Quantitative X-ray Analysis via Absorption Correction

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Solution Overview

Problem

In X-ray diffraction measurements, transmission geometry is hindered by X-ray absorption in samples, making quantitative analysis challenging due to unknown absorption coefficients and variable sample thickness and composition, which complicates the determination of crystalline phases and elemental composition.

Innovation Solution

A method that involves making correction measurements by directing incident X-rays at a similar angle to the diffraction measurement and measuring background intensity at a slightly deviated angle, allowing for the calculation of a linear intensity ratio that cancels out absorption effects, enabling quantitative analysis without explicit knowledge of sample thickness.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If transmission geometry is used for X-ray diffraction measurements, then measurements can be made through the sample, but X-ray absorption in the sample makes quantitative analysis difficult

Engineering Contradiction:
Improvemeasurement geometryVSAvoidquantitative analysis accuracy
Core Design Contradiction:
Adaptability or versatilityVSMeasurement precision

Solution Approach 1:

The patent introduces an intermediary substance (reference material with known composition and thickness) placed in the same beam path as the sample. This intermediary serves as a reference that experiences the same absorption conditions, allowing the system to calculate and correct for absorption effects mathematically by comparing sample measurements to reference measurements taken under identical geometric and absorption conditions.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent changes the measurement parameters by taking measurements at multiple different incident angles and detector angles. By varying these angular parameters and applying the measured values to mathematical models that account for absorption paths, the system can calculate absorption coefficients and correct quantitative analysis results without needing to know the sample thickness in advance.

Inventive Principle:
Principle #35Parameter changes

2Strength

If sample thickness is increased to ensure sufficient sample strength, then sample handling is improved, but X-ray absorption increases making quantitative analysis more difficult

Engineering Contradiction:
Improvesample strengthVSAvoidquantitative analysis accuracy
Core Design Contradiction:
StrengthVSMeasurement precision

Solution Approach 1:

The reference material acts as a mediator that allows the system to measure and quantify absorption effects in thicker samples. By placing the reference material in the same beam path and measuring its attenuation, the system can calculate the absorption coefficient for the sample matrix, thereby correcting the quantitative analysis even when samples are thick enough to be handled properly.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent implements a feedback mechanism where the measured attenuation of the reference material provides information about the actual absorption conditions in the beam path. This measured feedback is used to calculate correction factors that are applied to the sample measurements, allowing the system to compensate for absorption effects in real-time based on actual measurement conditions.

Inventive Principle:
Principle #23Feedback

3Adaptability or versatility

If sample composition varies, then real-world applicability is improved, but absorption becomes a function of composition making quantitative analysis more complex

Engineering Contradiction:
Improvesample composition variabilityVSAvoidanalysis complexity
Core Design Contradiction:
Adaptability or versatilityVSDevice complexity

Solution Approach 1:

The reference material with known composition serves as a mediator that allows the system to determine the absorption characteristics of any sample composition. By measuring how the reference material is attenuated by the sample matrix, the system can calculate the effective absorption coefficient for that specific composition, thereby handling composition variability without increasing analysis complexity.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Ease of manufacture

If pressed powder samples are used with binder, then sample preparation is simplified, but binder absorbs X-rays and interferes with quantitative analysis

Engineering Contradiction:
Improvesample preparationVSAvoidquantitative analysis accuracy
Core Design Contradiction:
Ease of manufactureVSMeasurement precision

Solution Approach 1:

The reference material acts as an intermediary that allows the system to measure and quantify the total absorption effects including those from the binder. By placing the reference material in the beam path through the pressed powder sample, the system measures the combined attenuation from both the sample material and binder, then uses this information to calculate correction factors that account for the binder's absorption interference.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 results in a linear calibration curve for determining the concentration of components like free lime, reducing the impact of absorption and sample inhomogeneities, and providing accurate quantitative measurements despite significant X-ray absorption and variable composition.

Implementation Method 1

Absorption of electromagnetic waves that pass directly through a medium is characterised by the Beer-Lambert law where I0 is the original intensity, I the intensity after passing through the material, μ the mass attenuation coefficient of the material, ρ the material density and d the material thickness

Methodology Applied
Scientific EffectAbsorption (EM radiation): Absorption (EM radiation)

Implementation Method 2

X-ray diffraction measurements allow the determination of the elemental composition of a sample. In some applications however this is not enough and there is a need not merely to determine the elemental composition but also to determine structure parameters such as the crystalline phases of a sample

Methodology Applied
Scientific EffectX-ray diffraction: Diffraction

Data Source

PatentEP3064932B1Quantitative x-ray analysis
Publication Date: 2019.11.13 PANALYTICAL BV
  • EP3064932B1 patent drawingFigure 1~2
  • EP3064932B1 patent drawingFigure 3
  • EP3064932B1 patent drawingFigure 4

AI summary

A method of X-ray analysis measures X-ray diffraction in transmission. In order to carry out quantitative measurements, a background measurement is taken slightly away from the diffraction peak and the ratio of measured intensities used to correct for variations in sample composition.