Advanced reactive system screening tool

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a particular test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein particular test conditions comprise particular test sample mass, particular test sample specific heat, and a particular test sample heat loss model;

• the improvement comprising a method for heater control during a test, the method comprising:
• a) initiating a test run with the particular test sample;
• tuning the heater means in an initial calibration stage to the particular test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• b) controlling said heater in a subsequent test stage during said test run with the particular test sample, said test stage using said heater control equation to calculate heater power to be applied;
• and
• c) said calibration stage having at least two temperature ramping intervals and at least two adiabatic holding intervals, said calibration stage determining a ramping polynomial control equation for use in ramping the sample, said calibration stage determining an adiabatic polynomial control equation for holding the sample in an approximate adiabatic state;
• and
• d) said test stage sequentially and repeatedly ramping said sample using said ramping polynomial control equation, and holding said sample adiabatic using said adiabatic control equation to search for an exothermic reaction, and said test stage holding said sample in an adiabatic state after an exothermic reaction has been detected.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a particular test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein particular test conditions comprise particular test sample mass, particular test sample specific heat, and a particular test sample heat loss model;

• the improvement comprising a method for heater control during a test the method comprising:
• a) initiating a test run with the particular test sample;
• tuning the heater means in an initial calibration stage to the particular test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• b) controlling said heater in a subsequent test stage during said test run with the particular test sample, said test stage using said heater control equation to calculate heater power to be applied;
• and
• c) further comprising foam detector means.

A calorimeter apparatus having a test sample with a tempering temperature, where thermal mass is equal to mass multiplied by specific heat, and where test conditions include sample mass, specific heat, and a sample heat loss model, comprising:

• a) a sealable containment vessel having pressure detection means;
• b) a test cell for containing the test sample, said cell housed within the containment vessel, a ratio of said test cell thermal mass to said test sample thermal mass of less than 1:8, said test cell having thermal insulation;
• c) test sample agitation means;
• d) a single thermocouple in direct contact with the test sample of measuring sample temperature,
• e) a single heater for heating the test sample;
• f) data acquisition means for recording data;
• g) foam detector means comprising a probe having a surface heated to a temperature substantially in excess of the material tempering temperature, having temperature measurement means for measuring the temperature of said probe surface, said surface being quickly cooled when it comes into contact with foam;
• and
• h) a heater control sequence comprising:
• i) a calibration stage for tuning said heater to the test conditions, said calibration stage having a control loop to tune said heater to achieve a desired sample ramp rate, said calibration stage having a control loop to tune said heater to achieve a desired sample adiabatic hold, said calibration stage determining a heater ramping control equation and a heater adiabatic control equation;
• and
• ii) a test stage for controlling said heater during a test, said test stage having a ramping mode using said ramping control equation, and said test stage having an adiabatic mode using said adiabatic control equation.

A calorimeter apparatus having a test sample with a surface and a tempering temperature, where thermal mass is equal to mass multiplied by specific heat, and where test conditions include sample mass, specific heat, and a sample heat loss model, comprising:

• a) a sealable containment vessel having pressure detection means;
• b) a test cell for containing the test sample, said cell housed within the containment vessel, a ratio of said test cell thermal mass to said test sample thermal mass of less than 1:8, said test cell having thermal insulation, said test cell being spherical with an open neck having an interior;
• c) test sample agitation means;
• d) a single thermocouple in direct contact with the test sample of measuring sample temperature,
• e) a single heater for heating the test sample;
• f) foam detector means comprising a cylindrical probe having a probe surface heated to a temperature substantially in excess of the material tempering temperature, having a thermocouple for measuring the temperature of said probe surface, said probe surface being quickly cooled when it comes into contact with foam, said probe placed in said test cell neck interior above said test sample surface level;
• g) data acquisition means for recording temperature, pressure, time, heater, and foam detector data;
• and
• h) a heater control sequence comprising:
• i) a calibration stage for tuning said heater to the test conditions, said calibration stage having a proportional integral derivative control loop to tune said heater to achieve a desired sample ramp rate, said calibration stage having a proportional integral derivative control loop to tune said heater to achieve a desired sample adiabatic hold, said calibration stage determining a heater ramping control polynomial equation and a heater adiabatic control polynomial equation;
• and
• ii) a test stage for controlling said heater during a test, said test stage having a ramping mode using said ramping control equation, and said test stage having an adiabatic mode using said adiabatic control equation.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein test conditions comprise sample mass, sample specific heat, and a sample heat loss model;

