Mixing Paper dev help needed

[crypt]

Dear forum members, first some background story. Due to continued increase of taxes for imported goods I decided to become autonomous and to start mixing Paper Developers at home. I've got the Darkroom Cookbook and chemicals (hydroquinone is still on it's way). Now I lack a technic to mix the chemistry. I either will do

a) will warm water at home, use respirator and mix chemicals one by one right in to the water,
b) will go to some other place with good ventilation and mix everything in one portion, then bring it home and dilute.

The question is if it's possible to dilute everything at once? Our domestic seller often divide chemistry in two parts. I really want to know by what principle.

The recipe for start is

FORMULA #72 W130B

 Water at 125/52C, 750.0ml
 Metol,2.2g
 Sodium sulfite, anhydrous, 50.0g
 Hydroquinone, 11.0 g
 Sodium carbonate, monohydrate, 78.0g
 Benzotriazole, 0.2 g
 Glycin, 11.0g
 Water to make 1.0 liter

Any general advice how to make mixing in comfortable manner or where to read about it is welcome.

[Payral]

You have to dissolve products one by one in the formula order. Waite to product be completely dissolve before adding next one.

[koraks]

The question is if it's possible to dilute everything at once? Our domestic seller often divide chemistry in two parts. I really want to know by what principle.

Yes, you can mix it all in one go, provided you use the developer up within a fairly short period of time and keep it stored in such a way that no oxygen can get to it (entirely full and well-capped glass bottles work OK).

As to your idea of mixing separate 'portion' (concentrates) and then compounding them at home: yes, that's also a possibility, but you have to keep an eye on solubility limits and the keeping properties of the different chemicals. It's really simpler to just mix it all together in the right order.

When dissolving metol, dissolve a small pinch of sulfite in the water first, then the metol, then the rest of the sulfite. It greatly helps if the water is warmed up when trying to dissolve it. From the chemicals you listed, metol is one of the more challenging ones to dissolve. The others are easier, with the exception of benzotriazole. For the benzotriazole, I would just mix a 1% solution (1g in 100ml) and dissolve it completely (this may take a few days), and then add the appropriate amount of this concentrate to your developer (i.e. for 0.2g, you can add 20ml of your 1% concentrate).

It's not all that complicated, just follow the instructions and it'll work OK. And good to hear that you're cautious. I have to admit I do not use a respirator, but that's not to suggest that you shouldn't either.

[Pere Casals]

Any general advice how to make mixing in comfortable manner or where to read about it is welcome.

Try to stir and not shaking (like dry martini, 007) to not mix air in, this may have a relative importance but better in the Bond's way.

If you are to mix often then a magnetic stirrer is quite convenient, in special when you mix chem that's difficult to disolve, now we have those devices new quite cheap.

201934


As you are starting to mix, let me recommend you to compare 130 with this alternative in the same book: FORMULA #84 E-72 (Chris Patton) “Environmentally friendly” Dektol-type developer. You may adjust a warm vs cold tone by susbtituing Bromide vs Benzotriazole in the equivalent amounts, in the same way than Ansco 130 vs W130B.

[Alan9940]

I've mixed my own chemistry for many years, but just recently started using a magnetic stirrer; highly recommended! Regarding the 130 formula, I would advise ensuring fresh glycin. Good luck and have fun! Mixing your own formulas saves money and enables you to use developers no longer available commercially.

[JMO]

I've mixed my own chemistry for many years, but just recently started using a magnetic stirrer; highly recommended! Regarding the 130 formula, I would advise ensuring fresh glycin. Good luck and have fun! Mixing your own formulas saves money and enables you to use developers no longer available commercially.


I think it's best to keep your glycin tightly sealed and in the freezer. I have made EC-130 from raw chemicals for 3-4 years now, and have had no problems. It's great with either glossy or warm tone FB papers.

[Alan9940]

I think it's best to keep your glycin tightly sealed and in the freezer. I have made EC-130 from raw chemicals for 3-4 years now, and have had no problems. It's great with either glossy or warm tone FB papers.

Yep, that's what I do, too. I have some glycin that's, at least, 3 years old now (kept in freezer) and it's fine.

[chuck461]

Where do you folks get your Glycin? I'm wondering if there is a source besides the Formulary.

