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Rust didn't change color when boiled?

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Hi All,
The 7th application of Mark Lee Slow Rust Blue rusted up fine. But when I boiled it the red rust didn't change to black. It did take on a brown tint but that was all. When I carded it the rust was hard and required "0" steel wool to remove it. The finish underneath returned to a smooth and satin metal grey.
I found several posts here and elsewhere mentioning this happening with no real explanation. Several posts mentioned further applications rusted and changed color as normal. Since my barrel hasn't changed color since the fifth application I suppose I'll leave it as it is. I was hoping for an nice blue but it's not going to happen on this barrel with the Mark Lee solution.

Any thoughts or comments, as always, would be most appreciated.

Thanks!
John
 
How long are you boiling it? A barrel will need 30 min-1 hour at least. You should not be carding so vigorously. The ideal is a soft stainless steel brush with bristles no thicker than 0.003". Put it in a drill press, lathe, or drill and spin at a slow speed. Grobet makes one version and they are sold by Brownell and Jantz Supply. Do not let the barrel rust for too long between applications. Let the first 2 sit for perhaps 4-6 hours and then the rest for no more than 2 hours before carding. Time depends on humidity and temp but the longer it rusts the bigger the pitting and the coarser the blue. The barrel below was blued using LMF browning solution.

dave
os4iFVv.jpg
 
Hi All,
The 7th application of Mark Lee Slow Rust Blue rusted up fine. But when I boiled it the red rust didn't change to black. It did take on a brown tint but that was all. When I carded it the rust was hard and required "0" steel wool to remove it. The finish underneath returned to a smooth and satin metal grey.
I found several posts here and elsewhere mentioning this happening with no real explanation. Several posts mentioned further applications rusted and changed color as normal. Since my barrel hasn't changed color since the fifth application I suppose I'll leave it as it is. I was hoping for an nice blue but it's not going to happen on this barrel with the Mark Lee solution.

Any thoughts or comments, as always, would be most appreciated.

Thanks!
John
First let me say that there are other ways to accomplish this task and get fine results but I find this works for me with what I have available to me. The items below are the materials that I use for rust bluing a barrel.

Mark Lee #1 Express Blue, small glass container, tap water (I have a water softening system in the house), Coarse cloth such as heavy denim, Terry cloth towel, or maybe burlap which I have not tried, rubber gloves or the like, heat source to heat up gutter + water to boiling or a little less, something to plug the openings in the barrel so no water can enter, a degreaser. DHC Silky Cotton Pads (or any soft cotton type applicator pads)

I use a length of steel gutter from Home Depot that I solder on end caps to contain water. I suggest to make the gutter length 2 to 4 inches longer than your barrel plus tang and muzzle plug.

Bend up some stiff wire (qty-2) to support the barrel at each ends in the gutter so that it does not contact the bottom. NOTE: if rust bluing a lock or small parts I use a small disposable aluminum “loaf pan” and just put the parts into the water without trying to support the parts off the bottom – the bluing comes out fine - might also work for a barrel but I have not tried it.

OK – now for the barrel preps. What I will be discussing here is what I did for this barrel and for the finish results I was looking for which was a dark blue/black non-polished look which is what I do the most of.

This is what the barrel looked like before and after the rust bluing process described here. These two barrels are the same, made by Ed Rayl as received from Dixon’s Muzzle Loading Shop.

I did not draw file the barrel. I did block sand with both 220 & 320 grit wet/dry paper quickly. I did not try to remove all surface marks just to “knock down” heavy machine marks. I then used a medium wire wheel to even the surface out as best as I could – the corners of the flats did get “eased” some – don’t go hard with the wire wheel unless you want a “distressed” look. At this point you want to degrease the barrel good - I used acetone. I made up a barrel holder from scrap wood so that I could apply the Mark Lee #1 Express Blue

I plugged the touch hole, my breach plug was already installed. I slipped the barrel into the barrel support and put on my “rubber”([PWB1] ) gloves. I degreased the barrel again. I poured a small amount of the bluing into a small glass container and dipped my cotton pad into it – squeezed out most of the excess and starting from one of the barrel made a continuous pass towards the other end of the barrel. I did the same with the other 7 flats. NOTE: reapply the bluing solution to the pad to keep it wet but not “dripping” wet. When completed set aside for 4 hours. NOTE: I did not have a “sweat box” I just left it as you see it in the picture above – temp in CA was 104 degrees outside at the time. After 4 hours I reapplied the bluing solution as above and set it aside for another 4 hours. I did this process two more times and left it overnight (13 hours).

