View Full Version : Pulling Down Some Old Handloads - Interesting Find...
So..Pulling down some hand loads that were from a development effort back on 06 - 07.
This was ammo for short range rapids in XC shooting. National Match stuff.
Everything was identical except for 2 powder types.
Berger 73gr LTB bullets
New Federal Gold Medal .223 brass - factory primed w/ FGM 205M primers.
Powder was various weights of N140 and N540. All slightly compressed
Pulled all the bullets w/ a Hornady LNL collet puller - the 140 loads came out a bit sticky - took a tad more oomph to get them out.
540 loads came out with ease. I noticed in all the 140 loads, the base of bullet was discolored. The 540 loads - base of the bullet looked brand new.
Here is the kicker; The 540 loads pour out after a little help with a toothpick - easy. Inside the cases - clean and bright - new brass just like when they were loaded.
The 140 loads...wow! Inside the cases were almost black. The powder had to be scraped off the walls and the walls were what appeared to be oxidized. Kind of a greenish grey discoloration.
I have never ever seen anything like this - anyone ever experience anything similar?
Theories?
Hunches?
Moisture/humidity when actually working up the load? It seems you are not the only person who has experienced this.
http://www.falfiles.com/forums/showthread.php?p=3745264
I use n135 and n140 and have never experienced this myself. Would be interesting to know what chemical reaction causes this and if there is a time frame/shelf life for VV loads.
Good find - I read through the whole thread. It is interesting to note that this ammo was loaded in brand new Fed GM brass w/ factory loaded FGM 205 M primers - both powders were dropped during the same loading session. Brass came from the same box - literally everything was exactly the same except the powder types. The two different powder type / loaded ammo were stored in the same MTM plastic box. My shop is temp / humidity controlled - the only difference between the corroded ammo and the non corroded was x number had N140 and x number had N540. Really is very strange.
Interestingly enough, I never had much luck with the N140. Far better results w/ N540.
I will dump the pull down powder in the garden (my wife thinks she has a green thumb - little does she know how much old powder goes in the flower beds LOL) :lol:
Sticking with N540 for a new effort.
Would love to get to the bottom of this though.
Interesting. Normally powder doesn't work as a fertilizer due to being non water soluble. But that stuff sounds like it might break down.
I am no chemist and hated it in high school.
I believe there are some significant differences in the chemistry of VV N140 and N540, 140 being a single base (nitrocellulose) propellant and 540 being double-based (nitrocellulose and nitroglycerin -- higher velocity at less pressure but higher temperature).
Smokeless powder manufacturers will add different stuff which affects powder in different ways. Each can affect how the powder deteriorates.
Deterrants affect burn rate. Stabilizers reduce decomposition and oxidation. Flash reducers come at the cost of added smoke. Other ingredients help in reducing powder or copper fouling, reducing barrel wear, aid production by keeping propellant grains round, reducing clumping, helping powder grains flow through machinery, or by helping to reduce static electricity and sparking.
If you leave powder in a powder measure with a clear plastic storage tube you may notice the transparency and color of the plastic changing over time as it's affected by chemical exposure or change. This may be from acids or other chemical interaction with the plastic.
Yep. I stained my Dillon powder hopper plastic by leaving Pistol powder in it years back.
28215
Here is a pic of a sectioned case - which was loaded with N140. Every case was like this as well as the bullet bases (see the ones on the right). The cases loaded w/ N540 were spotless - I didn't even bother sectioning them. The bullets were fine as well. Again - this was a development effort - the brass came from the same lot, was prepped all at the same time, loaded within minutes of one another - bullets from the same box.
The only variable was the powder. This was loaded in 2007.
I'd love to get Vihtavouri's take on it, but I highly doubt they'd even comment on it.
BTW - all ammo is stored in GI cans, with desiccant bags. Shop is climate controlled as well.
Baffled here...
Anyone want to buy some N140? 24lbs available....:blink:
Nitrocellulose smokeless powder begins to deteriorate as soon as it's produced. Diphenylamine is usually added at 2 percent by weight to help slow the oxidation process.
Army Quality Assurance Specialist Ammunition Surveillance folks monitor ammo for heat and decomposition. Once ammo gets old, stale, or acid (by measuring fumes and heat) they'll test ammo by lots (including sealed ammo). Some stuff like .50 cal, .45 ACP, 30-06, and 105mm howitzer ammo produced during WWII and Korea is still serviceable and soldiering on.
