Claims
- 1. An apparatus for parallel processing of reaction mixtures comprising:
vessels for containing the reaction mixtures; a stirring system for agitating the reaction mixtures; and a temperature control system that is adapted to maintain a first group of the vessels at a different temperature than a second group of the vessels.
- 2. The apparatus of claim 1, further comprising a reactor block;
wherein the vessels comprise wells formed in the reactor block.
- 3. The apparatus of claim 2, wherein the vessels further comprise removable liners, each of the liners having an interior surface defining a cavity for containing one of the reaction mixtures and an exterior surface dimensioned so that the liners fit within the wells formed in the reactor block.
- 4. The apparatus of claim 3, wherein the removable liners are glass vials.
- 5. The apparatus of claim 3, further comprising an insulating material filling gaps between the removable liners and the wells.
- 6. The apparatus of claim 5, wherein the insulating material is glass wool or silicone rubber.
- 7. The apparatus of claim 3, further comprising a conductive material filling gaps between the removable liners and the wells.
- 8. The apparatus of claim 7, wherein the conductive material is a thermal paste.
- 9. The apparatus of claim 2, wherein the wells comprise holes extending from a top surface of the reactor block to a bottom surface of the reactor block, the apparatus further comprising:
a removable lower plate disposed on the bottom surface of the reactor block, the removable lower plate defining a base of each of the wells; and a removable upper plate disposed on the top surface of the reactor block, the removable upper plate defining an upper end of each of the wells.
- 10. The apparatus of claim 9, wherein the removable upper plate further comprises vessel seals in substantial alignment with the wells, the vessel seals allowing processing of the reaction mixtures at pressures different than atmospheric pressure.
- 11. The apparatus of claim 2, further comprising a passageway formed in the reactor block adapted to provide a flow path for a thermal fluid and adapted to provide heat exchange between the vessels and the thermal fluid.
- 12. The apparatus of claim 1, further comprising a chamber enclosing the vessels, wherein the chamber is substantially gas impermeable.
- 13. The apparatus of claim 1, further comprising a plurality of modules, each of the modules containing a portion of the vessels.
- 14. The apparatus of claim 13, wherein each of the modules comprises a block and wherein vessels comprise wells formed in the block.
- 15. The apparatus of claim 1, further comprising a robotic material handling system for loading the vessels with starting materials, the robotic liquid handling system comprising:
a probe adapted to dispense starting materials into each of the vessels; a three-axis translation system coupled to the probe for manipulating the probe position; and a processor that communicates with the probe and the three-axis translation system; wherein the processor controls the probe position and an amount of the starting materials dispensed in each of the vessels.
- 16. The apparatus of claim 1, wherein the temperature control system includes a temperature monitoring system comprising:
temperature sensors in thermal contact with the vessels; and a temperature monitor that communicates with the temperature sensors and converts signals received from the temperature sensors to a standard temperature scale.
- 17. The apparatus of claim 16, wherein the temperature sensors are thermocouples, resistance thermometric devices, or thermistors, alone or in combination.
- 18. The apparatus of claim 16, further comprising a processor that communicates with the temperature monitor, wherein the processor performs calculations on data received from the temperature monitor.
- 19. The apparatus of claim 16, wherein the temperature sensors are attached to the vessels.
- 20. The apparatus of claim 16, wherein the temperature sensors are contained in the vessels.
- 21. The apparatus of claim 1, wherein the temperature control system includes a remote temperature monitoring system comprising an infrared-sensitive camera positioned to detect infrared radiation emanating from each of the vessels.
- 22. The apparatus of claim 21, wherein each of the vessels are fitted with a cap that transmits infrared radiation.
- 23. The apparatus of claim 21, further comprising an isolation chamber enclosing the vessels.
- 24. The apparatus of claim 23, wherein the isolation chamber has a window that transmits infrared radiation so that the camera positioned outside of the isolation chamber detects infrared radiation passing through the window.
- 25. The apparatus of claim 1, wherein the temperature control system further comprises temperature sensors and heat transfer devices;
wherein the temperature sensors and the heat transfer devices are in thermal contact with the vessels, and the heat transfer devices are adapted to transfer heat to or from the vessels in response to signals received from the temperature sensors.
- 26. The apparatus of claim 25, wherein each of the vessels is associated with at least one of the temperature sensors and with at least one of the heat transfer devices so that the temperature of each of the vessels can be controlled independently.
- 27. The apparatus of claim 25, wherein the temperature control system further comprises:
a processor that communicates with the temperature sensors and the heat transfer devices; wherein the processor and the heat transfer devices are adapted to adjust heat flow to or from the heat transfer devices in response to signals received by the processor from the temperature sensors.
- 28. The apparatus of claim 27, wherein the temperature control system further comprises:
a temperature monitor that communicates with the temperature sensors and the processor; wherein the temperature monitor converts signals received from the temperature sensors to temperature data and sends the temperature data to the processor which adjusts heat transfer to or from the heat transfer devices in response to the temperature data.
- 29. The apparatus of claim 27, wherein the heat transfer devices are electric resistance heaters, the temperature control system further comprising:
a heater control system that communicates with the electric resistance heaters and the processor; wherein the heater control system regulates the heat output from the electric resistance heaters by adjusting the amount of electrical current in each of the electric resistance heaters in response to signals from the processor.
- 30. The apparatus of claim 27, wherein the heat transfer devices are thermoelectric devices, the temperature control system further comprising:
a thermoelectric device control system that communicates with the thermoelectric devices and the processor; wherein the thermoelectric device control system regulates the heat flow to or from the thermoelectric devices by adjusting the magnitude and direction of the electrical current in each of the thermoelectric devices in response to signals from the processor.
