DIY Smokeless Powder - A4 Smokeless Powder Manufacturing

[MUSTANG]

This is another series of DIY home manufacturing Smokeless Powders
Using instructions from the source reference written in 1944 on page 33 of PRIMERS for Small Arms Cartridges by M. J. ALBERT and H. F. OELBERG, Copyright, March-1944. A pdf copy is available at: https://www.aardvarkreloading.com/re...%20Oelberg.pdf


The production of the A4 Smokeless Powder formula is similar to my other thread on the No.7 smokeless powder formula. The A4 Formula by weight is:

Ammonium Nitrate NH4NO3 7.5 grams (115.74 grains)
Potassium Nitrate KNO3 4.0 grams (61.73 grains)
Lead Nitrate Pb(NO3)2 4.0 grams (61.73 grains)
Hydrocellulose C12H22O11 3.4 grams (52.47 grains)

The original Instructions call for mixing the above with an equal quantity of RAIN WATER or Tap water, but soft water is better. Water should not if not softened by alkalis.

[MUSTANG]

My first hurdle is creation of Hydrocellulose. The original Paper Instructions called for producing Hydrocellulose through the following Instructions:

TO SECURE HYDROCELLULOSE: Into the bottom of a 2-quart glass jar place 300 sheets of NORTHERN TISSUE - about half the roll. Pour over this tissue enough pure commercial MURIATIC ACID to cover the paper and rise an inch above – about 1 1/2 pints. Jar somewhat over half full. Place the glass lid, with rubber scaling ring, on the jar loosely, but so that it will not fall off and so that it will prevent fumes climbing out. Boil the jar slowly for 30 minutes IN A KETTLE OF WATER. Keep jar off the bottom of the kettle by setting jar on pieces of coiled wire. Stir your acid and paper two or three times during the 30 minutes. And keep the lid on the jar, not tightly, but by its own weight to retain the fumes. Set kettle and all off the fire and let cool.

When cool, dump the whole tannish-gray colored thick soup into a cotton sack – a good 10 pound clean sugar sack - and flood and wash the contents of your sack UNDER RUNNING WATER. DO ALL OF THIS DUMPING AND WASHING OUT OF DOORS. The acid will not hurt your hands - remember we are talking of MURIATIC ACID. Don't lose any of your hydrocellulose out of your sack in the washing. Work the sack from the bottom with your left hand, holding the top shut with your right. After washing many times, drop into your sack 3/4 full of hydrocellulose and water, 2 teaspoonful of Bi- carbonate of Soda - common baking soda. Shake the sack, and add water, and then wash many times. Wash until you can taste neither soda nor acid. Test with blue litmus paper if you like. If neutral, squeeze out all of the water possible, crumble the hydrocellulose finely, spread out on newspaper in a hot and dry place, clean and ventilated, and let dry 24 hours. It is then ready to weigh and use in powder mixtures.

[MUSTANG]

My first dilemma was creation of the “Tools” necessary to accomplish this task. Muriatic Acid was procured at ACE Hardware. Toilet Paper was procured from the guest bathroom via a previous Costco Purchase. The roll was mostly expended, so I counted out 75 sheets (vs the referenced ~ 300 sheets in the original paper). I retrieved a clean Glass Peanut Butter Jar from storage that was destined for Fall vegetable canning. The Toilet Paper was placed into the wide mouth Peanut Butter jar and compressed with a wooden Chop stick onto the bottom of the Jar. Muriatic Acid was poured onto the toilet paper and up to a level 1 inch above the paper per the original instructions.

[MUSTANG]

Directions called for a Glass lid and Rubber Scaling ring; not available in today’s common market – so I improvised and used a small Stainless Steel Bowl from the reloading room, with the curve on the bottom of the Stainless Steel Bowl fitting into the wide mouth jar – forming a light seal to keep the fumes in.

BIG MISTAKE!!!!

