Amidol soluble in TEA or Glycol?

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avandesande

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Gerald Koch said:
BTW, by creating a large volume of solution you create the potential problem of spills and the difficulty of cleaning them up. Trading one problem for another.

Handling liquids is preferable to handling solids 99% of the time. Any chemist will tell you this.

Gerald Koch said:
I would be inclined to look around for granular forms of these two chemicals.
Yeah right. Nobody seems to be able to find it at a reasonable price in any form.
 

Steve Hamley

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I have to agree with Gerald, having a similar background. Also, any chemical used as a dye in hair dyes is not likely to be immediately dangerous in gram quantities, although I concur it would be a bad idea to drink hair dye, developer, or use any chemical or chemicals in a manner that wasn't intended. As far as I can tell, amidol is simply a sensitizer or irritant at worst in any reasonable quantity and use.

MSDS precautions are also based on sort of "worst case" scenarios, to help protect emergency responders under accident conditions where large quantities may be airborne, releasing fumes or vapors from fire, and so on, hence the famous "Lava soap" MSDS. If I were responding to a burning tractor trailer wreck that had spilled a ton of amidol, I'd certainly want a Level A suit as I rescued the amidol. I'd want a newspaper covering my work surface in the developer mixing area and gloves in the developer tray.

That said, the Amidol I got from Artcraft is indeed more dense and granular than the stuff from PF, and contains khaki-colored lumps which appears to be the same thing - amidol. It also mixes up a rather orange color, darker orange than the lighter, fluffier, more consistently textured PF stuff. The Artcraft stuff is clearly filter cake. There's a thread over on M&P that said the Arcraft stuff stained prints, but I can't tell it compared to the same picture developed in any other developer (including PF amidol), including the base paper.

So maybe give the Artcraft stuff a try.

Steve
 

avandesande

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So i guess pipetting or filling a graduate over a sink isn't more sanitary or easier than pulling out a scale and weighing a solid.
 

Tom Hoskinson

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Steve Hamley said:
So maybe give the Artcraft stuff a try.

Steve

Been there, done that. My Artcraft amidol is fluffy and in solution it's blue.

I agree with avandesande's statement: "Handling liquids is preferable to handling solids 99% of the time. Any chemist will tell you this."
 

Steve Hamley

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I've done both, and sooner or later you will dribble or spill liquids and you will spill powders. Your handling practices and housekeeping are everything when it comes to chemical or radiological safety. I generally cover my work surface with newspaper and use a small paper on the balance pan. When I'm done weighing amidol powder, I take the small square of paper, slowly fold it up and pitch it in the garbage. When I'm done same for the newspaper and wipe the work surface.

You should of course, handle powders deliberately to avoid airborne dust - "spoon" it out of the bottle rather than shaking the bottle, etc. You should also handle liquids with care if you want to minimize spills or dribbles.

I just don't think it makes much difference for most photo chemicals if you have decent chemical handling technique and clean up when youre done.

Steve
 

Gerald Koch

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My comment about an amidol solution addressed the problem one would have if the bottle were dropped not in handling the solution. I would suggest investing in shatter proof glass bottles for all solutions of this type (amidol, pyro, ...) if you exceed several ounces total volume.
 

gainer

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Tom Hoskinson said:
"Would the amidol base, dissolved in glycol, be blue?"

Well, the amidol (2,4-diaminophenol dihydrochloride) that I've dissolved in glycol is certainly a very deep dark blue.

Maybe you've done it, Pat.

Then again, maybe you HAVE re-created Woad!
Then I should piddle on my woad and let it stand several days until it begins to smell like ammonia, than trample around in it to get it all properly mixed, according to an ancient recipe. And we worry about amidol?
 

gainer

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I have summarizing to do and more questions to ask. It occurred to me that if almost any base can separate the HCl from amidol, even one as mild as baking soda, why not TEA? All it needs to start is a little water. A very little. TEA is an analog in a way of ammonia, but not a gas. With water in the amount of 2 moles of water for one mole of amidol, in more than enough TEA to satisfy the balance of whatever reaction occurs, there should be the TEA equivalent of ammonium chloride and the amidol base and water as products. Will the TEA equivalent of ammonium diaminophenolate also form with the excess TEA? I don't know.

I put 10 grams of amidol and a few ml of water in a pyrex pitcher, stirred it to make a slurry, and poured TEA over it to make 100 ml. To paraphrase a pseudo folk song, black, black black is the color of my amidol, but it is not yet oxidized. Stuff settled out, but 5 ml of the clear part in 250 ml of water with half a tbs of sulfite made a nice honey colored solution that blackened a film snippet almost before I could get it out. I diluted the stuff with glycol up to 250 ml and it is still about as active as stock D-76 in the above proportions. There is still sediment, which I take to be mostly the chloride. It is just as well to leave it there as ammonium chloride is not what you want in a developer, so I don't suppose the TEA analog is either.

