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MODULATED DSC

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From this experiment, the standard Heat Flow curve is separated into two ... as a function of temperature (Vincent Mathot, 1997 NATAS Conference Proceedings) ... – PowerPoint PPT presentation

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Title: MODULATED DSC


1
MODULATED DSC?
2
WHAT IS MDSC??
  • In MDSC, a sinusoidal heating profile is
    overlaid on the standard linear ramp
  • From this experiment, the standard Heat Flow
    curve is separated into two components called the
    Reversing Heat Flow and the Non-Reversing Heat
    Flow
  • Total Heat Flow is the same as in standard DSC
  • Reversing Heat Flow is the Cp component
  • Non-Reversing Heat Flow is the Kinetic Component

3
MDSC heating profile
4
Experimental conditions
5
Raw data
6
MDSC? EXAMPLE ON PET
7
Tzero? MDSC?
  • Results obtained using current MDSC practice are
    strongly dependent on modulation period
  • Long periods are required
  • Low heating rates necessary
  • Tzero MDSC greatly reduces period dependence
  • Shorter periods may be used
  • Higher heating rates are possible

8
FAST MDSC?
9
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10
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11
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12
Lactose
13
HEAT CAPACITY SIGNAL
14
WHAT IS HEAT CAPACITY?
  • Heat capacity is the amount of heat required to
    raise or lower the temperature of a material.
  • Specific heat capacity refers to a specific mass
    and temperature change for the material (J/gC)

15
WHY IS HEAT CAPACITY IMPORTANT?
  • Thermodynamic property of material(vs. heat flow)
  • Measure of molecular mobility
  • Provides useful information about physical
    properties of the material as a function of
    temperature

16
BENEFITS OF MEASURING HEAT CAPACITY
  • Structure-property information
  • Can compare samples run at different heating
    rates
  • Can compare samples during heating and cooling to
    better identify transitions associated with heat
    capacity and kinetic processes
  • Can be used to measure absolute crystallinity of
    polymers as a function of temperature (Vincent
    Mathot, 1997 NATAS Conference Proceedings)

17
MDSC? METHOD
  • MDSC heat capacity equation applies to heat flow
    to a single body
  • DSC heat flow is the difference between sample
    and reference heat flows
  • The method does not properly account for phase
    and amplitude differences between sample and
    reference heat flows and temperatures

18
Tzero? MDSC? METHOD
  • Tzero DSC gives independent sample and reference
    heat flow
  • Deconvolute sample and reference heat flow
    separately
  • Subtract reference reversing and non-reversing
    heat flow from sample reversing and non-reversing
    heat flow
  • Period dependence is greatly reduced
  • Cp units available for all signals

19
Tzero? MDSC? HEAT CAPACITY CALIBRATION
20
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21
HEAT CAPACITY UNITS ON ALL SIGNALS
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