- 31. The apparatus of claim 25, wherein the heat transfer devices are electric resistance heaters.
- 32. The apparatus of claim 31, wherein the electric resistance heaters are coiled around the vessels.
- 33. The apparatus of claim 31, wherein the temperature sensors and the electric resistance heaters are the same.
- 34. The apparatus of claim 33, wherein the temperature sensors and the electric resistance heaters are thermistors.
- 35. The apparatus of claim 25, wherein the heat transfer devices are thermoelectric devices.
- 36. The apparatus of claim 25, wherein the temperature control system further comprises a uniform temperature reservoir in thermal contact with the vessels.
- 37. The apparatus of claim 36, wherein the uniform temperature reservoir is adapted to contain a thermal fluid.
- 38. The apparatus of claim 37, wherein the vessels are suspended in the uniform temperature reservoir.
- 39. The apparatus of claim 37, wherein the temperature control system further comprises a heat pump in thermal contact with the uniform temperature reservoir, the heat pump adapted to maintain the uniform temperature reservoir at a selected temperature.
- 40. The apparatus of claim 37, further comprising:
a reactor block, wherein the vessels comprise wells formed in the reactor block; a passageway formed in the reactor block adapted to provide a flow path for the thermal fluid and adapted to provide heat exchange between the thermal fluid and the vessels; conduits providing fluid communication between the uniform temperature reservoir and the passageway; and a fluid pump located along one of the conduits for transporting the thermal fluid from the uniform temperature reservoir to the passageway and from the passageway to the uniform temperature reservoir.
- 41. The apparatus of claim 40, wherein the temperature control system further comprises:
a heat pump having a heat transfer coil immersed in the uniform temperature reservoir; a first temperature sensor in thermal contact with the uniform temperature reservoir, and a second temperature sensor in thermal contact with the passageway; and a processor that communicates with the heat pump, the first temperature sensor, and the second temperature sensor; wherein the processor and the heat pump are adapted to adjust heat transfer to or from the heat transfer coil in response to signals received by the processor from the first temperature sensor and the second temperature sensor.
- 42. The apparatus of claim 40, further comprising:
a valve located along one of the conduits; and a processor that communicates with the valve; wherein the valve is adapted to adjust flow rate of the thermal fluid through the passageway in response to a signal from the processor.
- 43. The apparatus of claim 25, wherein the heat transfer devices are thermoelectric devices and the apparatus further comprises:
a reactor block, wherein the vessels comprise wells formed in the reactor block; and a heat transfer plate in thermal contact with the thermoelectric devices, each of the thermoelectric devices disposed between the reactor block and the heat transfer plate such that the thermoelectric devices transfer heat from the vessels to the heat transfer plate or from the heat transfer plate to the vessels.
- 44. The apparatus of claim 43, wherein each of the thermoelectric devices transfers heat predominantly to or from a single vessel.
- 45. The apparatus of claim 43, wherein the heat transfer plate further comprises a passageway formed in the heat transfer plate adapted to provide a flow path for a thermal fluid.
- 46. The apparatus of claim 1, wherein the stirring system comprises:
stirring members at least partially contained in the vessels; and a drive mechanism coupled to the stirring members, the drive mechanism adapted to rotate the stirring members.
- 47. The apparatus of claim 46, wherein the drive mechanism comprises motors coupled to the stirring members so that the speed, torque, or speed and torque of the stirring members can be independently varied.
- 48. The apparatus of claim 47, wherein the motors are air-driven motors, constant-speed AC motors, variable-speed AC motors, DC motors, or stepper motors.
- 49. The apparatus of claim 47, further comprising strain gauges for measuring torque exerted by the motors on the reaction mixtures, wherein the motors are rigidly attached to a motor support, and the strain gauges are mounted between the motor support and the motors.
- 50. The apparatus of claim 47, further comprising speed sensors integral to the motors for monitoring rotational speed of the stirring members.
- 51. The apparatus of claim 50, wherein the speed sensors are encoders, resolvers, or Hall effect sensors.
- 52. The apparatus of claim 50, further comprising a processor in communication with the speed sensors;
wherein the processor adjusts power supplied to each of the motors in response to signals received from the speed sensors to maintain the rotational speed of the stirring members at selected values.
- 53. The apparatus of claim 46, further comprising strain gauges for measuring torque exerted by the drive mechanism on the reaction mixtures;
wherein one end of each of the strain gauges is rigidly attached to the vessel support, and an opposite end of each of the strain gauges is rigidly attached to the vessels so that each of the vessels is attached to one of the strain gauges.
- 54. The apparatus of claim 53, further comprising:
first permanent magnets attached to the opposite end of each of the strain gauges; and second permanent magnets attached to the vessels so that magnetic coupling between the first permanent magnets and the second permanent magnets prevents the vessels from rotating.
- 55. The apparatus of claim 46, wherein the drive mechanism comprises:
a motor; and a drive train coupling the motor to the stirring members.
- 56. The apparatus of claim 55, wherein the drive train comprises:
gears attached to the motor and to portions of the stirring members located external to the vessels, each of the gears dimensioned and arranged to mesh with at least one adjacent gear so that rotational energy is transmitted along the drive train from the motor to the stirring members.
- 57. The apparatus of claim 55, wherein the drive train comprises:
sprockets attached to the motor and to portions of the stirring members located external to the vessels; and a chain linking the sprockets so that rotation energy is transmitted along the drive train from the motor to the stirring members.
