Testing plain hypo fixer for salt prints


Marek Matusz
 

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.

Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.

I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.

This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.

Time to make some prints.

 

Have fun and test your workflow.

 

Marek Matusz

 

Sent from Mail for Windows

 


Christina Z. Anderson
 

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 


Pfriedrichsen
 

Coincidentally, the 30 min soak is what I came up with for removing most of the residual iron from a cyanotype print on HPR. One can check this by soaking afterwards in a tannin soln (unlike the light exposure here) So maybe it is just a slow diffusion out of those fibres and whatever sizing is in there regardless of the type of sensitizer?

Thanks Marek!

Peter

On Jan 22, 2022, at 12:45 PM, Marek Matusz <marekmatusz@...> wrote:



I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.

<17334E4A083649228425EBEBE2AB1A11.jpg>

Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.

I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.

This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.

Time to make some prints.

 

Have fun and test your workflow.

 

Marek Matusz

 

Sent from Mail for Windows

 


Serdar Bilici
 

Christina,

I am using TF-2 fixer at stock strength that is %20 percent sodium thiosulfate. I do not worry about prolonged fixing since alkaline fixers do not bleach image in my experience. I have used TF-2 for all my silver processes (vdb, collodion, silver gelatin film, plate and print). I have prepared Agfa 304 since Marek tested it but I haven’t tried it yet. 

I have not noticed any bleaching in old prints as well alkaline fixers are easier to wash away in my experience, so I never worried about residual hypo in prints.

Ammonium chloride wash is in the right spot.

Serdar




On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 



Christina Z. Anderson
 

Thanks, Serdar,
I’ve been working on a revision of my salted paper chapter in my first gum book and I am going to add your step in that chapter.
It is easy to produce fading at will by fixing a salt print and not rinsing afterwards. Goes to a nice yellow brown in a short time. For illustration purposes only, of course :)
For the record, I have never seen fading of a salt print in fixer. I see drastic color shifts in the salt baths and fixer but it’s not fading. I’ve never worried about fading with overlong fixing, just archivalness of the print with overlong fixing.
What is your formula for TF-2? Is it different than PhotoFormulary TF-4? TF-4 looks to be 10–15% ammonium thiosulfate but otherwise is a “secret” formula, from the SDS sheet. I wonder what percentage of something they can add before it is listed on the SDS.
Chris

On Jan 23, 2022, at 2:33 AM, Serdar Bilici <sbilici@...> wrote:

Christina,

I am using TF-2 fixer at stock strength that is %20 percent sodium thiosulfate. I do not worry about prolonged fixing since alkaline fixers do not bleach image in my experience. I have used TF-2 for all my silver processes (vdb, collodion, silver gelatin film, plate and print). I have prepared Agfa 304 since Marek tested it but I haven’t tried it yet. 

I have not noticed any bleaching in old prints as well alkaline fixers are easier to wash away in my experience, so I never worried about residual hypo in prints.

Ammonium chloride wash is in the right spot.

Serdar




On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 




Serdar Bilici
 

Christina,

TF-4 formula is secret as you have said. TF-2 is a simple alkaline sodium thiosulfate fixer I link the formula.

When I feel lazy I replace 10gr sodium metaborate with 6 gr sodium carbonate. (Carbonated version is not ideal if the material is carried from an acidic wash since it can create bubbles.)

If necessary  will link the method for sodium metaborate. I keep a stock of it and use it as necessary.

Serdar


On 23 Jan 2022, at 18:01, Christina Z. Anderson <christinazanderson@...> wrote:

Thanks, Serdar,
I’ve been working on a revision of my salted paper chapter in my first gum book and I am going to add your step in that chapter.
It is easy to produce fading at will by fixing a salt print and not rinsing afterwards. Goes to a nice yellow brown in a short time. For illustration purposes only, of course :)
For the record, I have never seen fading of a salt print in fixer. I see drastic color shifts in the salt baths and fixer but it’s not fading. I’ve never worried about fading with overlong fixing, just archivalness of the print with overlong fixing.
What is your formula for TF-2? Is it different than PhotoFormulary TF-4? TF-4 looks to be 10–15% ammonium thiosulfate but otherwise is a “secret” formula, from the SDS sheet. I wonder what percentage of something they can add before it is listed on the SDS.
Chris


