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  1. #81

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    Quote Originally Posted by Kirk Keyes View Post
    Temperature affects the rates of ALL reactions.
    The rule of thumb is that for every 10C increase in temperature, the reaction rate doubles. So a reaction at 30C will be twice as fast as one at 20C.
    Also, for precipitation, temperature affects solubility, so that affects the concentration that precipitation begins.
    Rule of thumb, solids are more soluble in water as the temperature increases. (The opposite is true for gases dissolved in water.)
    Kirk, you were right! I re-ran the precipitation-experiment at 20C (instead of 30C), and sure enough, slight cloudiness became visible after 40 min instead of 20 min. That means at 24C, it'll be 30 minutes, so this rule applies to the concentrate:
    "If using hard tap-water, develop promptly, making sure development is finished within 30 minutes after mixing."

    But I'd like to do better than that, so I'll investigate chelating agents.

    I also waited one hour and then developed a test-strip to see what harm this cloudiness does. I'll scan it in 1-2 days.

    @Relayer: I haven't forgotten your request to test your modified formula. I'd like to in a few days as time permits.

    Mark Overton

  2. #82

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    Quote Originally Posted by albada View Post
    @Relayer: I haven't forgotten your request to test your modified formula. I'd like to in a few days as time permits.
    thanks.

    I was still experimenting with my borax-carbonate version. LegacyPro 400 5.5min look ok. my other experiment is decreasing amount of sodium sulphite from 90g/l to 30g/l. amount of borax is same, but I need increase amount of carbonate for correct pH 8.3. formula:

    Sodium sulfite 30g
    Phenidone 0.1g
    Ascorbic acid 8.5g
    Borax 6.3g
    Sodium carbonate 3.3g
    Water 1l
    pH=8.3

    compared to 90g/l version this developer give less density for same time. more grainly, but sharpness is excellent. sample images for LegacyPro 400 5.5min in attach

    Click image for larger version. 

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  3. #83

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    Thanks for the work on this, I've wanted to try XTOL but making 5 ltrs is impracticable. I'm about to purchase the chemicals and the Sodium Metaborate (Kodalk) I can obtain is 8 mol. Could you advise on any correction to the amount of this to use, although I did Chemistry that was over 35 years ago!

    Many Thanks.

  4. #84

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    Quote Originally Posted by Relayer View Post
    I was still experimenting with my borax-carbonate version. LegacyPro 400 5.5min look ok. my other experiment is decreasing amount of sodium sulphite from 90g/l to 30g/l. amount of borax is same, but I need increase amount of carbonate for correct pH 8.3. formula:
    Sodium sulfite 30g
    Phenidone 0.1g
    Ascorbic acid 8.5g
    Borax 6.3g
    Sodium carbonate 3.3g
    Water 1l
    pH=8.3
    compared to 90g/l version this developer give less density for same time. more grainly, but sharpness is excellent. sample images for LegacyPro 400 5.5min in attach
    Sulfite helps the developer to develop faster, so when sulfite is reduced, density will decrease, even at the same pH. You need to develop longer if using low sulfite.

    6.3 g of Borax has the same number of boron atoms as 6.7 g of metaborate, but it has much fewer moles of molecules, so I think buffering will be worse. I suggest increasing acid and alkalis to improve buffering like this:
    sulfite=90, ascorbicAcid=9, borax=10, s.carbonate=??, phenidone=0.1
    Adjust s.carbonate to give pH=8.3. More than 10g of borax would be better, but it might take too long to dissolve.

    The left scan in your images looks like the scanner was slightly out of focus. It is difficult to focus scanners accurately to measure grain. Can you re-scan that negative with manual focus on that part?

    Mark Overton

  5. #85

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    Quote Originally Posted by richydicky View Post
    Thanks for the work on this, I've wanted to try XTOL but making 5 ltrs is impracticable. I'm about to purchase the chemicals and the Sodium Metaborate (Kodalk) I can obtain is 8 mol. Could you advise on any correction to the amount of this to use, although I did Chemistry that was over 35 years ago!
    Many Thanks.
    Firstly, Welcome to apug! (I notice this is your first posting).

    You'll need 9.1 g of sodium metaborate 8 mol.
    The ratio of the molecular weights of 8 mol and 4 mol = 137.88/101.83 = 1.354, which multiplied by 6.7 gives 9.1.
    8 mol contains more water than 4 mol, so if you're mixing it into propylene glycol, I suggest letting it sit for 15 minutes at 90C to steam-out the water.
    Don't let it get much over 90C or the PG itself will evaporate. Don't ask how I know.