- 58. The apparatus of claim 55, wherein the drive train comprises:
pulleys attached to the motor and to portions of the stirring members located external to the vessels; and belts linking the pulleys so that rotation energy is transmitted along the drive train from the motor to the stirring members.
- 59. The apparatus of claim 46, wherein each of the stirring members comprises:
a spindle, each spindle having a first end and a second end; and a stirring blade attached to the first end of the spindle.
- 60. The apparatus of claim 59, wherein the second end of the spindle is mechanically coupled to the drive mechanism.
- 61. The apparatus of claim 59, wherein the second end of the spindle is magnetically coupled to the drive mechanism.
- 62. The apparatus of claim 59, further comprising a strain gauge located within the spindle.
- 63. The apparatus of claim 59, further comprising an optical speed sensor mounted adjacent to the spindle for monitoring rotational speed of the spindle.
- 64. The apparatus of claim 46, wherein the stirring members are magnetic stirring bars, and the drive mechanism comprises an array of electromagnets that produce rotating magnetic fields in the vessels.
- 65. The apparatus of claim 64, wherein the array of electromagnets is arranged so that each of the vessels is located between four electromagnets, the four electromagnets defining four corners of a quadrilateral sub-array.
- 66. The apparatus of claim 65, wherein the array of electromagnets is arranged so that the ratio of electromagnets to vessels is about 1:1, 2:1, or 4:1.
- 67. The apparatus of claim 66, wherein the array of electromagnets further comprises:
a first group of electromagnets; and a second group of electromagnets; wherein, the first group of electromagnets are electrically connected in series so that pairs of successive electromagnets define two opposite corners of each quadrilateral sub-array, and the second group of electromagnets are electrically connected in series so that pairs of successive electromagnets define two opposite corners of each quadrilateral sub-array.
- 68. The apparatus of claim 64, wherein the drive mechanism further comprises:
a drive circuit and a processor, wherein the drive circuit is controlled by the processor and is adapted to independently and temporally vary electrical current in the first group of electromagnets and in the second group of electromagnets.
- 69. The apparatus of claim 68, wherein the drive circuit further comprises a power source that is adapted to provide sinusoidal electrical currents.
- 70. The apparatus of claim 68, wherein the drive circuit further comprises a power source that is adapted to provide pulsed electrical currents.
- 71. The apparatus of claim 64, wherein the array of electromagnets is mounted on a printed circuit board.
- 72. The apparatus of claim 46, wherein the stirring system further comprises a system for measuring phase lag between the stirring members and the drive mechanism.
- 73. The apparatus of claim 72, wherein the system for measuring phase lag comprises:
inductive sensing coils located adjacent to the vessels and displaced laterally from the axes of rotation of the stirring members; and a phase-sensitive detector adapted to monitor phase differences among signals generated by the inductive sensing coils and a reference signal having the same phase behavior as the drive mechanism; wherein the stirring members include permanent magnets having magnetic moments that are nonparallel to the axes of rotation of the stirring members so that rotation of the stirring members result in signals generated by the inductive sensing coils having the same phase behavior as the stirring members.
- 74. The apparatus of claim 73, wherein the inductive sensing coils are gradient coils.
- 75. The apparatus of claim 73, wherein the phase-sensitive detector is a lock-in amplifier.
- 76. The apparatus of claim 73, wherein the stirring members are magnetic stirring bars, and the drive mechanism comprises an array of electromagnets that produce rotating magnetic fields in the vessels.
- 77. The apparatus of claim 73, wherein each of the stirring members comprises:
a spindle having a first end and a second end, the second end of the spindle attached to the drive mechanism; and a magnetic stirring blade attached to the first end of the spindle; wherein, the spindle is torsionally soft.
- 78. The apparatus of claim 1, further including a system for evaluating reaction mixtures comprising:
mechanical oscillators located within the vessels, each of the mechanical oscillators adapted to receive a variable frequency excitation signal and to transmit a response signal that depends on one or more material properties of the reaction mixtures; a source in communication with the mechanical oscillators, the source providing each of the mechanical oscillators with the variable frequency excitation signal; and a receiver in communication with the mechanical oscillators, the receiver monitoring the response signal from each of the mechanical oscillators.
- 79. The apparatus of claim 78, wherein the source and the signal comprise a network analyzer.
- 80. The apparatus of claim 79, wherein the network analyzer further comprises a wide band receiver.
- 81. The apparatus of claim 79, wherein the system for evaluating reaction mixtures further comprises a high impedence buffer amplifier located in a communication link between the mechanical oscillators and the network analyzer.
- 82. The apparatus of claim 78, wherein the mechanical oscillators are tuning forks or bimorph/unimorph resonators.
- 83. The apparatus of claim 1, further including a system for evaluating reaction mixtures comprising:
a mechanical oscillator adapted to receive a variable frequency excitation signal and to transmit a response signal that depends on one or more material properties of the reaction mixtures; a source in communication with the mechanical oscillators, the source providing the mechanical oscillator with the variable frequency excitation signal; a receiver in communication with the mechanical oscillator, the receiver monitoring the response signal from the mechanical oscillator; a three-axis translation system coupled to the mechanical oscillator for manipulating the mechanical oscillator position; and a processor in communication with the three-axis translation system, the processor adapted to direct the three-axis translation system to place the mechanical oscillator in each of the vessels.