Jim Patterson,
 

Hi All,
If is not very toxic, any ingredient less than 1% does not have to be listed in US, OSHA, etc
Jim


On Jan 23, 2022, at 9:01 AM, Christina Z. Anderson <christinazanderson@...> wrote:

Thanks, Serdar,
I’ve been working on a revision of my salted paper chapter in my first gum book and I am going to add your step in that chapter.
It is easy to produce fading at will by fixing a salt print and not rinsing afterwards. Goes to a nice yellow brown in a short time. For illustration purposes only, of course :)
For the record, I have never seen fading of a salt print in fixer. I see drastic color shifts in the salt baths and fixer but it’s not fading. I’ve never worried about fading with overlong fixing, just archivalness of the print with overlong fixing.
What is your formula for TF-2? Is it different than PhotoFormulary TF-4? TF-4 looks to be 10–15% ammonium thiosulfate but otherwise is a “secret” formula, from the SDS sheet. I wonder what percentage of something they can add before it is listed on the SDS.
Chris

On Jan 23, 2022, at 2:33 AM, Serdar Bilici <sbilici@...> wrote:

Christina,

I am using TF-2 fixer at stock strength that is %20 percent sodium thiosulfate. I do not worry about prolonged fixing since alkaline fixers do not bleach image in my experience. I have used TF-2 for all my silver processes (vdb, collodion, silver gelatin film, plate and print). I have prepared Agfa 304 since Marek tested it but I haven’t tried it yet. 

I have not noticed any bleaching in old prints as well alkaline fixers are easier to wash away in my experience, so I never worried about residual hypo in prints.

Ammonium chloride wash is in the right spot.

Serdar




On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 




Jim Patterson,
 

Me Again,
On further reviewing OSHA trade secret rules, the specific name and/or specific % can be claimed as a trade secret.  It should not be in general use in similar products.

A health care provider can request the specific name and % in case of poisoning and the mfg must provide it for patient safety.
Jim


On Jan 23, 2022, at 9:13 AM, Jim Patterson, <jimbobnola@...> wrote:

Hi All,
If is not very toxic, any ingredient less than 1% does not have to be listed in US, OSHA, etc
Jim


On Jan 23, 2022, at 9:01 AM, Christina Z. Anderson <christinazanderson@...> wrote:

Thanks, Serdar,
I’ve been working on a revision of my salted paper chapter in my first gum book and I am going to add your step in that chapter.
It is easy to produce fading at will by fixing a salt print and not rinsing afterwards. Goes to a nice yellow brown in a short time. For illustration purposes only, of course :)
For the record, I have never seen fading of a salt print in fixer. I see drastic color shifts in the salt baths and fixer but it’s not fading. I’ve never worried about fading with overlong fixing, just archivalness of the print with overlong fixing.
What is your formula for TF-2? Is it different than PhotoFormulary TF-4? TF-4 looks to be 10–15% ammonium thiosulfate but otherwise is a “secret” formula, from the SDS sheet. I wonder what percentage of something they can add before it is listed on the SDS.
Chris

On Jan 23, 2022, at 2:33 AM, Serdar Bilici <sbilici@...> wrote:

Christina,

I am using TF-2 fixer at stock strength that is %20 percent sodium thiosulfate. I do not worry about prolonged fixing since alkaline fixers do not bleach image in my experience. I have used TF-2 for all my silver processes (vdb, collodion, silver gelatin film, plate and print). I have prepared Agfa 304 since Marek tested it but I haven’t tried it yet. 

I have not noticed any bleaching in old prints as well alkaline fixers are easier to wash away in my experience, so I never worried about residual hypo in prints.

Ammonium chloride wash is in the right spot.

Serdar




On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 




Christina Z. Anderson
 

Thanks Serdar and Jim for the quick answers!
So either up to 10 g per liter, Jim, or, if trade secret, it can be anything. I don’t think anyone is going to be poisoned by TF-4 anytime soon in order to find out the secret sauce. 
I’m going to go stick a print outside in the sun today a la Marek.
Chris

On Jan 23, 2022, at 8:33 AM, Jim Patterson, <jimbobnola@...> wrote:

Me Again,
On further reviewing OSHA trade secret rules, the specific name and/or specific % can be claimed as a trade secret.  It should not be in general use in similar products.