Some stuff gets to a certain identified safety level or level of decomposition and gets pulled down. Components might be sold as pulled powder, brass, and bullets, while the primers are chemically inerted (usually by immersing in an oil).
Interesting to note the N140 seems to have a fairly aggressive corrosion rate in this particular case.
A spin-off the Army found with its WWI 30-06 was tin-plated bullet jackets cold-soldering to the inside of case necks. Hatcher explained this would boost pressures to near-proof levels.
I also found that the powder completely corroded the primer too - they wouldn't even go bang.. ?!?!
it would be interesting to find out whether the n140 you had issues with is the same lot# as the person at falfiles, perhaps it was more something to do with that lot of powder than n140 in general. that said, in my experience VV powder is generally very consistent lot to lot and it seems that there is a 3-4 year gap between the falfiles poster loadings and yours opsoff so the chances of this are likely very low.
it would be interesting to find out whether the n140 you had issues with is the same lot# as the person at falfiles, perhaps it was more something to do with that lot of powder than n140 in general. that said, in my experience VV powder is generally very consistent lot to lot and it seems that there is a 3-4 year gap between the falfiles poster loadings and yours opsoff so the chances of this are likely very low.
I am curious too - I joined Falfiles so I could contact him - definitely wanted to compare lot #'s. I have always had pretty good luck with VV powders, until they got so expensive. Luckily I'm sitting on a lot (other than the N140)
Finding really good results with 73 Bergers and N540 right now.
Also - N140 is a single base powder - the 5 series are double base. I know that single base powders are hygroscopic - so maybe on some weird outside chance, there was some moisture in that powder. If not - it has to be some type of chemical reaction.
I am finding it hard to believe that it was moisture though - I have probably 20+ different powders on hand, some of which are 15 - 20 yrs old - still use them occasionally - never an issue with any of the others new or old and they are all stored in the same place right next to each other.
agree with the thoughts on it likely not being moisture, i too have some powder that has been around for a long time (I have about two pounds of the original Thunderbird, no it is not for sale ;) ) and it is all fine/useable, in fact I am still using varget from the same 8 lb keg my grandfather gave me when he started teaching me to handload (14 years ago). hopefully you are able to find a cause for the degredation of the ammo using n140.
Did you tumble the brass before loading it? Is it possible that lubricant used during the brass forming process interacted chemically with the N140? Do you think the chemicals used to effect the hygroscopic properties of the powder interacted with the brass?
One manufacturing process uses organic solvents and another process uses water. The water or solvents must be dried before packaging the powder. Could it be that the batch of N140 powder you used was not dried enough after the manufacture process and prior to packaging at the factory?
Getting a manufacturer to reveal the chemicals used in their powder making process may be an exercise in futility.
rcoodyar15
09-01-14, 04:08
Well I have 8# of n140
It shoots good
guess I will have to use it up quick before it goes bad
Lets see you get about 250 rounds of 223 out of a lb
and about half of that out of a .308
won't take long
none go in the storage bin. Load them and use them
opsoff1,
Let us know what you determine is the problem. You have my attention and I would really like to know the answer to this mystery.
I have pulled bullets from 1971 vintage Korean surplus 30-06 that was starting to deteriorate and the brass did not look that bad.
Did you tumble the brass before loading it? Is it possible that lubricant used during the brass forming process interacted chemically with the N140? Do you think the chemicals used to effect the hygroscopic properties of the powder interacted with the brass?
One manufacturing process uses organic solvents and another process uses water. The water or solvents must be dried before packaging the powder. Could it be that the batch of N140 powder you used was not dried enough after the manufacture process and prior to packaging at the factory?
Getting a manufacturer to reveal the chemicals used in their powder making process may be an exercise in futility.
T2C,
Good questions - the brass was new Federal Gold Medal - factory primed w/ 205M's - right out of the carton. The only things that were done: neck size with a TiN bushing, so no lube involved or tumbling or really any other operation. The interesting or perplexing point is all the brass came out of the same box, was processed at the same time, loaded with bullets out of the same box. The only variable was half the brass got N140 and half got N540. I also have some ammo development / tests using the same components (loaded at a different session) using N135 - no issues with that either. Appears to be specific to N140.
