–0.04
–0.03
–0.02
–0.01
Rev Heat Flow (W/g)
–80
–60
–40
–20
Temperature (ºC)
Exo Up
Universal V4.5A TA Instruments
0
2 0
0.0
–0.3
–33.16ºC(I)
–35.27ºC(I)
Nonrev Heat Flow (W/g)
Heat Flow (W/g)
–35.02ºC(I)
File: C:\TA\Data\DSC\2019\300719.001 Run Date: 30-Jul-2019 09:17
Program: Universal V4.5A Run Number: 1
TA Instruments Thermal Analysis – DSC Standard – Modulated RC
Method Log:
1: Isothermal for 2.00 min
2: Ramp 10.00ºC/min to –90.00ºC
3: Mark end of cycle 1
4:Data storage: Off
5:Modulate +/- 1.00ºC every 60 seconds
6: Isothermal for 8.00 min
7: Data storage: On
8: Samping interval 1.00 sec/pt
9: Isothermal for 8.00 min
10: Data storage: On
11: Samping interval 1.00 sec/pt
12: Ramp 3.00ºC/min to 25.00ºC
13: Mark end of cycle 2
14: End of method
–37ºC 18µbar sample drying
–Sample frozen
(plane polarised light)
–35ºC
Collapse
beginning
Sample: histidine sucrose
Size: 74.8000 mg
Method: MDSC – 3c minramp 1cminc modulat
DSC
File: C:\TA\Data\DSC\2019\300719.002
Operator: pm
Run Date: 30–Jul-2019 10:30
Instrument: DSC Q2000 V24.10 Build 122
Fig. 2 Thermal analysis of 5% w/v sucrose, 20 mM histidine buffer 0.01% Tween 20 pH 6.5, showing (a) FDM
profile from frozen (left-hand side image) to drying (middle image) to collapse at À35
C (right-hand side
image) and (b) mDSC profile with total heat flow (À35.0
C), reversing (À33.2
C), and non-reversing
(À35.3
C) profiles. Sample 75 mg in high-volume steel pan, temperature ramp rate 3
C/min with 1
C/min
modulation. Exothermic events shown as upward peaks
Principles of Freeze-Drying
119
–0.03
–0.02
–0.01
Rev Heat Flow (W/g)
–80
–60
–40
–20
Temperature (ºC)
Exo Up
Universal V4.5A TA Instruments
0
2 0
0.0
–0.3
–33.16ºC(I)
–35.27ºC(I)
Nonrev Heat Flow (W/g)
Heat Flow (W/g)
–35.02ºC(I)
File: C:\TA\Data\DSC\2019\300719.001 Run Date: 30-Jul-2019 09:17
Program: Universal V4.5A Run Number: 1
TA Instruments Thermal Analysis – DSC Standard – Modulated RC
Method Log:
1: Isothermal for 2.00 min
2: Ramp 10.00ºC/min to –90.00ºC
3: Mark end of cycle 1
4:Data storage: Off
5:Modulate +/- 1.00ºC every 60 seconds
6: Isothermal for 8.00 min
7: Data storage: On
8: Samping interval 1.00 sec/pt
9: Isothermal for 8.00 min
10: Data storage: On
11: Samping interval 1.00 sec/pt
12: Ramp 3.00ºC/min to 25.00ºC
13: Mark end of cycle 2
14: End of method
–37ºC 18µbar sample drying
–Sample frozen
(plane polarised light)
–35ºC
Collapse
beginning
Sample: histidine sucrose
Size: 74.8000 mg
Method: MDSC – 3c minramp 1cminc modulat
DSC
File: C:\TA\Data\DSC\2019\300719.002
Operator: pm
Run Date: 30–Jul-2019 10:30
Instrument: DSC Q2000 V24.10 Build 122
Fig. 2 Thermal analysis of 5% w/v sucrose, 20 mM histidine buffer 0.01% Tween 20 pH 6.5, showing (a) FDM
profile from frozen (left-hand side image) to drying (middle image) to collapse at À35
C (right-hand side
image) and (b) mDSC profile with total heat flow (À35.0
C), reversing (À33.2
C), and non-reversing
(À35.3
C) profiles. Sample 75 mg in high-volume steel pan, temperature ramp rate 3
C/min with 1
C/min
modulation. Exothermic events shown as upward peaks
Principles of Freeze-Drying
119