A health care provider can request the specific name and % in case of poisoning and the mfg must provide it for patient safety.
Jim


On Jan 23, 2022, at 9:13 AM, Jim Patterson, <jimbobnola@...> wrote:

Hi All,
If is not very toxic, any ingredient less than 1% does not have to be listed in US, OSHA, etc
Jim


On Jan 23, 2022, at 9:01 AM, Christina Z. Anderson <christinazanderson@...> wrote:

Thanks, Serdar,
I’ve been working on a revision of my salted paper chapter in my first gum book and I am going to add your step in that chapter.
It is easy to produce fading at will by fixing a salt print and not rinsing afterwards. Goes to a nice yellow brown in a short time. For illustration purposes only, of course :)
For the record, I have never seen fading of a salt print in fixer. I see drastic color shifts in the salt baths and fixer but it’s not fading. I’ve never worried about fading with overlong fixing, just archivalness of the print with overlong fixing.
What is your formula for TF-2? Is it different than PhotoFormulary TF-4? TF-4 looks to be 10–15% ammonium thiosulfate but otherwise is a “secret” formula, from the SDS sheet. I wonder what percentage of something they can add before it is listed on the SDS.
Chris

On Jan 23, 2022, at 2:33 AM, Serdar Bilici <sbilici@...> wrote:

Christina,

I am using TF-2 fixer at stock strength that is %20 percent sodium thiosulfate. I do not worry about prolonged fixing since alkaline fixers do not bleach image in my experience. I have used TF-2 for all my silver processes (vdb, collodion, silver gelatin film, plate and print). I have prepared Agfa 304 since Marek tested it but I haven’t tried it yet. 

I have not noticed any bleaching in old prints as well alkaline fixers are easier to wash away in my experience, so I never worried about residual hypo in prints.

Ammonium chloride wash is in the right spot.

Serdar




On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

Marek and Serdar,

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

But my question is, is it possible something else is going on?

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

Chris

  1. Immerse in a tray of 5% salted water, agitating continually for 4 minutes. Be sure to submerge the print all at once to prevent uneven tones.
  2. Transfer the print to a second tray of 5% salted water and agitate continually for 4 minutes.
  3. Wash the print in 20% ammonium chloride for 3-5 mins. (%20 Ammonium chloride is reusable for more than 10 prints. You can put the solution under the sun, metallic silver will precipitate and you can filter it. and add more amm. chloride and continue using it.)
  4. Transfer the print to a third tray of plain water and agitate continually for 4 minutes to remove excess salt that can slow toning action.
  5. Lift, drain, and transfer the print to the toner, face up, agitating all the while until the desired tone is reached, from 3–15 minutes.
  6. Lift, drain, and transfer the print to an alkaline water wash, plain water made slightly alkaline by the addition of  ¼ teaspoon of  washing soda (sodium carbonate) per liter, for 4 minutes to remove any toner and acidity before fixing. This is very important with an acid toner, because acid will precipitate sulfur in the fix and weaken the fix, both which lead to staining and fading of the print.  Note: if thiourea toning, use the 5% salt bath instead of the alkaline bath in this step, or you will get instant brown staining.
  7. Lift, drain, and transfer the print to the first tray of fixer and agitate continually for 4 minutes. 
  8. Transfer the print to the second tray of fixer and agitate continually for 4 minutes. If printing lots of prints in one day, after 10–15 8˝ × 10˝ prints have gone through the first tray, discard it, move Tray 2 to Tray 1’s spot and mix up a new tray of fixer. 
  9. Lift, drain, and rinse the print for 4 minutes in plain water.
  10. Transfer the print to the 1% sodium sulfite hypoclear bath for 4 minutes to remove any residual fixer.
  11. Transfer the print to a final running water wash for 30–60 minutes or much longer if desired.


On Jan 22, 2022, at 10:45 AM, Marek Matusz <marekmatusz@...> wrote:

I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.<17334E4A083649228425EBEBE2AB1A11.jpg>
Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.
I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.
This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.
Time to make some prints.
 
