Kallitype solution and Potassium Dichromate. Help.

DMJ · Nov 20, 2020

Hello,

This is my first time posting here. I hope I can find some help to fix a mistake I made. I added by mistake 1ml of potassium dichromate to a kallitype solution of Ferric Oxalate/Oxalic Acid and Silver Nitrate, instead of adding it to the developer of choice. I don't want to use any dichromate anymore but I had a small amount leftover from some gum prints, and I thought that using it with a few kallitypes could be a good way to get rid of it.

When I developed in Borax and Rochelle Salt, the image fades completely after fixing with sodium thyosulfate and ammonia.
When I developed with 20% sodium citrate, the image fades completely during a clearing bath of citric acid.

So that is when I realized that I added the dichromate to the silver solution instead of the developer. Is there a way to fix the solution or do something different ? What if I tone with gold before fixing ? It would be a pity to throw the silver but mistakes happen.

Thanks.

Andrew O'Neill · Nov 21, 2020

Did the image look fine after sodium citrate development? I mainly use sodium citrate, followed by a very weak citric acid bath... I've read somewhere that this bath isn't necessary if you develop in sodium citrate. After development, give the print a good rinse (in water that is neutral PH), then stick it in the gold toner, and see what happens. Rinse and then fix.

DMJ · Nov 21, 2020

Thanks for the quick reply Andrew. Yes, the image looked good after the citrate development but it took two minutes to fully develop. With the borax, it developed in normal time (seconds) and looked great. I will try to tone and see what happens. My understanding is that when toning, the metallic silver is replaced by the metal of the toner, hopefully one that does not oxidate and perdures so I hope it doesn't get washed away during the fix.

stefano_ber · Nov 21, 2020

DMJ said:
Thanks for the quick reply Andrew. Yes, the image looked good after the citrate development but it took two minutes to fully develop. With the borax, it developed in normal time (seconds) and looked great. I will try to tone and see what happens. My understanding is that when toning, the metallic silver is replaced by the metal of the toner, hopefully one that does not oxidate and perdures so I hope it doesn't get washed away during the fix.

Hi!
development must last from 8 to 10 minutes. Clarification does not last more than 4 minutes with citric acid. dichromate how many ml did you put? EDTA avoid it. Also, what concentration did you use of the fixing? sodium thiosulfate must be a maximum of 3%
I had the same problem and I solved it by removing the edta and clarifying only 4/5 minutes with a pinch of citric acid in distilled water.

stefano_ber · Nov 21, 2020

Andrew O'Neill said:
Did the image look fine after sodium citrate development? I mainly use sodium citrate, followed by a very weak citric acid bath... I've read somewhere that this bath isn't necessary if you develop in sodium citrate. After development, give the print a good rinse (in water that is neutral PH), then stick it in the gold toner, and see what happens. Rinse and then fix.

hi Andrew!
Do you know if sodium citrate made with soda and citric acid works well? I tried to make it at home, it works well alone, but adding the potassium dichromate (4ml) does not increase the contrast.
I use this formula:
sodium carbonate (soda): 266gr
citric acid: 162gr
water: 1440ml

all two component I bought in supermarket

thank you!!!
Stefano

nmp · Nov 21, 2020

stefano_ber said:
hi Andrew!
Do you know if sodium citrate made with soda and citric acid works well? I tried to make it at home, it works well alone, but adding the potassium dichromate (4ml) does not increase the contrast.
I use this formula:
sodium carbonate (soda): 266gr
citric acid: 162gr
water: 1440ml

all two component I bought in supermarket

thank you!!!
Stefano

Hi, Stefano:

Unless I am missing something, it looks like your recipe is deficient in citric acid - how much depends on whether you are using anhydrous or hydrated forms of the two. For example, using both anhydrous CA and soda, 266 gm of soda should equate to 321 gm of CA by my calculation. Have you checked the pH of your developer?