So now I have some kind of tar-like solution that I can treat as if it were 5% amidol, that clears when sulfite is added and alone will develop film, and I did not have to use caustic alkali. I think it will store well, as there is very little water in the solution. I doubt that it needs to be kept in glass. The only heat I had to use was enough to thin out the TEA. If it were the kind of tea you drink, you would probably send it back to be reheated. Use a little in PMK instead of a pinch of dry amidol. Use some in Pyrocat XX just to see what happens. Use it to make the world's finest developer for chloride paper.

The same treatment should work with metol.

My questions? I guess you can see that I'm not sure exactly what I produced, but only that it seems to be working as desired. I'm sure someone will tell me if I really have a fertile imagination or if I'm just full of equine excrement.

Now I'm going to try to get the stain off my hands. Whatever you do, do not mix Clorox with any kind of acid.
 

Tom Hoskinson

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Fascinating, Pat! Time for me to grab my jug of TEA and head for MY dungeon. I'll keep your methanol suggestion in mind, avandesande.
 

gainer

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avandesande said:
You could try a little methanol instead of water.
Why would methanol activate the alkaline behavior of TEA? If it would do that, propylene glycol might also.

The reaction with ammonia as I see it would be:
M H2SO4 + 2NH3 + 2HOH => M + (NH4)2SO4 + 2H2O, M being short for 2[4(methyl-amino)phenol].

It looks like the H2O cancels, but if you put NH4OH in you see that water is formed from the H in the hydrosulfate and the OH in the ammonium hydroxide. TEA is like the ammonia with all 3 H substituted by ethanol. It needs water to be like ammonium hydroxide.

TEA does appear to debase (my pun) metol and appears to cause less oxidation in the process. Just enough water to make a paste is all you need. Add TEA to make a 10% solution and warm it. Whatever the product is, dilute one part of it with 50 parts of about a 3% sodium sulfite solution and you have a pretty good developer.
 
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sanking

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gainer said:
TEA does appear to debase (my pun) metol and appears to cause less oxidation in the process. Just enough water to make a paste is all you need. Add TEA to make a 10% solution and warm it. Whatever the product is, dilute one part of it with 50 parts of about a 3% sodium sulfite solution and you have a pretty good developer.

How would making a paste and then adding the TEA differ from just adding a small amount of very hot water, dissolving the metol and then adding this to TEA? I have done this and the solution appeared to dissolve into the TEA with no problem, but later when the TEA cooled I could see that much of the metol had come out of solution.

Sandy
 

gainer

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sanking said:
How would making a paste and then adding the TEA differ from just adding a small amount of very hot water, dissolving the metol and then adding this to TEA? I have done this and the solution appeared to dissolve into the TEA with no problem, but later when the TEA cooled I could see that much of the metol had come out of solution.

Sandy
Are you sure that what settled out after cooling was metol and not the sulfate salt of TEA? For every 10 grams of metol you put in, about 3 grams of sulfate ion are released from the metol. The sulfate of TEA has quite a large molecular weight, and if it is not soluble in TEA it may look like a lot of metol settled out. Then too, the hot water may have oxidized some of the metol. You might try 10 grams of metol and a teaspoon or two of COOL water. Make it into a paste and add a little TEA. Work this around some and add enough TEA at room temperature to make 100 ml. In other words, keep the temperature down until the metol is well covered by the TEA. Stir it well and warm it to maybe 140 F. Let it sit for hours or until it cools and test the liquid for activity by mixing 5 ml of it in 250 ml of water with a teaspoon (about 8 grams) of sulfite. In my experiments, this solution is about as active as full strength D-23, an 8 minute developer for, say, HP5+.

The solution should be a light honey color. I made some last night and some a few days ago and both are still that color.
 

gainer

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There is a slightly different way to go about this. I calculate, based on typical 149.19 molecular weight of TEA supplied by Dow, that it would take 0.87 grams of TEA to release the base of a gram of metol and 1.57 grams to do that for amidol. That translates to 0.77 ml and 1.4 ml at room temperature. One could make the paste with, say, 7 ml TEA and 10 g metol and then add cool water. In theory, it would take only a little more than 1 ml to satisfy the equation for 10 grams metol or 1.9 ml for 10 grams amidol. Now the sludge or solution as the case may be should be about neutral. The rest of the 100 ml to make 10% could be TEA or glycol or an alcohol.
I cannot seem to find a way to make amidol solutions that don't look like the stuff that comes out of a lot of wells here in West Virginia. Of course, that stuff burns. No matter how black my amidol solution, it is a very potent developing agent. 1:100 dilution in 3% sulfite will develop HP5+ to normal contrast for diffusion enlargement, with a lot of density. Metol takes more.
 