I placed the gutter over the two gas burners of MY kitchen stove and filled it with MY tap water to 1” – 1-1/2” above the top of the barrel (try to keep this water level throughout the process). I placed the stiff wire supports for the barrel that I previously bent to shape into both ends of the gutter. Turn on the gas to high. While the water is heating up put on your “rubber” (Nitrile) gloves and plug the muzzle of the barrel. Reapplied the bluing solution but this time I wetted the pad with more of [PWB2] bluing solution then above and set it aside until the water was as hot as I could get it (just about to bubble). I then placed the barrel into the water and leave it there for 10 to 15 minutes. Removed the barrel (be sure you have your “rubber” gloves on – also the barrel WILL be HOT), dry it quickly and reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to 15 minutes. Remove the barrel after the allotted time and take your course cloth and buff the heck out of the barrel (1 or 2 minutes). Reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to 15 minutes. Remove the barrel after the allotted time and take your course cloth and buff the heck out of the barrel (1 or 2 minutes). Reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to15 minutes. Remove the barrel after the allotted time and buff the heck out of it for 1 to 2 minutes then check if it is the color you are happy with - if not repeat the above process. If the barrel IS the color you are happy with you can now do two things to the warm barrel; First – remove all plugs then either apply oil or a wax LIBERALY – TWICE – let stand for ½ hour then wipe off excess oil or buff the wax. Set aside for at least 12 hours keeping an eye on it for signs of rust – if so buff out with cloth and reapply oil or wax. NOTE: I use a half & half wax mixture consisting of melted carnauba flakes and a high quality paste wax. That’s it – hope it works out like you want – does for me.
qa2djcZ.jpg

MPxgHTw.jpg
 
How long are you boiling it? A barrel will need 30 min-1 hour at least. You should not be carding so vigorously. The ideal is a soft stainless steel brush with bristles no thicker than 0.003". Put it in a drill press, lathe, or drill and spin at a slow speed. Grobet makes one version and they are sold by Brownell and Jantz Supply. Do not let the barrel rust for too long between applications. Let the first 2 sit for perhaps 4-6 hours and then the rest for no more than 2 hours before carding. Time depends on humidity and temp but the longer it rusts the bigger the pitting and the coarser the blue. The barrel below was blued using LMF browning solution.

dave

Hi Dave,
Thanks for the reply. I'm trying to figure out what you are telling me in comparison to my results. I've been placing the barrel in a length of PVC pipe and adding boiling distilled water. Every time the rust has changed color, from red to blue/black within a couple of minutes, no more than five. Actually I've treated the barrel each time to a second bath immediately after the first just to make sure. This matches up exactly with the Mark Lee instructions. I used the "0" steel wool because the "0000" steel wool bounced off the rust and didn't touch it. . I used LMF browning solution on my last barrel; had no issues and the color is quite similar to yours. I'll have to check your wire wheel suggestion.

Are you suggesting if I had actually boiled the barrel longer the rust would have changed color?
Any thoughts on why the rust didn't change color?
 
First let me say that there are other ways to accomplish this task and get fine results but I find this works for me with what I have available to me. The items below are the materials that I use for rust bluing a barrel.

Mark Lee #1 Express Blue, small glass container, tap water (I have a water softening system in the house), Coarse cloth such as heavy denim, Terry cloth towel, or maybe burlap which I have not tried, rubber gloves or the like, heat source to heat up gutter + water to boiling or a little less, something to plug the openings in the barrel so no water can enter, a degreaser. DHC Silky Cotton Pads (or any soft cotton type applicator pads)

I use a length of steel gutter from Home Depot that I solder on end caps to contain water. I suggest to make the gutter length 2 to 4 inches longer than your barrel plus tang and muzzle plug.

Bend up some stiff wire (qty-2) to support the barrel at each ends in the gutter so that it does not contact the bottom. NOTE: if rust bluing a lock or small parts I use a small disposable aluminum “loaf pan” and just put the parts into the water without trying to support the parts off the bottom – the bluing comes out fine - might also work for a barrel but I have not tried it.

OK – now for the barrel preps. What I will be discussing here is what I did for this barrel and for the finish results I was looking for which was a dark blue/black non-polished look which is what I do the most of.

This is what the barrel looked like before and after the rust bluing process described here. These two barrels are the same, made by Ed Rayl as received from Dixon’s Muzzle Loading Shop.

