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Rev. 0
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Reliable Measurements: A Guidebook for Trace Analysts
Foundations
1. Laying the Foundation
i. What is Trace Analysis?
ii. Stages of a Trace Analysis
iii. Training
iv. Recommended References
Sample Collection
2. Planning the Project
i. Overview
ii. Defining The Problem
iii. Detection Limits and Uncertainties
iv. Constructing the Sampling Plan
3. Sampling and Sub-sampling
i. Overview
ii. Sampling Publications
iii. Developing the Sampling Plan
iv. Constructing the Sampling Plan
v. Different Approaches to Sampling
vi. Sub-sampling
vii. Determination of Sampling and Sub-Sampling Errors
viii. Contamination Issues During Sampling;
Geological
Soils
Air
Water
Biological
Contamination Data
Contamination From Speciation Change
Sample Preparation
4. An Introduction to Sample Preparation
i. Overview
ii. Preliminary Issues
iii. Selecting a Sample Preparation Method
5. Container Material Properties
i. Materials;
Borosilicate Glass
Porcelain
Quartz
Platinum
Graphite
Plastics
ii. The Purity and Cleaning of Plastics
6. Container Transpiration
i. Overview
ii. Initial Transpiration Study
iii. Additional Transpiration Studies
iv. Summary of Findings
7. Stability of Elements at ppb Concentration Levels
i. Overview
ii. Adsorption
iii. PPB Stability Study
iv. Summary of Findings
Contamination
8. Environmental Contamination
i. Overview
ii. Reducing Environmental Contamination
iii. Avoiding Environmental Contamination
9. Contamination From Reagents
i. High Purity Water
ii. Storage of High Purity Water;
Quartz
HDPE and LDPE
Fluoropolymers
High Purity Acids
iii. Other Reagents
10. Contamination From the Analyst and Apparatus
i. Contamination From the Analyst;
Common Contaminants
Tips for the Analyst
ii. Apparatus Contamination;
A Closer Look at Quartz
Apparatus Tips
Preparation Techniques
11. Acid Digestions of Inorganic Samples
i. Overview of Sample Preparation Techniques
ii. Nitric Acid Digestions;
Facts About Nitric Acid
12. Acid Digestions of Organic Samples
i. Nitric and Perchloric Acid Digestions
ii. Sample Preparation Procedure;
Introduction and Scope
Apparatus and Chemicals
Glassware Cleaning
Sample Handling, Identification, and Storage
Sample Preparation of Tissues and Serum
iii. Microwave Digestion References
13. Sample Preparation by Fusion
i. Useful Fusions for Trace Analysts
ii. Lithium Carbonate Fusions
iii. Sample Preparation Procedure;
Scope and Summary
Equipment
Chemicals
Standard Preparation
Sample Preparation
14. Ashing
Ashing Techniques
Advantages of Ashing
Disadvantages of Ashing
Examples of Ashing Procedures
Sample Measurement
15. ICP-OES Measurement
i. Line Selection;
Sensitivity
Precision
Spectral Interferences
Standard Preparation
Example of a Method
(PDF file, 25K)
ii. Matrix Effects
16. ICP-MS Measurement
i. ICP-MS References
ii. Resolution
iii. Interferences;
Isobaric Interference
Polyatomic (Molecular) Interferences
Doubly Charged Ion Interferences
iv. Matrix Effects;
Space Charge Effects
Salt Buildup
v. Quantitative Analysis Measurement Techniques;
External Calibration using Calibration
Standard Additions
Isotope Dilution
Conclusions
17. Method Validation
i. Purpose of Method Validation
ii. References: The Validation Process
iii. Confirm Basic Performance Criteria
iv. Robustness
v. Collaborative and Cooperative Testing
vi. Concluding Statement
ICP Operations: A Guide for New ICP Users
Multi-Element Standard Blends
1. Elemental and Matrix Compatibility
i. Nitric Acid Matrices
ii. Hydrochloric Acid Matrices
iii. Water at pH of 7
iv. Hydrofluoric Acid Matrices
v. Sulfuric Acid Matrices
vi. Phosphoric Acid Matrices
2. ICP Quality Issues
i. Accuracy
ii. Purity
iii. Chemical Compatibility
iv. Stability
v. Availability
vi. Documentation
vii. Traceability
3. Handling, Calculations, Preparation, and Storage
i. Handling
ii. Calculations
iii. Preparation;
> Weight ≠ Volume
> Acid Content
> Acid Content in Molarity
> Avoiding Precipitates
iv. Storage