Keep in mind, I am not a chemist. I had read in my research that Muriatic Acid would react with some metals. My research did not reveal which metals it reacts with. Turns out that Stainless Steel is one of the metals it will react with. The bottom of the stainless steel bowl had a greenish substance collect/form on the bottom of the bowl during the subsequent production process where the mixture was heated. The greenish substance that formed also caused a slight staining of the underside of the Stainless Steel Bowl; when cleaned after the production process was completed.

ADDITIONAL CAUTION!!!

Upon completion of the cooking and washing process (described later) I dumped the residual Muriatic Acid mixture into the Gravel on the Driveway and washed the Hydrocellulose Product with water. I then washed some of the glassware in the kitchen sink; another mistake. Evidently there was sufficient acid remaining in the glassware that it left some slight discoloration of the Kitchen Stainless Steel sink where it was placed before washing. Not enough to upset my wife; but enough that I can see it. For marital harmony; wash outside in a manner that avoids the stains.
I am thinking a small ceramic bowl may be the solution for a “Lid” to keep fumes within the Jar when making Hydrocellulose in the future.

[MUSTANG]

To “Cook” the Toilet Paper/Muriatic Mixture; I used a 2 quart cooking pot with about 2 – 3 inches of water in it. To keep the Peanut Butter Jar off the bottom of the pan (allowing the temperature of the TP/Acid to be boiling water temp, and not higher due to contacting the Steel Pot on the Flame) I used 3 Small Mouth Caning Jar Screw on Rings as elevation platforms on which the Peanut Butter Jar sat in the boiling water.

The TP/Acid mixture was cooked in boiling water for 30 minutes. Be Aware; if one lifts the “Lid” to stir the TP mass as recommended in the original directions, there is a foul smell from the fuming of the Muriatic Acid. If possible; cooking this mixture is best done outside.

As time passes, the Toilet Paper in the mixture will start to turn brown on the bottom of the Glass jar and then become totally black over the 30 minute period.

[MUSTANG]

After cooking, I took the pot and Jar of TP/Acid outside and let it sit to cool for 45 minutes. After noting the problem with the small Stainless steel bowl used as a “Lid”; I did not want to use any of my Stainless Steel/Steel screens or Kitchen Strainers in my arsenal of “Shop Tools” due to probable corrosion if coming into contact with the Muriatic Acid.

ENTER PROBLEM #2.

I had previously bought an inexpensive Nylon/Plastic screener from amazon with a 100 mesh non-metal screen. See: https://www.amazon.com/dp/B0B7XMJLW7...t_details&th=1

Turns out that whatever the Mesh material is that forms the 100 mesh screen; it is incompatible with Muriatic Acid. I had read that some plastics were not compatible with Muriatic Acid; but once again there was no specifications of which ones. Results of pouring a small amount of the cooled TP/ACID Mixture through the screen:



The Mesh was destroyed by slight contact with the mixture; but the outside handle and ring were undamaged as they seem to be another material (Nylon?).

The original instructions had called for using a cotton Flour Sack. Once again, not currently available in todays market environment (Have not seen a cloth flour sack for at least 10 years). I had a “EUREKA” moment. I haven been taking my worn out cotton underwear (Cotton Briefs not Cotton Boxers)and washing them, then cutting them up to make cotton cleaning patches for Rifles and Pistols (Frugal – Not Broke). I took a set that had not been cut up yet and cut a large piece that I could pour the TP/ACID mixture through; using another jar to capture the filtered liquid from. I the Pored some water through the captured mixture. Then I twisted the neck of the material and squeezed out the Liquid – repeated while rinsing with additional clean water numerous times until I felt the Muriatic Acid was out of the mixture.

I did not use any baking soda to neutralize the Muriatic Acid as discussed in the original paper; this was due to the difficulties of the adhoc use of Cotton Underwear to capture and clean the captured Hydrocellulose material. I am thinking of buying some of the small cotton sacks listed on Amazon or Walmart ON LINE sites for future efforts in order to more closely follow the original instructions.