I did not draw file the barrel. I did block sand with both 220 & 320 grit wet/dry paper quickly. I did not try to remove all surface marks just to “knock down” heavy machine marks. I then used a medium wire wheel to even the surface out as best as I could – the corners of the flats did get “eased” some – don’t go hard with the wire wheel unless you want a “distressed” look. At this point you want to degrease the barrel good - I used acetone. I made up a barrel holder from scrap wood so that I could apply the Mark Lee #1 Express Blue

I plugged the touch hole, my breach plug was already installed. I slipped the barrel into the barrel support and put on my “rubber”([PWB1] ) gloves. I degreased the barrel again. I poured a small amount of the bluing into a small glass container and dipped my cotton pad into it – squeezed out most of the excess and starting from one of the barrel made a continuous pass towards the other end of the barrel. I did the same with the other 7 flats. NOTE: reapply the bluing solution to the pad to keep it wet but not “dripping” wet. When completed set aside for 4 hours. NOTE: I did not have a “sweat box” I just left it as you see it in the picture above – temp in CA was 104 degrees outside at the time. After 4 hours I reapplied the bluing solution as above and set it aside for another 4 hours. I did this process two more times and left it overnight (13 hours).

I placed the gutter over the two gas burners of MY kitchen stove and filled it with MY tap water to 1” – 1-1/2” above the top of the barrel (try to keep this water level throughout the process). I placed the stiff wire supports for the barrel that I previously bent to shape into both ends of the gutter. Turn on the gas to high. While the water is heating up put on your “rubber” (Nitrile) gloves and plug the muzzle of the barrel. Reapplied the bluing solution but this time I wetted the pad with more of [PWB2] bluing solution then above and set it aside until the water was as hot as I could get it (just about to bubble). I then placed the barrel into the water and leave it there for 10 to 15 minutes. Removed the barrel (be sure you have your “rubber” gloves on – also the barrel WILL be HOT), dry it quickly and reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to 15 minutes. Remove the barrel after the allotted time and take your course cloth and buff the heck out of the barrel (1 or 2 minutes). Reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to 15 minutes. Remove the barrel after the allotted time and take your course cloth and buff the heck out of the barrel (1 or 2 minutes). Reapplied the bluing solution with a new pad. NOTE: keep the pad very wet with the bluing solution but do not “puddle” the solution on the barrel. Replace the barrel into the hot water for another 10 to15 minutes. Remove the barrel after the allotted time and buff the heck out of it for 1 to 2 minutes then check if it is the color you are happy with - if not repeat the above process. If the barrel IS the color you are happy with you can now do two things to the warm barrel; First – remove all plugs then either apply oil or a wax LIBERALY – TWICE – let stand for ½ hour then wipe off excess oil or buff the wax. Set aside for at least 12 hours keeping an eye on it for signs of rust – if so buff out with cloth and reapply oil or wax. NOTE: I use a half & half wax mixture consisting of melted carnauba flakes and a high quality paste wax. That’s it – hope it works out like you want – does for me.

Thanks for the reply. I'll have to look into your gutter boiling container. I've been using a length of PVC pipe. My wife is fairly tolerant and should allow me to use the stove as you have.

Any thoughts on why the rust didn't change color?

Thanks!
John
 
Hi John,
I have to admit that I never used Mike Lee's but with other rust bluing solutions my barrels needed at least 30 minutes in boiling water to fully and evenly turn color. I usually give them about an hour to be sure. You really should not need coarse steel wool to card. That suggests to me that you may be letting the barrel rust to long before carding. Moreover, steel wool can contain oil and needs to be degreased before use. The passage below was copied from a thread of mine on another forum. It was written by John Cholin who is a fire chemist and knows his stuff. It describes what happens to turn a brown rust to blue-black rust:

" The red/orange brown is ferric oxide, Fe2O3. When ferric oxide is allowed to accumulate an additional oxygen it converts to ferrosoferric oxide, Fe3O4 which usually exists as a nonahydrate, -9(H2O), The brown color of a browned barrel is due to a mixture of ferric oxide and ferrosferric oxide - red and black make brown. That's why boiling a browned barrel turns it black - the red ferric oxide is being converted to ferrosoferric oxide nonahydrate due to the boiling process."

A nonahydrate contains 9 molecules of water in crystalline form, which is why you boil the barrel to drive the water into the ferric oxide creating ferrosoferric oxide. The reaction takes some time. The reaction also may work faster the thinner the coat of rust.

dave
 
Hi John,
I have to admit that I never used Mike Lee's but with other rust bluing solutions my barrels needed at least 30 minutes in boiling water to fully and evenly turn color. I usually give them about an hour to be sure. You really should not need coarse steel wool to card. That suggests to me that you may be letting the barrel rust to long before carding. Moreover, steel wool can contain oil and needs to be degreased before use. The passage below was copied from a thread of mine on another forum. It was written by John Cholin who is a fire chemist and knows his stuff. It describes what happens to turn a brown rust to blue-black rust:

" The red/orange brown is ferric oxide, Fe2O3. When ferric oxide is allowed to accumulate an additional oxygen it converts to ferrosoferric oxide, Fe3O4 which usually exists as a nonahydrate, -9(H2O), The brown color of a browned barrel is due to a mixture of ferric oxide and ferrosferric oxide - red and black make brown. That's why boiling a browned barrel turns it black - the red ferric oxide is being converted to ferrosoferric oxide nonahydrate due to the boiling process."

