Ilford Microphen/ID-68, origins and replenishment?

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Ian Grant

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The 1996 X-Tol datasheet says 70 ml: https://125px.com/docs/techpubs/kodak/j108-1996_09.pdf
I don't ever remember another figure for replenishing X-Tol, but I wasn't using X-Tol back then.
The recommended replenishment amount for T-Max RS is/was 45 ml per roll - perhaps that is what you were thinking of.

Thanks Matt, I don't have any data sheet on hand pre 2008 for Xtol, which is odd as I never throw anything out. I used Xtol replenished from its UK release until around 2007 but definitely didn't use 70ml per film (or 4 sheets of 5x4). I mainly used Xtol for commercial shoots, often around 20 rolls of APX100 per session, sometimes TMax 400, and I'm certain that replenishment was far less than 70ml.

Ian
 

MattKing

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FWIW, the 1999 German datasheet for X-Tol also appears (I don't read or speak German), to also recommend 70 ml.
https://125px.com/docs/techpubs/kodak/xtolEntwickler.pdf
I know that over the years there were lots of Kodak Ltd. products that were specific to the UK market, but I would be surprised to learn that a developer that was designed by Eastman Kodak in the mid 1990s in the US, and finalized and put into production in 1996, would have ever been made in two very different versions, with one such version being specific to the UK.
 

Steven Lee

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I would expect the replenishment volume to depend on film speed. Kodak's recommendation is probably based on a typical mix of B&W film speeds processed by an average lab at the time of publishing. I am not surprised by Ian's experience given his heavy use of APX 100. 90% of my shooting is ISO 400 with a bit of Delta 100 and 3200, and 70ml leads to gradual decline in activity.

By the way, I never realized how young Xtol is by B&W chemistry standards. I was already alive and exposing film in 1996! Anyway, this thread made me want to experiment with Microphen more. It beats the shit out of Xtol when processing Delta 3200 but I have not tried it for anything else.
 

Alain Deloc

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I did double-check the 9ml, Perceptol was replenished with 21ml of the then available replenisher.

A bit weird. I am pretty sure that your notes don't lie. But I am wondering why in the current Microphen datasheet, Ilford recommends extending developing time with 10% after each roll? That would give the idea that every roll consumes some 100ml of the working solution. The replenisher is much stronger than the working solution, indeed, but it doesn't seem to be that strong (according with ID68R formula) so 9ml of it could compensate the exhaustion of 100ml of working solution. Maybe that 10% time extension from current datasheet is too high?
 

Matroskin

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Hey guys
I found such a recipe for Microphen and it seems to be the most correct:

Sodium Tripolyphosphate 3.4g
Sodium sulphite 100g
Sodium metabisulphite 0.65g
Hydroquinone 5g
Borax 6.8g
Boric acid 2.8g
Potassium bromide 1g
Phenidone 0.2g

If consider this recipe and split it into 2 packages what should be in pack A and B?
 

albada

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First of all, welcome to Photrio!

The metabisulphite is probably present to protect the developers in packet A, which would contain:
sodium metabisulphite
hydroquinone
phenidone

Packet B would contain everything else. Actually, boric acid is acidic, so it could probably go in packet A. In general, it's important to keep the alkalis separate from the developers.

Mark
 

Ian Grant

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Hey guys
I found such a recipe for Microphen and it seems to be the most correct:

Sodium Tripolyphosphate 3.4g
Sodium sulphite 100g
Sodium metabisulphite 0.65g
Hydroquinone 5g
Borax 6.8g
Boric acid 2.8g
Potassium bromide 1g
Phenidone 0.2g

If consider this recipe and split it into 2 packages what should be in pack A and B?

That's definitely NOT the formula for Microphen, it's the powder version of Ilford Autophen, it was published incorrectly as Microphen in the Photo Lab Index many years ago and carried through many US books. The number of errors in the Photo Lab Index is around the 25% to 30% level.

Autophen was a PQ version of ID-11/D76 for commercial photofinishing, it was sold as a powder or liquid with two different replenishers, one for topping up the other bleed replenishment. Part B was the Sulphite and Borax.

There were a series of articles in the BJP in the 1950s, from Ilford research, which chronicle the evolution of what was termed the Axford-Kendal PQ Fine Grain Developer by Curt Jacobson. Essentially Ilford were looking at more effective replenishment. Unlike ID-11/D76 which collapses with Bromide build up inhibiting the Metol, that doesn't happen when you switch to Phenidone.

It was noted that Autophen gave a slight speed increase, so Ilford created a new developer to exploit the speed increase that using Phenidon gave compared to using Metol, they dropped the Sulphite level by 15%. It was already known that MQ developers like Adox Borax MQ and Agfa 44/Agfa Ansco 17 gave better shadow detail and a slight speed increase compared to ID-11/D76.