I'll definitely keep on this as I want to find out the root cause. The big question is this a byproduct of too long in storage - so if I load and shoot N140 now it'll be ok or is it an issue where the powder has gone bad?
opsoff1,
Let us know what you determine is the problem. You have my attention and I would really like to know the answer to this mystery.
I have pulled bullets from 1971 vintage Korean surplus 30-06 that was starting to deteriorate and the brass did not look that bad.
This is an extract from the FBI (Forensic Science Communications, April 2002 - Volume 4 - Number 2, Research and Technology)
The Manufacture of Smokeless Powders and their Forensic Analysis: A Brief Review
Robert M. Heramb
Graduate Student
Bruce R. McCord
Associate Professor of Analytical and Forensic Chemistry
Department of Chemistry
Ohio University
Athens, Ohio
Composition and Manufacturing
The major classes of compounds in smokeless propellants include energetics, stabilizers, plasticizers, flash suppressants, deterrents, opacifiers, and dyes (Bender 1998; Radford Army Ammunition Plant 1987).
Energetics facilitate the explosion. The base charge is nitrocellulose, a polymer that gives body to the powder and allows extrudability. The addition of nitroglycerine softens the propellant, raises the energy content, and reduces hygroscopicity. Adding nitroguanidine reduces flame temperature, embrittles the mixture at high concentration, and improves energy-flame temperature relationship.
Stabilizers prevent the nitrocellulose and nitroglycerine from decomposing by neutralizing nitric and nitrous acids that are produced during decomposition. If the acids are not neutralized, they can catalyze further decomposition. Some of the more common stabilizers used to extend the safe life of the energetics are diphenylamine, methyl centralite, and ethyl centralite.
It sounds like this particular lot of N140 might not have been properly manufactured.
I'll definitely keep on this as I want to find out the root cause. The big question is this a byproduct of too long in storage - so if I load and shoot N140 now it'll be ok or is it an issue where the powder has gone bad?
I have powder from 1998 that is still usable. I am perplexed why your powder went bad so soon.
This is an extract from the FBI (Forensic Science Communications, April 2002 - Volume 4 - Number 2, Research and Technology)
It sounds like this particular lot of N140 might not have been properly manufactured.
Sinister,
Good stuff - I looked on the containers of the powder before I saw your post - interestingly enough, Vihtavouri lists all the ingredients in the powder. I want to look again and compare it to what you found in the article.
Looking at putting together a letter with pictures to send off to Vihtavouri Oy. Best case scenario is they replace the powder / worst case they tell me to pound sand. The lot(s) that I have are actually from 1995....
Didn't realize it was that old.
I'm interested to see what you find out and what they say.
Hmmm. 20 years really isn't that old, considering you had the ammo in sealed cans and I'm assuming indoor storage?
Nitrocellulose single-based powder is manufactured with lots of water to rinse out excessive acid content, then the powder is dried by running across heated rollers. If the acid isn't rinsed out it works as a catalyst and would explain the corrosion inside the case, the bottom of the bullets, and killing your primers.
When Olin moved their powder manufacturing facilities from Illinois to Florida they got away from freezing with the large quantities of water needed to make smokeless. What they hadn't completely thought out was the threat of lightning and static electricity on the gulf coast.
I'm not sure your powder is still usable. Can you tell by a sour-acidic smell? It might be best used for fertilizer now.
Curious to hear what VihtaVuori says. I believe their US headquarters are now co-located with Lapua in Sedalia, Missouri.
Hmmm. 20 years really isn't that old, considering you had the ammo in sealed cans and I'm assuming indoor storage?
Nitrocellulose single-based powder is manufactured with lots of water to rinse out excessive acid content, then the powder is dried by running across heated rollers. If the acid isn't rinsed out it works as a catalyst and would explain the corrosion inside the case, the bottom of the bullets, and killing your primers.
When Olin moved their powder manufacturing facilities from Illinois to Florida they got away from freezing with the large quantities of water needed to make smokeless. What they hadn't completely thought out was the threat of lightning and static electricity on the gulf coast.
I'm not sure your powder is still usable. Can you tell by a sour-acidic smell? It might be best used for fertilizer now.
Curious to hear what VihtaVuori says. I believe their US headquarters are now co-located with Lapua in Sedalia, Missouri.
