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US 5,346,306 AGranted
Method and apparatus for modulated differential analysis
AssigneeTA Instruments, Inc.
InventorsMichael Reading, Brian K. Hahn, Benjamin S. Crowe
Life of this patent
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Abstract
The present invention relates to differential analytical techniques for determining the composition, phase, structure, identification or other properties of a material that undergoes a transition as function of a driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises: (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; and (2) deconvoluting the resultant heat flow signal into rapidly reversible and non-rapidly reversible components.
Claims44
A method for analyzing a material using a differential scanning calorimeter comprising the steps of:
- (a) selecting an underlying heating rate, modulation frequency and modulation amplitude;
- (b) lacing a sample of the material in the differential scanning calorimeter;
- (c) varying the temperature of the sample in the differential scanning calorimeter according to the selected underlying heating rate, the selected modulation frequency and the selected modulation amplitude;
- (d) recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (e) deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute at least one deconvoluted signal.
3 more elements
A method for analyzing a material using a differential thermal analyzer comprising the steps of:
- (a) selecting an underlying heating rate, modulation frequency and modulation amplitude;
- (b) placing a sample of the material in a differential thermal analyzer;
- (c) varying the temperature of the sample in the differential thermal analyzer according to the selected underlying heating rate, the selected modulation frequency and the selected modulation amplitude;
- (d) recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (e) deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute at least one deconvoluted signal.
3 more elements
A differential scanning calorimeter comprising:
- (a) means for varying the temperature of a sample in the differential scanning calorimeter according to an underlying heating rate;
- (b) means for selecting a modulation frequency and a modulation amplitude;
- (c) means for controlling the temperature of the sample according to the selected underlying heating rate, modulation frequency and modulation amplitude;
- (d) means for detecting the heat flow to and from the sample with respect to a reference as a function of temperature, as the temperature is varied according to the modulation frequency and the modulation amplitude;
- (e) means for recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (f) means for deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute at least one deconvoluted signal.
4 more elements
A differential thermal analyzer comprising:
- (a) means for varying the temperature of a sample in the differential thermal analyzer according to an underlying heating rate;
- (b) means for selecting a modulation frequency and a modulation amplitude;
- (c) means for controlling the temperature of the sample according to the selected underlying heating rate, modulation frequency and modulation amplitude;
- (d) means for detecting the heat flow to and from the sample with respect to a reference as a function of temperature, as the temperature is varied according to the modulation frequency and the modulation amplitude;
- (e) means for recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (f) means for deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute at least one deconvoluted signal.
4 more elements
A method for analyzing a material comprising the steps of:
- (a) placing a sample of the material in an apparatus for detecting differential changes in the heat flow to a sample material with respect to a reference, as a function of temperature;
- (b) varying the temperature at an underlying heating rate modulated by a modulation function, said modulation function having a preselected modulation frequency and a preselected modulation amplitude;
- (c) monitoring a differential signal representative of the differential change in the heat flow to the sample material with respect to the reference;
- (d) recording the differential signal representative of the differential change in the heat flow to the sample material with respect to the reference;
- and
- (e) deconvoluting the signal representative of the differential change in the heat flow to the sample material with respect to the reference to compute at least one deconvoluted signal.
3 more elements
A thermal analysis instrument comprising:
- (a) a furnace comprising a heater, a heater controller, and a furnace chamber;
- (b) a sample pan and a reference pan in the furnace chamber;
- (c) means for monitoring the temperature of the sample pan and the temperature difference between the sample pan and the reference pan;
- (d) means for controlling the temperature of the furnace chamber;
- (e) means for receiving a signal representative of the temperature of the sample pan and of the temperature difference between the sample pan and the reference pan, for calculating a signal representative of differential changes in heat flow to the sample pan with respect to heat flow to the reference pan from the signal representative of the temperature of the sample pan and of the temperature difference between the sample pan and the reference pan, and for controlling the means for controlling the temperature of the furnace chamber;
- (f) means for (i) selecting an underlying heating rate for the furnace chamber, (ii) selecting a modulation frequency and a modulation amplitude, and (iii) controlling the temperature of the sample pan according to the selected underlying heating, modulation frequency and modulation amplitude;
- (g) means for recording the signal representative of differential changes in the heat flow to the sample pan with respect to the heat flow to the reference pan;
- and
- (h) means for deconvoluting the signal representative of differential changes in the heat flow to the sample pan with respect to the heat flow to the reference pan to compute at least one deconvoluted signal.
6 more elements
A thermal analysis instrument comprising:
- (a) a sample position and a reference position;
- (b) means for heating a sample placed at the sample position and a reference placed at the reference position;
- (c) means for monitoring the heat flow to the sample and the heat flow to the reference;
- (d) means for receiving a signal representative of the heat flow to the sample and the heat flow to the reference;
- (e) means for recording the signal representative of the heat flow to the sample and the heat flow to the reference;
- (f) means for selecting an underlying heating rate, modulation frequency and modulation amplitude;
- (g) means for controlling the temperature of the sample according to the selected underlying heating rate, modulation frequency and modulation amplitude;
- (h) means for calculating a signal representative of differential changes in the heat flow to the sample with respect to the heat flow to the reference;
- and
- (i) means for deconvoluting the signal representative of differential changes in the heat flow to the sample with respect to the heat flow to the reference to compute at least one deconvoluted signal.
7 more elements
A method for analyzing a material using a differential scanning calorimeter comprising the steps of:
- (a) selecting an underlying heating rate, modulation frequency and modulation amplitude;
- (b) placing a sample of the material in the differential scanning calorimeter;
- (c) varying the temperature of the sample in the differential scanning calorimeter according to the selected underlying heating rate, the selected modulation frequency and the selected modulation amplitude;
- (d) recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (e) deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute two deconvoluted signals.
3 more elements
A method for analyzing a material using a differential thermal analyzer comprising the steps of:
- (a) selecting an underlying heating rate, modulation frequency and modulation amplitude;
- (b) placing a sample of the material in a differential thermal analyzer;
- (c) varying the temperature of the sample in the differential thermal analyzer according to the selected underlying heating rate, the selected modulation frequency and the selected modulation amplitude;
- (d) recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (e) deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute two deconvoluted signals.
3 more elements
A differential scanning calorimeter comprising:
- (a) means for varying the temperature of a sample in the differential scanning calorimeter according to an underlying heating rate;
- (b) means for selecting a modulation frequency and a modulation amplitude;
- (c) means for controlling the temperature of the sample according to the selected underlying heating rate, modulation frequency and modulation amplitude;
- (d) means for detecting the heat flow to and from the sample with respect to a reference as a function of temperature, as the temperature is varied according to the modulation frequency and the modulation amplitude;
- (e) means for recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (f) means for deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute two deconvoluted signals.
4 more elements
A differential thermal analyzer comprising:
- (a) means for varying the temperature of a sample in the differential thermal analyzer according to an underlying heating rate;
- (b) means for selecting a modulation frequency and a modulation amplitude;
- (c) means for controlling the temperature of the sample according to the selected underlying heating rate, modulation frequency and modulation amplitude;
- (d) means for detecting the heat flow to and from the sample with respect to a reference as a function of temperature, as the temperature is varied according to the modulation frequency and the modulation amplitude;
- (e) means for recording a signal representative of differential changes in the heat flow to and from the sample;
- and
- (f) means for deconvoluting the signal representative of differential changes in the heat flow to and from the sample to compute two deconvoluted signals.
4 more elements
Dependencies are inferred from the claim text.