Actually the fish remains breathing even while its cells and blood are forming ice crystals (eew!). Whether it is aware of this I don't know, I can't imagine that this feels all too great. I think this is the most humane for the person doing the killing: pop it in a baggie, fling it in the freezer and walk away.
One of the best methods I've heard of is to put the fish (or whatever creature you are trying to do in) in a bowl of very cold water. They instantly have a heart attack and all organs shut down and the critter is dead.
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Christy's Reef Blog
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