Table 1.

Overview of process parameters of the different freeze-drying cycles employed. All cycles had a loading step of 60 min at 5 °C prior to freezing. End of primary drying time was determined as ∆p_c ≤ 1 mTorr between Pirani and capacitance probe.

Cycle	Freezing	Primary Drying			Secondary Drying
		Ramp (°C/min)	Ts (°C)	pc (mTorr)	Ramp (°C/min)	Ts (°C)	Hold Time (min)	Pressure (mTorr)
0	Ramp 0.3 °C/min Temp. −35 °C Hold 180 min	0.2	−10	100	0.2	+25	360	100
1		0.2	+10	100	0.2	+25	360	100
2		0.2	+30	100	0.2	+40	360	100
3		1.0	+30	100	0.2	+40	360	100
4		0.2	+30	155	0.2	+40	360	155
5		0.2	+30	100	-

T_s: shelf temperature, p_c: chamber pressure.