    Mark Overton

  6. #86

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    Tap-water scan

    Here are full-resolution (2900dpi) neg-scans of photos of a Stouffer wedge shot on TMY2. The left scan was developed in distilled water, and the right in a tap-water solution that was allowed to sit for one hour at 20C before usage. It had some cloudiness visible in specular side-lighting, which was the beginning of precipitation.

    Distilled: Click image for larger version. 

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    Yes these pictures are boring. But I don't see any degradation in the dark or light areas in the right scan. Nor do I see any issue in a 22X loupe on the light-table. The cloudiness appears to have had no effect. If waiting an hour doesn't hurt anything with hard tap-water, I'm questioning whether it's worth putting a chelating agent into this one-shot formula. I guess I should run more tests to see how severe the cloudiness must be before it affects image-quality.

    Mark Overton
    Last edited by albada; 07-25-2012 at 01:49 AM. Click to view previous post history.

  7. #87

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    What's in your tap water? Your local water bureau can tell you that. PE has said that Kodak had water with extra minerals found in some municiple waters on tap for use in their lab testing!

  8. #88

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    Quote Originally Posted by Kirk Keyes View Post
    What's in your tap water? Your local water bureau can tell you that. PE has said that Kodak had water with extra minerals found in some municiple waters on tap for use in their lab testing!
    According to my shower, plenty of calcium. We get an annual report from the water district, and I'll look closer next time.

    Last night, I let tap-water-based developer sit for an hour at 30C, which is roughly equal to two hours at 20C (thanks again for that correction). The test-strip shows no sign of speckling, despite obvious cloudiness in the dev. BTW, the precipitation was still staying in suspension, so it hadn't gotten far enough along to start settling to the bottom. This dev will be used soon after mixing, so I don't think any precipitation will progress enough to cause harm.

    But remember that white cloudiness and scale in the concentrate (not water-solution) that I reported a week ago? It was triggered by mixing-in the Dimezone last, but did not occur when mixed first. Well, it even occurred in the concentrate where the Dimezone was mixed first. It just took a week to start. This also happened months ago with a highly concentrated dev I tried. But it has not happened in less concentrated samples that are six months old, nor has Alan Johnson reported it about his bottle of D316.

    If you define "concentration ratio" as GramsOfPowders / MlOfFinalVolume, then the failing samples had ratios of .46 and .63, and the successful samples had ratios of .35 and .33. So I'm suspecting that when concentration ratio gets much above .35, the concentrate becomes susceptible to this crystallization-problem that PE described here. If so, then I need to reduce concentration, and I have some ideas for that. One is to reduce the ascorbic acid some, which will also reduce the metaborate. Another is to replace some of the metaborate with TEA. Or one could simply add more propylene glycol. If somebody has suggestions about this, I welcome them...

    Mark Overton

  9. #89

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    Just to confirm that D-316 is still clear with no precipitate at 6 months old.
    It has a concentration ratio (2.2+4.5)/20 = 0.335

  10. #90
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    Get your hands on potassium sulphite or potassium metabisulphite (and react it with potassium hydroxide beforehand) if you want to make a high-sulphite concentrate.

    I've made a very high phenidone-ascorbate concentrate, but using potassium ascorbate. React the AA prior with a potassium salt like KOH. Shouldn't need as much sulphite for preservative with high ascorbate content. If you want to add salicylic acid, just use supermarket aspirin, it will hydrolyse in solution to salicylate.

    If then the only role left for sulphite is to act as a fine grain solvent. You could use a very small amount of potassium thiocyanate (as in a non-highlight clearing/non-reversal amount for the process times).

    My current concentrate is a bit different I made is similar, 4-aminophenol, potassium ascorbate and CD-2, still good after over a year, with some floating precipitate (saturated solution, like this since fresh). It is 1+24 to 1+49 dilution (20 min for HP5+ etc at 1+49), produces a negative that has higher local contrast with better micro details, but prints on a higher grade filter for the same black to white range (good for high contrast subjects already printing at 0), has more accentuated grain though.


    If you want a very high keeping life of concentrates, if you're going to split it into a 2 part solution anyway, making the part with the developing agents pH 4-6, with potassium metabisulphite and/or ascorbic acid etc, should increase the shelf life due to lower pH.
    Last edited by Athiril; 07-27-2012 at 11:30 PM. Click to view previous post history.



 

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