Sample Homogenization Loop for ppq ICP Trace Element Detection

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Inductively Coupled Plasma (ICP) spectrometry systems face challenges in accurately measuring low parts per quadrillion (ppq) levels of chemicals due to limitations in sample homogenization, leading to inaccurate detection of trace elemental concentrations, which is critical in stringent industrial processes like semiconductor fabrication.

Innovation Solution

A sample concentration and homogenization system that includes a first valve, an exchange column, a liquid mass-flow meter, and a homogenization valve, which concentrates and homogenizes samples to create a uniform distribution of chemical species, allowing for multiple analysis modes without peak timing restrictions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional sample introduction systems are used for ICP spectrometry, then the system structure is simple, but the measurement precision for ultra-low concentrations (ppq levels) is insufficient due to poor sample homogenization

Engineering Contradiction:
Improvedetection accuracy of trace elementsVSAvoidsystem complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The sample introduction system is divided into separate functional modules: a sample concentration system with exchange columns for different chemical elements, a homogenization system with dedicated loops and valves, and an ICP analysis system. This segmentation allows each module to be optimized independently for its specific function, improving overall measurement precision while managing complexity through modular design.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The system performs preliminary concentration and homogenization of samples before they reach the ICP spectrometer. Exchange columns pre-concentrate trace elements from large sample volumes, and homogenization loops ensure uniform distribution of chemical species prior to analysis, enabling accurate detection of ultra-low concentrations at ppq levels.

Inventive Principle:
Principle #10Preliminary action

2Measurement precision

If sample concentration and homogenization systems are implemented, then measurement precision for trace elements improves, but the device complexity increases due to additional components

Engineering Contradiction:
Improvedetection accuracy of trace elementsVSAvoidnumber of system components
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The homogenization system uses a single homogenization loop that can accommodate multiple exchange columns for different chemical elements. The same loop and pump system serve both concentration and homogenization functions, reducing the need for separate dedicated components for each function and managing overall device complexity.

Inventive Principle:
Principle #6Universality (Multi-functionality)

Solution Approach 2:

The homogenization loop acts as an intermediary between the concentration system and the ICP analysis system. It receives concentrated samples from exchange columns, ensures uniform distribution of chemical species through controlled circulation, and delivers homogenized samples to the nebulizer, mediating the transition from concentration to analysis.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Productivity

If manual sampling methods are used, then the device complexity is low, but the productivity for analyzing large numbers of samples is insufficient

Engineering Contradiction:
Improvesample analysis throughputVSAvoidautomation system complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The automated sampling system performs sample introduction, concentration, and homogenization without manual intervention. The system automatically cycles through exchange columns, controls valve operations for sample routing, and manages homogenization loop circulation, enabling high-throughput analysis of large numbers of samples while minimizing operator involvement.

Inventive Principle:
Principle #25Self-service

Solution Approach 2:

The system maintains continuous operation by automatically cycling through multiple exchange columns and samples without interruption. The homogenization loop continuously circulates samples to ensure uniform distribution, and the automated valve system continuously routes samples and reagents, eliminating idle time between analysis steps and maximizing productivity.

Inventive Principle:
Principle #20Continuity of useful 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

The system enables accurate detection of trace elements at ppq levels by ensuring a uniform sample distribution, allowing for simultaneous analysis of multiple chemical species and improving detection accuracy and efficiency in industrial processes.

Implementation Method 1

at least a first exchange column configured to retain at least one chemical of interest

Methodology Applied
Scientific EffectIon exchange: Ion Exchange

Implementation Method 2

a homogenization valve that introduces the concentrated sample into a sample homogenizer loop which creates a homogenized concentrated sample

Methodology Applied
Scientific EffectFluid mixing: Stirring

Implementation Method 3

a liquid mass-flow meter fluidically coupled with the valve and configured to measure at least one of a mass or volume of liquid passed through the first exchange column

Methodology Applied
Scientific EffectFlow measurement:

Implementation Method 4

ICP spectrometry employs electromagnetically generated partially ionized argon plasma which reaches a temperature of approximately 7,000K

Methodology Applied
Scientific EffectPlasma: Plasma

Implementation Method 5

the high temperature causes sample atoms to become ionized or emit light

Methodology Applied
Scientific EffectIonization: Ionisation

Implementation Method 6

measuring the spectra of the emitted mass or light allows the determination of the elemental composition

Methodology Applied
Scientific EffectAtomic emission spectroscopy: Luminescence

Data Source

PatentUS11823884B2Automated system for remote inline concentration and homogenization of ultra-low concentrations in pure chemicals
Publication Date: 2023.11.21 ELEMENTAL SCI
  • US11823884B2 patent drawing
  • US11823884B2 patent drawing
  • US11823884B2 patent drawing

AI summary

Systems and methods are described to concentrate and homogenize a remote sample for analysis. A sample concentration and homogenization system embodiment includes, but is not limited to, at least a first valve, at least a first column fluidically coupled to the first valve, a flow meter fluidically coupled with the first column when the first valve is in a first flow path configuration to measure an amount of the liquid sample passed through the first column, and a homogenization valve including a sample homogenizing loop in which the concentrated sample is homogenized.