Alliant Unique powder issue, can you help

[KeithK]

I prepped a bunch of 9mm for loading and planned on Unique because I had 5lb's left of the 8 lb container. But when the first load came out of the Chargemaster I noticed a color difference in maybe 10-15 percent of the pan.

I kept loading the pan hoping to see a normal pan full of powder (or maybe this color has always been there but I hadn't' noticed, i'm not sure)

There is no smell like you get when powder is going bad, no other indications that I can notice. The powder is from a 2008 lot and has been kept inside my office/house at temps between 65-74 and sealed in original container in dark powder enclosure.

To be honest this powder could have always had this color difference but I didn't notice, but it seems like one half of a flake of powder has a different color on one side than the other, pretty hard manipulating one piece of powder.

I am going to try and upload the picture of the powder, not sure if it will be good enough to see but will try. I am hoping by posting this someone who has and uses Unique can tell me if there is a slight color difference or not.

I was going to order or pickup a new container of Unique but seems like no one as any, I wanted to see if there is a difference or I just have a bad container. Sorry for the long post, if you got this far and can comment it will be appreciated. I was going to call Alliant tomorrow but will have to see if they can help via phone or net, but we shall see.

Thanks again, Keith

 

[ericuda]

Color always been there you are gtg. Mine has mix of duller flakes to too.

 

[.45Coltguy]

I just looked at my opened bottle of Unique and it looks the same from what I can tell. A call to Alliant may help. I'm thinking your powder is good.

 

[GeoDudeFlorida]

I prepped a bunch of 9mm for loading and planned on Unique because I had 5lb's left of the 8 lb container. But when the first load came out of the Chargemaster I noticed a color difference in maybe 10-15 percent of the pan.

I kept loading the pan hoping to see a normal pan full of powder (or maybe this color has always been there but I hadn't' noticed, i'm not sure)

There is no smell like you get when powder is going bad, no other indications that I can notice. The powder is from a 2008 lot and has been kept inside my office/house at temps between 65-74 and sealed in original container in dark powder enclosure.

To be honest this powder could have always had this color difference but I didn't notice, but it seems like one half of a flake of powder has a different color on one side than the other, pretty hard manipulating one piece of powder.

I am going to try and upload the picture of the powder, not sure if it will be good enough to see but will try. I am hoping by posting this someone who has and uses Unique can tell me if there is a slight color difference or not.View attachment 1146385

I was going to order or pickup a new container of Unique but seems like no one as any, I wanted to see if there is a difference or I just have a bad container. Sorry for the long post, if you got this far and can comment it will be appreciated. I was going to call Alliant tomorrow but will have to see if they can help via phone or net, but we shall see.

Thanks again, Keith

Looks pretty normal to me. I think you’re good.

 

[KeithK]

Thanks so very much, I feel a lot better, you guys are the best, I will update after my call to Alliant.

Keith

 

[Soonerpesek]

I am going to try and upload the picture of the powder, not sure if it will be good enough to see but will try. I am hoping by posting this someone who has and uses Unique can tell me if there is a slight color difference or not

Here is a pic of Unique from a 1lber from 2016 ish..............
Looks the same as yours to my eyes............

 

[ms6852]

Choooot it.

 

[RikSors]

Looks normal from the picture.

Form a thin line and burn one end. Powder still burns if it finishes the line with consistency.

Next step would be to load a couple of test rounds and compare with your old reloaded rounds with the same powder. Good luck and be safe.

 

[ericuda]

I'm curious why are you going to call aliant. The powder is fine and just curious have you even shot any loads loaded with it.

 

[KeithK]

I'm curious why are you going to call aliant. The powder is fine and just curious have you even shot any loads loaded with it.

You're right, my thinking was did I miss a normal color change after opening or with normal aging or was it always like that and I just missed it. Yes I have shot it a lot but not lately, I was in the process of making rounds for my sons and grandkids for use when i'm gone. I have an awful lot of components and I have the time now but just a different purpose than my old one of shooting every week.

