Old syrup HC-110 with crystals?

I was about to mix up developer to process a roll of Verichrome (the ortho version -- has to be at least seventy years old, found film that came with my Autographic Vest Pocket Kodak), when i noticed both of my clear containers of HC-110 concentrate have crystals in the bottom, looking like snow. I was about to open the unopened one, then stopped; that one has been in the same shed for the same time.

I understand this crystallization is most likely due to freezing temperatures while these bottles were stored in my shed (six winters for the unopened bottle, most of a seventh for the clear bottles).

Has anyone successfully gotten them to redissolve, for instance by gently heating the concentrate? Or should I mix it all up as stock solution (and have an HC-110-fest)? Or is it gone off and useless (in my defense, I didn't know these were going to be stored through even one winter, never mind six or seven)?

Just use it normally. The un-crystallized stuff is probably slightly more concentrated now.

I would try to dissolve the crystals. Get a bowl and put the bottle in some hot water. If you can get the contents up to 125°F or so see if it will dissolve. Ilford had instructions similar for Ilfochrome developer concentrate. I remember freaking out when I got a kit that had solids in the developer bottle.

It may have been from heat not cold. If it goes back in solution my guess is it will work normally. Worth a try, real HC-110 is hard to find.

I have a bottle of the new formula (non-syrup) purchased last year that has about 1/4 remaining, it has crystals and works fine. It’s mostly been stored in my warm laundry room. I’ve read this is common and nothing to be concerned about.

mshchem said:

I would try to dissolve the crystals.

Click to expand...

What are these crystals chemically?

Here is the formula of HC-110 old version concentrate:
diethanolamine - sulfur dioxide addition product.............31g
diethanolamine.................................................................9g
diethanolamine hydrobromide........................................1.5g
phenidone.......................................................................0.5g
hydroquinone...................................................................6g
monoethanolamine.............................................................5g
ethylene glycol.................................................................10ml
polyvinylpyrolidone................add .25g to 1L of above
Something must crystalize out of that.
from FDC 2020 p75

My last bottle grew crystals, used it anyway, it worked ok. I was down to the last few CC's so I discarded the remainder.

Given the shape of the crystals (thin flat plates, reminiscent of snowflakes) I was thinking it was the diethanolamine or its sulfonate. I'll try warming up to 120 F or so (slowly) and see if it helps; if not, I'll just use it.

I would also go with the diethanolamine -SO2 addition product, which may be near the limit of its solubility in the various solvents included and crystalizes on cooling.

How safe is heating HC-110 concentrate? Would the diethanolamine -SO2 addition product break down into its constituents when heated and thereby releasing SO2?

mshchem said:

I would try to dissolve the crystals. Get a bowl and put the bottle in some hot water. If you can get the contents up to 125°F or so see if it will dissolve. Ilford had instructions similar for Ilfochrome developer concentrate. I remember freaking out when I got a kit that had solids in the developer bottle.

It may have been from heat not cold. If it goes back in solution my guess is it will work normally. Worth a try, real HC-110 is hard to find.

Click to expand...

This is what I would do too. Also a clip test.

In fact I will be practising what i'm now preaching, tomorrow morning - I have 12 rolls of Kodak Panatomic-X I've had refrigerated (but not frozen) since 1991 or 1992, which I'll be processing in a batch of newly-mixed Adox MQ borax developer. If this choice of developer results in any screams of outrage or otherwise from other members here, let me say in my defence that I've done a fair few rolls of Panatomic-X in this brew, and it works well. The film is now so old anyway, any images I've taken with it were purely for my own enjoyment and nothing I cannot live without or not be able to reshoot again. So.

I've used this developer to process several rolls of old (circa 1980) Tri-X film, with good results. Also an undated roll of Agfacolor negative film, probably from the 1950s or 1960s, which I left in the developer at 20C for two hours but for all that I got nothing at all, no images whatsoever, for my effort. Not that I expected anything from it, but I was still disappointed to open the tank and find a blank roll, which did have some faint edge markings, so the processing did work, in a way.

For especially valuable films, I wouldn't run the risk of using old HC-110 with crystals.

That ancient film the OP has may well harbor some interesting images, that is if anything at all comes out of the processing. To coin an old, old funny line, Mr Qualls, when you've processed this film, please let us know what develops, or rather developed...

I expect there'll be a specific "found film" thread with discussion and any images I get. I've gotten barely distinguishable images from film old enough to be on nitrate base once before, so we'll see what I get.

Okay, didn't intend to get two threads going for the same end purpose; I'm requesting this one to be close, as I've decided on cold D-23 with benzotriazole, and will post results (good or bad) there: https://www.photrio.com/forum/threads/how-much-extra-time-for-d-23-with-benzotriazole.189958/

Thread closed, with thanks.