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Thermal cover:Layout 1 1/18/11 3:56 PM Page 3
SIMULTANEOUS TGA/DSC
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Thermal Brochure 2011:Layout 1 1/18/11 3:34 PM Page 66
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Thermal Brochure 2011:Layout 1 1/18/11 3:34 PM Page 68
APPLICATIONS
102 0.9
96 Dehydration
High Sensitivity Heat Flow (W/g) 7 0.6
90
Weight (%)
16 in which a small (3 mg) sample of sodium tungstate is 84
468.7J/g 459.1J/g 459.2J/g 464.4J/g
0 analyzed at 10 ˚C/min from ambient to 800 ˚C. The TGA
14 and derivative TGA (DTG) signals quantitatively record the 78 1 0.0
-2 dehydration step. The DSC trace quantitatively shows the loss
Weight (mg)
-4 -2 -0.3
11.27mg melting transitions respectively. The latter pair are thermal 66
In SDT experiments, superior accuracy in DSC data is -6 10 events where no weight loss occurs. Solid State and Melting Transitions
obtained when the instantaneous weight (rather than the 9.379mg 60 -0.6
7.628mg 8
initial sample weight) is used in heat flow calculations. This -8 0 200 400 600 800
figure shows data for sodium chloride (which loses weight on Temperature (˚C)
-10 Heat of Fusion using Original Weight (13.26mg) 6
heating) cycled through its melt four times, and the heat of
fusion (J/g) determined using the instantaneous weight. The 468.7J/g 384.1J/g 324.7J/g 266.9J/g
-12 4 Polymorphic Phase Transitions
accompanying table shows a comparison of this data versus 100
20 40 60 80 100 Simultaneous DSC/TGA
an identical experiment where the initial sample weight Time (min) Melting
was used for calculating the DSC data in each cycle. Transition -2
This figure contains simultaneous DSC and TGA data to Dehydration
The differences in reproducibility are significant.
Weight (%)
Cycle 1 Cycle 2 Cycle 3 Cycle 4 the dehydration and the onset of a higher temperature
decomposition. The DSC signal reveals transitions associated -4
Heat of Fusion
468.7 384.1 324.7 266.9 with the dehydration, a polymorphic phase transition and
Initial Weight (J/g)
the high temperature melt. The inset shows details about the 80
Heat of Fusion phase transition. In the Q600, heat flow integrations are -6
468.7 459.1 459.2 464.4 automatically normalized using the dynamic weight at the
Instantaneous Weight (J/g)
start of each transition. 300 400 500 600
70 -8
0 200 400 600 800 1000 1200 1400
Temperature (˚C)
68 69
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