 

[ericuda]

Gotcha if I was even worried a bit I'd shoot some standby loads over chroni.

 

[AJC1]

You're right, my thinking was did I miss a normal color change after opening or with normal aging or was it always like that and I just missed it. Yes I have shot it a lot but not lately, I was in the process of making rounds for my sons and grandkids for use when i'm gone. I have an awful lot of components and I have the time now but just a different purpose than my old one of shooting every week.

How well you label everything matters a lot after your gone... put as much information as possible! I say this as a second generation bullet squisher teaching a third generation shooting his grandpa's loads.

 

[mdi]

If you're really concerned. load a half dozen and shoot them over a chrony, if you have one. Wide swings in velocity may indicate powder going bad. BTDT...

But IMO, it's still good...

 

[Ironicaintit]

Not much wrong with an abundance of caution when we're discussing controlled explosions near our face. My old Hercules Unique, as well as my new Alliant stuff all had slight color variations like yours shows. I say load em up!
-some guy on the internet

 

[KeithK]

How well you label everything matters a lot after your gone... put as much information as possible! I say this as a second generation bullet squisher teaching a third generation shooting his grandpa's loads.

AJC1

You are very good, I am labeling all my reloads with more than the usual so the kids know the date and all the specs for the reloads, Thank You. I have always believed like you to document every container and these past few months I have included more.

 

[KeithK]

Well I finished up early my reloading and said heck i'll call Alliant. Got a really nice fellow right away no numbers to push, no secretary's to get through. He said just do the 3 test thing and if it passes all three then you're good to go. If it fails any one then it doesn't pass. Now he had a better name for it but of course I didn't t write it down or remember exactly.

1. Smell test- If acidic or any odor not likely to pass the wife's nose is bad.
2. Color test- Put about a teaspoon on a white sheet of paper and roll it up and shake and roll it back and forth then look at the paper, you don't squeeze or smash the paper, just roll it around. charcoal, black or no color is good. Yellow, rust, red colors its bad.
3. Burn test- put a 1 inch square pile of powder followed by a line of powder a safe distance away and light the line, it should burn completely to your square of powder and all burn up. If it sputters, goes out and back on, or sparkles then it's bad.

So of course I went and did the 3 tests as he said and my powder passed all three as most of you probably already know, I was sure it was going to pass after all the replies I have received but figured why not, and I thought I can post the test procedures and maybe it might help someone in the future.

I really appreciate all the help and advice, this forum and it's members are truly the best, Thanks

Keith

 

[BushMaster-15]

Well I finished up early my reloading and said heck i'll call Alliant. Got a really nice fellow right away no numbers to push, no secretary's to get through. He said just do the 3 test thing and if it passes all three then you're good to go. If it fails any one then it doesn't pass. Now he had a better name for it but of course I didn't t write it down or remember exactly.

1. Smell test- If acidic or any odor not likely to pass the wife's nose is bad.
2. Color test- Put about a teaspoon on a white sheet of paper and roll it up and shake and roll it back and forth then look at the paper, you don't squeeze or smash the paper, just roll it around. charcoal, black or no color is good. Yellow, rust, red colors its bad.
3. Burn test- put a 1 inch square pile of powder followed by a line of powder a safe distance away and light the line, it should burn completely to your square of powder and all burn up. If it sputters, goes out and back on, or sparkles then it's bad.

So of course I went and did the 3 tests as he said and my powder passed all three as most of you probably already know, I was sure it was going to pass after all the replies I have received but figured why not, and I thought I can post the test procedures and maybe it might help someone in the future.

