decontruction of Microphen

Recent Classifieds

Forum statistics

Threads
199,124
Messages
2,786,531
Members
99,818
Latest member
Haskil
Recent bookmarks
0

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
Hi there,
I got so much knowledge lurking into the discussions in this forum, and it is time I start sharing some of mine. I wanted to have some sort of reference developer with the idea of using it occasionally, and commercial Microphen seemed like a perfect candidate.

Commercial Ilford Microphen powder for 1 liter contains, according to the MSDS,
Part A (13.47 g) hydroquinone, phenidone, boric acid, sodium metabisulfite
Pat B (117.35 g) sodium sulfite, borax, sodium tripolyphosphate, potassium bromide

Obviously Ilford added chelator and sodium metabisulfite to the formula of ID-68, to protect hydroquinone and phenidone from oxidation during dissolution of Part A at high temperature. Thus, there is more borax in part B to compensate for added bisulfite. Its amount is somewhat uncertain since it comes in several hydrated forms, and it is unknown which one Ilford used. I thought this formulation is a perfect candidate for a two solution “long-lived” developer that can be prepared without any additional chemicals (well, not quite, read on).

First, I warmed 200 ml of water to 50 degree Celsius, and attempted to dissolve Part A contents in it. Some pellet remained, which is likely phenidone, so I carefully decanted most of the solution into another jar, and added 10 ml of rubbing alcohol, and after slight mixing the pellet dissolved. I returned the remainder of the Part A solution into this jar and mixed. The resultant concentrate is clear and colorless, is 5X with regard to the stock developer and contains ~3.5% isopropanol. This solution has pH of 5. It was distributed into 4x50 ml tubes, each of 3 filled to the top, and the last one had 20 ml left.

Solution B, containing a lot of sulfite cannot be concentrated, so it was dissolved in 800 ml volume and was dispensed in glass beer bottles with rubberized spring-latch caps, 400 ml each.

For preparation of working developer one needs to mix 50 ml of solution A and 200 ml of solution B.

For 1:1, take 125 ml water, 25 ml solution A and 100 ml solution B. Given that the stock is rated for 10 films, using 1:1 as one shot allows to develop 8 films, using every time a fresh solution. So far this works perfectly after 3 months and counting. Both solutions are still colorless and the development time is the same. Example: Kentmere 100, 10 min at 20 C in 1:1.

Now, obviously, this principle could be applied to a variety of powder developers of the same family (D-76, ID-11, Perceptol etc), but I have no interest in testing all of them. Incidentally, this two-solution preparation also opens a venue for additional experimentation, as in how this developer would work in the near absence of sulfite, with different alkaline buffers and so on. I hope someone would find this helpful.
 
Last edited:

trendland

Member
Joined
Mar 16, 2012
Messages
3,398
Format
Medium Format
Hi there,
I got so much knowledge lurking into the discussions in this forum, and it is time I start sharing some of mine. I wanted to have some sort of reference developer with the idea of using it occasionally, and commercial Microphen seemed like a perfect candidate.

Commercial Ilford Microphen powder for 1 liter contains, according to the MSDS,
Part A (13.47 g) hydroquinone, phenidone, boric acid, sodium metabisulfite
Pat B (117.35 g) sodium sulfite, borax, sodium tripolyphosphate, potassium bromide

Obviously Ilford added chelator and sodium metabisulfite to the formula of ID-68, to protect hydroquinone and phenidone from oxidation during dissolution of Part A at high temperature. Thus, there is more borax in part B to compensate for added bisulfite. Its amount is somewhat uncertain since it comes in several hydrated forms, and it is unknown which one Ilford used. I thought this formulation is a perfect candidate for a two solution “long-lived” developer that can be prepared without any additional chemicals (well, not quite, read on).

First, I warmed 200 ml of water to 50 degree Celsius, and attempted to dissolve Part A contents in it. Some pellet remained, which is likely phenidone, so I carefully decanted most of the solution into another jar, and added 10 ml of rubbing alcohol, and after slight mixing the pellet dissolved. I returned the remainder of the Part A solution into this jar and mixed. The resultant concentrate is clear and colorless, is 5X with regard to the stock developer and contains ~3.5% isopropanol. This solution has pH of 5. It was distributed into 4x50 ml tubes, each of 3 filled to the top, and the last one had 20 ml left.

Solution B, containing a lot of sulfite cannot be concentrated, so it was dissolved in 800 ml volume and was dispensed in glass beer bottles with rubberized spring-latch caps, 400 ml each.

For preparation of working developer one needs to mix 50 ml of solution A and 200 ml of solution B.

For 1:1, take 125 ml water, 25 ml solution A and 100 ml solution B. Given that the stock is rated for 10 films, using 1:1 as one shot allows to develop 8 films, using every time a fresh solution. So far this works perfectly after 3 months and counting. Both solutions are still colorless and the development time is the same. Exanple: Kentmere 100, 10 min at 20 C in 1:1.

Now, obviously, this principle could be applied to a variety of powder developers of the same family (D-76, ID-11, Perceptol etc), but I have no interest in testing all of them. Incidentally, this two-solution preparation also opens a venue for additional experimentation, as in how this developer would work in the near absence of sulfite, with different alkaline buffers and so on. I hope someone would find this helpful.

