The method 4 wherein said cooling rate in step is {HEAD ~ about 0.2° C.} per {TAIL ~ minute} or less 
per
The method 4 wherein said cooling rate in step is { HEAD ~ about 0.2 ° C. } per { TAIL ~ minute } or less
OTH OTH OTH OTH OTH OTH OTH OTH OTH OTH HEAD HEAD HEAD HEAD HEAD HEAD HEAD HEAD REL TAIL TAIL TAIL TAIL TAIL OTH OTH