I really appreciate all the help and advice, this forum and it's members are truly the best, Thanks

Keith

For future general powder quality assurance ; Have a strong light behind you ,so You can open the can of powder while looking at the open portion of the canister with light behind . IF You see any Red or fume ,the powder has lost it's stabilizer and when You smell it it will have an acrid acid smell .
IF it smells like solvent ,either or alcohol ,IT'S OK . Red color or acid smell is immediate RED FLAG ,as Nitro aka Nitric acid is and has been separated from base . That powder should go in the garden or lawn or strung out and burned .

IF You are making long term rounds ,proper storage of those is somewhat important , depending on term Long ?

 

[lightman]

I'm another that thinks it looks normal. Load it and shoot it! I'm also another that realized that I won't be around forever and have gotten better about labeling my ammo. I also write the purchase dates on powder and primers.

 

[Slamfire]

Red color or acid smell is immediate RED FLAG ,as Nitro aka Nitric acid is and has been separated from base . That powder should go in the garden or lawn or strung out and burned .

One of these days I will have find my picture of Krag 30-40 powder that came out of a 1898 cartridge. The grains are red. I pulled the picture as I became tired of deniers claiming that was the original color of issue Krag powder, as I could not find a period source stating color.

I will mention something that is still absolutely unbelievable to me. I was given about 100 30-40 cartridges, all 1898 head stamp, and all had cracked case necks. I could pull bullets with my fingers, and some I did. I poured out the powder in a metal tablespoon and returned it to the case. But one, what I saw in that tablespoon were beautiful ruby red pin points distributed among the powder. The powder grains were all small, not the tubes of the other cartridges, and these ruby red pin points were clearly visible in the dark. I found a magnifying glass and looked at them. They were wavy in appearance, like charcoal briquet wavy. I had no idea what I was looking at. But now, I believe the things were on fire! I do not know how the powder could have deteriorated to the point that some grains exhibited flames, tiny as they were, without the whole pile going poof!.

Wish I had taken a picture, and I gave most of those rounds to a collector. But I saw it. Never seen it again.

 

[BushMaster-15]

One of these days I will have find my picture of Krag 30-40 powder that came out of a 1898 cartridge. The grains are red. I pulled the picture as I became tired of deniers claiming that was the original color of issue Krag powder, as I could not find a period source stating color.

I will mention something that is still absolutely unbelievable to me. I was given about 100 30-40 cartridges, all 1898 head stamp, and all had cracked case necks. I could pull bullets with my fingers, and some I did. I poured out the powder in a metal tablespoon and returned it to the case. But one, what I saw in that tablespoon were beautiful ruby red pin points distributed among the powder. The powder grains were all small, not the tubes of the other cartridges, and these ruby red pin points were clearly visible in the dark. I found a magnifying glass and looked at them. They were wavy in appearance, like charcoal briquet wavy. I had no idea what I was looking at. But now, I believe the things were on fire! I do not know how the powder could have deteriorated to the point that some grains exhibited flames, tiny as they were, without the whole pile going poof!.

Wish I had taken a picture, and I gave most of those rounds to a collector. But I saw it. Never seen it again.

Remember before turn of the century ,NO explosive powder included had stabilizers at least to MY knowledge . IF people only knew what commercial dynamite was really made of ,they'd freak out . Notice you DON'T see people with Blackpowder ( Real Blackpowder ) showing tins of it ; There's a reason

The ONLY ammunition I've ever personally seen IGNITE were Phosphorous rounds . There's a few different types and not simply tracer either .

 

[peeplwtchr]

Well I finished up early my reloading and said heck i'll call Alliant. Got a really nice fellow right away no numbers to push, no secretary's to get through. He said just do the 3 test thing and if it passes all three then you're good to go. If it fails any one then it doesn't pass. Now he had a better name for it but of course I didn't t write it down or remember exactly.