Sample Introduction
4. Sample Introduction Systems
i. System Components
ii. Troubleshooting;
> Connection Checks
> Spray Chambers
> Peristalic Pump Tubing
iii. Maintenance
5. Nebulizers, Spray Chambers, and Torches
i. Nebulizers;
> Pneumatic Nebulizers
> Ultrasonic Nebulizers
ii. Spray Chambers
iii. Torches
iv. Considerations
6. Compatibility and Precision Issues
i. Solutions Containing HF;
> When HF Attacks
> Glass Introduction Systems
> Recommendations
ii. High Disovled Solids
iii. Suspended Solids
iv. Closing Remarks
Performance Characteristics
7. Linearity and Detection Limits
i. Defining ICP Performance Characteristics;
> Examples of Spectra
ii. Confirm Basic Performace Criteria
8. Spectral Interferences: Types, Avoidance, and Correction
i. Types: ICP-OES
ii. Avoidance: ICP-OES
iii. Correction: ICP-OES;
> Background Interference
> Spectral Overlap
iv. Types: ICP-MS
v. Avoidance: ICP-MS
9. Key Instrument Parameters
i. Gas Flow Rates;
> Sample Ar Gas Flow for ICP-OES
ii. Applied Power for ICP-OES
Calibration Techniques
10. Calibration Curve and Standard Additions Techniques
i. Basic Considerations
ii. Calibration Standards;
> Recommendations
> Discussions
11. Internal Standardization and Isotope Dilution
i. Standard Additions
ii. Internal Standardization
iii. Isotope Dilution Mass Spectrometry
Problem Elements
12. Common Problems with Hg, Au, Si, Os, and Na
i. Mercury (Hg)
ii. Gold (Au)
iii. Silicon (Si)
iv. Osmium (Os)
v. Sodium (Na)
13. Common Problems with Ag, As, S, Ba, Pb, and Cr
i. Silver (Ag)
ii. Arsenic (As)
iii. Sulfur (S)
iv. Barium (Ba)
v. Lead (Pb)
v. Chromium (Cr)
Basic Calculations
14. Accuracy, Precision, Mean and Standard Deviation
i. Accuracy
ii. Precision
iii. Mean
iv. Standard Deviation
15. Significant Figures and Uncertainty
i. Significant Figures
ii. Uncertainty;
> Recommended Reading
16. Traceability
i. Background
ii. Terms and Explanations
iii. Discussion
Sample Preparation Guide: Considerations In the Preparation of Elemental Chemical Solutions
1. Guide Overview
i. Background
ii. Topics
iii. Resources
iv. References
2. Lithium, Sodium, Potassium, Rubidium and Cesium
i. The Metals
ii. Minerals — Natural and Manufactured
iii. Water and Acid Soluble Material
iv. Organic Matrices;
> Wet Ash
> Sulfate Ash
v. Hydrolytic Stability, Preferred Matrices and More
vi. Detailed Elemental Profiles
3. Beryllium
i. The Metal
ii. BeO
iii. Minerals
iv. Alloys
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. Detailed Elemental Profile
4. Magnesium
i. The Metal
ii. Mg Oxide, Hydroxide, Carbonat
iii. Minerals and Ores
iv. Alloys
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. Detailed Elemental Profile
5. Calcium
i. The Metal
ii. Ca Oxide, Hydroxide, Carbonat
iii. Minerals and Ores
iv. Alloys
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. Detailed Elemental Profile
6. Strontium and Barium
i. The Metals
ii. Oxides, Hydroxides, Carbonates
iii. Minerals and Ores
iv. Alloys
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. Detailed Elemental Profile
7. Scandium
i. The Metal
ii. Sc Oxide, Hydroxide, Carbonate
iii. Minerals and Ores
iv. Alloys
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. Detailed Elemental Profile
8. Rare Earth Elements
i. The Metals
ii. Oxides, Hydroxides, and Salts
iii. Minerals
iv. Catalysts
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. ICP Measurement
viii. Detailed Elemental Profile
9. Thorium and Uranium
i. The Metals
ii. Oxides, Hydroxides, and Salts
iii. Minerals
iv. Catalysts
v. Organic Matrices
vi. Hydrolytic Stability and Preferred Matrices
vii. ICP Measurement
viii. Detailed Elemental Profile
10. Titanium
i. Sampling and Handling
ii. The Metal
iii. Ti Oxides
iv. Minerals and Ores
v. Alloys
vi. Organic Matrices
vii. Hydrolytic Stability and Preferred Matrices
viii. Detailed Elemental Profile
Guides and Articles
News Archive
Product Index
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Wavelength Calibration for ICP and ICP-MS
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