Sabrina, I'm not an expert, but I have read a lot about this and there can be multiple things that caused your pollen to not work:
1) Is the pollen from a daylily known to be pollen fertile? If not, the pollen might have been infertile to start.
2) Try letting your pollen dry for a short while (maybe twenty minutes up to an hour) in your air conditioned home, especially if it is a humid day, before putting in the freezer.
3) Don't use pollen that has been rained on. (May apply if you had heavy morning dew and your daylily is an early opener, or "EMO", too.)
4) If you open your freezer repeatedly and your pollen is at the front/top where it is exposed to room temp air more readily, the repeayed freezing/thawing process might affect it, especially if you see signs of condensate (moisture).
5) Exposure to high heat (especially temperatures in excess of 80-90° F) can cause pollen fertility to deteriorate. As can time.
6) Make sure to pull off the stem-it has a lot of moisture-and only keep the anther head. (Or even just brush off the pollen into your container?)
Good luck with future pollen freezing. I used frozen pollen successfully last year, but this will be my first year carrying frozen pollen over from a previous season in order to try to pollinate my early bloomers with it.
I'm also really excited about a microscope I just recently purchased that allows me to see Daylily pollen. ..I need to do research to find out if I'll be able to use it to identify 'bad pollen' that is no longer viable. It probably isn't strong enough, but I'm hoping it is. It's possible that's a way you could we'd out infertile pollen in the future, though.
