I am using NHS chemistry to activate DNA oligos. I purify by HPLC and need to put them on the lyophilizer. Every time I put them on the lyophilizer I've been left with no product. I read that it could be because they weren't frozen enough and were boiling/entering liquid phase instead of going straight from solid to gas. So this time I froze them for over 48 hours at -80 degrees. But when I put them on the lyo, I immediately saw bubbles at the surface of the samples and liquid was forming. So I took them off and put them back in -80. Any idea why this is still happening and how to prevent it?