Method and apparatus for parsed dynamic differential analysis
AssigneeTA Instruments, Inc.
InventorMichael Reading
Life of this patent
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Abstract
The interpretation of dynamic differential calorimetry ("DDSC") data is enhanced by parsing the data according to whether it is obtained while the sample is being heated, cooled, or re-heated. Each DDSC scan is split up into three separate components, depending upon whether the sample is undergoing heating, cooling or reheating. Each component can then be analyzed separately to investigate the sample response to temperature change as the sample is being heated, cooled, or re-heated. Each file is deconvoluted separately, using a deconvolution routine that first removes the effect of the phase lag due to the instrument's finite response time.
Claims69
A method for analyzing a material using a differential scanning calorimeter, said differential scanning calorimeter having a sample pan and a reference pan comprising the steps of:
- (a) selecting an underlying heating rate;
- (b) selecting a first modulation function characterized by a first modulation amplitude and a first modulation frequency;
- (c) placing a sample of the material in the sample pan of the differential scanning calorimeter;
- (d) varying the temperature of the sample pan of the differential scanning calorimeter according to the selected underlying heating rate and the first selected modulation function;
- (e) recording a signal representative of differential changes in the heat flow to and from the sample pan with respect to the reference pan to obtain differential heat flow data;
- (f) parsing the differential heat flow data according to the temperature conditions the sample was experiencing as the differential heat flow data was collected;
- and
- (g) storing the parsed differential heat flow data in separate files.
A differential scanning calorimeter comprising:
- (a) a sample position and a reference position;
- (b) means for varying the temperature of the sample position according to an underlying heating rate;
- (c) means for selecting a modulation function characterized by a modulation frequency and a modulation amplitude;
- (d) means for controlling the temperature of the sample position according to the selected underlying heating rate and modulation function;
- (e) means for detecting the heat flow to and from the sample position with respect to a reference as a function of temperature, as the temperature is varied according to the modulation function;
- (f) means for recording a signal representative of differential changes in the heat flow to and from the sample position with respect to the reference position;
- and
- (g) means for parsing the differential heat flow data according to the temperature conditions the sample was experiencing as the differential heat flow data was collected.
A differential scanning calorimeter comprising:
- (a) a sample position and a reference position;
- (b) means for varying the temperature of the sample position according to an underlying heating rate;
- (c) means for selecting a multiplex modulation function characterized by a first modulation frequency, a second modulation frequency, a first modulation amplitude and a second modulation frequency;
- (d) means for controlling the temperature of the sample position according to the selected underlying heating rate and multiplex modulation function;
- (e) means for detecting the heat flow to and from the sample position with respect to a reference as a function of temperature, as the temperature is varied according to the multiplex modulation function;
- and
- (f) means for recording a signal representative of differential changes in the heat flow to and from the sample position with respect to the reference position.
A method for analyzing a material comprising the steps of:
- (a) providing a heat flux differential scanning calorimeter having a sample position;
- (b) selecting an underlying heating rate;
- (c) selecting a modulation function characterized by a modulation frequency and a modulation amplitude;
- (d) placing a reference material at the sample position;
- (e) varying the temperature of the sample position at the selected underlying heating rate;
- (f) recording a reference signal representative of the heat flow to the sample position;
- (g) placing a sample of the material on the sample position of the differential scanning calorimeter;
- (h) varying the temperature of the sample position such that the average temperature of the sample position increases at the underlying heating rate, and applying an oscillating heat flow to the sample position, said heat flow oscillating according to the selected modulation function;
- (i) recording a differential signal representative of the average differential total heat flow to the sample position compared to the reference signal, and recording the average temperature of the sample position;
- and
- (j) parsing the differential signal according to whether the signal was obtained as the sample was being heated, cooled or re-heated;
- (k) storing the data obtained from the differential signal while the sample was being heated in a first file, storing the data obtained from the differential signal while the sample was being cooled in a second file, and storing the data obtained from the differential signal while the sample was being re-heated in a third file.
A heat flux differential scanning calorimeter comprising:
- (a) a sample position;
- (b) means for selecting an underlying heating rate;
- (c) means for selecting a modulation function characterized by a modulation frequency and a modulation amplitude;
- (d) means for varying the temperature of the sample position at the selected underlying heating rate;
- (e) means for recording a reference signal representative of the heat flow to the sample position;
- (f) means for varying the temperature of the sample position such that the average temperature of the sample position increases at the underlying heating rate, and applying an oscillating heat flow to the sample position, said heat flow oscillating according to the selected modulation function;
- (g) means for recording a differential signal representative of the average differential total heat flow to the sample position compared to the reference signal, and recording the average temperature of the sample position;
- and
- (h) means for parsing the differential signal according to whether the signal was obtained as the sample was being heated, cooled or re-heated;
- and
- (i) means for storing the data obtained from the differential signal while the sample was being heated in a first file, storing the data obtained from the differential signal while the sample was being cooled in a second file, and storing the data obtained from the differential signal while the sample was being re-heated in a third file.
A method for analyzing a material using a differential scanning calorimeter, said differential scanning calorimeter having a sample pan and a reference pan comprising the steps of:
- (a) selecting an underlying heating rate;
- (b) selecting a multiplex modulation function characterized by at least two different modulation frequencies;
- (c) placing a sample of the material in the sample pan of the differential scanning calorimeter;
- (d) varying the temperature of the sample pan of the differential scanning calorimeter according to the selected underlying heating rate and the selected multiplex modulation function;
- and
- (e) recording a signal representative of differential changes in the heat flow to and from the sample pan with respect to the reference pan to obtain multiplexed differential heat flow data.
Dependencies are inferred from the claim text.