Thanks
CW

[Mick Fagan]

Crypt, possibly the best way to mix or stir photo chemistry, is to use a Patterson chemical mixer. I have used these for around 35 years, on my second one now, they are very good as the bottom is flat which enables you to crush solid lumps of chemicals. This mixer works perfectly in any photographic measuring graduate, or most plastic cooking jugs you can buy from a supermarket cooking accessories section.

https://www.patersonphotographic.com/product/paterson-chemical-mixer/

As for your second question about halving, I assume you mean mixing up 500ml instead of 1 litre. This is simple, you would measure Metol 1.1gm, Sodium Sulphite Anhydrous 25.0gm and so on, with the end result that you have 500ml of solution. With 500ml of solution you can mix this with 500ml of water to make up 1,000ml of working paper developer for your tray and at the end of the session you can discard the developer or keep it in tightly closed containers with no air. I use glass marbles to remove as much air as possible, this has worked for me for over 50 years.

Mick.

[Alan9940]

Where do you folks get your Glycin? I'm wondering if there is a source besides the Formulary.

Thanks
CW

I get mine from the Formulary, but I request fresh powder when ordering. Who knows how fresh it really is, but I've never had any problems with it.

[Mick Fagan]

Just re-read you question, mixing chemistry in powder form does require you to be a bit careful. In an ideal world you would have a clean air supply across your face, a powered clean air mask is one solution. But living in the real world, you could mix your chemistry in a very well ventilated place, or even mix it outside, providing there is no wind.

Wearing a face mask is probably one of the safer ways to mix powdered chemicals.

You may not have a set of scales, this would be required to measure your chemistry into different amounts. A cheap set of electronic scales should be alright, if you really get into mixing your own chemistry from bulk purchased chemicals, then by that time you would have an idea of what kind of scales you may find best. I myself have a triple beam set of scales, no batteries, no electronics, just weights. I've had my current scale set for maybe 30 years, they will see me out.

https://en.wikipedia.org/wiki/Triple_beam_balance

Mick.

[Pere Casals]

Where do you folks get your Glycin? I'm wondering if there is a source besides the Formulary.

Thanks
CW


Glycin is an orphan chemical with no other "industrial" photo production known beyond Photographer's Formulary, CAS number is 122-87-2 , it is also made in very expensive reagent grade by Merk / sigma aldrich: https://www.sigmaaldrich.com/catalog/search?term=122-87-2&interface=CAS%20No.&N=0&mode=partialmax&lang=es&region=ES&focus=product

[crypt]

WoW! Guys! You are so helpfull! Thanks a lot! Sorry I didn't replied for a few days, I was mixing and testing:) At the moment I'm using room out of my home with a very strong ventilation. The air pressure is so strong, you have trouble to open the door. No, it's not chemistry lab unfortunately, but it feels much safer. Especially Benzotriazol has a very strong smell, I thought it may be poisonous at home.:)

My current results are not very satisfactory. I mixed three different fomulas and they all went out dark colored like Rodinal.:( Either water is too hot, or I hadn't patience to dissolve everything. Maybe something other is wrong. Today I will try to be more systematic and write you later.


I shook the bottle and now I will try to stir. Also today I will try Ansel Adams variant of Ansco 130, divided in two parts. Chances are that it will dissolve better while on a shelf.

While I'm already aware about Metol/Sodium Sulfite trick, it was new to me that Glycin may need some additional treatment. Could you please tell my why so? All the chemistry I've got in plastic bags and plastic cans. Far from hermetic. I don't currently have special glass bottle to keep all these 8 components... What do you advise?

I have some doubts about Potassium bromide which is in one big piece and it probably absorbed water. Also I found it started to darken here and there. Also need special treatment?

Anyway how long do you usually wait before something is dissolved?

> For the benzotriazole, I would just mix a 1% solution (1g in 100ml) and dissolve it completely (this may take a few days),

Wow! A few days?! I was so urgent to try, it didn't come to my mind! I will definitely try this trick. Does it make difference if I dissolve it with Sodium Sulfite (like in Adams formula) or alone (like in other recipe)?


--

Regards,
Konstantin

[crypt]

Just re-read you question, mixing chemistry in powder form does require you to be a bit careful. In an ideal world you would have a clean air supply across your face, a powered clean air mask is one solution. But living in the real world, you could mix your chemistry in a very well ventilated place, or even mix it outside, providing there is no wind.