Have fun and test your workflow.
 
Marek Matusz
 
Sent from Mail for Windows
 





Marek Matusz
 

Chris and Serdar

 

The grey stain that is present in my sun test with very short fixing times is likely at least partially silver chloride being reduced to metallic silver. The yellow stain is perhaps  underneath, but masked by grey color of silver. The yellow stain is likely silver sulfide that forms by decomposition of residual silver thiosulfate complex. I have tested a number of stains with farmers reducer and the yellow stain stays, which is a likely indication of it being silver sulfide (plus the color).

The reason that fixers have evolved to have high concentrations of thiosulfate is that you need large excess of thiosulfate to make soluble silver complexes. SO you need time and concentration for thiosulfate to diffuse in sufficient concentration to solubilize and remove silver chloride. The chemistry of thiosulfate complexation is quite complex and goes through several stages.

I do have a stack of prints, well over 100 all on heavy paper like HPR and Revere Platinum 310g all showing some degree of yellow stain after 3-5 years of storage. AT one point I moved to two very short TF2 fixing baths (I thought rapid fixing would apply to salt prints, BIG MISTAKE) and that was a mystery that it took me a long time to solve. By the way, I did not see issues on lightweight papers like Strathmore Bristol 500 1ply.

 

I was prompted to do some more research by correspondence with a few members of alt community on the subject of salt printing and especially paper recommendations, so I re-read all period articles cited by Chris and decided to start my processing from ground zero (that is what would have been best practice at the turn of century). Kind of distilling all combined literature into a practice. That actually lead me to systematically test fixers and fixing times.

 

By the way pH of plain thiosulfate that I tested is about 7, but it has very little buffering capacity.

Here is an example of the action of Farmers Reducer on a freshly generated stain resulting from short fixing time. You can see severe bleaching of silver (shadows), but underneath is the yellow component of silver sulfide stain that is not removed in this test (highlights)

Serdar, I wonder if you ammonium chloride dip actually solubilizes silver chloride (one way to test would be to expose to sunlight at that point) or just supplies ammonium ions that have much higher mobility than sodium.

I do like constructive discussion on the subject and love the fact that I am able to make salted paper prints on Revere platinum again. They are so fabulously yellow/red brown in shade.

Marek

 

 

 



On 23 Jan 2022, at 02:23, Christina Z. Anderson <christinazanderson@...> wrote:

 

Marek and Serdar,

 

Marek, I do not do water washes first, but immediate 5% salted water washes (not 2%), 2 trays in a row, for a total of 8 minutes.

 

I also use an alkaline water wash before fixing, AND an alkaline fixer, two baths, total of 8 minutes (sodium carbonate in fix). Actually, to be honest, I use Formulary TF-4 Fixer at the recommended dilution.

 

Back in 1855 they attributed fading of prints to too long fixing and residual thiosulfate left in the paper fibers and in one of Ware’s articles/books he also says this. (BTW the Salted Paper Printing Troubleshooting chapter is 34 whopping pages with 73 illustrations but you know that since you and I collaborated on some areas in that book!). Are you worried about overly long fixing?

 

So what I am seeing in your prints is a continued sensitivity to light exposure as if you have not removed all the sensitive silver chloride. 

 

I promise, now that I am home I am sticking a print outside in the sun and see if I can create this, too. 

 

But my question is, is it possible something else is going on?

 

Serdar, tell me if I have added your step in my usual workflow in the right spot, below?

 

Chris

 

 


Paul Barden
 

Has anyone done the sun exposure test on paper that has only been sized with gelatin? Is it possible there’s something happening between the chemistry of the paper and gelatin together? Maybe Photo grade gelatin behaves differently from Knox food grade? Just pondering out loud. 


On Jan 22, 2022, at 9:46 AM, Marek Matusz <marekmatusz@...> wrote:



I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.

Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.

I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.

This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.

Time to make some prints.

 

Have fun and test your workflow.