- 84. The apparatus of claim 1, further including a system for evaluating reaction mixtures comprising:
a mechanical oscillator located within a separate vessel, the mechanical oscillator adapted to receive a variable frequency excitation signal and to transmit a response signal that depends on one or more material properties of the reaction mixtures; a source in communication with the mechanical oscillators, the source providing the mechanical oscillator with the variable frequency excitation signal; a receiver in communication with the mechanical oscillator, the receiver monitoring the response signal from the mechanical oscillator; a probe adapted to withdraw and dispense the reaction mixtures; a three-axis translation system coupled to the probe for manipulating the probe position; and a processor that communicates with the probe and the three-axis translation system, the processor adapted to direct the probe to withdraw a portion of one of the reaction mixtures from one of the vessels and to dispense the portion of one of the reaction mixtures in the separate vessel.
- 85. The apparatus of claim 1, further comprising a pressure control system, wherein each of the vessels has a gas inlet for introducing a vapor-phase component of the reaction mixtures into the vessels, and each of the vessels has an open end for loading the vessels with condensed-phase components of the reaction mixtures, the pressure control system further comprising:
caps removably attached to the open end of each of the vessels, the caps minimizing gas flow through the open end of each of the vessels; pressure sensors in fluid communication with the vessels; conduits providing fluid communication between a source of the vapor-phase component and the gas inlet of each of the vessels; valves located along the conduits between the source of the vapor-phase component and the gas inlet of each of the vessels; a valve controller communicating with the valves, the valve controller regulating the amount of the vapor-phase component entering the vessels by selectively opening or closing the valves; and a processor communicating with the valve controller and the pressure sensors, the processor directing the valve controller to selectively open or close the valves in response to signals received from the pressure sensors.
- 86. The apparatus of claim 85, further comprising temperature sensors in thermal contact with the vessels, the temperature sensors communicating with the processor and providing the processor with data for determining pressure corrections based on temperature changes of the reaction mixtures.
- 87. The apparatus of claim 85, wherein the valves are multi-port valves, each of the valves providing selective fluid communication between the gas inlet and an exhaust port, and between the gas inlet and the source of the vapor-phase component.
- 88. The apparatus of claim 85, further comprising flow sensors located along the conduits between the valves and the gas inlet of each of the vessels, the flow sensors communicating with the processor and providing the processor with data for determining amounts of the vapor-phase component entering each of the vessels during processing.
- 89. The apparatus of claim 1, further comprising a pressure control system, wherein each of the vessels has a gas inlet for introducing a vapor-phase component of the reaction mixtures into the vessels, and each of the vessels has an open end for loading the vessels with condensed-phase components of the reaction mixtures, the pressure control system further comprising:
caps removably attached to the open end of each of the vessels, the caps minimizing gas flow through the open end of each of the vessels; conduits providing fluid communication between a source of the vapor-phase component and the gas inlet of each of the vessels, the source of the vapor-phase component having about constant pressure during processing of the reaction mixtures; flow sensors located along the conduits between the source of the vapor-phase component and the gas inlet of each of the vessels; and a processor communicating with the flow sensors, the flow sensors providing the processor with data for determining amounts of the vapor-phase component entering each of the vessels during processing.
- 90. An apparatus for monitoring rates of production or consumption of a gas-phase component of a reaction mixture comprising:
a vessel for containing the reaction mixture, the vessel having a gas inlet for introducing a gas-phase component of the reaction mixture into the vessels and an open end for loading the vessel with one or more condensed-phase components of the reaction mixture; a stirring system for agitating the reaction mixture; a temperature control system for regulating the temperature of the reaction mixture; and a pressure control system comprising: caps removably attached to the open end of vessel, the cap minimizing gas flow through the open end of vessel; a pressure sensor in fluid communication with the vessel; a conduit providing fluid communication between a source of the gas-phase component and the gas inlet of the vessel; a valve located along the conduit between the source of the gas-phase component and the gas inlet of the vessel; a valve controller communicating with the valve, the valve controller regulating the amount of the gas-phase component entering the vessel by selectively opening or closing the valve; and a processor communicating with the valve controller and the pressure sensor, the processor directing the valve controller to selectively open or close the valve in response to a signal received from the pressure sensor.
- 91. The apparatus of claim 90, further comprising a temperature sensor in thermal contact with the vessel, the temperature sensor communicating with the processor and providing the processor with data for determining pressure corrections based on temperature changes of the reaction mixture.
- 92. The apparatus of claim 90, wherein the valve is a multi-port valve, the valve providing selective fluid communication between the gas inlet and an exhaust port, and between the gas inlet and the source of the gas-phase component.
- 93. The apparatus of claim 90, further comprising a flow sensor located along the conduit between the valve and the gas inlet of the vessel, the flow sensor communicating with the processor and providing the processor with data for determining an amount of the gas-phase component entering the vessel.
- 94. An apparatus for monitoring rates of consumption of a gas-phase reactant of a reaction mixture comprising:
a vessel for containing the reaction mixture, the vessel having a gas inlet for introducing the gas-phase reactant into the vessels and an open end for loading the vessel with one or more condensed-phase components of the reaction mixture; a stirring system for agitating the reaction mixture; a temperature control system for regulating the temperature of the reaction mixture; and a pressure control system comprising: caps removably attached to the open end of vessel, the cap minimizing gas flow through the open end of vessel; a pressure sensor in fluid communication with the vessel; a conduit providing fluid communication between a source of the gas-phase reactant and the gas inlet of each of the vessels; a flow sensor located along the conduit between the source of the gas-phase component and the gas inlet of the vessel; and a processor communicating with the flow sensor, the flow sensor providing the processor with data for determining an amount of the gas-phase reactant entering the vessel during processing.
