I've had similar problems with Hannah Alk and Calcium reagents. Since I have a Trident, I'm not testing manually very often, and I find that when I do the tests are unreliable with older Hannah reagent bottles that have been open for a while, even tough they are still within the expiration date. I think this is one of the reasons that Neptune advises to just throw out any leftover Alk reagent after 30 days.