Mick.

Thank you Mick, I'll keep it in mind. At this point I'm in a temporary situation and don't want to make it more expensive. If I found something that works approximately the same as ID MG, I will optimize the process. I would be happy just using Ilford Multigrade dev, but my current place of living means two things. Firstly domestic regulations (aka greed) make it harder and harder to order something from abroad. Secondly it needs about 3 weeks to get something (and you don't want to know the cost of delivery). And I'm expecting to print often, but not that much in regards of paper meters. These means I start using a working solution and soon it became dark just because waits for next session. My own stock supposedly will help.

Currently I've borrowed cheap Chinese scales from friend. Well, it says 0.1 precision. I have trouble to weight small amounts like 0.2 benzotriazol, but at least I can try the idea in general.

> mix it outside, providing there is no wind.

Not an option. Windy as hell. Also ... wait, I have a photo... Here! Snow in May! https://www.flickr.com/photos/crypt47/34272223552/in/dateposted-public/

[Pere Casals]

> For the benzotriazole,

does it make difference if I dissolve it with Sodium Sulfite (like in Adams formula) or alone (like in other recipe)?



It dissolves better in mild alkali, if you add it in the order stated in the formula then the soup is alkaline by then.

For darkroom mixing you may find suitable having a 0.001gr scale, this is $15, and a Weight calibration set, $10.

Checking scale calibration is very good practice, some dirt particle may obstruct the platform movement of the 0.001gr scale, or other issues may happen.

202010

Me, I use two scales, a larger one and a 0.001grs precision one. A 0.01gr scale may introduce a 10% error in a 0.2g dose. Of course you may also dilute chem in a liquid for an easier dosing, but many times a precision (cheap) scale is the most convenient.

Try to handle powders with care an use a face mask (covid-19 type :)), safety first. Read some general darkroom safety literature, no hazard if following rules with some common sense.

[crypt]

What I see at this point, Metol is oxidizing very fast and makes the solution purple. A 'pinch' of sodium sulfite seems to be not enough. I've added a bit more - better, but gradually darkens anyway. After adding full portion of Sodium Sulfite it continues to darken... Confused... I'm using so called distilled water for cars and have the last liter. What should I do?

[koraks]

Metol does not oxidize that fast in water, not even without any sulfite present. Are you sure it's distilled water and not battery acid you're using? ;)

[crypt]

Metol does not oxidize that fast in water, not even without any sulfite present. Are you sure it's distilled water and not battery acid you're using? ;)

Well, I don't know what to think! It was sold as CAS rn 55-55-0 and the title says Metol 99%. Maybe it have to be 99.8%? The water is marked as distilled and solution is totally dark. Will now try water from tap just to check.

Used 4.5 g of sodium sulfite. Then this 'Metol'. It dissolves very easily. Maybe it's not metol at all.

[crypt]

Metol does not oxidize that fast in water, not even without any sulfite present. Are you sure it's distilled water and not battery acid you're using? ;)

Will the seller, though without much hope. What about Potassium bromide? The seller tells it becomes darker on sunlight. But I only opened the can when mixing. Does it really goes that fast? I've made a photo of Metol while it's not too dark 202017 Strange color, isn't it?

[koraks]

Yeah, that's very odd. I've never seen metol in solution go that color. It goes a pale straw yellow with time in a neutral to slightly acid solution, or brown in an alkaline solution.
Your potassium bromide looks weird too; mine also has some discolorations, but that's because of minor contamination with developer compounds which oxidize and give a brown coloration to it. The potassium bromide itself should not change color. Hence, I suspect yours is quite severely contaminated with something that oxidizes.

I don't know what's going on there, to be honest. If you mix a small amount of developer this way (accepting that it turns weird colors), does it actually develop paper at all?

[crypt]

Yeah, that's very odd. I've never seen metol in solution go that color. It goes a pale straw yellow with time in a neutral to slightly acid solution, or brown in an alkaline solution.
Your potassium bromide looks weird too; mine also has some discolorations, but that's because of minor contamination with developer compounds which oxidize and give a brown coloration to it. The potassium bromide itself should not change color. Hence, I suspect yours is quite severely contaminated with something that oxidizes.