gainer

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gainer said:
There is a slightly different way to go about this. I calculate, based on typical 149.19 molecular weight of TEA supplied by Dow, that it would take 0.87 grams of TEA to release the base of a gram of metol and 1.57 grams to do that for amidol. That translates to 0.77 ml and 1.4 ml at room temperature. One could make the paste with, say, 7 ml TEA and 10 g metol and then add cool water. ...
I meant that to say 8 ml. which is 7.7 in government terms. A heaping (this is possible with TEA) 1/2 tbs will do it. Half a tablespoon comes in most measuring spoon sets and is 7.5 ml.

It's like when I was a kid making mud pies and the like. When you add the tiny bit of water, 1/4 teaspoon, things change, but slowly. The paste gets semi-fluid so it won't hold a dimple...very long.
 
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sanking

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gainer said:
You might try 10 grams of metol and a teaspoon or two of COOL water. Make it into a paste and add a little TEA. Work this around some and add enough TEA at room temperature to make 100 ml. In other words, keep the temperature down until the metol is well covered by the TEA. Stir it well and warm it to maybe 140 F. Let it sit for hours or until it cools and test the liquid for activity by mixing 5 ml of it in 250 ml of water with a teaspoon (about 8 grams) of sulfite. In my experiments, this solution is about as active as full strength D-23, an 8 minute developer for, say, HP5+.

The solution should be a light honey color. I made some last night and some a few days ago and both are still that color.

OK, I mixed the metol with a little water, made a paste, and then added the TEA at room temperature. I did not heat it, but frankly everything appears to be in solution at this time. I will test it tomorrow. I think you are right in that the hot water caused oxidation.

Sandy
 
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sanking

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gainer said:
Now there is joy on Croagh Padraic!

Did you mean Croagh Padraig?

If so, how can anyone be happy in a place where the major gratification is flagellation?

Meanwhile, back in Easley, South Carolina, we found that the metol mixed in TEA according to your instructions worked nicely.

Sandy
 

Tom Hoskinson

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gainer said:
Now there is joy on Croagh Padraic!

Not a Snake or Frog anywhere in sight - maybe just a few faint echos from your bell, eh? St. Patrick?
 

gainer

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sanking said:
Did you mean Croagh Padraig?

If so, how can anyone be happy in a place where the major gratification is flagellation?

Meanwhile, back in Easley, South Carolina, we found that the metol mixed in TEA according to your instructions worked nicely.

Sandy
When you get to the pearly gates you can ask my father, Patrick Ward Gainer, why he named it thus. I'm not sure of the spelling, but he told me it meant "Patrick's Mountain". His doctorate was in philosophy and philology of English, from St. Louis University. His ancestors came from Ireland, where the name is now spelled Gainor, but when they came over in 1745, a county clerk or some recorder spelled it our way. The same sort of thing caused the Monongahela river to run through Monongalia county. He married Antoinette Kizinski who came from Poland when she was 5, and he learned Polish, so he said, in self defence. She spoke Polish and English both without accent.

I'm happy it worked for you.

An Irish lady friend told us once that St. Patrick got rid of all the pests in Ireland except the beer drinking Irishmen.
 

mohmad khatab

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It's probably not going to be used alone. The pH requirements depend lso on whatever is used with the amidol. I have done both, and prefer to use glycol because it allows playing with the alkali. The following is a pretty good developer.

10 grams ascorbic or erythorbic acid.
0.1 gram amidol
Propylene glycol to 100 ml.

!0 ml of this in 250 ml water will require 2 ml of TEA to work in a reasonable time. With 10 ml TEA it will develop HP5+ or whatever the current Arista II in about 6 minutes. In this case, of course, you can figure that almost 2 ml went to neutralize the ascorbic acid.
Dear brother ,,
This is an odd and inconsistent recipe.
Is it a one-shot recipe or what?
The amount of amidol in the recipe is very low (0.1). Is this number correct?
Written in the recipe (! 0 ml of this in 250 ml water will require 2 ml of TEA) and I wonder, what is meant by (0ml)?
Have you tested and tried that recipe?
- Please, the recipe needs more clarifications and explanations.
God bless you
 

Anon Ymous

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Dear brother ,,
This is an odd and inconsistent recipe.
Is it a one-shot recipe or what?
The amount of amidol in the recipe is very low (0.1). Is this number correct?
Written in the recipe (! 0 ml of this in 250 ml water will require 2 ml of TEA) and I wonder, what is meant by (0ml)?
Have you tested and tried that recipe?
- Please, the recipe needs more clarifications and explanations.
God bless you
Patrick Gainer passed away many years ago, so...
 
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