:Niranjan.

stefano_ber · Nov 21, 2020

nmp said:
Hi, Stefano:

Unless I am missing something, it looks like your recipe is deficient in citric acid - how much depends on whether you are using anhydrous or hydrated forms of the two. For example, using both anhydrous CA and soda, 266 gm of soda should equate to 321 gm of CA by my calculation. Have you checked the pH of your developer?

:Niranjan.

thank you Niranjan!
I don't know which kind of soda is. You can read its specifications here.
Soda Solvay® light - PDS - Orig. Eur - EN

which PH should the development have?

nmp · Nov 21, 2020

stefano_ber said:
thank you Niranjan!
I don't know which kind of soda is. You can read its specifications here.
Soda Solvay® light - PDS - Orig. Eur - EN

which PH should the development have?

The spec looks like that of the anhydrous sodium carbonate as water of hydration is not mentioned anywhere. I am guessing CA is anhydrous too as it is the most common one in the grocery stores.

Here is the link where you can calculate the amounts of all by plugging in one if the ingredients the table below.

https://www.webqc.org/balance.php?reaction=C6H8O7+Na2CO3=Na3C6H5O7+CO2+H2O

:Niranjan.

nmp · Nov 21, 2020

Regarding pH, it should be slightly on the alkaline side - since it is a salt of a mild acid and a strong base...may be like 8 or so. Prepared trisodium citrate stoichiometrically, that is. I wonder if the commercial deveiopers have some excess citric acid to make it neutral.

Andrew O'Neill · Nov 21, 2020

Be sure to develop thoroughly. With sodium citrate, and sodium acetate developers, 10 minutes. As far as making sodium citrate at home, I've never done that. I have made sodium acetate, though.

DMJ · Nov 21, 2020

stefano_ber said:
Hi!
development must last from 8 to 10 minutes. Clarification does not last more than 4 minutes with citric acid. dichromate how many ml did you put? EDTA avoid it. Also, what concentration did you use of the fixing? sodium thiosulfate must be a maximum of 3%
I had the same problem and I solved it by removing the edta and clarifying only 4/5 minutes with a pinch of citric acid in distilled water.

Hi Stefano,
I think my timing is right because I never had problems before but I'm not an expert either. My citric acid bath is 3% one shot. I usually leave the print there until all yellow is gone.
I'm going to replace the citric acid bath clearing for a solution of 12% potassium oxalate. Since it is difficult to get it in powder form here in the US, does anyone know if the Bostick & Sullivan's Pt/Pd potassium oxalate developer works as a clearing bath for kallitypes?

I think I'm going to get rid of the dichromate entirely, it is not needed and only causes problems. There must be a "non toxic" way in 2020 to control contrast besides working the negative?

Since the thread has already gone somewhere else, I will ask one more question here. Is it possible to add a drop of blue food coloring to the sensitizer to be able to see it under yellow light without compromising the solution ? I read about it in a book about salt printing but the solution for salted prints only uses silver nitrate.

Cheers

Andrew O'Neill · Nov 21, 2020

DMJ said:
Hi Stefano,
I think my timing is right because I never had problems before but I'm not an expert either. My citric acid bath is 3% one shot. I usually leave the print there until all yellow is gone.
I'm going to replace the citric acid bath clearing for a solution of 12% potassium oxalate. Since it is difficult to get it in powder form here in the US, does anyone know if the Bostick & Sullivan's Pt/Pd potassium oxalate developer works as a clearing bath for kallitypes?

I think I'm going to get rid of the dichromate entirely, it is not needed and only causes problems. There must be a "non toxic" way in 2020 to control contrast besides working the negative?

Since the thread has already gone somewhere else, I will ask one more question here. Is it possible to add a drop of blue food coloring to the sensitizer to be able to see it under yellow light without compromising the solution ? I read about it in a book about salt printing but the solution for salted prints only uses silver nitrate.

Cheers

Citric Acid is hard to get in the US? Here in Canada, I get a kg bag from a local DIY wine shop. It's also easily purchased from amazon. As far as blue food colouring, it's probably okay, but I'm only guessing. You need to work in a brighter space.

