Method and apparatus for rapid determination of fries rearrangement products in aromatic polycarbonate resins
OwnerJames Claude Carnahaninventor
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Abstract
A rapid analysis method for the determination of Fries rearrangement products in aromatic polycarbonate resins utilizes in-line determination of polymer concentration and in-line fluorescence detection of Fries rearrangement products. The method avoids time consuming sample preparation required by previous methods, allows for separation of interfering low molecular weight components, and is suitable for automation.
Claims27
A method for analysis of Fries rearrangement products in aromatic polycarbonate resins, comprising:
- providing an analytical sample comprising an aromatic polycarbonate;
- optionally, separating the analytical sample to yield a high molecular weight fraction;
- performing an in-line determination of aromatic polycarbonate concentration in the analytical sample;
- and
- performing an in-line determination of the fluorescence signal due to Fries rearrangement products in the analytical sample;
- wherein the total analysis time is not greater than about 5 minutes per sample.
A method for analysis of Fries rearrangement products in aromatic polycarbonate resins, comprising:
- providing a plurality of analytical samples each comprising aromatic polycarbonate;
- optionally, separating each analytical sample to yield a high molecular weight fraction;
- performing an in-line determination of aromatic polycarbonate concentration in each analytical sample;
- and
- performing an in-line determination of the fluorescence signal due to Fries rearrangement products in each analytical sample;
- wherein the total analysis time is not greater than about 5 minutes per sample.
A method for analysis of Fries rearrangement products in aromatic polycarbonate resins, comprising:
- providing an analytical sample comprising aromatic polycarbonate synthesized from at least one dihydric phenol comprising bisphenol A;
- optionally, separating the analytical sample to yield a high molecular weight fraction;
- performing an in-line determination of aromatic polycarbonate concentration in the analytical sample using differential refractive index detection;
- and
- performing an in-line determination of the fluorescence signal due to Fries rearrangement products in the analytical sample using an excitation wavelength of about 280 to about 360 nm and an emission wavelength of about 420 to about 650 nm;
- wherein the total analysis time is not greater than about 5 minutes per sample.
A system for analysis of Fries rearrangement products in analytical samples comprising aromatic polycarbonate, comprising:
- a solvent delivery system;
- an autoinjector for injecting a portion of the analytical sample;
- optionally, a chromatographic column for separating said analytical sample to yield a aromatic polycarbonate high molecular weight fraction;
- an in-line concentration detector for determining the aromatic polycarbonate concentration in the analytical sample;
- an in-line fluorescence detector for determining the fluorescence signal due to Fries rearrangement products in each analytical sample;
- wherein the system's total analysis time is not greater than 5 minutes per sample.
An analysis system, comprising:
- a sample preparation module for preparing a plurality of analytical samples, each sample being prepared by dissolving an aromatic polycarbonate resin in a suitable solvent.
- an autoinjector for injecting a portion of each analytical sample;
- a chromatographic column for separating each analytical sample to yield an aromatic polycarbonate high molecular weight fraction;
- an in-line concentration detector for determining the aromatic polycarbonate concentration in each analytical sample;
- an in-line fluorescence detector for determining the fluorescence signal due to Fries rearrangement products in each analytical sample;
- and
- a computer for calculating the concentration of Fries rearrangement products in the aromatic polycarbonate based on the aromatic polycarbonate concentration in the analytical sample and the concentration of Fries rearrangement products in the analytical sample, and for reversibly controlling the sample preparation module, the solvent delivery system, the autoinjector, the fluorescence detector, and the concentration detector;
- wherein the system's total analysis time is not greater than 5 minutes per sample;
- and wherein computer control of the sample preparation module, the solvent delivery system, the autoinjector, the fluorescence detector, and the concentration detector enables analysis of the plurality of samples without human intervention.
Dependencies are inferred from the claim text.