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ICP Operations ICP Operations
A Guide for New ICP Users  [ Tell-A-Friend ]

By Paul Gaines, Ph.D.
Edited and prepared for the Web by Brian Brolin

This guide is intended for anyone operating and preparing samples and standards for measurement using ICP (ICP hereafter refers to either ICP-MS or ICP-OES). Our last guide, Reliable Measurements: A Guide for Trace Analysts, focused upon the task of achieving reliable trace measurements by ICP. This series will not focus on any single topic but rather upon a multitude of day-to-day tasks required by all ICP operators. The topics will be fundamental in nature and are intended as an aid for the analyst who is completely new or somewhat new to the technique of ICP.

Table of Contents

MULTI-ELEMENT STANDARD BLENDS

1.  Elemental and Matrix Compatibility
  1. Nitric Acid Matrices

  2. Hydrochloric Acid Matrices

  3. Water at pH of 7

  4. Hydrofluoric Acid Matrices

  5. Sulfuric Acid Matrices

  6. Phosphoric Acid Matrices

2.  ICP Quality Issues
  1. Accuracy

  2. Purity

  3. Chemical Compatibility

  4. Stability

  5. Availability

  6. Documentation

  7. Traceability

3.  Handling, Calculations, Preparation, and Storage
  1. Handling

  2. Calculations

  3. Preparation;
    > Weight ≠ Volume
    > Acid Content
    > Acid Content in Molarity
    > Avoiding Precipitates
  4. Storage

SAMPLE INTRODUCTION

4.  Sample Introduction Systems
  1. System Components

  2. Troubleshooting;
    > Connection Checks
    > Spray Chambers
    > Peristalic Pump Tubing
  3. Maintenance

5.  Nebulizers, Spray Chambers, and Torches
  1. Nebulizers;
    > Pneumatic Nebulizers
    > Ultrasonic Nebulizers
  2. Spray Chambers

  3. Torches

  4. Considerations

6.  Compatibility and Precision Issues
  1. Solutions Containing HF;
    > When HF Attacks
    > Glass Introduction Systems
    > Recommendations
  2. High Disovled Solids

  3. Suspended Solids

  4. Closing Remarks

PERFORMANCE CHARACTERISTICS

7.  Linearity and Detection Limits
  1. Defining ICP Performance Characteristics;
    > Examples of Spectra
  2. Confirm Basic Performace Criteria

8.  Spectral Interferences: Types, Avoidance, and Correction
  1. Types: ICP-OES

  2. Avoidance: ICP-OES

  3. Correction: ICP-OES;
    > Background Interference
    > Spectral Overlap
  4. Types: ICP-MS

  5. Avoidance: ICP-MS

9.  Key Instrument Parameters
  1. Gas Flow Rates;
    > Sample Ar Gas Flow for ICP-OES
  2. Applied Power for ICP-OES

CALIBRATION TECHNIQUES

10.  Calibration Curve and Standard Additions Techniques
  1. Basic Considerations

  2. Calibration Standards;
    > Recommendations
    > Discussions
11.  Internal Standardization and Isotope Dilution
  1. Standard Additions

  2. Internal Standardization

  3. Isotope Dilution Mass Spectrometry

PROBLEM ELEMENTS

12.  Common Problems with Hg, Au, Si, Os, and Na
  1. Mercury (Hg)

  2. Gold (Au)

  3. Silicon (Si)

  4. Osmium (Os)

  5. Sodium (Na)

13.  Common Problems with Ag, As, S, Ba, Pb, and Cr
  1. Silver (Ag)

  2. Arsenic (As)

  3. Sulfur (S)

  4. Barium (Ba)

  5. Lead (Pb)

  6. Chromium (Cr)

BASIC CALCULATIONS

14.  Accuracy, Precision, Mean and Standard Deviation
  1. Accuracy

  2. Precision

  3. Mean

  4. Standard Deviation

15.  Significant Figures and Uncertainty
  1. Significant Figures

  2. Uncertainty;
    > Recommended Reading
16.  Traceability
  1. Background

  2. Terms and Explanations

  3. Discussion


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