• the improvement comprising a method of heater control comprising:
• (a) tuning the heater means in a calibration stage to the test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• said calibration stage having at least two temperature ramping intervals and at least two adiabatic holding intervals, said calibration stage determining a heater ramping control equation and a heater adiabatic control equation;
• and
• (b) controlling said heater in a test stage during a test, said test stage using said heater control equation to calculate heater power to be applied;
• wherein said test stage controls said heating means with said ramping control equation to ramp the sample temperature until an exothermic reaction is detected, and said test stage controls said heating means with said adiabatic control equation to hold the sample adiabatic after an exothermic reaction has been detected.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein test conditions comprise sample mass, sample specific heat, and a sample heat loss model;

• the improvement comprising a method of heater control comprising:
• a) tuning the heater means in a calibration stage to the test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• said calibration stage having at least two temperature ramping intervals and at least two adiabatic holding intervals, said calibration stage determining a ramping polynomial control equation for use in ramping the sample, said calibration stage determining an adiabatic polynomial control equation for holding the sample in an approximate adiabatic state;
• and
• b) controlling said heater in a test stage during a test, said test stage using said heater control equation to calculate heater power to be applied;
• said test stage sequentially and repeatedly ramping said sample using said ramping polynomial control equation, and holding said sample adiabatic using said adiabatic control equation to search for an exothermic reaction, and said test stage holding said sample in an adiabatic state after an exothermic reaction has been detected.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein test conditions comprise sample mass, sample specific heat, and a sample heat loss model;

• the improvement comprising:
• a. a method of heater control comprising:
• (i) tuning the heater means in a calibration stage to the test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• (ii) controlling said heater in a test stage during a test, said test stage using said heater control equation to calculate heater power to be applied;
• and
• b. wherein the heater control method further comprises foam detection means.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a particular test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein particular test conditions comprise particular test sample mass, particular test sample specific heat, and a particular test sample heat loss model;

• the improvement comprising a method for heater control during a test, the method comprising:
• a) initiating a test run with the particular test sample;
• tuning the heater means in an initial calibration stage to the particular test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• said initial calibration stage comprising at least one ramping interval and at least one holding interval;
• and
• b) controlling said heater in a subsequent test stage during said test run with the particular test sample, said test stage using said heater control equation to calculate heater power to be applied;
• said test stage comprising at least one ramping interval and at least one adiabatic interval.

An improved heater control method for a calorimeter apparatus, the calorimeter of the type having an exterior containment vessel, a test cell containing a particular test sample, temperature measurement means for measuring the test sample temperature, heating means for heating the test sample, data acquisition means for recording data, wherein particular test conditions comprise particular test sample mass, particular test sample specific heat, and a particular test sample heat loss model, wherein the test sample undergoes an exothermic reaction;

• the improvement comprising a method for heater control during a test, the method comprising:
• a) initiating a test run with the particular test sample;
• tuning the heater means in an initial calibration stage to the particular test conditions, said calibration stage having a control loop to tune said heater, said calibration stage determining a heater control equation relating temperature to heater power;
• and
• b) controlling said heater in a subsequent test stage during said test run with the particular test sample, said test stage using said heater control equation to calculate heater power to be applied, and wherein said heater control equation controls the heater to maintain the particular test sample in a substantially adiabatic condition while the test sample undergoes an exothermic reaction.