Integrated aTREF-rGPC Polymer Characterization System

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Solution Overview

Problem

Current methods for polymer microstructure characterization, specifically the combination of temperature rising elution fractionation (TREF) and gel permeation chromatography (GPC), are inefficient due to offline processing requirements and limited ability to differentiate between polymers with similar melting points and varying molecular weights, leading to lengthy analysis times of several months.

Innovation Solution

An integrated analytical method and device that concurrently determines chemical composition and molecular weight distribution using analytical temperature rising elution fractionation (aTREF) and rapid gel permeation chromatography (rGPC), enabling online and real-time analysis through a synchronized system with a valve scheme and computer control, allowing for rapid characterization of polymer samples.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If offline processing of polymer sample fractions is used, then comprehensive characterization data can be obtained, but analysis time increases to two to three months

Engineering Contradiction:

Improvecharacterization data completenessVSAvoidanalysis time

Core Design Contradiction:

Measurement precisionVSLoss of time

Solution Approach 1:

The patent combines aTREF and GPC analyses into a single integrated system where polymer fractions are simultaneously separated by crystallizability (aTREF) and molecular weight (GPC) in one continuous process, eliminating the need for separate offline processing steps and reducing total analysis time from months to hours

Inventive Principle:

Principle #5Merging (Combining)

Solution Approach 2:

The patent implements continuous online analysis where the aTREF column effluent is continuously fed to the GPC column without interruption, maintaining continuous separation and detection throughout the analysis process, thereby eliminating idle time between sequential offline measurements

Inventive Principle:

Principle #20Continuity of useful action

2Measurement precision

If aTREF analysis alone is used, then polymer composition can be determined, but molecular weight distribution information is not provided

Engineering Contradiction:

Improvecomposition determinationVSAvoidmolecular weight distribution data

Core Design Contradiction:

Measurement precisionVSLoss of information

Solution Approach 1:

The patent merges aTREF and GPC capabilities into a single integrated instrument where the aTREF column is directly coupled to the GPC column, allowing simultaneous determination of both polymer composition (from aTREF) and molecular weight distribution (from GPC) for the same sample without requiring separate analyses

Inventive Principle:

Principle #5Merging (Combining)

Solution Approach 2:

The integrated system provides multi-functionality by enabling the same instrument to perform both aTREF analysis (for composition and crystallizability) and GPC analysis (for molecular weight distribution), making the system universally applicable for comprehensive polymer characterization

Inventive Principle:

Principle #6Universality (Multi-functionality)

3Quantity of substance

If pTREF fractionation is used, then sufficient sample can be generated, but thermal history differences make data not applicable to aTREF

Engineering Contradiction:

Improvesample amountVSAvoiddata applicability

Core Design Contradiction:

Quantity of substanceVSReliability

Solution Approach 1:

The patent performs preliminary fractionation of the polymer sample into discrete temperature slices using aTREF before the GPC analysis, ensuring that the thermal history is controlled and standardized from the outset. This preliminary action ensures that the subsequent GPC analysis reflects the same thermal conditions, making the data directly applicable and eliminating the need for separate pTREF preparation

Inventive Principle:

Principle #10Preliminary action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach significantly reduces analysis time to less than 8 hours, providing comprehensive and efficient characterization of polymer samples by integrating aTREF and rGPC, enabling simultaneous determination of composition and molecular weight distribution in a fully online process.

Implementation Method 1

The fractionation may be performed across a temperature gradient

Methodology Applied

Scientific EffectTemperature gradient: Temperature Gradient

Implementation Method 2

Temperature rising elution fractionation (TREF) separates polymeric molecules based on their crystallizability

Methodology Applied

Scientific EffectCrystallization: Crystallisation

Implementation Method 3

Gel permeation chromatography (GPC), also known as size-exclusion chromatography (SEC), is a useful technique for characterizing the molecular weight or molecular weight distribution (MW/MWD) of a polymer sample

Methodology Applied

Scientific EffectSize exclusion chromatography: Molecular Sieve

Data Source

PatentUS8722416B2Integrated on-line two-dimensional method and device for synchroned analytical temperature rising elution fractionation and gel permeation chromatography

Publication Date: 2014.05.13 CHEVRON PHILLIPS CHEMICAL COMPANY LP

AI summary

An analytical method comprising performing a first fractionation of a polymer sample based on differences in crystallizability to provide a first set of sample fractions, performing a first analysis on the first set of sample fractions, performing a second fractionation of the first set of sample fractions to produce a second set of sample fractions, performing a second analysis on the second set of sample fractions, and synchronizing the first fractionation and second fractionation to provide about concurrent analysis of the polymer sample.