 

Marek Matusz

 

Sent from Mail for Windows

 


Marek Matusz
 

Paul
The stain only happens on part that had silver nitrate sensitizer. I never see any in part that was salted/sized. Always stays paper white
Marek


On Jan 23, 2022, at 3:20 PM, Paul Barden via groups.io <castlebravo@...> wrote:

 Has anyone done the sun exposure test on paper that has only been sized with gelatin? Is it possible there’s something happening between the chemistry of the paper and gelatin together? Maybe Photo grade gelatin behaves differently from Knox food grade? Just pondering out loud. 


On Jan 22, 2022, at 9:46 AM, Marek Matusz <marekmatusz@...> wrote:



I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.

Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.

I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.

This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.

Time to make some prints.

 

Have fun and test your workflow.

 

Marek Matusz

 

Sent from Mail for Windows

 


Paul Barden
 

Good to know, Marek, thanks!


On Jan 23, 2022, at 1:28 PM, Marek Matusz <marekmatusz@...> wrote:

 Paul
The stain only happens on part that had silver nitrate sensitizer. I never see any in part that was salted/sized. Always stays paper white
Marek


On Jan 23, 2022, at 3:20 PM, Paul Barden via groups.io <castlebravo@...> wrote:

 Has anyone done the sun exposure test on paper that has only been sized with gelatin? Is it possible there’s something happening between the chemistry of the paper and gelatin together? Maybe Photo grade gelatin behaves differently from Knox food grade? Just pondering out loud. 


On Jan 22, 2022, at 9:46 AM, Marek Matusz <marekmatusz@...> wrote:



I am posting an additional fixer test in my latest salt print research. This time it is plain 15% thiosulfate solution, most common recommendation for a fixer. The paper is Hahnemuhle Platinum Rag, salting/size is gelatin based. After exposure the print was washed in 3 changes of water and soaked in 2% salt. The print is NOT toned. It was placed in a solution of plain 15% hypo fixer and test strips cut after indicated fixing times. This is one bath fixing. After fixing the strips were soaked in 2% sodium sulfite for 3 minutes and washed. Dry strip showed no stain at this point. They were put out in full sun for 4 hours to accelerate stain formation.

Clearly there is only partial fixing at 5 minutes. 10 minute fixing time is still not sufficient with some surface stain evident in the test strip on top. At 15 min the surface of the print looks fixed, but you can see the stain if you look through the paper. The print is well fixed at 20 min, no further tonal change or otherwise happens with 30 min fixing. I do not see a progressive bleaching in this test.

I was surprised that I did not get a clear yellow stain as before. This might be due to the fact that it was a freshly made fixer and it did not have any silver build in.

This confirms my observation that long fixing times are needed to completely clear salted paper prints to avoid stain formation.

Time to make some prints.

 

Have fun and test your workflow.

 

Marek Matusz

 

Sent from Mail for Windows

 


Niranjan Patel
 

If you are toning with sulfide or selenium toners, which is what I do, you would have a built in test to see if the fixing is adequate.  Since those toners will react with both the silver metal and the salt, unlike gold toner, you would get staining if fixer did not remove all of the silver salts.  This is also the basis for Kodak's silver test solution ST-1 used in traditional silver gelatin papers.  

:Niranjan.


Serdar Bilici
 

Marek,

Sorry for my late reply. I was distracted. I have prepared agfa 304 fixer to test later.

What type of testing procedure do you recommend to test the effects of ammonium chloride wash? 

BTW, in case it didn't come to your attention, this information is from from silver chloride solubility tables. I am sure we can find some scientific text to clarify it.

NOTE: About Silver Chloride and solubility in general
When Silver Chloride is freshly prepared in solution, it looks and feels exactly like soft, white Cottage Cheese. This freshly prepared Silver Chloride, when rinsed and damp, before it is dry, or exposed to any light, will tend to be more soluble than commercially prepared, dry, blended, sifted Silver Chloride. During the drying, sifting and blending process, Silver Chloride undergoes subtle changes that are not always visible to the human eye. When dry, Silver Chloride hardens into pretty tough, but very tiny, little particles. The very outer layers of the dry Silver Chloride powder pieces tend to undergo changes when exposed to even dim lighting and oxygen that make the Silver Chloride powder less soluble in solutions. The more the light and heat, the more pronounced this effect becomes.

