Capillary Tube Sample Presentation for X-ray Diffraction
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Solution Overview
Problem
Current sample presentation devices for radiation-based analytical equipment, such as X-ray diffraction, are limited by large volume reaction chambers that hinder rapid gas changes, cannot handle liquids or corrosive gases, and suffer from dead volumes and poor flow patterns, restricting kinetic data determination and real-world condition representation.
Innovation Solution
A sample presentation device featuring a capillary tube with coaxial connectors, an infrared radiant heater, and a thermocouple, allowing for adjustable positioning and heating, and using compression seals to maintain high pressures and temperatures, enabling the use of liquids and vapors in feed and product streams.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Temperature
If a large volume reaction chamber is used, then the sample can be inserted on a plate-like sample holder and heated to high temperatures, but the gas changeover time is prolonged and dead volumes are created
Solution Approach 1:
The invention divides the reaction chamber into a capillary tube configuration instead of a large volume chamber, segmenting the sample presentation area to eliminate dead volumes and enable rapid gas exchange while maintaining heating capability
Solution Approach 2:
The invention transitions from a planar plate-like sample holder to a three-dimensional capillary tube structure, allowing gas flow through the entire sample volume and eliminating the dead space problems associated with two-dimensional sample presentation
2Reliability
If beryllium or similar X-ray invisible windows are used, then the reaction chamber can be sealed, but the temperature and pressure ranges are limited
Solution Approach 1:
The invention changes the material parameters of the reaction chamber from beryllium windows with limited temperature/pressure tolerance to a capillary tube design that can withstand higher temperatures and pressures while maintaining X-ray transparency through its geometric structure
Solution Approach 2:
The invention uses a composite approach combining the capillary tube material with the surrounding heating and sealing mechanisms, allowing the system to achieve high temperature and pressure resistance without relying on limited-window materials
3Illumination intensity
If a plate-like sample holder is used, then the sample can be presented to X-ray radiation, but dead volumes are created and plug flow pattern is poor
Solution Approach 1:
The invention segments the sample presentation from a continuous plate into a capillary tube structure, creating defined flow paths that eliminate dead volumes while maintaining adequate X-ray exposure through the tube walls
Solution Approach 2:
The invention applies fluid dynamics principles by designing the capillary tube to facilitate laminar plug flow through its circular cross-section, eliminating the poor flow patterns and dead zones characteristic of plate-like configurations
4Reliability
If the reaction chamber is designed for dry conditions, then corrosion is avoided, but liquids and vapors cannot be used in feed or product streams
Solution Approach 1:
The invention changes the operating parameters from dry condition limitations to a design that accommodates liquids and vapors by using a capillary tube configuration that prevents corrosion through its geometric design and material selection
Solution Approach 2:
The invention creates a universal reaction chamber design that can handle multiple fluid types including gases, liquids, and vapors, eliminating the need for dry condition-only operation while maintaining corrosion resistance
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
Enables rapid gas changes, accurate temperature control, and near-ideal plug flow, facilitating kinetic data collection and reducing turn-over time in materials screening, while being cost-effective and compatible with commercial X-ray diffraction equipment.
Implementation Method 1
at least one radiant heater radially offset from the axis of the coaxial connectors for heating, in use, a capillary tube mounted by way of the coaxial connectors
Implementation Method 2
a thermocouple associated with that sleeve is employed to measure the temperature of the sleeve
Data Source
AI summary
A sample presentation device for radiation-based analytical equipment comprising a mounting base, a carrier carried by, and adjustable in position, relative to the mounting base, and an arm extending from the carrier and having at its opposite end a terminal member; Each of the carrier and terminal member has a coaxial connector for receiving two opposite end regions of a capillary tube that forms, in use, a reaction cell; A radiant heater, typically an infrared heater, is radially offset from the axis of the coaxial connectors for heating, in use, a capillary tube mounted by way of the coaxial connectors; The carrier and terminal member preferably have heaters associated therewith for heating the flow passages through them; The terminal member preferably has a passage generally coaxial with the connector for receiving a communications conductor carrying a temperature sensor at its end that is operatively located generally centrally within a capillary.