Yes - why not. Be sure there might be people here who find this helpful.
To me one question is of very special interest : " Have you intention to create your own developer from homebrew chems later ?"

with interest
 
OP
OP

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
My intentions are of a more general type, like finding out if one can dispense with copious amounts of sulfite and/or carbonate/borate. I am currently looking at a chemical called THAM (tris-hydroxymethyl-aminomethane), which acts as a restrainer and an alkali at the same time. Kind of a paradox, right? At this point I am pretty far from anything that qualifies as "my own developer" but I may be trying to reincarnate some forgotten ideas of the past.
 

faberryman

Member
Joined
Jun 4, 2016
Messages
6,048
Location
Wherever
Format
Multi Format
Interesting. What are you trying to achieve with your experiments?
 
OP
OP

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
Ultimately, I think, to get rid of some persistent myths in photochemistry.
 

Rudeofus

Member
Joined
Aug 13, 2009
Messages
5,081
Location
EU
Format
Medium Format
Restraining action of THAM is something I have not heard of, and which would not make a whole lot of sense to me either. It's a primary amine after all, so it should have moderate solvent property, which typically translates into acceleration, not restraint of development action.

One thing which is most definitely not a myth: you need Sulfite if you want to mix a normal photographic developer that uses Hydroquinone as main developer. There may be patents for photographic developers, where Sulfite is replaced by other Oxygen scavengers, there are developers which don't need Sulfite at all, but neither trick will work with MQ or PQ type developers.
 
OP
OP

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
Thank you, Rudeofus, especially for the links. However, since patents were filed mostly by companies interested in commercial production, there seems to be a historical bias towards research that produced one-bottle solution capable of long term storage. Keeping the alkaline part separately always seemed like too much of a hassle. I only made a few experiments so far, but the trick of replacing part B of Microphen entirely with THAM actually works, even though one needs a longer development time to get box speed. Since THAM can be adjusted to any pH between 11 and 7, there are plenty of possibilities.
 

Gerald C Koch

Member
Joined
Jul 12, 2010
Messages
8,131
Location
Southern USA
Format
Multi Format
The formula for Microphen was never disclosed however Ilford did publish the formula for a similar developer Autophen. As you have probably found out an MSDS does not give specific amounts but rather ranges and is not that helpful when trying to construct a formula.
 
OP
OP

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
The formula for Microphen was never disclosed however Ilford did publish the formula for a similar developer Autophen. As you have probably found out an MSDS does not give specific amounts but rather ranges and is not that helpful when trying to construct a formula.

Gerald, I am not trying to emulate Microphen, so its exact composition is not important. In fact, in part A published weights of components add up within the margin of error, but part B weighs a good 10 g more than I would expect. The point is, part A as such can be used both in the two-part original formula as a reference and in new combinations with different alkaline components. For example, it was an easy way to find out how this PQ combination operates in the near absence of sulfite.
 

Rudeofus

Member
Joined
Aug 13, 2009
Messages
5,081
Location
EU
Format
Medium Format
Thank you, Rudeofus, especially for the links. However, since patents were filed mostly by companies interested in commercial production, there seems to be a historical bias towards research that produced one-bottle solution capable of long term storage. Keeping the alkaline part separately always seemed like too much of a hassle. I only made a few experiments so far, but the trick of replacing part B of Microphen entirely with THAM actually works, even though one needs a longer development time to get box speed. Since THAM can be adjusted to any pH between 11 and 7, there are plenty of possibilities.
pH is not the only thing determining properties of a developer, you also need to look at buffer capacity, and at buffer capacity over pH. Fortunately you don't need such a thing. Tripotassium Phosphate, Potassium Hydroxide and Potassium Metabisulfite are much more soluble than Trisodium Phosphate and Sodium Sulfite, so you could easily formulate a decent concentrate as stock solution B.
 
OP
OP

Pixophrenic

Member
Joined
Mar 30, 2017
Messages
370
Location
Canada
Format
Multi Format
Where did you get the idea of THAM?
Possibly it has never been investigated.
Is it difficult to obtain?

I think it may have never been investigated as it used to be hard to obtain, but not anymore. Today it is a common chemical in medical investigations and tests. Mike from Artcraft said he could source it, if needed. I can't be sure for the rest of the world, but all regular lab reagent suppliers should carry it. The working concentration is in the order of 1 g/L.
 

Rudeofus

Member
Joined
Aug 13, 2009
Messages
5,081
Location
EU
Format
Medium Format
THAM is quite present in older patent literature, but only as an antioxidant and as alkali. I am still not sure what Pixophrenic expects from it. It will not replace sulfite in a PQ type developer, period.
 
Joined
Jul 28, 2016
Messages
2,770
Location
India
Format
Multi Format
the trick of replacing part B of Microphen entirely with THAM actually works, even though one needs a longer development time to get box speed. Since THAM can be adjusted to any pH between 11 and 7, there are plenty of possibilities.

Just curious to know. Was there any further progress in using THAM?
 
Photrio.com contains affiliate links to products. We may receive a commission for purchases made through these links.
To read our full affiliate disclosure statement please click Here.

PHOTRIO PARTNERS EQUALLY FUNDING OUR COMMUNITY:



Ilford ADOX Freestyle Photographic Stearman Press Weldon Color Lab Blue Moon Camera & Machine
Top Bottom