So by dropping the Sulphite level, optimising the PQ ratio & buffering Ilford release Microphen, the formula was published as ID-68 along with the replenisher. The packaged versions have Metabisulphite as a preservative in Part A so the buffering is adjusted to compensate.

Ian
 
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Ilfotec DD is the latest Ilford large volume film developer and replenishment product and probably more suitable for the current range of available films.
 

Matroskin

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First of all, welcome to Photrio!

The metabisulphite is probably present to protect the developers in packet A, which would contain:
sodium metabisulphite
hydroquinone
phenidone

Packet B would contain everything else. Actually, boric acid is acidic, so it could probably go in packet A. In general, it's important to keep the alkalis separate from the developers.

Mark
Thank you :smile:

That's definitely NOT the formula for Microphen, it's the powder version of Ilford Autophen, it was published incorrectly as Microphen in the Photo Lab Index many years ago and carried through many US books. The number of errors in the Photo Lab Index is around the 25% to 30% level.

Autophen was a PQ version of ID-11/D76 for commercial photofinishing, it was sold as a powder or liquid with two different replenishers, one for topping up the other bleed replenishment. Part B was the Sulphite and Borax.

There were a series of articles in the BJP in the 1950s, from Ilford research, which chronicle the evolution of what was termed the Axford-Kendal PQ Fine Grain Developer by Curt Jacobson. Essentially Ilford were looking at more effective replenishment. Unlike ID-11/D76 which collapses with Bromide build up inhibiting the Metol, that doesn't happen when you switch to Phenidone.

It was noted that Autophen gave a slight speed increase, so Ilford created a new developer to exploit the speed increase that using Phenidon gave compared to using Metol, they dropped the Sulphite level by 15%. It was already known that MQ developers like Adox Borax MQ and Agfa 44/Agfa Ansco 17 gave better shadow detail and a slight speed increase compared to ID-11/D76.

So by dropping the Sulphite level, optimising the PQ ratio & buffering Ilford release Microphen, the formula was published as ID-68 along with the replenisher. The packaged versions have Metabisulphite as a preservative in Part A so the buffering is adjusted to compensate.

Ian
Yes, I read it, but in the same time a guy from other forum told that he had been provided this recipe by Ilford plant employee.

Ok, if I want to make powder developer and store it over couple of years, should I add Sodium metabisulphite (0.65g) ?

A:
Sodium sulphite 85g
Hydroquinone 5g
Phenidone 0.13g
Sodium metabisulphite (0.65g)

B:
Borax 7g
Boric acid 2g
Potassium bromide 1g


PS By the way, what is the point to split it into 2 different packs? Dilution temperature?
 

Alain Deloc

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Thank you :smile:


Yes, I read it, but in the same time a guy from other forum told that he had been provided this recipe by Ilford plant employee.

Ok, if I want to make powder developer and store it over couple of years, should I add Sodium metabisulphite (0.65g) ?

A:
Sodium sulphite 85g
Hydroquinone 5g
Phenidone 0.13g
Sodium metabisulphite (0.65g)

B:
Borax 7g
Boric acid 2g
Potassium bromide 1g


PS By the way, what is the point to split it into 2 different packs? Dilution temperature?

It seems that you have all the necessary powders. Why would you want to mix them now as Microphen or Autophen or ID-68 (it really doesn't matter) and store it mixed for few years? You can keep all powders separated in bottles for as many years as you want and mix them from time to time.

You're probably using the expression "store it over the couple of years" as a replacement for "mix and sell it without degradation problems" 🙂 . In case if you're thinking to mix some powders and pack it in ziplock bags for sale, you should be aware that metabisulfite won't solve the oxygen problems. Commercial powder kits are packed and sealed in a inert gas atmosphere and the metabisulfite is added only for the minimal oxygen exchange that can occur through sealing or bag.
 
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Ian Grant

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Thank you :smile:


Yes, I read it, but in the same time a guy from other forum told that he had been provided this recipe by Ilford plant employee.

Ok, if I want to make powder developer and store it over couple of years, should I add Sodium metabisulphite (0.65g) ?

A:
Sodium sulphite 85g
Hydroquinone 5g
Phenidone 0.13g
Sodium metabisulphite (0.65g)

B:
Borax 7g
Boric acid 2g
Potassium bromide 1g


PS By the way, what is the point to split it into 2 different packs? Dilution temperature?

It's only split for dry packaging.

