Rapid characterization of polymers
AssigneeSymyx Technologies, Inc.
InventorsAdam Safir, Miroslav Petro, Ralph B. Nielsen, Thomas S. Lee, Jean M. J. Fréchet
Life of this patent
Estimating the term…
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.
Claims112
A method for characterizing a combinatorial library of non-biological polymer samples, the method comprising
- providing a combinatorial library comprising four or more spatially separated non-biological polymer samples, the four or more polymer samples being polymerization polymer mixtures resulting from polymerization reactions that are varied with respect to a factor affecting polymerization,
- serially injecting the 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, 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.
A method for characterizing a combinatorial library of non-biological polymer samples, the method comprising
- providing a combinatorial library comprising a plurality of non-biological polymer samples, each of the plurality of polymer samples being polymerization polymer mixtures resulting from polymerization reactions that are varied with respect to a factor affecting polymerization and residing in separate sample containers,
- withdrawing a first non-biological polymer sample from a first sample container,
- injecting at least a portion of the withdrawn first sample into a mobile phase of a liquid chromatography system at a first injection time, tLCI1,
- chromatographically separating at least one sample component or polymer molecule of the injected first sample from other sample components or polymer molecules thereof in a chromatographic column,
- detecting a property of at least one of the separated sample components or polymer molecules of the first sample,
- withdrawing a second non-biological polymer sample from a second sample container,
- injecting at least a portion of the withdrawn second sample into the mobile phase of the liquid chromatography system at a second injection time, tLCI2, the difference in time, tLCI2−tLCI1, being not more than about 10 minutes,
- chromatographically separating at least one sample component or polymer molecule of the injected second sample from other sample components or polymer molecules thereof in the chromatographic column, and
- detecting a property of at least one of the separated sample components or polymer molecules of the second sample.
A method for characterizing a combinatorial library of non-biological polymer samples, the method comprising
- providing a combinatorial library comprising four or more different, spatially separated, non-biological polymer samples, the four or more polymer samples being polymerization polymer mixtures resulting from polymerization reactions that are varied with respect to a factor affecting polymerization,
- serially injecting each of the forty-eight or more non-biological polymer samples into a mobile-phase of a liquid chromatography system, and
- determining a weight-average molecular weight of at least one chromatographically separated component or polymer molecule of each of the forty-eight or more samples with the liquid chromatography system, the average sample-throughput being not more than about 10 minutes per sample.
A method for characterizing a plurality of non-biological polymer samples comprising a polymerization product mixture, the method comprising
- (a) injecting a non-biological polymer sample into a mobile-phase of a liquid chromatography system,
- (b) chromatographically separating a low molecular-weight fraction of the injected sample from a high molecular-weight fraction thereof in a chromatographic column having a stationary-phase, the low molecular-weight fraction comprising sample components having molecular weights of not more than about 1000 D, the high molecular-weight fraction comprising sample components having molecular weights of more than about 1000 D,
- (c) passing the high molecular-weight fraction of the injected sample through the chromatographic column without substantial separation thereof,
- (d) detecting a property of the high molecular-weight fraction or of a component thereof, and
- (e) repeating steps (a), (b), (c) and (d) for the plurality of polymer samples.
A method for characterizing a combinatorial library of non-biological polymer samples, the method comprising
- providing a combinatorial library comprising a plurality of non-biological polymer samples, each of the plurality of polymer samples being polymerization polymer mixtures resulting from polymerization reactions that are varied with respect to a factor affecting polymerization,
- serially injecting the plurality of polymer samples into a mobile phase of a liquid chromatography system,
- chromatographically separating at least one sample component or polymer molecule of the injected samples from other sample components or polymer molecules thereof in a chromatographic column having a stationary-phase and an aspect ratio ranging from about 0.1 to about 1, and
- detecting a property of at least one of the separated components of the plurality of samples.
A method for characterizing a combinatorial library of non-biological polymer samples, the method comprising
- providing a combinatorial library comprising four or more non-biological polymer samples, the four or more polymer samples being polymerization polymer mixtures resulting from polymerization reactions that are varied with respect to a factor affecting polymerization,
- serially screening four or more non-biological polymer samples of the library for a first property of interest with a first flow characterization system, the first flow characterization system being a liquid chromatography system having an average sample throughput of not more than about 10 minutes per sample, the four or more polymer samples being screened by a method that includes injecting the four or more polymer samples into a mobile phase of the liquid chromatography system, chromatographically separating one or more components or polymer molecules of the four or more injected samples from other components or polymer molecules thereof, and detecting the first property of interest, and
- screening at least one of the four or more samples screened with the first characterization system for a second property of interest with a second characterization system.
The method of claims, 53, 60, 64 or 81 wherein at least one sample component or polymer molecule of the injected samples are separated from other sample components or polymer molecules thereof by size-exclusion chromatography.
A method for characterizing a plurality of polymer samples comprising a polymerization product mixture, the method comprising
- providing an array of four or more spatially separated polymer samples, and
- serially detecting a property of the four or more polymer samples or of components thereof with a liquid chromatography system at an average sample-throughput ranging from about 1 minute per sample to about 30 seconds per sample.
A method for characterizing a plurality of polymer samples comprising a polymerization product mixture, the method comprising
- providing an array of four or more spatially separated polymer samples, and
- serially detecting a property of the four or more polymer samples or of components thereof with a liquid chromatography system at an average sample-throughput of not more than about 30 seconds per sample.
Dependencies are inferred from the claim text.