[MUSTANG]

I Placed the mixture in the Dehydrator yesterday evening; but turned it off over night as I am not sure what temps the Hydrocellulose can tolerate; my concerns are that if it replicates “Gun Cotton” (Totally different Acid Mixtures) it could ignite when moisture is gone and temp is too high.

I currently have the Hydrocellulose mixture in the Dehydrator for the day and will see how removing the water is progressing. Dehydrator is set at 100 degrees. It is taking some time to dry; still damp inside if the clump is broken open.

[MUSTANG]

I have been doing additional research on the "Ignition Temperatures" today for Nitro Cellulose (Not what is being used for the A4 Powder), and HydroCelllulose (This is what IS being used for the A4 Powder). The information seems to be sparse to minor conflicts in various sources (written Papers) on the Internet.

Generally I found:

Nitro Cellulose Ignition Temperatures: Most references give a range of 180 °C to 210 °C (Max 221 °C).
Cellulose 410 °C, hemicellulose 370 °C and lignin 405 °C ignition temperatures.
Charcoal 349 °C ignition temperature .
I found no data on Ignition Temperature for Hydrocellulose (What is being used in the A4 formula).

My obvious concern is to ensure that the Dehydrator does not represent and Ignition Source for the Hysdrocellulose production. My extrapolation is that the Hydrocellulose Ignition will be significantly higher than the Nitrocellulose used in Single/Double/Triple base conventional Rifle and Pistol powders. Once again; not Hydrocellulose as used in the A4 powder; but a paper found in the US Naval Institute Proceedings Magazine/Paper an article by
By Lieutenant R. W. Henderson, U. S. Navy entitled The Evolution of Smokeless Powder, dated April 1904 Proceedings Vol. 30/2/110 addressed the production of Gun Cotton for making Single Based Powder (Nitrocellulose). This article stated the US Navy's powder was dried at a temperature of 95 °F to 105 °F depending on weather. Not that this is helping alleviate my concerns; but it does provide some level of comparison and consideration as I move forward.

[perotter]

FWIW. If one wants to study NC powder making, the best source of detailed information is the volume of the series of books that Urbanowski wrote that contains that information. His books are available for download free of charge.

One thing I learned that was that what I've been doing the last few years is that I won't be able to exactly be able to duplicate in the future. There would be be a bit of back to the drawing board and testing to see what I get. That's the reason why I don't share publicly or freely what I've done, as some people seem not to excrise proper caution - they seem to think that they are making something akin to normal store bought powder.

[MUSTANG]

Pulled the Hydrocellulose Product out of the Dehydrator today after having been dried for about 24 hours over a two day period with Dehydrator turned off over night. Interesting result. The water had been squeezed out from the black sludge that formed, by twisting and squeezing it through the cotton cloth, then placed in the dehydrator. (Pic of the "Hydrocellulose" product):



The product produced by the Muriatic Acid Treatment of Toilet Paper is very, very, very hard when dried. I tried grinding it down with the face of a claw hammer in a small stainless bowl. After about 10 minutes I only created about 15 Grains that would pass through a 40 mesh screen. I got out the Ceramic Mortar and Pestal I use in my variety of Primer Making efforts; and after another 7 minutes, I had achieved grinding another 17 grains (total of 32 grains) that passed through a 40 mesh screen. I'll use this in producing five test rounds of the A4 Smokeless Powder over the next week or so.

I have a quandary -

I have been looking for papers on the Term "Hydrocellulose"; as spelled and referred to in the instructions from 1944. There is next to no links to that term on the Internet. A variety of other Cellulose products and papers can be found. I located one on Line "Dictionary" that indicated the Term Hydro Cellulose came into use back in the 1830 to 1840 period; and the use of the word dramatically increased until the late 1930's then has fallen to infrequent use in today's world.