- 95. A method of making and characterizing materials comprising the steps of:
providing vessels with starting materials to form reaction mixtures; confining the reaction mixtures in the vessels to allow reaction to occur; stirring the reaction mixtures for at least a portion of the confining step; and evaluating the reaction mixtures by tracking at least one characteristic of the reaction mixtures for at least a portion of the confining step; wherein the confining step is carried out at about the same time for each of reaction mixtures.
- 96. The method of claim 95, wherein the providing step includes loading the vessels with starting materials using a robotic material handling system, the robotic liquid handling system comprising:
a probe adapted to dispense starting materials into each of the vessels; a three-axis translation system coupled to the probe for manipulating the probe position; and a processor that communicates with the probe and the three-axis translation system; wherein the processor controls the probe position and an amount of the starting materials dispensed in each of the vessels.
- 97. The method of claim 95, wherein the providing step further comprises the step of blanketing the vessels in an inert gas atmosphere.
- 98. The method of claim 95, wherein the evaluating step further comprises the step of monitoring temperatures of each of the reaction mixtures.
- 99. The method of claim 98, wherein the monitoring step comprises detecting infrared emissions from the reaction mixtures.
- 100. The method of claim 95, wherein the evaluating step comprises the step of monitoring heat transfer rates into or out of the vessels.
- 101. The method of claim 100, wherein the monitoring step includes the steps of:
measuring temperature differences between each of the reaction mixtures and a thermal reservoir surrounding the vessels; and determining heat transfer rates from a calibration relating the temperature differences to heat transfer rates.
- 102. The method of claim 100, wherein the evaluating step further comprises the step of computing conversion of the starting materials based on the heat transfer rates of the monitoring step.
- 103. The method of claim 102, wherein the evaluating step further comprises the step of determining rates of reaction based on conversion of the starting materials.
- 104. The method of claim 95, wherein the stirring step comprises the steps of:
supplying the reaction mixtures with stirring members; and rotating each of the stirring members.
- 105. The method of claim 104, wherein the stirring members rotate at the same rate in the rotating step.
- 106. The method of claim 104, wherein the evaluating step further comprises the step of monitoring the torque needed to rotate the stirring members in the rotating step.
- 107. The method of claim 106, wherein the torque is monitored by measuring phase lag between the torque and the stirring members.
- 108. The method of claim 106, wherein the evaluating step further comprises the step of determining viscosity of each of the reaction mixtures from a calibration relating the torque and viscosity.
- 109. The method of claim 108, wherein the evaluating step further comprises the steps of:
measuring heat transfer rates into or out of the vessels; computing conversion of the starting materials based on heat transfer rates into or out of the vessels; and calculating molecular weight of a component of the reaction mixtures based on conversion of the starting materials and on viscosity of each of the reaction mixtures.
- 110. The method of claim 104, wherein the evaluating step further comprises the step of monitoring the power needed to rotate each of the stirring members in the rotating step.
- 111. The method of claim 110, wherein the evaluating step further comprises the step of determining viscosity of each of the reaction mixtures from a calibration relating power and viscosity.
- 112. The method of claim 111, wherein the evaluating step further comprises the steps of:
measuring heat transfer rates into or out of the vessels; computing conversion of the starting materials based on heat transfer into or out of the vessels; and calculating molecular weight of a component of the reaction mixtures based on conversion of the starting materials and on viscosity of each of the reaction mixtures.
- 113. The method of claim 104, wherein the evaluating step further comprises the step of monitoring stall frequencies of the stirring members in the rotating step.
- 114. The method of claim 113, wherein the evaluating step further comprises the step of determining viscosity of each of the reaction mixtures from a calibration relating stall frequencies and viscosity.
- 115. The method of claim 114, wherein the evaluating step further comprises the steps of:
measuring rates of heat transfer into or out of the vessels; computing conversion of the starting materials based on rates of heat transfer into or out of the vessels; and calculating molecular weight of a component of the reaction mixtufes based on conversion of the starting materials and on viscosity of each of the reaction mixtures.
- 116. The method of claim 95, wherein the evaluating step further comprises the steps of:
stimulating mechanical oscillators with a variable frequency excitation signal, the mechanical oscillators located within the vessels; monitoring response signals from the mechanical oscillators; determining a property of each of the reaction mixtures from a calibration relating response signals and the property.
- 117. The method of claim 116, wherein the property of the determining step is molecular weight, specific gravity, elasticity, dielectric constant or conductivity.
- 118. The method of claim 116, wherein the evaluating step further comprises the steps of:
placing a mechanical oscillator in one of the vessels containing a particular reaction mixture; stimulating the oscillator with a variable frequency excitation signal; monitoring a response signal from the mechanical oscillator; and determining a property of the particular reaction mixture from a calibration relating response signals and the property; wherein the placing step, the stimulating step, the monitoring step, and the determining step are carried out for each of the reaction mixtures.
- 119. The method of claim 116, wherein the evaluating step further comprises the steps of:
supplying a separate vessel with a mechanical oscillator; placing a portion of a particular reaction mixture in the separate vessel; stimulating the oscillator with a variable frequency excitation signal; monitoring a response signal from the mechanical oscillator; and determining a property of the particular reaction mixture from a calibration relating response signals and the property; wherein the placing step, the stimulating step, the monitoring step, and the determining step are carried out for each of the reaction mixtures.