I am thinking ammonium chloride wash turns excess nitrate salts to chloride as expected but I  assume other silver salts are turned into the halogen from as well in the presence of such excess. Since they are freshly formed and they haven't undergone changes they are so easily dissolved by amm. chloride wash and remaining changed salts are easily removed by thiosulfate. 


Marek Matusz
 

Serdar
Just cut the strip after ammonium chloride bath and expose it to sun for a few hours together with time test fix strips. It would be interesting to see if this treatment shortens fixing times vs print has has not been treated. 
Marek


On Jan 25, 2022, at 11:03 AM, Serdar Bilici <sbilici@...> wrote:

Marek,

Sorry for my late reply. I was distracted. I have prepared agfa 304 fixer to test later.

What type of testing procedure do you recommend to test the effects of ammonium chloride wash? 

BTW, in case it didn't come to your attention, this information is from from silver chloride solubility tables. I am sure we can find some scientific text to clarify it.

NOTE: About Silver Chloride and solubility in general
When Silver Chloride is freshly prepared in solution, it looks and feels exactly like soft, white Cottage Cheese. This freshly prepared Silver Chloride, when rinsed and damp, before it is dry, or exposed to any light, will tend to be more soluble than commercially prepared, dry, blended, sifted Silver Chloride. During the drying, sifting and blending process, Silver Chloride undergoes subtle changes that are not always visible to the human eye. When dry, Silver Chloride hardens into pretty tough, but very tiny, little particles. The very outer layers of the dry Silver Chloride powder pieces tend to undergo changes when exposed to even dim lighting and oxygen that make the Silver Chloride powder less soluble in solutions. The more the light and heat, the more pronounced this effect becomes.

I am thinking ammonium chloride wash turns excess nitrate salts to chloride as expected but I  assume other silver salts are turned into the halogen from as well in the presence of such excess. Since they are freshly formed and they haven't undergone changes they are so easily dissolved by amm. chloride wash and remaining changed salts are easily removed by thiosulfate. 


Clay Harmon
 

Thanks to Serdar and Marek for these fascinating threads. This seems to be the (extreme) summary of what is being discussed:

Serdar: a pre-fix clearing bath of ammonium chloride is advantageous in solubilizing unexposed silver chloride from the paper fibers and removing it.

Marek: Extended fixing times are also necessary for removing any remaining unexposed silver chloride from the paper fibers to prevent subsequent fogging of highlights. This necessarily means that hypoclearing is also important to prevent later sulfiding of the silver particles remaining in the paper fiber.

Is this perhaps a belt-and-suspenders best processing practice incorporating both? :

- initial clearing of print with ammonium chloride bath for ca. 5-10 minutes (which needs to be replenished as necessary)
- wash 
- toning if desired
- extended fix in alkaline fixers of 15 minutes or more
- hypoclearing for 5-10 minutes
- wash for ca. 45-60 minutes

For the chemists in the group, is there any conceivable downside to this set of steps?

I made some prints two days ago with exactly these steps and they are now roasting in the window to see if I can get any highlight fogging. So far, so good.

Clay


On 2022-01-25, at 13:41 :29, Marek Matusz <marekmatusz@...> wrote:

Serdar
Just cut the strip after ammonium chloride bath and expose it to sun for a few hours together with time test fix strips. It would be interesting to see if this treatment shortens fixing times vs print has has not been treated. 
Marek


On Jan 25, 2022, at 11:03 AM, Serdar Bilici <sbilici@...> wrote:

Marek,

Sorry for my late reply. I was distracted. I have prepared agfa 304 fixer to test later.

What type of testing procedure do you recommend to test the effects of ammonium chloride wash? 

BTW, in case it didn't come to your attention, this information is from from silver chloride solubility tables. I am sure we can find some scientific text to clarify it.