I don't know what's going on there, to be honest. If you mix a small amount of developer this way (accepting that it turns weird colors), does it actually develop paper at all?

When I use darkened solution it works somehow (dark brown tones, lith-like look mostly), but since there are several active developers I'm not sure which works. I believe I have to get as much information as I can before posting here. And make some photographs for you to see.

The test I've made so far:
* Tried Glycin only formula. (Substituted Potassium Carbonate with Sodium Carbonate) Glycin only mix. SS: 50g, SC: 48g, G: 8g. - Dilution clean, but doesn't work, paper doesn't darken.
* When some HQ solution added to the above the solution becomes colored at once so as the paper. Presumably HQ works as super-additive, but for some reason changes it's color. The color is dark-purple.
* HQ only solution first has light-yellow color but to the next day becomes bright-red.

I will repeat test with metol only solution and make a photo.

As for the potassium bromide the seller made an excuse like it usually becomes darker when present on the light. Though I've kept it in the dark mostly. I'll use your suggestion to place it another bag. Anyway, PB is cheap, but metol is the most important component.

[Bernard_L]

You state in your OP that cost matters. Yet you chose a glycin formula. Gycin is expensive. And has a limited shelf lifetime in powder form.

Internet is full of claims about this or that "wonderful" developer; you will also find professionals with lots of experience who rely on an "ordinary" developer, e.g. Dektol. Why don't you start with D-72, similar to Dektol, or ID-62, an Ilford formula PQ formula similar to Bromophen? These formulas were finalized by teams of professional chemists at Kodak or Ilford, not by an enthusiast trying to do "something different".

and now i start to run before the Gycin and Amidol crowds catch me

[Pere Casals]

lots of experience who rely on an "ordinary" developer

I agree, beyond colder-warmer tone... I see a very limited impact of the paper developer choice in the image control, as we usually develop to completion. Many other factor have a deep impact in the image, but what was not done with those factors it would be very difficult to control with paper developer choice.


IMO, since Variable Contrast paper popularization (many decades ago) there is less a need to go beyond "ordinary" developers.


Personally, I consider two factors in a paper developer:

> Tone modification, depending on developing agents we get a warmer or colder tone... > but anyway it is the paper type what rules... and if we later use a toner then the toner is the key, in fact. Also the kind or restrainer has an effect (Benzo vs Br)

> Amount of restrainer, using more or less restrainer it modifies the paper toe that's responsible for the highlights, but again the natural paper curve is very important.


IMHO it's not necessary to go much beyond ordinary developers to have all that control, by selecting an ordinary warm/cold tone soup, and adding some benzotriazole/bromide if wanting to cut toe for an effect in the highlights.

At least, IMO, no paper developer is a magic bullet, what counts is knowing what we want in an image and mastering the tools we have at hand. So, personally, I prefer a ECO one.

[crypt]

You state in your OP that cost matters. Yet you chose a glycin formula. Gycin is expensive. And has a limited shelf lifetime in powder form.

Internet is full of claims about this or that "wonderful" developer; you will also find professionals with lots of experience who rely on an "ordinary" developer, e.g. Dektol. Why don't you start with D-72, similar to Dektol, or ID-62, an Ilford formula PQ formula similar to Bromophen? These formulas were finalized by teams of professional chemists at Kodak or Ilford, not by an enthusiast trying to do "something different".

and now i start to run before the Gycin and Amidol crowds catch me

As I've written above, I have some weird problem with metol. It doesn't behave like it should. And it needs about 3 weeks to get any new chemicals here. Also the virus situations adds more time. That's why I tried something different with what I have. As for the price in my case, Glycin costs 5 time less then Metol and only 2 times more then PB. So actually it's not _that_ expensive here. And it would be great if I found a recipe that works without metol and phenidone. But it doesn't work. May be because I've tried to substitute PC with SC. As for ID-62, Phenidone is what's really expensive. And it's hard to get cause it doesn't used in other industries and hence seems to be not produced widely anymore.

[Bernard_L]

But it doesn't work. May be because I've tried to substitute PC with SC.
No way. Should be equivalent, provided you substitute mole for mole; and even if you just take the same mass, you should have a working developer

As I've written above, I have some weird problem with metol. It doesn't behave like it should.