- 120. The method of claim 95, wherein there is a net loss of moles of gas-phase components of each of the reaction mixtures due to reaction, the evaluating step further comprising the steps of:
filling the vessels with a gas-phase reactant until gas pressure in each of the vessels exceeds an upper-pressure limit, PH; allowing gas pressure in each of the vessels to decay below a lower-pressure limit, PL; monitoring the gas pressure in each of the vessels during the filling and allowing steps so as to generate a record of pressure versus time for each of the vessels; repeating the filling step and the allowing step at least once; and determining rates of consumption of the gas-phase reactant in each of the reaction mixtures from the record of pressure versus time for each of the vessels.
- 121. The method of claim 120, wherein the determining step further comprises the steps of:
converting the record of pressure versus time for each of the vessels to partial pressure of the gas-phase reactant versus time for each of the vessels; calculating rates of consumption of the gas-phase reactant in each of the reaction mixtures from time rates of change of the partial pressure of the gas-phase reactant versus time during the allowing steps.
- 122. The method of claim 120, wherein the determining step further comprises the step of calculating rates of consumption of the gas-phase reactant in each of the reaction mixtures from frequencies of the filling steps over particular time intervals.
- 123. The method of claim 120, wherein the determining step further comprises the steps of:
estimating a volumetric flow rate of the gas-phase reactant entering a given vessel during a particular filling step; multiplying the volumetric flow rate of the gas-phase reactant entering the given vessel during the particular filling step by an amount of time elapsed during the particular filling step to obtain an estimate of an amount of the gas-phase reactant entering the given vessel during the particular filling step; dividing the estimate of the amount of the gas-phase reactant entering the given vessel during the particular filling step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of consumption of the gas-phase reactant in the given vessel for the particular filling step and the subsequent allowing step.
- 124. The method of claim 120, wherein the determining step further comprises the steps of:
measuring an amount of the gas-phase reactant entering a given vessel during a particular filling step; dividing the amount of the gas-phase reactant entering the given vessel during the particular filling step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of consumption of the gas-phase reactant in the given vessel for the particular filling step and the subsequent allowing step.
- 125. The method of claim 95, wherein there is a net gain of moles of gas-phase components of each of the reaction mixtures due to reaction, the evaluating step further comprising the steps of:
allowing gas pressure in each of the vessels to rise above an upper-pressure limit, PH; venting the vessels until gas pressure in each of the vessels falls below a lower-pressure limit, PL; monitoring the gas pressure in each of the vessels during the allowing and venting steps so as to generate a record of pressure versus time for each of the vessels; repeating the allowing step and the venting step at least once; and determining rates of production of a gas-phase product in each of the reaction mixtures from the record of pressure versus time for each of the vessels.
- 126. The method of claim 125, wherein the determining step further comprises the steps of:
converting the record of pressure versus time for each of the vessels to partial pressure of the gas-phase product versus time for each of the vessels; calculating rates of production of the gas-phase product in each of the reaction mixtures from time rates of change of the partial pressure of the gas-phase product versus time during the allowing steps.
- 127. The method of claim 125, wherein the determining step further comprises the step of calculating rates of production of the gas-phase product in each of the reaction mixtures from frequencies of the venting steps over particular time intervals.
- 128. The method of claim 125, wherein the determining step further comprises the steps of:
estimating a volumetric flow rate of the gas-phase product leaving a given vessel during a particular venting step; multiplying the volumetric flow rate of the gas-phase product leaving the given vessel during the particular filling step by an amount of time elapsed during the particular venting step to obtain an estimate of an amount of the gas-phase product leaving the given vessel during the particular venting step; dividing the estimate of the amount of the gas-phase product leaving the given vessel during the particular venting step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of production of the gas-phase product in the given vessel for the particular venting step and the subsequent allowing step.
- 129. The method of claim 125, wherein the determining step further comprises the steps of:
measuring an amount of the gas-phase product leaving a given vessel during a particular venting step; dividing the amount of the gas-phase product leaving the given vessel during the particular venting step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of production of the gas-phase product in the given vessel for the particular venting step and the subsequent allowing step.
- 130. The method of claim 95, further comprising the step of controlling temperatures of each of the reaction mixtures.
- 131. The method of claim 130, wherein temperatures of each of the reaction mixtures are controlled independently in the controlling step.
- 132. A method of monitoring a rate of consumption of a gas-phase reactant where there is a net loss of moles of gas-phase components in a reaction mixture due to reaction, the method comprising the steps of:
providing a vessel with starting materials to form the reaction mixture; confining the reaction mixtures in the vessel to allow reaction to occur; stirring the reaction mixture for at least a portion of the confining step; filling the vessel with the gas-phase reactant until gas pressure in the vessel exceeds an upper-pressure limit, PH; allowing gas pressure in the vessel to decay below a lower-pressure limit, PL; monitoring the gas pressure in the vessel during the filling and allowing steps so as to generate a record of pressure versus time for the vessel; repeating the filling step and the allowing step at least once; and determining rates of consumption of the gas-phase reactant in the reaction mixture from the record of pressure versus time.
- 133. The method of claim 132, wherein the determining step further comprises the steps of:
converting the record of pressure versus time to partial pressure of the gas-phase reactant versus time; calculating rates of consumption of the gas-phase reactant from time rates of change of the partial pressure of the gas-phase reactant versus time during the allowing steps.
- 134. The method of claim 132, wherein the determining step further comprises the step of calculating rates of consumption of the gas-phase reactant from frequencies of the filling steps over particular time intervals.
- 135. The method of claim 132, wherein the determining step further comprises the steps of:
estimating a volumetric flow rate of the gas-phase reactant entering the vessel during a particular filling step; multiplying the volumetric flow rate of the gas-phase reactant entering the vessel during the particular filling step by an amount of time elapsed during the particular filling step to obtain an estimate of an amount of the gas-phase reactant entering the vessel during the particular filling step; dividing the estimate of the amount of the gas-phase reactant entering the vessel during the particular filling step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of consumption of the gas-phase for the particular filling step and the subsequent allowing step.