NOTE: About Silver Chloride and solubility in general
When Silver Chloride is freshly prepared in solution, it looks and feels exactly like soft, white Cottage Cheese. This freshly prepared Silver Chloride, when rinsed and damp, before it is dry, or exposed to any light, will tend to be more soluble than commercially prepared, dry, blended, sifted Silver Chloride. During the drying, sifting and blending process, Silver Chloride undergoes subtle changes that are not always visible to the human eye. When dry, Silver Chloride hardens into pretty tough, but very tiny, little particles. The very outer layers of the dry Silver Chloride powder pieces tend to undergo changes when exposed to even dim lighting and oxygen that make the Silver Chloride powder less soluble in solutions. The more the light and heat, the more pronounced this effect becomes.

I am thinking ammonium chloride wash turns excess nitrate salts to chloride as expected but I  assume other silver salts are turned into the halogen from as well in the presence of such excess. Since they are freshly formed and they haven't undergone changes they are so easily dissolved by amm. chloride wash and remaining changed salts are easily removed by thiosulfate. 


Serdar Bilici
 

It is great to hear Clay, I am hoping to test Marek’s suggestion today or tomorrow.

I think combining both approaches will guarantee permanent trouble free prints. 

I find that using thiourea gold toners before fixing can create very subtle fog in highlights. Alkaline borax or carbonate toners don’t seem cause a similar problem. It is probably due to the sulfur in thiourea.

Serdar

On 26 Jan 2022, at 17:22, Clay Harmon <w.clay.harmon@...> wrote:

Thanks to Serdar and Marek for these fascinating threads. This seems to be the (extreme) summary of what is being discussed:

Serdar: a pre-fix clearing bath of ammonium chloride is advantageous in solubilizing unexposed silver chloride from the paper fibers and removing it.

Marek: Extended fixing times are also necessary for removing any remaining unexposed silver chloride from the paper fibers to prevent subsequent fogging of highlights. This necessarily means that hypoclearing is also important to prevent later sulfiding of the silver particles remaining in the paper fiber.

Is this perhaps a belt-and-suspenders best processing practice incorporating both? :

- initial clearing of print with ammonium chloride bath for ca. 5-10 minutes (which needs to be replenished as necessary)
- wash 
- toning if desired
- extended fix in alkaline fixers of 15 minutes or more
- hypoclearing for 5-10 minutes
- wash for ca. 45-60 minutes

For the chemists in the group, is there any conceivable downside to this set of steps?

I made some prints two days ago with exactly these steps and they are now roasting in the window to see if I can get any highlight fogging. So far, so good.

Clay


On 2022-01-25, at 13:41 :29, Marek Matusz <marekmatusz@...> wrote:

Serdar
Just cut the strip after ammonium chloride bath and expose it to sun for a few hours together with time test fix strips. It would be interesting to see if this treatment shortens fixing times vs print has has not been treated. 
Marek


On Jan 25, 2022, at 11:03 AM, Serdar Bilici <sbilici@...> wrote:

Marek,

Sorry for my late reply. I was distracted. I have prepared agfa 304 fixer to test later.

What type of testing procedure do you recommend to test the effects of ammonium chloride wash? 

BTW, in case it didn't come to your attention, this information is from from silver chloride solubility tables. I am sure we can find some scientific text to clarify it.

NOTE: About Silver Chloride and solubility in general
When Silver Chloride is freshly prepared in solution, it looks and feels exactly like soft, white Cottage Cheese. This freshly prepared Silver Chloride, when rinsed and damp, before it is dry, or exposed to any light, will tend to be more soluble than commercially prepared, dry, blended, sifted Silver Chloride. During the drying, sifting and blending process, Silver Chloride undergoes subtle changes that are not always visible to the human eye. When dry, Silver Chloride hardens into pretty tough, but very tiny, little particles. The very outer layers of the dry Silver Chloride powder pieces tend to undergo changes when exposed to even dim lighting and oxygen that make the Silver Chloride powder less soluble in solutions. The more the light and heat, the more pronounced this effect becomes.

I am thinking ammonium chloride wash turns excess nitrate salts to chloride as expected but I  assume other silver salts are turned into the halogen from as well in the presence of such excess. Since they are freshly formed and they haven't undergone changes they are so easily dissolved by amm. chloride wash and remaining changed salts are easily removed by thiosulfate. 

_._,_._,_

Groups.io Links:

You receive all messages sent to this group. 