Sinister,
It shouldn't be an issue (20 yrs) I have a lot of other powder that is of the same age and it shoots fine. The N540 was sitting right next to the N140 and was fine.
I'm tying to dig up a POC for an inquiry / letter - I'd prefer to deal with someone in the US vs Finland.
I did the Mk-I nose smell test - seems ok.
In the mean time - I may run a test with some of it to see how it shoots in a few test rounds. Probably burn some first though.
Yeesh, I'd hate to trash 24 lbs of the stuff...
rcoodyar15
09-02-14, 12:02
N140 works so much better than varget for me with the 77 MK
guess I will not put in a stock of them though.
This is an extract from the FBI (Forensic Science Communications, April 2002 - Volume 4 - Number 2, Research and Technology)
It sounds like this particular lot of N140 might not have been properly manufactured.
Composition and Manufacturing
The major classes of compounds in smokeless propellants include energetics, stabilizers, plasticizers, flash suppressants, deterrents, opacifiers, and dyes (Bender 1998; Radford Army Ammunition Plant 1987).
Energetics facilitate the explosion. The base charge is nitrocellulose, a polymer that gives body to the powder and allows extrudability. The addition of nitroglycerine softens the propellant, raises the energy content, and reduces hygroscopicity. Adding nitroguanidine reduces flame temperature, embrittles the mixture at high concentration, and improves energy-flame temperature relationship.
Stabilizers prevent the nitrocellulose and nitroglycerine from decomposing by neutralizing nitric and nitrous acids that are produced during decomposition. If the acids are not neutralized, they can catalyze further decomposition. Some of the more common stabilizers used to extend the safe life of the energetics are diphenylamine, methyl centralite, and ethyl centralite.
So...
I looked at the ingredients in N140 & N540
N140
Nitrocellulose
Diphenylamine
Diethyldiphenyurea
N540 (actually gave max percentages)
Nitrocellulose 90%
Nitroglycerin 20%
2-nitrodiphenylamine
Ethyldiphenylurea
Potassium Sulphate
Graphite
Did the Mk-1 Nose Smell Test again - sniffing 8lb jugs of N135, N140, N165, N540 and N550 - they all smelled the same - I know the 540 & 550 are good as well as the 135. So ???
ETA: Did a rudimentary burn test - 25grs of N140 vs 25grs of N540 - 140 lit right up, burned bright and fast. 540 burned a little softer and longer - interesting - not sure what it proves other than it'll probably still go bang.
Bizarre
Sending a letter with pics to VihtaVouri Oy tomorrow.
Single base powders have a shorter shelf life than double base. Even when under good storage conditions, single base is expected to last only ~15 years from my recollection.
Of course, it could also be an error in mfg. but I'd hazard a guess to say you've exceeded this powder's lifespan.
Arrrghhh.... no offense intended at all... but this thread sucks. ;)
I truly held Viht. powder as VERY well made powder. Not susceptible to the same somewhat common US manufacturers problems... I guess every company can mess up. Dang.
I also am very interested in there response. Thanks for taking the time to share with us.
I hear ya...
I wrote to Nammo a week ago and provided a very detailed description, with lot #'s, temp / humidity readings, photos etc.
Haven't heard anything back. (yet)
I'm tying to dig up a POC for an inquiry / letter - I'd prefer to deal with someone in the US vs Finland.
If you are over on Snipers Hide there is a Lapua/VV rep over there that has been helpful to me in the past. He might know who to send you to if you cant find anything.
If you are over on Snipers Hide there is a Lapua/VV rep over there that has been helpful to me in the past. He might know who to send you to if you cant find anything.
Any idea of who it is over there?
Any idea of who it is over there?
pm incoming
Given this is a single base powder, I could see this happening. I had some late 80's/early 90's IMR powder that some gave to me go bad. It smelled odd and gave off a red rust powder. As a science experiment I still shot some of it and it all went bang and still provided OK accuracy.
Interestingly though the same lot of powder, when I harvested it from some old loaded rounds, was still fresh and looked like new. When I fired it, it was indistinguishable from the new IMR I also had.
I personally believe that storage and humidity exposure plays a big part in powder longevity, I think the caps on the powder container must have allowed moisture/humidity/oxygen intrusion.
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