- 136. The method of claim 132, wherein the determining step further comprises the steps of:
measuring an amount of the gas-phase reactant entering the vessel during a particular filling step; dividing the amount of the gas-phase reactant entering the vessel during the particular filling step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of consumption of the gas-phase reactant for the particular filling step and the subsequent allowing step.
- 137. A method of monitoring a rate of production of a gas-phase product where there is a net gain of moles of gas-phase components in a reaction mixture due to reaction, the method comprising the steps of:
providing a vessel with starting materials to form the reaction mixture; confining the reaction mixtures in the vessel to allow reaction to occur; stirring the reaction mixture for at least a portion of the confining step; allowing gas pressure in the vessel to rise above an upper-pressure limit, PH; venting the vessel until gas pressure in the vessel falls below a lower-pressure limit, PL; monitoring the gas pressure in the vessel during the allowing and venting steps so as to generate a record of pressure versus time for the vessel; repeating the allowing step and the venting step at least once; and determining rates of production of the gas-phase product from the record of pressure versus time.
- 138. The method of claim 137, wherein the determining step further comprises the steps of:
converting the record of pressure versus time to partial pressure of the gas-phase product versus time; calculating rates of production of the gas-phase product from time rates of change of the partial pressure of the gas-phase product versus time during the allowing steps.
- 139. The method of claim 137, wherein the determining step further comprises the step of calculating rates of production of the gas-phase product from frequencies of the venting steps over particular time intervals.
- 140. The method of claim 137, wherein the determining step further comprises the steps of:
estimating a volumetric flow rate of the gas-phase product leaving the vessel during a particular venting step; multiplying the volumetric flow rate of the gas-phase product leaving the vessel during the particular filling step by an amount of time elapsed during the particular venting step to obtain an estimate of an amount of the gas-phase product leaving the vessel during the particular venting step; dividing the estimate of the amount of the gas-phase product leaving the vessel during the particular venting step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of production of the gas-phase product for the particular venting step and the subsequent allowing step.
- 141. The method of claim 137, wherein the determining step further comprises the steps of:
measuring an amount of the gas-phase product leaving the vessel during a particular venting step; dividing the amount of the gas-phase product leaving the vessel during the particular venting step by an amount of time elapsed during a subsequent allowing step to obtain an average rate of production of the gas-phase product for the particular venting step and the subsequent allowing step.
- 142. An apparatus for parallel processing of reaction mixtures comprising:
vessels for containing the reaction mixtures; a stirring system for agitating the reaction mixtures; a temperature control system for regulating the temperature of the reaction mixtures; and an injection system for introducing a fluid into the vessels at a pressure different than ambient pressure.
- 143. The apparatus of claim 142, wherein the injection system comprises:
fill ports adapted to receive a fluid delivery probe; first conduits and valves, the first conduits providing fluid communication between the fill ports and the valves; and second conduits and injectors, the second conduits providing fluid communication between the valves and the injectors; wherein the injectors are located in the vessels.
- 144. The apparatus of claim 143, further comprising a robotic handling system, wherein the robotic handling system is adapted to manipulate the fluid delivery probe.
- 145. The apparatus of claim 144, further comprising a computer to control both the robotic handling system and the valves.
- 146. The apparatus of claim 143, wherein the fill port comprises:
an elongated body having a longitudinal axis and a bore centered on the longitudinal axis, the bore extending the length of the elongated body and characterized by first, second, and third diameters, wherein the first diameter is greater than the second diameter, and the second diameter is greater than the third diameter; an elastomeric o-ring seated within the bore of the elongated body on a first ledge defined by the second diameter and the third diameter; and a cylindrical sleeve having a hole centered on its axis of rotation, the hole extending the length of the cylindrical sleeve; wherein the cylindrical sleeve is seated within the bore of the elongated body on a second ledge defined by the first diameter and the second diameter and the cylindrical sleeve abuts the elastomeric o-ring.
- 147. The apparatus of claim 146, wherein the cylindrical sleeve is made of a chemically resistant plastic material.
- 148. The apparatus of claim 147, wherein the chemically resistant plastic material is a perfluoro-elastomer or polyethylethylketone or polytetrafluoroethylene.
- 149. The apparatus of claim 143, wherein the fill port comprises:
an elongated body having a longitudinal axis and a bore centered on the longitudinal axis, the bore extending the length of the elongated body and characterized by a first diameter and a second diameter, wherein the first diameter is greater than the second diameter; and a cylindrical insert having a tapered hole centered on its axis of rotation, the tapered hold extending the length of the cylindrical insert; wherein the cylindrical insert is seated within the bore of the elongated body on a ledge defined by the first diameter and the second diameter.
- 150. The apparatus of claim 149, wherein the cylindrical insert is made of a chemically resistant plastic material.
- 151. The apparatus of claim 150, wherein the chemically resistant plastic material is a perfluoro-elastomer or polyethylethylketone or polytetrafluoroethylene.
- 152. The apparatus of claim 143, further comprising a reactor block;
wherein the vessels comprise wells formed in the reactor block.
- 153. The apparatus of claim 152, further comprising an injector manifold associated with the reactor block and wherein the fill ports and valves are in fluid communication with the injector manifold.
- 154. The apparatus of claim 153, wherein the injector manifold is attached to the reactor block and the first conduits and the second conduits are passageways formed in the injector manifold.