Christina Z. Anderson
 

Serdar,
I have alleviated that fog with an after-toner salted water wash in place of the alkaline water wash. Have you used that and still gotten the fog? I really do like the thiourea gold toners even though they are a bit more of a PITA to make...
Chris

On Jan 26, 2022, at 8:02 AM, Serdar Bilici <sbilici@...> wrote:

It is great to hear Clay, I am hoping to test Marek’s suggestion today or tomorrow.

I think combining both approaches will guarantee permanent trouble free prints. 

I find that using thiourea gold toners before fixing can create very subtle fog in highlights. Alkaline borax or carbonate toners don’t seem cause a similar problem. It is probably due to the sulfur in thiourea.

Serdar

On 26 Jan 2022, at 17:22, Clay Harmon <w.clay.harmon@...> wrote:

Thanks to Serdar and Marek for these fascinating threads. This seems to be the (extreme) summary of what is being discussed:

Serdar: a pre-fix clearing bath of ammonium chloride is advantageous in solubilizing unexposed silver chloride from the paper fibers and removing it.

Marek: Extended fixing times are also necessary for removing any remaining unexposed silver chloride from the paper fibers to prevent subsequent fogging of highlights. This necessarily means that hypoclearing is also important to prevent later sulfiding of the silver particles remaining in the paper fiber.

Is this perhaps a belt-and-suspenders best processing practice incorporating both? :

- initial clearing of print with ammonium chloride bath for ca. 5-10 minutes (which needs to be replenished as necessary)
- wash 
- toning if desired
- extended fix in alkaline fixers of 15 minutes or more
- hypoclearing for 5-10 minutes
- wash for ca. 45-60 minutes

For the chemists in the group, is there any conceivable downside to this set of steps?

I made some prints two days ago with exactly these steps and they are now roasting in the window to see if I can get any highlight fogging. So far, so good.

Clay


On 2022-01-25, at 13:41 :29, Marek Matusz <marekmatusz@...> wrote:

Serdar
Just cut the strip after ammonium chloride bath and expose it to sun for a few hours together with time test fix strips. It would be interesting to see if this treatment shortens fixing times vs print has has not been treated. 
Marek


On Jan 25, 2022, at 11:03 AM, Serdar Bilici <sbilici@...> wrote:

Marek,

Sorry for my late reply. I was distracted. I have prepared agfa 304 fixer to test later.

What type of testing procedure do you recommend to test the effects of ammonium chloride wash? 

BTW, in case it didn't come to your attention, this information is from from silver chloride solubility tables. I am sure we can find some scientific text to clarify it.

NOTE: About Silver Chloride and solubility in general
When Silver Chloride is freshly prepared in solution, it looks and feels exactly like soft, white Cottage Cheese. This freshly prepared Silver Chloride, when rinsed and damp, before it is dry, or exposed to any light, will tend to be more soluble than commercially prepared, dry, blended, sifted Silver Chloride. During the drying, sifting and blending process, Silver Chloride undergoes subtle changes that are not always visible to the human eye. When dry, Silver Chloride hardens into pretty tough, but very tiny, little particles. The very outer layers of the dry Silver Chloride powder pieces tend to undergo changes when exposed to even dim lighting and oxygen that make the Silver Chloride powder less soluble in solutions. The more the light and heat, the more pronounced this effect becomes.

I am thinking ammonium chloride wash turns excess nitrate salts to chloride as expected but I  assume other silver salts are turned into the halogen from as well in the presence of such excess. Since they are freshly formed and they haven't undergone changes they are so easily dissolved by amm. chloride wash and remaining changed salts are easily removed by thiosulfate. 



Serdar Bilici
 

Chris, 
I used the toners after ammonia chloride wash. I rinse the paper of chloride then tested the toners. It is not pronounced as if it is a fog but it is especially visible with colder toners. Dmin values are different than paper white. 
I am totally into thiourea toners but you have point.

Serdar

On 26 Jan 2022, at 18:07, Christina Z. Anderson <christinazanderson@...> wrote:

Serdar,
I have alleviated that fog with an after-toner salted water wash in place of the alkaline water wash. Have you used that and still gotten the fog? I really do like the thiourea gold toners even though they are a bit more of a PITA to make...
Chris