it to go to one of the fine non-corrosive primers that you have graciously shared with us. We all appreciate you work and are grateful that you share it with us. Until reading this post, I had no idea the it was not used as primer in the past. Now that I can no longer find much reference to it on the internet, I cant even research the history and historical uses of it. If it is too dangerous/sensitive to be using as primer I certainly would like to know. I am sure that everyone else would also. I think that if the govt got wind of this they would take it off the market. Don't know if I care for that solution though. Reply Reply With Quote Yesterday, 05:57 PM #448 Marshall Boolit Man Join Date Mar 2014 Posts 113 @Traffer, Regarding your comment: "Why would Google or the powers of the internet purge Armstrong Mix?" I think some other folks in this thread have experienced similar search difficulties. You might try some different search engines other than google. I did a search on the terms " armstrong's mixture" and got over 159,000 hits. If you are getting less, I think google or the government is restricting your access to data they think is dangerous for the public to know. This is probably just a small taste of what we can expect in the future after the turnover of the internet to the UN. If you can, get your important information NOW while you still can. Same thing with ordering chemicals to make primers. The time may be coming when access will be restricted to the pyro chem sites. I don't want people to think I am paranoid, but there are many people in government who do not trust the common man. And it is not likely to get better any time soon. Buying a pound of potassium chlorate now beats trying to make it in the future from bleach and potassium chloride. Marshall Reply Reply With Quote Yesterday, 06:26 PM #449 perotter Boolit Master Join Date May 2009 Location SE Minnesota Posts 3,524 From what I've read the Dreyse rifle used a red phosphorous/potassium chlorate primer mix. I'll have to dig out a few books I have stored away to see which one or one's have that information in. If one has or can get red phosphorous, it would be better to use a nitrate like barium/lead nitrate instead of potassium chlorate for the primer mix. Reply Reply With Quote Today, 01:58 AM #450 M.A.D Boolit Bub Join Date Sep 2011 Location Australia Philippines (Good) Posts 45 With 25 year experience as a explosives technician... All i can say is, DON'T EVEN THINK ABOUT IT. But if you wish to make an attempt at a Darwin award... Then The History of Powder and Explosives By Dr Tenny L Davis is your safest bet.. Look forward to reading about you in the Obituary.. Reply Reply With Quote Today, 07:58 AM #451 Duckdog Boolit Master Join Date Dec 2007 Location Northern Wisconsin Posts 213 I can assume your referring to the Armstrong mix? I use the H48 mix and consider it very stable when handled properly. Reply Reply With Quote