Abstract: A method and apparatus for reacting a plurality of different mixtures in parallel in a semi-batch or continuous mode is provided. Each reaction is contained within a reactor vessel, the reactor vessels combined into a reactor block. Reactant(s) to be added during the reaction are kept in a header barrel, which has a plunger to feed reactant(s) from the header barrel through a transfer line into the reactor vessel. The plunger is moved using a drive system. The header barrels are optionally combined in a header block. The header block is sealed to a plate containing the transfer lines, which in turn is sealed to the reactor block. A latch mechanism is provided for easy sealing of the reactor and header blocks to the plate. The entire apparatus may be placed on a rocker or rotating plate for mixture as the reaction is proceeding.

Abstract: A method is disclosed for characterizing a plurality of non-biological polymer samples. The method includes the steps of injecting four or more non-biological polymer samples into a mobile-phase of a liquid chromatography system, chromatographically separating at least one sample component or polymer molecule of each of the four or more injected polymer samples from other sample components or polymer molecules thereof in a chromatographic column, and serially detecting a property of the four or more non-biological polymer samples or of components or polymer molecules thereof with a flow-through detector at an average sample throughput of not more than about 10 minutes per sample.

Abstract: Controlled stable free radical emulsion polymerization processes employ nitroxide control agents having an alpha carbon atom bearing a destabilizing substituent such as hydrogen. The emulsion polymerizations have living characteristics, including the re-initiation of polymer chains, and provide a high degree of control over molecular weight, particle size, polydispersity and polymer composition and architecture. The processes are useful for the preparation of polymer emulsions, including block copolymers, star and graft copolymers, telechelics and macromonomers from a wide range of monomers.

Abstract: An apparatus and method for carrying out and monitoring the progress and properties of multiple reactions is disclosed. The method and apparatus are especially useful for synthesizing, screening, and characterizing combinatorial libraries, but also offer significant advantages over conventional experimental reactors as well. The apparatus generally includes multiple vessels for containing reaction mixtures, and systems for controlling the stirring rate and temperature of individual reaction mixtures or groups of reaction mixtures. In addition, the apparatus may include provisions for independently controlling pressure in each vessel. In situ monitoring of individual reaction mixtures provides feedback for process controllers, and also provides data for determining reaction rates, product yields, and various properties of the reaction products, including viscosity and molecular weight.

Abstract: A method is disclosed for characterizing non-biological polymers using liquid chromatography that is particularly useful in polymer research programs. The method includes the steps of providing a library of four or more non-biological polymer samples, with each of the four or more polymer samples being polymerization product mixtures that result from polymerization reactions that are varied with respect to a factor affecting polymerization. Each of the four or more polymer samples resides in the reaction vessel in which they were formed.

Abstract: A method is disclosed for characterizing a plurality of non-biological polymer samples. The method includes the steps of injecting a first non-biological polymer sample into a mobile-phase of a liquid chromatography system, chromatographically separating at least one sample component of the injected first sample from other sample components thereof in a chromatographic column, detecting at least one property of the separated sample component of the first sample, injecting a second non-biological polymer sample into the mobile-phase of the liquid chromatography system while advancing the first sample to the chromatographic column, chromatographically separating at least one sample component of the injected second sample from other sample components thereof, and detecting at least one property of the separated sample component of the second sample.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Abstract: Controlled stable free radical emulsion polymerization processes employ nitroxide control agents having an alpha carbon atom bearing a destabilizing substituent such as hydrogen. The emulsion polymerizations have living characteristics, including the re-initiation of polymer chains, and provide a high degree of control over molecular weight, particle size, polydispersity and polymer composition and architecture. The processes are useful for the preparation of polymer emulsions, including block copolymers, star and graft copolymers, telechelics and macromonomers from a wide range of monomers.

Abstract: An apparatus and method for screening combinatorial libraries of materials by measuring the response of individual library members to mechanical perturbations is described. The apparatus generally includes a sample holder for containing the library members, an array of probes for mechanically perturbing individual library members, and an array of sensors for measuring the response of each of the library members to the mechanical perturbations. Library members undergoing screening make up a sample array, and individual library members constitute elements of the sample array that are confined to specific locations on the sample holder. During screening, the apparatus mechanically perturbs individual library members by displacing the sample array (sample holder) and the array of probes. Typically, all of the elements of the sample array are perturbed simultaneously, but the apparatus also can also perturb individual or groups of sample array elements sequentially.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Abstract: Nitroxides having an alpha-carbon atom with a destabilizing moiety are effective control agents for emulsion and water-based polymerizations, including the formation of block copolymers from a wide range of monomers. The nitroxide radicals may be used as a free radical or as an adduct with a residue from the initiator. The emulsions have living characteristics, including the re-initiation of polymer chains. Also, a seeded process for emulsions, which includes the step-wise addition of monomer is disclosed, providing access to a wide range of initiator types.

Abstract: Block copolymers are disclosed having at least one polymer segment characterized by a high degree of control over molecular weight, particle size, polydispersity and polymer composition and architecture. The block copolymers feature at least on polymer segment produced using a controlled free radical polymerization process in an emulsion. Additional polymer segments can be generated using the controlled free radical emulsion process or any other polymerization process. The block copolymers include polymers having unique structure, such as stars, grafts, telechelics and macromonomers. Block copolymers having hard/soft and amphiphilic characteristics are also disclosed. The block copolymers may also include adducts with nitroxide control agents capable of free radical re-initiation.

Abstract: An apparatus and method for carrying out and monitoring the progress and properties of multiple reactions is disclosed. The method and apparatus are especially useful for synthesizing, screening, and characterizing combinatorial libraries, but also offer significant advantages over conventional experimental reactors as well. The apparatus generally includes multiple vessels for containing reaction mixtures, and systems for controlling the stirring rate and temperature of individual reaction mixtures or groups of reaction mixtures. In addition, the apparatus may include provisions for independently controlling pressure in each vessel. In situ monitoring of individual reaction mixtures provides feedback for process controllers, and also provides data for determining reaction rates, product yields, and various properties of the reaction products, including viscosity and molecular weight.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Abstract: A method and apparatus for reacting a plurality of different mixtures in parallel in a semi-batch or continuous mode is provided. Each reaction is contained within a reactor vessel, the reactor vessels combined into a reactor block. Reactant(s) to be added during the reaction are kept in a header barrel, which has a plunger to feed reactant(s) from the header barrel through a transfer line into the reactor vessel. The plunger is moved using a drive system. The header barrels are optionally combined in a header block. The header block is sealed to a plate containing the transfer lines, which in turn is sealed to the reactor block. A latch mechanism is provided for easy sealing of the reactor and header blocks to the plate. The entire apparatus may be placed on a rocker or rotating plate for mixture as the reaction is proceeding.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. In preferred high-temperature embodiments, the polymer sample is maintained at a temperature of not less than about 75° C. during sample preparation, loading into a liquid chromatography or flow-injection analysis system, injection into a mobile phase of a liquid chromatography or flow-injection analysis system, and/or elution from chromatographic column. The described methods, systems, and device have primary applications in combinatorial polymer research and in industrial process control.

Abstract: Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.