1. Smell test- If acidic or any odor not likely to pass the wife's nose is bad.
2. Color test- Put about a teaspoon on a white sheet of paper and roll it up and shake and roll it back and forth then look at the paper, you don't squeeze or smash the paper, just roll it around. charcoal, black or no color is good. Yellow, rust, red colors its bad.
3. Burn test- put a 1 inch square pile of powder followed by a line of powder a safe distance away and light the line, it should burn completely to your square of powder and all burn up. If it sputters, goes out and back on, or sparkles then it's bad.

So of course I went and did the 3 tests as he said and my powder passed all three as most of you probably already know, I was sure it was going to pass after all the replies I have received but figured why not, and I thought I can post the test procedures and maybe it might help someone in the future.

I really appreciate all the help and advice, this forum and it's members are truly the best, Thanks

Keith

Thanks for posting these tests, I have some new IMR 8208 that has a strong odor. This test process is going into my loading note book.

 

[Slamfire]

Remember before turn of the century ,NO explosive powder included had stabilizers at least to MY knowledge ..

I don't know when the first stabilizers were used for nitrocellulose, but I do recall reading that it was very early. Nitrocellulose was too unstable. I recall reading that European cities banned gunpowder mills after too many went kaboom! This reference provides an idea of the history of one stabilizer. They had to have been using earlier compositions as stabilizers that where not as satisfactory as later formulations.

Stabilizers for nitrate ester-based energetic materials and their mechanism of action: a state-of-the-art review

https://link.springer.com/article/10.1007/s10853-017-1474-y

J Mater Sci (2018) 53:100–123

The continuous decomposition of nitrate esters is mainly due to the low bonding energy of nitrate ester functional group, CH2–O–NO2 [15]. Consequently, gaseous products, especially nitrogen oxides, are released and nitrous and nitric acids are produced under severe environments (high temperature or acid chemical environment) [27–29]. Without the incorporation of any stabilizer, these generated products play a catalytic effect on the decomposition processes [30]. The additives, however, cannot prevent the nitrate ester decomposition, but are able to inhibit it and avoid the catalytic effect caused by the decomposition products such as NO, NO2, HNO2 and HNO3 [21]. The stabilizers react more and more with the gases released by the energetic composition until they depleted completely [31, 32]. The decrease in these primary stabilizers is accompanied by the formation of different derivatives considered as secondary stabilizers, since they also play a stabilizing action [33]. The conventional stabilizers employed for nitrate ester-based energetic materials belong to (a) aromatic amines such as diphenylamine (DPA), 2-nitrodiphenylamine (2-NDPA) and p-nitro-N-ethy[1]laniline and (b) urea compounds such as N,N0 -di[1]ethyl-N,N0 -diphenylurea (C1), N,N0 -dimethyl-N,N0 - diphenylurea (C2) and N-methyl N0 ,N0 -diphenylurea (AK-II) [34–36]. The Swedish Alfred Nobel was the first to introduce DPA as stabilizer of energetic composition as reported in a German patent in 1889 [32, 37–39]. By reacting with nitrogen oxides, the conventional stabilizers are converted to a range of nitrosamines and nitroamines. The reactions of these stabilizing agents are complex, and different successive prod[1]ucts of the primary stabilizer, named also daughter products, are generated. These latter components may themselves act as stabilizers. Nevertheless, the generated nitroso derivatives are considered toxic and carcinogenic [36, 40]. Therefore, these stabilizers need to be replaced as soon as possible

The shooting society is more familiar with the history of paper clips than stabilizers. Can't say I am all that interested in when stabilizers were discovered, or their evolution.

 

[AJC1]

I don't know when the first stabilizers were used for nitrocellulose, but I do recall reading that it was very early. Nitrocellulose was too unstable. I recall reading that European cities banned gunpowder mills after too many went kaboom! This reference provides an idea of the history of one stabilizer. They had to have been using earlier compositions as stabilizers that where not as satisfactory as later formulations.

