Yes, the water would freeze. Instead of having a layer of water in the bottom of a tank, that layer would become a layer of ice.
But, ... the better way to get water out of the diesel, is to drain it out of the drainage plug (if it has one) when it's not froze, and leave the diesel in the tank.
Water if any, goes to the bottom. Draining the tank at the drian plug until nothing but diesel comes out, will remove any water that is in there. If tank doesn't have a drain plug, you obviously aren't going to be able to remove the water this way. But, if your planning on re-using the tank, you aren't going to be able to remove the ice this way either.
So, ... I'm not seeing that there would be much benefited from messing around with it when the water is froze. Unless of course, you were just retrieving diesel from a tank that you wasn't planning on using the tank again, and you knew the tank has some water in it as well.
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