Birdsandbees - same story here (only at end of first year, but have been trying for a whole year and getting nowhere). Like you, this is the cornerstone not just of my PhD but of the work that will be done downstream of here - it's even written into the contract that this method must be developed. CC: glad you got there in the end. When you say "column", is that chromatography or protein purification? I would like to try some new HPLC columns but they're so expensive.

yeah its a pretty difficult situation to be in. I suppose im similar- in that although its not written into a contract or anything, this is really important- and while my superviser has a back up plan of a bucch of data that needs analysing if it were to fall through, it still needs to be done and i dont want to be the one that failed it.
We're currently trying to decide whether to carry on or cut our losses and hand me some data to analyse just so i can get a phd. At the moment this is looking pretty appealing, but seems like a waste of two years work and doesnt exactly give you a warm glow about what you've done.....