Stabilizers for nitrate ester-based energetic materials and their mechanism of action: a state-of-the-art review

https://link.springer.com/article/10.1007/s10853-017-1474-y

J Mater Sci (2018) 53:100–123

The continuous decomposition of nitrate esters is mainly due to the low bonding energy of nitrate ester functional group, CH2–O–NO2 [15]. Consequently, gaseous products, especially nitrogen oxides, are released and nitrous and nitric acids are produced under severe environments (high temperature or acid chemical environment) [27–29]. Without the incorporation of any stabilizer, these generated products play a catalytic effect on the decomposition processes [30]. The additives, however, cannot prevent the nitrate ester decomposition, but are able to inhibit it and avoid the catalytic effect caused by the decomposition products such as NO, NO2, HNO2 and HNO3 [21]. The stabilizers react more and more with the gases released by the energetic composition until they depleted completely [31, 32]. The decrease in these primary stabilizers is accompanied by the formation of different derivatives considered as secondary stabilizers, since they also play a stabilizing action [33]. The conventional stabilizers employed for nitrate ester-based energetic materials belong to (a) aromatic amines such as diphenylamine (DPA), 2-nitrodiphenylamine (2-NDPA) and p-nitro-N-ethy[1]laniline and (b) urea compounds such as N,N0 -di[1]ethyl-N,N0 -diphenylurea (C1), N,N0 -dimethyl-N,N0 - diphenylurea (C2) and N-methyl N0 ,N0 -diphenylurea (AK-II) [34–36]. The Swedish Alfred Nobel was the first to introduce DPA as stabilizer of energetic composition as reported in a German patent in 1889 [32, 37–39]. By reacting with nitrogen oxides, the conventional stabilizers are converted to a range of nitrosamines and nitroamines. The reactions of these stabilizing agents are complex, and different successive prod[1]ucts of the primary stabilizer, named also daughter products, are generated. These latter components may themselves act as stabilizers. Nevertheless, the generated nitroso derivatives are considered toxic and carcinogenic [36, 40]. Therefore, these stabilizers need to be replaced as soon as possible

The shooting society is more familiar with the history of paper clips than stabilizers. Can't say I am all that interested in when stabilizers were discovered, or their evolution.

These stabilizers need to be replaced.... price going up!!!

 

[PapaG]

As Troy says, "choot it".

 

[Slamfire]

I have some new IMR 8208 that has a strong odor.

I can't tell what your odor smells like. New gunpowder does have a strong smell, and what is in the air, I don't know. But bad gunpowder is outgassing NOx which is a chemical spectrum. One of them is NO2, nitrogen dioxide. The same NO2 that gives a brown color to the air above Los Angeles. Fly to LAX and you go through this brown layer of air. Only goes away when it rains, and then you see things at distance you have not seen before. Within the week, the brown will be back. An additional bad thing about NO2 is that when it runs into a water molecule, called humidity, it converts into nitric acid gas. I think that is colorless. So while the description is technically correct, as the bottle is fuming nitric acid gas, what you see is nitrogen dioxide.



I had a 8lb jug of pulldown IMR 4895 and it fumed. I did not know what I was looking at as this knowledge had been driven from the shooting community. But I what I did figure out after sniffing, was that it was one of the worst sniffs I had ever taken. Hard to describe how horrible it was, but it was like my nostrils were being ripped out of my skull!

A sniff test is not a sophisticated test. I have WW2 era 4831 that is obviously going bad, but I can't smell anything. A more sensitive test is the Methly Violet test, or Talliani test in Mil Std 286. Methyl violet paper, is put into a test tube with gunpowder and if the paper changes color over time, the gunpowder is outgassing NOx. I don't know the time

I found this, but no criteria for color change time


Big Chemical Encyclopedia

https://chempedia.info/info/methyl_violet_tests/

Methyl violet test

Stability. Heat stabihty is determined by measuring the time required for a specific amount of CN, held at 134.5°C, to decompose and discolor methyl violet test paper (75). [Pg.268]