Ian
 
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Hey guys
I found such a recipe for Microphen and it seems to be the most correct:

Sodium Tripolyphosphate 3.4g
Sodium sulphite 100g
Sodium metabisulphite 0.65g
Hydroquinone 5g
Borax 6.8g
Boric acid 2.8g
Potassium bromide 1g
Phenidone 0.2g

If consider this recipe and split it into 2 packages what should be in pack A and B?

Have a look at the MSDS for microphen on Ilford s website for what is in parts A and B.

I can't remember what it is from memory.
 

Matroskin

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It seems that you have all the necessary powders. Why would you want to mix them now as Microphen or Autophen or ID-68 (it really doesn't matter) and store it mixed for few years? You can keep all powders separated in bottles for as many years as you want and mix them from time to time.

You're probably using the expression "store it over the couple of years" as a replacement for "mix and sell it without degradation problems" 🙂 . In case if you're thinking to mix some powders and pack it in ziplock bags for sale, you should be aware that metabisulfite won't solve the oxygen problems. Commercial powder kits are packed and sealed in a inert gas atmosphere and the metabisulfite is added only for the minimal oxygen exchange that can occur through sealing or bag.
Exactly, I store all reagents in the lab where I work and I'd like to have some prepared powder developers at home. Like I have several packs of D76 at home and when I need it I just add water and ready to go.

It's only split for dry packaging.
Yep, that's what I need :smile:

Have a look at the MSDS for microphen on Ilford s website for what is in parts A and B.

I can't remember what it is from memory.
Thanks.
They say pack A: Hydroquinone, 1-phenyl-3-pyrazolidone (i.e Phenidone), Sodium metabisulphite

To summarize:

A:
Hydroquinone 5g
Phenidone 0.13g
Sodium metabisulphite 0.65g (optional)

B:
Sodium sulphite 85g
Borax 7g
Boric acid 2g
Potassium bromide 1g
 

Alain Deloc

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Exactly, I store all reagents in the lab where I work and I'd like to have some prepared powder developers at home. Like I have several packs of D76 at home and when I need it I just add water and ready to go.

Phenidone won't mix like metol (from D76). You will have to stir a lot, even if the water is heated at 50-60 Celsius. D76 mixes very quick because of the metol, you just need some 50C hot water, and you're done in 2 minutes. If you want to have a convenient usage, you will have to mix your phenidone in propylene glycol, like 1 gram in 100 ml., and then add 10 or 13 or 20 ml of your solution in that water where you already dissolved the sodium sulfite, borax, bromide, etc.
 

Matroskin

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Phenidone won't mix like metol (from D76). You will have to stir a lot, even if the water is heated at 50-60 Celsius. D76 mixes very quick because of the metol, you just need some 50C hot water, and you're done in 2 minutes. If you want to have a convenient usage, you will have to mix your phenidone in propylene glycol, like 1 gram in 100 ml., and then add 10 or 13 or 20 ml of your solution in that water where you already dissolved the sodium sulfite, borax, bromide, etc.
Hmm, when I used Ilford miсrophen I don't remember any problems with solubility (it was only once long time ago..). Anyway thank you for the advice! And do you have an idea how stable is the solution of phenidone in propylene glycol?

Ps according to Ilford microphen box label it also contains Sodium Tripolyphosphate (may be also to prevent oxidation)

PPS My observations about oxidation: I store my reagents in sealed plastic containers and of cause there is some air inside. I open it from time to time to prepare powder developers and I didn't notice any problems with my developers over time. As I understand the main problem is a high humidity.


And I found some discrepancy in packages contents:

1) according to https://www.ilfordphoto.com/1173875 pack A contains: Hydroquinone, Phenidone, Sodium metabisulphite

2) according to MSDS https://www.ilfordphoto.com/wp/wp-content/uploads/2022/10/Microphen-Dev-PartA-J22.pdf pack A contains: Hydroquinone, Phenidone, Sodium metabisulphite, Boric acid
 
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Anon Ymous

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@Matroskin Sodium tripolyphosphate is there to take care of water hardness. Otherwise you'd get precipitate in most of the cases of tap water.


Phenidone in propylene glycol is stable for years in my experience. Assume a minimum of a year to be very safe.
 

Alain Deloc

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Hmm, when I used Ilford miсrophen I don't remember any problems with solubility (it was only once long time ago..). Anyway thank you for the advice! And do you have an idea how stable is the solution of phenidone in propylene glycol?

Ps according to Ilford microphen box label it also contains Sodium Tripolyphosphate (may be also to prevent oxidation)

PPS My observations about oxidation: I store my reagents in sealed plastic containers and of cause there is some air inside. I open it from time to time to prepare powder developers and I didn't notice any problems with my developers over time. As I understand the main problem is a high humidity.


