Oxidation Sensitivity Analysis of Bituminous Binder via EPR

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Solution Overview

Problem

Current methods fail to effectively analyze the aging stability of bituminous binders, particularly their sensitivity to oxidation, especially for raw binders and long-term aging, which is crucial for evaluating their resistance to cracking and structural changes.

Innovation Solution

A method involving electronic paramagnetic resonance (EPR) analysis of bituminous binders to measure the integral of stable carbon-centered radicals, combined with accelerated aging through heating and pressure testing, allowing for the classification of binders based on their oxidation sensitivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional methods are used to analyze bituminous binder aging stability, then the analysis process is simple, but the reliability and accuracy for measuring oxidation sensitivity are insufficient

Engineering Contradiction:
Improveoxidation sensitivity measurementVSAvoidanalysis method complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent uses electron paramagnetic resonance (EPR) spectroscopy as an intermediary technique to detect stable carbon-centered radicals formed during oxidation. This intermediary method provides precise measurement of oxidation sensitivity by quantifying radical concentrations, which serve as indicators of aging progression, thereby resolving the contradiction between measurement precision and method simplicity.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent replaces conventional mechanical or chemical analysis methods with EPR spectroscopy, which uses electromagnetic radiation to detect unpaired electrons in radical species. This substitution enables accurate, non-destructive measurement of oxidation sensitivity without complex chemical preparations, addressing the contradiction between precision and complexity.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

2Adaptability or versatility

If existing EPR methods are applied to bituminous binders, then spectroscopic parameters can be measured, but they do not apply to raw bituminous binder or long-term aging assessment

Engineering Contradiction:
Improveapplicability to raw binder and long-term agingVSAvoidaging stability assessment reliability
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent changes the measurement parameters by focusing on stable carbon-centered radicals rather than transient radical species. This parameter change enables the method to be applied to raw bituminous binders and to assess long-term aging stability, as stable radicals persist and accumulate over time, providing reliable indicators of aging progression that existing methods cannot detect.

Inventive Principle:
Principle #35Parameter changes

3Duration of action of moving object

If accelerated aging through heating and pressure is applied, then long-term aging effects can be simulated, but the analysis time and process complexity increase

Engineering Contradiction:
Improveaging simulation durationVSAvoidanalysis time
Core Design Contradiction:
Duration of action of moving objectVSLoss of time

Solution Approach 1:

The patent applies preliminary accelerated aging treatment (heating and pressurization) to simulate long-term aging effects before EPR analysis. This preliminary action condenses years of natural aging into hours or days of controlled treatment, allowing rapid assessment of aging stability while maintaining reliability through the subsequent EPR measurement of stable radical formation.

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 method provides a rapid and reliable assessment of bituminous binder stability to oxidation, enabling classification and continuous monitoring, thereby ensuring resistance to aging and adapting production processes for improved quality.

Implementation Method 1

Electron paramagnetic resonance analysis of a sample of the bituminous binder and measurement of the integral of the signal of the stable carbon-centered radicals

Methodology Applied
Scientific EffectElectron paramagnetic resonance: Electron Paramagnetic Resonance

Implementation Method 2

The aging of a bituminous binder is primarily due to the presence of oxidation mechanisms

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 3

heating of said bituminous binder, followed by ii) heating under pressure of the bituminous binder

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 4

heating under pressure of the bituminous binder obtained at the end of step i)

Methodology Applied
Scientific EffectPressure: Pressure Increase

Data Source

PatentEP3887809B1Method for determining the sensitivity to oxidation of a bituminous binder by electron spin resonance
Publication Date: 2023.04.19 TOTALENERGIES ONETECH
  • EP3887809B1 patent drawingFigure 1
  • EP3887809B1 patent drawingFigure 2

AI summary

The invention relates to a method for analysing ageing stability, in particular by the sensitivity to oxidation, of a bituminous binder, comprising: a) electron spin resonance analysis of a sample of the bituminous binder and measurement of the integral of the signal of the stable carbon-centred radicals; b) accelerated ageing of the bituminous binder, comprising: i) heating the bituminous binder, followed by ii) heating under pressure of the bituminous binder obtained at the end of step i); c) electron spin resonance analysis of a sample of the aged bituminous binder obtained in step b) and measurement of the integral of the signal of the stable carbon-centred radicals; d) comparing the integral of the signal of the stable carbon-centred radicals of the bituminous binder obtained in step a) and that obtained in step c).