High-temperature characterization of polymers

A method for characterizing a polymer sample, the method comprising

• withdrawing a polymer sample from a sample container into an injection probe of an auto-sampler, the injection probe being heated to maintain the withdrawn sample at a temperature of not less than about 75° C. while resident in the injection probe, the heated injection probe residing in a first environment maintained at about ambient temperature,
• loading at least a portion of the withdrawn sample into an injection port or a loading port of a flow-injection analysis system, the injection port being adaptable for fluid communication with a continuous-flow detector,
• injecting the loaded sample into a mobile phase of the flow-injection analysis system,
• detecting a property of the sample or of a component thereof, and
• maintaining the sample at a temperature of not less than about 75° C. during a period of time including from when the sample is withdrawn from the sample container to when the property of the sample or of a component thereof is detected.

A method for characterizing a polymer sample, the method comprising

• loading a polymer sample into a liquid chromatography system,
• maintaining the loaded polymer sample at a temperature of not less than 75° C.,
• eluting one or more sample components of the polymer sample with a mobile-phase eluant having a temperature of not less than about 75° C.,
• controlling the composition of the mobile-phase eluant to vary over time to separate at least one sample component of the sample from other sample components thereof, and
• detecting a property of at least one of the separated sample components.

An apparatus for automated sampling of polymer samples for characterization, the apparatus comprising

• an injection probe having a surface defining a sample-cavity and an inlet port for fluid communication between the sample cavity and a polymer sample, the probe being adapted for fluid communication with an injection port or a loading port of a continuous-flow polymer characterization system,
• a microprocessor for controlling three-dimensional motion of the injection probe between various spatial addresses,
• a pump for withdrawing a polymer sample into the injection probe, and
• a temperature-control element in thermal communication with the injection probe for maintaining a polymer sample residing in the probe at a predetermined temperature or within a predetermined range of temperatures.

A method for characterizing a polymer sample, the method comprising

• withdrawing a polymer sample from a sample container into an injection probe of an autosampler, the injection probe being heated to maintain the withdrawn sample at a temperature of not less than about 100° C. while resident in the injection probe, the heated injection probe residing at a first spatial address in a first environment while withdrawing the polymer sample, the first environment being external to a second heated environment,
• moving the probe from the first spatial address to a second spatial address,
• loading at least a portion of the withdrawn sample into an injection port or a loading port of a high performance liquid chromatography system while the probe is at the second spatial address, the injection port or loading port being internal to the second heated environment and being adaptable for fluid communication with a chromatographic column, the chromatographic column being internal to the second heated environment, the second heated environment being maintained at a temperature of not less than about 100° C.,
• injecting the loaded sample into a mobile phase of the liquid chromatography system,
• maintaining the sample at a temperature of not less than about 100° C. during a period of time including from when the sample is withdrawn from the sample container to when the sample is loaded into the injection port or loading port,
• chromatographically separating the injected sample, and
• detecting a property of the sample or of a component thereof.