And I found some discrepancy in packages contents:

1) according to https://www.ilfordphoto.com/1173875 pack A contains: Hydroquinone, Phenidone, Sodium metabisulphite

2) according to MSDS https://www.ilfordphoto.com/wp/wp-content/uploads/2022/10/Microphen-Dev-PartA-J22.pdf pack A contains: Hydroquinone, Phenidone, Sodium metabisulphite, Boric acid

Why do you care about the content of those packs? There is Microphen/ID-68 formula available, there is Autophen also. Make a pack of 5 grams of HQ, make another pack of everything else and have 1 gram pf Phenidone dissolved in glycol that can be measured with a 10ml. syringe. It's going to mix in 1 minute in warm water. Why is so important to clone Ilford packs?
 

Matroskin

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@Matroskin Sodium tripolyphosphate is there to take care of water hardness. Otherwise you'd get precipitate in most of the cases of tap water.


Phenidone in propylene glycol is stable for years in my experience. Assume a minimum of a year to be very safe.

Good to know, thank you.
Why do you care about the content of those packs? There is Microphen/ID-68 formula available, there is Autophen also. Make a pack of 5 grams of HQ, make another pack of everything else and have 1 gram pf Phenidone dissolved in glycol that can be measured with a 10ml. syringe. It's going to mix in 1 minute in warm water. Why is so important to clone Ilford packs?
May be because the is some logic in splitting it into 2 packs al long as my curiosity and perfectionism :smile:
 

Alain Deloc

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There isn't any particular logic. It's only for selling. That's why they are sealing the bags in inert gas atmosphere. If you are a perfectionist, you should measure and mix your powders separated. Keeping them pre-mixed it's already prone to errors. Ilford sells it in 2 bags because 3 bags would make the product harder to use for average amateur-photographer and sales would drop.
 

relistan

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MSDS sheets don’t have to list everything that is in the pack. Only the things that require labeling and are in an amount high enough (over 1% by weight I believe). So a slight change in the amount of boric acid, or new legislation requiring labeling would be the easy explanation for different MSDS sheets.

The important thing for storage longevity is to keep the alkali away from the developing agents, and to prevent either group from oxidizing. Here there are two packs and the one with the developing agents contains metabilsulfite (also acidic, like the developing agents) as a preservative. When mixed into the solution, the metabisulfite will also form part of the silver solvency for the developer.
 

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There will be a way to use microphen stock as a replenisher for itself like Xtol ?
 

Matroskin

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There isn't any particular logic. It's only for selling. That's why they are sealing the bags in inert gas atmosphere. If you are a perfectionist, you should measure and mix your powders separated. Keeping them pre-mixed it's already prone to errors. Ilford sells it in 2 bags because 3 bags would make the product harder to use for average amateur-photographer and sales would drop.
Actually there is :smile: Otherwise it would be one pack.
Of cause it's better to store separated, but not very handy.

MSDS sheets don’t have to list everything that is in the pack. Only the things that require labeling and are in an amount high enough (over 1% by weight I believe). So a slight change in the amount of boric acid, or new legislation requiring labeling would be the easy explanation for different MSDS sheets.

The important thing for storage longevity is to keep the alkali away from the developing agents, and to prevent either group from oxidizing. Here there are two packs and the one with the developing agents contains metabilsulfite (also acidic, like the developing agents) as a preservative. When mixed into the solution, the metabisulfite will also form part of the silver solvency for the developer.
That's a good point and quite consistent of what Ilford put in different packs
 

Alain Deloc

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Actually there is :smile: Otherwise it would be one pack.
Of cause it's better to store separated, but not very handy.


That's a good point and quite consistent of what Ilford put in different packs

There is, but only to minimize oxidizing during long periods of time. You don't need 2 packs. You can keep in 4, if you aim for perfection.
 

pentaxuser

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Anyway, this thread made me want to experiment with Microphen more. It beats the shit out of Xtol when processing Delta 3200 but I have not tried it for anything else.
It makes you wonder why Ilford ceased to make a replenisher for Microphen given its great economy when used that way?

A real pity for you, Steven. Ilford's price direct to the U.K. customer is now £8.28 and unless you use it 1+1 or better still 1+3 it remains relatively expensive. This is especially true when using higher speed films such as D3200 where Ilford give no times for anything other than stock. If its a 120 film that only 2 films per litre

That only leaves the re-use method where 10 films can be developed but as Ilford says, some inconsistencies in its action may arise and from another forum called FADU some experimentation may be needed on where in the 10 films an increase in the percentage time may be called for. From film 6 onwards times appear to increase dramatically by the addition of 90%

It isn't clear to me why it is not possible to replenish Microphen from stock as is the case with Xtol or is it but the quantities of stock replenisher is so large as to be uneconomical?

Can anyone help with the "why not"


Thanks

pentaxuser
 
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