DMJ · Nov 21, 2020

Andrew O'Neill said:
Citric Acid is hard to get in the US? Here in Canada, I get a kg bag from a local DIY wine shop. It's also easily purchased from amazon. As far as blue food colouring, it's probably okay, but I'm only guessing. You need to work in a brighter space.

I was referring to potassium oxalate in powder form. Citric acid is very easy to get here in LA, I bought a 5lb bag at the Indian supermarket for really cheap.

DMJ · Nov 21, 2020

Update.

I got a negative that I use for testing (without a curve), cheap canson paper and kept the solutions in a warm water bath because last night was too cold.
I developed with a solution of 48gr Borax/36gr Sodium Potassium Tartrate in 500ml of water. I washed the print before clearing (this is something that I skipped last time) and put it in a very short clearing bath of 3% citric acid. Image still there without any major changes, only slightly lighter. Washed thoroughly and put in 50gr sodium Thyosulfate/12ml ammonia fixer for 5 minutes, then washed again. Image still present!.

The variables I changed were the washing before the clearing and the temperature of the solutions. The problem now is that the print is too orange but I am using a black developer. I'm sure this happens because of the dichromate. The image I uploaded is actually darker and more orange.I'm going to get rid of the solutions unless there are other creative possibilities. The good thing is that my city takes care of hazmats even during the pandemic.

Thanks.

stefano_ber · Nov 21, 2020

DMJ said:
Update.

I got a negative that I use for testing (without a curve), cheap canson paper and kept the solutions in a warm water bath because last night was too cold.
I developed with a solution of 48gr Borax/36gr Sodium Potassium Tartrate in 500ml of water. I washed the print before clearing (this is something that I skipped last time) and put it in a very short clearing bath of 3% citric acid. Image still there without any major changes, only slightly lighter. Washed thoroughly and put in 50gr sodium Thyosulfate/12ml ammonia fixer for 5 minutes, then washed again. Image still present!.

The variables I changed were the washing before the clearing and the temperature of the solutions. The problem now is that the print is too orange but I am using a black developer. I'm sure this happens because of the dichromate. The image I uploaded is actually darker and more orange.I'm going to get rid of the solutions unless there are other creative possibilities. The good thing is that my city takes care of hazmats even during the pandemic.

Thanks.

I never had problems with dichromate, but in the developer! Fixing bath I think is too longer! it is always advisable not to exceed 1 minute due to fading problems that thiosulphate normally causes on the print. Certainly the addition of dichromate in the sensitizer did not help. So basically I will redo the solution and it should be fine.

stefano_ber · Nov 21, 2020

nmp said:
The spec looks like that of the anhydrous sodium carbonate as water of hydration is not mentioned anywhere. I am guessing CA is anhydrous too as it is the most common one in the grocery stores.

Here is the link where you can calculate the amounts of all by plugging in one if the ingredients the table below.

https://www.webqc.org/balance.php?reaction=C6H8O7+Na2CO3=Na3C6H5O7+CO2+H2O

:Niranjan.

yes Niranjan!
they are all anidro component, but I don't understand as I can use that table.

nmp · Nov 21, 2020

stefano_ber said:
yes Niranjan!
they are all anidro component, but I don't understand as I can use that table.

What you do is enter a number, say in the Weight column against the soda (Na2CO3) row. For example, enter 266 which was the amount you used and hit enter. Rest of the numbers will be automatically filled. In this case, CA (C6H8O7) will show 321.4493. In the top, there is also a tool that will balance the equation for you which you would do before you get the table.

:Niranjan.

koraks · Nov 25, 2020

nmp said:
The spec looks like that of the anhydrous sodium carbonate as water of hydration is not mentioned anywhere.

Molecular weight is the give-away; the pdf says 106 which means anhydrous. I've only encountered monohydrate and decahydrate in my local supermarkets.

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