As for the price in my case, Glycin costs 5 time less then Mitol and only 2 times more then PB.

Are you sure you are being sold good quality chemicals? Or outdated, oxidized chemicals? Or "technical" grade chemicals with impurities that are fatal for your intended photographic use?
Why not start with a clean slate, a different supplier of chemicals. You do not state where you reside; I had a look on fotoimpex (probably the best-stocked photo store in Europe) and they have shipping restrictions to many countries for "dangerous" chemicals like Dektol in powder form(???:confused:). But here are two possible sources for raw chemicals; I have reasons to believe that either of them might be less fussy about shipping regulations than regular photo stores.

https://www.moersch-photochemie.de/content/rohchemie
(this does not appear in the English language version)
http://moersch-photochemie.de/moersch/webroot/files/Preisliste_online_2018final.pdf
E-Mail: fotosuvatlar@live.de ask them if they will ship to your country.
They even have ingredients for making your own color developers.

Also:
https://keten.com.pl/
They used to have all the usual developing agents, now only hydroquinone, but they state:
If you do not see something, please visit the old page HERE or CONTACT US. The list is updated on a regular basis.
The old page is a broken link, the contact is: office@keten.com.pl


And it needs about 3 weeks to get any new chemicals here. Also the virus situations adds more time.
That is a fact you cannot change. Your time (experiments with doubtful chemicals) also is valuable, I guess.

[crypt]

No way. Should be equivalent, provided you substitute mole for mole; and even if you just take the same mass, you should have a working developer


Thanks, I've checked everything again. It's not Glycin that I've used, it's glycinE. :(




Are you sure you are being sold good quality chemicals? Or outdated, oxidized chemicals? Or "technical" grade chemicals with impurities that are fatal for your intended photographic use?


Well... There are some figures about purity on cans (you can on the photo above), but seller is untrusted.

With help of this thread (https://www.photrio.com/forum/threads/home-made-d76-with-raw-chemistry.53129/page-2#post-775919) I did 3 cases:

a) SS + HQ + M - This should prevent Metol from oxidizing and also restores it. The solution darkens, maybe because HQ restores M but oxidizes itself.

b) SS + M - This shouldn't restore Metol, but should prevent from oxidizing. It does not. The solution darkens. Bad 99% SS?

c) M + citric stop bath - the most stable solution, doesn't become dark. Metol is not active this way, but addition of PB disables acid. So it's only to keep it in two solutions and for development of film. After mixing the solutions becomes dark. Nothing like D76 from store.





Why not start with a clean slate, a different supplier of chemicals.

Not happy to spend more money for testing honestly. But have a little choice. Anyway the store I was going to use doesn't work because of moratorium till 3d of April. So I have time to think and thanks for the links. Soon ordering from EU willn't be an options because of the taxes, but for now it's fine. Taxes changes gradually.

[Bernard_L]

a) SS + HQ + M - This should prevent Metol from oxidizing and also restores it. The solution darkens, maybe because HQ restores M but oxidizes itself.
Still something abnormal. Not buying your explanation. The first stages of preparation of D-76 are:
- pinch of sulfite
- Metol (2g)
-all the sulfite (100g)
- Hydroquinone (5g)
Note that you are not supposed to dissolve the main part of the sulfite first.
I've mixed D-76 numerous times, last time 2 days ago, and the liquid remains clear. Water at 50°C. Stir and dissolve completely each chemical before adding the next. Do not shake, and if using an electric stirrer make sure you do not create a vortex; reason: to avoid oxidizing prematurely your developer. Advice already given by other posters earlier in this thread.

The solution darkens. Bad 99% SS?
I would more readily suspect the Metol than the Sodium sulfite. From US patent 2,686,718:
Various suggestions have been made to in prove dry packages of developers. The developing substance such as hydroquinone, pyrogallol, monomethyl paraminophenol (metol) and other organic developing agents are easily oxidized in storage, particularly in the presence of humidity, the slightest degree of oxidation showing up as discoloration.
My own metol powder tends to darken, but still works, and dissolves into a clear solution. On the other hand, sulfite in storage remains a pure white powder. Of course, there might also be an impurity "X" in the sulfite.

If you replace suspect chemicals one at a time, you will spend substantial time. And extra money, because of shipping costs. This is why I suggest to take a clean start.

Good luck.