- 155. The apparatus of claim 153, wherein the wells comprise holes extending from a top surface of the reactor block to a bottom surface of the reactor block, the apparatus further comprising:
a lower plate disposed on the bottom surface of the reactor block, the lower plate defining a base of each of the wells; an injector adapter plate disposed on the top surface of the reactor block, the injector adapter plate having holes substantially aligned with the wells and having channels extending from a front edge of the injector adapter plate to a bottom surface of the injector adapter plate, wherein the injectors are attached to the bottom surface of the injector adapter plate and are in fluid communication with the channels, and the injector manifold is attached to the front edge of the injector adapter plate so that the second conduits are in fluid communication with the channels of the injector adapter plate; and an upper plate disposed on the injector adapter plate, the upper plate defining an upper end of each of the wells.
- 156. The apparatus of claim 155, wherein the injectors extend into the reaction mixtures.
- 157. An apparatus for parallel processing of reaction mixtures comprising:
vessels for containing the reaction mixtures; a temperature control system for regulating the temperature of the reaction mixtures; and a stirring system for agitating the reaction mixtures, the stirring system comprising: spindles contained in the vessels, each of the spindles having a first end and a second end; a stirring blade attached to the first end of each of the spindles; a drive mechanism located external to the vessels that is adapted to rotate the spindles; and magnetic feed through devices for magnetically coupling the drive mechanism to the second end of each of the spindles.
- 158. The apparatus of claim 157, wherein each of the magnetic feed through devices comprises:
a rigid cylindrical pressure barrier having an interior surface that together with one of the vessels defines a closed chamber; a magnetic driver rotatably mounted concentrically with the pressure barrier and external to the closed chamber; and a magnetic follower rotatably mounted within the closed chamber; wherein the drive mechanism is mechanically coupled to rotate the magnetic driver and the magnetic follower follows the magnetic driver, and the second end of one of the spindles is attached to the magnetic follower so that the spindles rotate as driven by the drive mechanism.
- 159. The apparatus of claim 158, wherein the drive mechanism further comprises:
a motor; and a drive train coupling the motor to the magnetic driver of the magnetic feed through devices.
- 160. The apparatus of claim 158, wherein the drive train comprises:
gears attached to the motor and to the magnetic driver of the magnetic feed through devices, each of the gears dimensioned and arranged so as to mesh with at least one adjacent gear so that rotational energy is transmitted along the drive train from the motor to the spindles through the magnetic feed through devices.
- 161. An apparatus for parallel processing of reaction mixtures comprising:
vessels for containing the reaction mixtures; a temperature control system for regulating the temperature of the reaction mixtures; and a stirring system for agitating the reaction mixtures, the stirring system comprising multi-piece spindles partially contained in the vessels, and a drive mechanism coupled to the spindles, the drive mechanism adapted to rotate the spindles; wherein each of the spindles includes: an upper spindle portion mechanically coupled to the drive mechanism; and a removable stirrer attached to the upper spindle portion and contained in one of the vessels.
- 162. The apparatus of claim 161, wherein the removable stirrer is made of a chemically resistant material.
- 163. The apparatus of claim 162, wherein the chemically resistant material is a perfluoro-elastomer or polyethylethylketone or polytetrafluoroethylene or glass.
- 164. The apparatus of claim 161, further comprising a coupler for reversibly attaching the removable stirrer to the upper spindle portion, wherein the coupler comprises:
a cylindrical body having first and second holes centered along an axis of rotation of the coupler, the first hole dimensioned to receive an end of the upper spindle portion, and the second hole of the coupler dimensioned to receive an end of the removable stirrer.
- 165. The apparatus of claim 164, further including a locking mechanism for preventing relative rotation of the coupler and the removable stirrer comprising:
a pin embedded in the end of the removable stirrer; a spring mounted between the coupler and a shoulder formed on the removable stirrer periphery; and an axial groove extending from an entrance of the second hole to a lateral slot cut through a wall of the coupler, the lateral slot extending partway around the coupler circumference to an axial slot cut through the wall of the coupler; wherein the axial groove, the lateral slot, and the axial slot are sized to accommodate the pin when the end of the removable stirrer is inserted into the second hole and rotated, and the pin is held in the axial slot by a force exerted by the spring.
- 166. The apparatus of claim 161, wherein the removable stirrer is snapped into the upper spindle portion.
- 167. A method of making and characterizing materials comprising the steps of:
providing vessels with starting materials to form reaction mixtures; confining the reaction mixtures in the vessels; stirring the reaction mixtures for at least a portion of the confining step; and evaluating the reaction mixtures by tracking at least one characteristic of the reaction for at least a portion of the confining step; wherein the confining step further includes a step of injecting a fluid into at least one of the vessels.
- 168. The method of claim 167, wherein the fluid of the injecting step comprises a catalyst.
- 169. The method of claim 167, wherein the fluid of the injecting step comprises a catalyst poison.
- 170. The method of claim 167, wherein the fluid of the injecting step comprises a comonomer.
RELATED APPLICATIONS
[0001] This application is a continuation in part of U.S. application Ser. No. 09/177,170, filed Oct. 22, 1998, which claims the benefit of U.S. Provisional Application No. 60/096,603, filed Aug. 13, 1998.
Provisional Applications (1)
|
Number |
Date |
Country |
|
60096603 |
Aug 1998 |
US |
Continuations (1)
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Number |
Date |
Country |
Parent |
09211982 |
Dec 1998 |
US |
Child |
09850916 |
May 2001 |
US |
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
09177170 |
Oct 1998 |
US |
Child |
09211982 |
Dec 1998 |
US |