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 Reliable Measurements
 
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Reliable Measurements Reliable Measurements
A Guidebook for Trace Analysts  [ Tell-A-Friend ]

By Paul Gaines, Ph.D.
Edited by Brian Brolin, John Fiorino, & Marge Gwynne

More than ever before, people are making decisions based on chemical measurements that affect us medically, environmentally, legally, and commercially. The reliability of these measurements is becoming a critical matter.

Dr. Paul Gaines presents an essential guide for trace analysts at any level of experience. Topics cover all phases of sample collection, preparation, measurement, and data analysis.

NOTE:  All references to trace analysis assume the use of either ICP-OES or ICP-MS for the purposes of this guide.

Table of Contents

FOUNDATIONS

1.  Laying the Foundation
  1. What is Trace Analysis?

  2. Stages of a Trace Analysis

  3. Training

  4. Recommended References

SAMPLE COLLECTION

2.  Planning the Project
  1. Overview

  2. Defining The Problem

  3. Detection Limits and Uncertainties

  4. Constructing the Sampling Plan

3.  Sampling and Sub-sampling
  1. Overview

  2. Sampling Publications

  3. Developing the Sampling Plan

  4. Constructing a Sampling Program

  5. Different Approaches to Sampling

  6. Sub-sampling

  7. Determination of Sampling and Sub-Sampling Errors

  8. Contamination Issues During Sampling;
    > Geological
    > Soils
    > Air
    > Water
    > Biological
    > Contamination Data
    > Contamination From Speciation Change

SAMPLE PREPARATION

4.  An Introduction to Sample Preparation
  1. Overview

  2. Preliminary Issues

  3. Selecting a Sample Preparation Method

5.  Container Material Properties
  1. Materials;
    > Borosilicate Glass
    > Porcelain
    > Quartz
    > Platinum
    > Graphite
    > Plastics
  2. The Purity and Cleaning of Plastics

6.  Container Transpiration
  1. Overview

  2. Initial Transpiration Study

  3. Additional Transpiration Studies

  4. Summary of Findings

7.  Stability of Elements at ppb Concentration Levels
  1. Overview

  2. Adsorption

  3. PPB Stability Study

  4. Summary of Findings

CONTAMINATION

8.  Environmental Contamination
  1. Overview

  2. Reducing Environmental Contamination

  3. Avoiding Environmental Contamination

9.  Contamination From Reagents
  1. High Purity Water

  2. Storage of High Purity Water;
    > Quartz
    > HDPE and LDPE
    > Fluoropolymers
    > High Purity Acids
  3. Other Reagents

10.  Contamination From the Analyst and Apparatus
  1. Contamination From the Analyst;
    > Common Contaminants
    > Tips for the Analyst
  2. Apparatus Contamination;
    > A Closer Look at Quartz
    > Apparatus Tips

PREPARATION TECHNIQUES

11.  Acid Digestions of Inorganic Samples
  1. Overview of Sample Preparation Techniques

  2. Nitric Acid Digestions;
    > Facts About Nitric Acid
12.  Acid Digestions of Organic Samples
  1. Nitric and Perchloric Acid Digestions

  2. Sample Preparation Procedure;
    > Introduction and Scope
    > Apparatus and Chemicals
    > Glassware Cleaning
    > Sample Handling, Identification, and Storage
    > Sample Preparation of Tissues and Serum
  3. Microwave Digestion References

13.  Sample Preparation by Fusion
  1. Useful Fusions for Trace Analysts

  2. Lithium Carbonate Fusions

  3. Sample Preparation Procedure;
    > Scope and Summary
    > Equipment
    > Chemicals
    > Standard Preparation
    > Sample Preparation
14.  Ashing
  1. Ashing Techniques

  2. Advantages of Ashing

  3. Disadvantages of Ashing

  4. Examples of Ashing Procedures

SAMPLE MEASUREMENT

15.  ICP-OES Measurement
  1. Line Selection;
    > Sensitivity
    > Precision
    > Spectral Interferences
    > Example of a Method (PDF file, 25K)
  2. Matrix Effects

16.  ICP-MS Measurement
  1. ICP-MS References

  2. Resolution

  3. Interferences
    > Isobaric Interference
    > Polyatomic (Molecular) Interferences
    > Doubly Charged Ion Interferences
  4. Matrix Effects
    > Space Charge Effects
    > Salt Buildup
  5. Quantitative Analysis Measurement Techniques
    > External Calibration using Calibration
    > Standard Additions
    > Isotope Dilution

CONCLUSIONS

17.  Method Validation
  1. Purpose of Method Validation

  2. References: The Validation Process

  3. Confirm Basic Performance Criteria

  4. Robustness

  5. Collaborative and Cooperative Testing

  6. Concluding Statement


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