My reference for the A4 powder states:

Hydrocellulose C12H22O11 (The C12H22O11 being the Chemical Formula).

My quandary is that researching the Chemical Formula C12H22O11; I find that formula is for good old white Table Sugar. If the Hydrocellulose created is actually a form of Table Sugar; why would the Authors go to the trouble to fabricate the product with Acid when the local Store of the time would have had sugar. If the formula for the Hydrocelulose created with the Acid treatment of Toilet Paper IS NOT C12H22O11; then what is the Formula for what I have actually replicated based on the Authors 1944 instructions?

Any chemists out there that can help with what the Chemical Formula (and alternate names if exist) for the Hydrocellulose created?

[ofitg]

I'm not a chemist, but if you go to Google Books and search for "hydrocellulose", there are several pages of documents/publications which date back to the 1900s and 1800s.... you might find the answer (?)

https://www.google.com/search?tbm=bks&q=hydrocellulose

[perotter]

....[/INDENT]

My quandary is that researching the Chemical Formula C12H22O11; I find that formula is for good old white Table Sugar. If the Hydrocellulose created is actually a form of Table Sugar; why would the Authors go to the trouble to fabricate the product with Acid when the local Store of the time would have had sugar. If the formula for the Hydrocelulose created with the Acid treatment of Toilet Paper IS NOT C12H22O11; then what is the Formula for what I have actually replicated based on the Authors 1944 instructions?

...

Because AN won't work with table sugar. It has to do with the melting points of the two. I've tried a few times to prove the experts wrong on this, didn't get a much more than smoke and a bunch of carbon residue.

FWIW. If one wants to go a with a simple to make AN based propellant, table sugar substitute sorbitol will work. Sorbitol melts at a low temperature and mix can be made without using water.

[MUSTANG]

Because AN won't work with table sugar. It has to do with the melting points of the two. I've tried a few times to prove the experts wrong on this, didn't get a much more than smoke and a bunch of carbon residue.

FWIW. If one wants to go a with a simple to make AN based propellant, table sugar substitute sorbitol will work. Sorbitol melts at a low temperature and mix can be made without using water.

Thanks. I was going to do a 5 round with the Hydrosol Test Mix and 5 rounds with Sugar as a test. Based on your experience/advice; I will not waste the chemicals on the sugar replacement in 5 rounds. For those 5 rounds, I will replace the Hydrosol with Fine Charcoal (the original paper indicated that a replacement with Charcoal was an alternative; so I will see how that performs).

I am also doing a lot of reading and contemplation/cogitation/analysis on the Links that ofitg cited in post #11.

[MUSTANG]

My Smokeless Powder source dated 1944, on page 33 of PRIMERS for Small Arms Cartridges by M. J. ALBERT and H. F. OELBERG, Copyright, March-1944. The Chemical formula cited for Hydrocellulose was:

HydroCellulose - C12H22O11.

A paper published in 1899; EWP Hydrocellulose and its Derivatives , By A GIRARD, page 379, provides the following Chemical Formulas:

Cellulose - C12H10O10

When transformed by hydration using acids it becomes HydroCellulose
Hydrocellulose - C12H11011

So, my original 1944 source document may or may not have a “Typo”, since it has the Hydrogen at 22 (Sugar); whereas the 1899 document has the Hydrogen listed as 11. In both cases; there is additional Hydrogen and additional Oxygen in the Hydro Cellulose, compared to the source Cellulose.

Currently I have not resolved anything; nor made the situation clear in my mind. Has the chemistry of Hydrocellulose disappeared from current societal focus/knowledge, been discovered to be incorrect, or simply not used as better products have replaced it in the last 90 to 120 years?

I will continue reading and researching. Doing a Firefox browser search on C12H11011 turns up a variety of “Mole Calculating” on line tools (of no use to me at this time), and reverts to numerous links where Sugar (C12H22O1) is listed. No actual discussions of Hydrocellulose or C12H11011 provided by search engine.