Note The Observation Test was intended to detect the initial decompn of propint, and was conducted at ail depots and posts where powder was stored. A 6oz sample of each lot of powder with a strip of methyl violet test paper was placed in a glass-stoppered bottle, with the paper not in contact with the powder. The test was conducted in the magazine in which the proplnt under test was stored. Bleaching of the test paper was taken as an indication that the powder had started to de-... [Pg.136]

Davis, Vol 2 (1943) Sensitivity of NG (p 209) Stability Tests for NC, which include Kl-Starch Test at 65.5°, Methyl Violet Test at 134.5°C, Bergmann-Junk and Vacuum Tests (267-69) Testing of Detonators by Nail Test and by US Bureau of Mines Sand Test (421-24)... [Pg.311]

Loss of Weight Test, Marqueyrol s Test, Meerscheidt-Hullessem Test, Mittasch s Test, Obermiiller s Test, Pavlik s Test, Methyl Violet Test, Silvered Vessel Test, Simon Thomas Test, Spica Test, Sy Test, Taliani Test, Taylor s Test, Tomanari s Test, Vacuum Stability Test, Vieille Test, Warmlagermethode 75° (German Storage Test), Will Test... [Pg.59]

It was adopted by the US Ordnance Dept (Ref 2), but the temperatures of the test were 120° for double-base propellants and 134.5° for single-base propellants for NC s (Ref 3). Litmus paper was originally used in this test (Refs 1 8c 2) but later this was changed id methyl violet paper and the test was called the Methyl Violet Test Apparatus ... [Pg.712]

Normal methyl violet test paper is prepd by soaking filter paper in a normal solution of rosaniline acetate-crystal violet and drying... [Pg.712]

The stability test for nitrocellulose powder at a temperature of 134.5°C the sample will not be considered serviceable unless the time necessary to produce the evolution of nitrogen oxides is at least 45 min and the powder withstands this temperature without exploding for 5 hr. The test can be combined with methyl violet test decoloration of the test paper should not occur before 30 min or longer according to particular specifications. [Pg.558]

The test for nitroglycerine powders at a temperature of 120°C (nitroglycerine powders cannot withstand higher temperatures) here the same conditions apply as in the test for nitrocellulose powders, viz. appearance of the nitrogen oxides after a lapse of at least 45 min and no explosion for 5 hr. The same test can be carried out in the presence of methyl violet test papers. Decoloration of the paper should not occur before 30 min. [Pg.558]

Tonegutti and Debenedetti [63] found that this test also agrees well with the methyl violet test at 120°C. [Pg.559]


Sample Date of manufacture NaN02 in mg % Decoloration of methyl violet test paper at 120°C after min... [Pg.559]

Test Papers. See under Methyl Violet Tests in Vol 8, M118-Lto M120-L, and Lead Acetate in Vol 1, A28-R... [Pg.563]

Methods in which the escaping nitrous gases can be recognized visually or by noting the color change of a strip of dyed filter paper. The former methods include the qualitative tests at 132, 100, 75, and 65.5 °C (270, 212, 167, and 150 °F). These tests include the U.S. supervision test, the methyl violet test, the Abel test, and the Vieille test. [Pg.235]


Methyl violet test for stability of explosives, 79 Mineral jelly, for use in explosives, examination of, 14 in nitroglycerine, 5a... [Pg.476]

Found a Vacuum Test with methyl violet paper, and the temps and times they used

Determination of Chemical Stability of Propellants Using the Vacuum Stability Test Method
file:///B:/Daily%20Dump/Determination_of_chemical_stability_of_propellants.pdf

Since no one I know is going to buy methyl violet paper and a special oven, nor a gas chromatography machine, all we cheap skates can do is look and sniff. I tossed this gunpowder because it was smelling vinegary bitter. Sort of a red pepper sauce smell, again, bitter. I am of the opinion that what we are sniffing for is bitter smells, that is traces of NO2 and nitric acid gas. Bitter is bad.