bishop pipefreezing services ltd based in UK did a number of pipe frezzing job . for us few years back. coolant used was nitorgen at minus 196C. in their presentation, they cited several factors that affect the time/plug formation such as the ambient temp, pipe wall thickness, heat sink, integrity of the seals between the pipe and the jacket and convection within the pipe. Freezing time can vary between 4-18 hours.
you may want to check out the article featured in pipingdesign.com regarding pipefreezing technique