A nonahydrate contains 9 molecules of water in crystalline form, which is why you boil the barrel to drive the water into the ferric oxide creating ferrosoferric oxide. The reaction takes some time. The reaction also may work faster the thinner the coat of rust.

dave

Hi Dave,
Thanks for the chemistry lesson! I was familiar with the basic transformation but now I know the complete chemistry.

You hit the nail squarely on the head! The barrel was in the sweat box for over eight hours while I was waiting for the rust to cover the whole barrel. Lee directions suggest it might take five hours or more for the rust to form and cover the barrel on successive applications. Obviously that was much too long. The rust never did cover the entire barrel. It was about 50/50 rust and blue/black. The rusted portions required the "0" steel wool while the blue/black sections carded easily with the "0000" steel wool.

I'm going to try another application and I'll remove the barrel as soon as a fine coating of rust appears or two hours which ever comes first. I'll try carding with canvas first and then "0000" steel wool, if neccessary. I de-greased a couple of pads with naptha.

This is what the barrel looks like now.
barrel3 web.jpg

I was hoping to achieve something a little darker with more blue.
 
If that picture is of the raw, unoiled barrel, it will become noticeably darker after you oil it.

Of course, if you do oil it and you want to try to make it darker by applying more of the bluing solution you will have to totally remove all traces of the oil you applied.
That isn't as easy as removing oil from a bare steel barrel because the existing bluing will absorb the oil and try to hang on to it.
 
If that picture is of the raw, unoiled barrel, it will become noticeably darker after you oil it.

Of course, if you do oil it and you want to try to make it darker by applying more of the bluing solution you will have to totally remove all traces of the oil you applied.
That isn't as easy as removing oil from a bare steel barrel because the existing bluing will absorb the oil and try to hang on to it.

Hi Jim,
Thanks for the reply. That is a photo of the raw, unoiled barrel. I applied one more coat of the slow rust blue with no change to the color. It will get a coat of oil later today.
 
Do ya'll blue the barrel with the breech plug installed or do you remove it and blue it off the barrel?

So far, I've blued my three barrels with the breech plug installed. You don't have to worry about lining up the breech plug-top barrel flat and possible damaging your finish and you only have to plug the muzzle to keep browning/rusting solution and boiling water out. Not my own idea, I'm following the lead of build books and experienced builders.
 
I apologize for hijacking the thread, but I am looking to blue a barrel but would like a softer, lighter more gray than blue than what you guys achieved. Similar to the Judson Brennan rendition of the Edward Marshall rifle as shown here.
http://judsonbrennan.blogspot.com/2017/11/

I am using the Jim Chambers solution for bluing. Do I just rub it back until I get what I'm looking for or is there another technique?
Also, is there a method to get the case hardening look on the lock without actually case hardening? I have zero experience in metallurgy...
 
Looks like your bringing up a whole new subject.

I suggest you start a topic that can delve into your questions without sidetracking this topic.

I'm not saying this because your question is a bit off track. I'm saying this because like you, there are others who might run a "search" for your issue and by having your own topic, it will pop up quickly so they can find the answer to their, and your question
 
I apologize for hijacking the thread, but I am looking to blue a barrel but would like a softer, lighter more gray than blue than what you guys achieved. Similar to the Judson Brennan rendition of the Edward Marshall rifle as shown here.
http://judsonbrennan.blogspot.com/2017/11/

Hi Buckskinn,
The second and third application of the rust blue solution I used produced a color similar to to what you're looking for. The color does start out light and gets darker with each application. Maybe you can achieve the same effect with the Chamber's product.
 
Hi Buckskinn,
The second and third application of the rust blue solution I used produced a color similar to to what you're looking for. The color does start out light and gets darker with each application. Maybe you can achieve the same effect with the Chamber's product.

Thanks, that's what I was hoping for.... As far as the color case hardening, a quick search revealed what I was looking for. And it's not something I'm going to play with at this time. I will either leave the lock as is or lightly blue it and play with different buffing methods to get as close to what I'm looking for as I can.
 
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