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2 days ago my 10G tank was great. After adding a few puffer fish I started feeding frozen food as I was told they won't eat dry foods. I bought various frozen foods and have since fed them 2 servings of brine shrimp.

Today my tank has a thick oily substance floating across the top, enough to stop air getting into the water. Also the smell is horrendous!!!

Is this the frozen food causing this?
Very well could be. What do you consider a serving to be ? Those portion packs are intended to keep the rest of the package fresh more so than being a suggested feeding amount. You could probably get by feeding 1/3 of a cube a day for a few small puffers.
 
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