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  1. #51
    Snapshot's Avatar
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    My friend indicated that extracting a "reasonably" pure solid from it would be difficult, since I don't have a laboratory like he has access to. Hmm.... maybe it's time to buy him a nice Christmas present this year?
    "The secret to life is to keep your mind full and your bowels empty. Unfortunately, the converse is true for most people."

  2. #52
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    Sciencelab lists the potassium salt. I have purchased form them in the past.

    The Link http://www.sciencelab.com/page/S/PVAR/10415/SLH1723

    Evan Clarke

  3. #53

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    [QUOTE=Snapshot;546219]Evidiently, you can create the the HQMS with sodium sulfite, hydroquinone and hydrogen peroxide.

    Hydroquinone Monosulfonate, Sodium

    25.0g of sodium sulfite, 11.0g of hydroquinone and 10ml of hydrogen peroxide (40% solution) in 500ml of water.

    ...
    30% H2O2 was fairly readily available until recently. Now the ATF people are worried about people making acetone peroxide explosives with it. Although it is still available, you may have trouble getting a chemical house to sell it to an individual. The 30% stuff is a little tamer than 40%, but it is still a powerful oxidizer that demands respect. The H2O2 used to bleach hair is considerably more powerful than the usual 3% solution. I think it runs about 15%, but I'm not sure. You might check beauty supply houses or art supply houses that cater to dyers and fabric workers.

  4. #54
    Photo Engineer's Avatar
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    Ok, by comparison, HQSulfonate free acid is rather insoluable by comparison, and so it might be possible to purify by acidification and then washing with DW or Acetone or something like that. I may play with this a bit and see what is up.

    I'll keep you posted.

    PE

  5. #55
    Photo Engineer's Avatar
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    I tried the following:

    25 grams of Sodium Sulfite (anh) or 0.2 moles

    Dissolve in 366 ml of distilled water

    Add 11 grams of HQ or 0.1 moles

    Temperature 68F or 20C.

    Add slowly with stirring 133 ml of 3% H2O2 or about 0.15 moles.

    Temperature rose slowly during addition to 100F or 38C. (this could boil over if you are not careful and ruin you and the mixture) The pH was about 7.0 at this time.

    The solution was clear and colorless this whole time but slowly began to turn straw colored as it cooled. A sample was taken and acidified strongly to try to form a precipitate of the sulfonic acid derivative, but there was no effect except for the evolution of some sulfur dioxide gas.

    It is now sitting in my sink with me wondering what I should try next. It appears to me that purification may be rather difficult due to the solubility and the excess of Sodium Sulfite. I'll let it stand overnight and try some other things and keep you posted.

    This seems too simple. Like all simple things, there may be a gotcha in here somewhere.

    PE

  6. #56
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    Well, it looks promising enough. I too agree that it's suspiciously simple. Is it possible to use the solution as is?
    "The secret to life is to keep your mind full and your bowels empty. Unfortunately, the converse is true for most people."

  7. #57
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    Not unless you want a 50% excess of sodium sulfite.

    There is too much missing from that formula such as addition rate, temperatures, addition method and purification method.

    Today the clear solution sits with no change. An acidified beaker of some with extra peroxided added has turned dark orange. The odor of sulfite is gone, so I've oxidized the excess sulfite to sulfate.

    Now, I might be able to purify it by adding calcium or magnesium sulfate, but then I have to reconvert to the HQMS sodium salt. This becomes tedious and expensive. The price on that reference earlier begins to look more and more attractive!

    PE

  8. #58
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    I know this is my chemistry ignorance speaking but will reducing the sodium sulphite to 16g ameliorate some of the problem. How much HQMS was produced? About 21 grams?

    I guess begging Photographer's Formulary to stock potassium hydroquinone monosulphonate might be easier.
    Last edited by Snapshot; 11-16-2007 at 11:33 AM. Click to view previous post history.
    "The secret to life is to keep your mind full and your bowels empty. Unfortunately, the converse is true for most people."

  9. #59

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    Patent on making Sodium Hydroquinone Monosulfate

    Here is a link to a patent from 1982 on making and using Sodium Hydroquinone Monosulfate. The patent describes what PE did, but does not try to dry it, instead they use it in a developer solution right away.

    http://www.freepatentsonline.com/4366234.html

    On another note, I have noticed some formulations of first / B&W developers use a borax/boric acid buffer system, and others use carbonate/bicarbonate. Is there much difference between these two, especially if the final product is pH balanced with NaOH?

  10. #60
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    Quote Originally Posted by Photo Engineer View Post
    I tried the following:

    25 grams of Sodium Sulfite (anh) or 0.2 moles

    Dissolve in 366 ml of distilled water

    Add 11 grams of HQ or 0.1 moles

    Temperature 68F or 20C.

    Add slowly with stirring 133 ml of 3% H2O2 or about 0.15 moles.

    Temperature rose slowly during addition to 100F or 38C. (this could boil over if you are not careful and ruin you and the mixture) The pH was about 7.0 at this time.

    The solution was clear and colorless this whole time but slowly began to turn straw colored as it cooled. A sample was taken and acidified strongly to try to form a precipitate of the sulfonic acid derivative, but there was no effect except for the evolution of some sulfur dioxide gas.

    It is now sitting in my sink with me wondering what I should try next. It appears to me that purification may be rather difficult due to the solubility and the excess of Sodium Sulfite. I'll let it stand overnight and try some other things and keep you posted.

    This seems too simple. Like all simple things, there may be a gotcha in here somewhere.

    PE
    How about doing it in ethanol? Sodium Sulfite is insoluble in it, but Hydroquinone is soluble in Ethanol (I -think- it's about 20g/L at 24.5 celsius, may be remembering it wrong), left over sulfite shouldn't be dissolved then and you could dry it?

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