The third pull doesnt take more time to crash out. It doesnt take time to precipitate, just temperature change. You may be experiencing problems due to your your solvent not being saturated enough. Was your solvent warm enough? How many ml of solvent are you freezing? Maybe you need to evap to solvent down to 25% of the original volume and then freeze precip. The last time my friend extracted 500g of bark he was left w. 7g of spice.