As stated; will continue to research, and read the articles from links the oftig provided in post 11. Chemists welcome to comment.

[perotter]

Thanks. I was going to do a 5 round with the Hydrosol Test Mix and 5 rounds with Sugar as a test. Based on your experience/advice; I will not waste the chemicals on the sugar replacement in 5 rounds. For those 5 rounds, I will replace the Hydrosol with Fine Charcoal (the original paper indicated that a replacement with Charcoal was an alternative; so I will see how that performs).

I am also doing a lot of reading and contemplation/cogitation/analysis on the Links that ofitg cited in post #11.

You're welcome.

[perotter]

Some might be interested in this patent. It does have a drying temp for the hydrocellulose, but a different process of making it. The final use of it is related.

https://patents.google.com/patent/US597565A/en

FWIW. For those that don't know, the reason for using hydrocellulose is to remove unburnable ash from the cellulose.

[Sandro_ventania]

This is another series of DIY home manufacturing Smokeless Powders
Using instructions from the source reference written in 1944 on page 33 of PRIMERS for Small Arms Cartridges by M. J. ALBERT and H. F. OELBERG, Copyright, March-1944. A pdf copy is available at: https://www.aardvarkreloading.com/re...%20Oelberg.pdf


The production of the A4 Smokeless Powder formula is similar to my other thread on the No.7 smokeless powder formula. The A4 Formula by weight is:

Ammonium Nitrate NH4NO3 7.5 grams (115.74 grains)
Potassium Nitrate KNO3 4.0 grams (61.73 grains)
Lead Nitrate Pb(NO3)2 4.0 grams (61.73 grains)
Hydrocellulose C12H22O11 3.4 grams (52.47 grains)

The original Instructions call for mixing the above with an equal quantity of RAIN WATER or Tap water, but soft water is better. Water should not if not softened by alkalis.

Interesting...I'll follow your Mustang efforts! One thing I found strange is that hydro cellulose seems to be the only fuel in the mixture, but the quantity seems to be very little. Another thing I would like to understand is how ammonium nitrate works...why not just use potassium nitrate?

[Sandro_ventania]

Studying here... Cellulose and hydrochloric or sulfuric acid cause the hydrolysis of cellulose. creating Nanocellulose. Something old that is being rediscovered as a fantastic material. Today it is possible to buy nanocellulose even on eBay.

[MUSTANG]

Finished producing the A4 (Rev-0) Powder as described in the 1944 Paper entitled - Primers for Small Arms Cartridges by Albert and Oelberg. The Test lot production amount was scaled to produce enough powder to load 5 rounds, with each round having 32 Grains. Batch size produced was:

Ammonium Nitrate NH4NO3 - 66.4 Grains
Potassium Nitrate KNO3 - 36.4 Grains
Lead Nitrate Pb(NO3)2 - 36.4 Grains
Hydrocellulose (C12H22O11 (? ? ?)) - 30.9 Grains

This batch was dehydrated for about 18 hours total at 100 degrees Fahrenheit in the Dehydrator. This Powder was produced with Hydrocellulose; but it was NOT cooked on a stove, rather its was thoroughly mixed in well water (about mili-liters) then placed into the dehydrator. Initially the mixture was a black color, but when dried it was somewhat a brownish color.



Powder was screened to fall through a 20 Mesh Screen; and all powder falling through that screen was mixed with about equal numbers of large and small kernels in each of the 5 rounds loaded.

Additionally, I am going to make some different versions of the A4 Powder (Some using Charcoal instead of the Hydrocellulose), and then do a 5 Round Test comparison of each Formulation after they are completed and loaded into 5 round test batches. Upon completion of each test batch being totally dried; I will load them into .308 cases with RCBS 200 Sil cast Bolts to preclude the powders picking up moisture from the air.