Elemental Analysis in Geochemistry, Volume 8

Preface

Chapter 1. Introduction

Chapter 2. Preparation and Decomposition of Samples

Preparation of samples

Common types of samples and methods of sampling

Sample size

Diminution of samples

Contamination of samples during preparation

Storage and care of samples

Decomposition of samples

Undecomposed sample powders and their use

Solution techniques

Fluxing techniques

Special fluxing techniques

Contamination of samples during decomposition

Storage of decomposed samples

Chapter 3. Statistical Evaluation and Sampling

Chapter 4. Factors Influencing the Selection of Methods of Separation and Analysis

Separation of elements

Gravimetric "absolute" methods

Instrumental nondestructive methods

Volumetric methods

Colorimetric methods

Flame-photometric methods

Atomic absorption

Emission spectroscopy

Chapter 5. Some Methods of Extraction and Ion Exchange Separation

Separation by extraction

Separation methods by ion exchange resins

Procedure to determine the capacity of a resin

Ion exchange separation method for systematic analysis of silicate rocks by Shibata

Chapter 6. The Classical Qualitative Separation Scheme

Chapter 7. Classical Gravimetric and Other Methods

Silicon

Gravimetric determination as silica, SiO2

Aluminum

Gravimetric method

Determination of aluminum by the oxine method

Iron

Ferric or total iron, volumetric procedure

Ferrous iron, volumetric procedure

Calcium

Procedure

Magnesium

Gravimetric procedure

EDTA titration methods for calcium and magnesium

Sodium and potassium

Decomposition of sample

J. Lawrence Smith method

Potassium Perchlorate method

Potassium tetraphenylboron method

Sodium as uranyl zinc acetate

Titanium

Titanium as peroxide

Manganese

Separation and determination of manganese

Colorimetric determination of manganese

Phosphorus

Gravimetric determination

Ammonium phosphomolybdate method

Precipitation of magnesium ammonium phosphate hexahydrate

Carbon

Simplified method

Combination of classical acid decomposition and combustion methods

Hydrogen and water

Total water

The Penfield method

Fluorine

Decomposition and preparation of fluorine-bearing samples

Sulfur

Gravimetric determination as barium sulfate

Decomposition of sulfide samples by aqua regia and bromine

The zinc oxide-sodium carbonate fusion

Barium

Procedure

Chlorine

Sample decomposition

Gravimetric method for chlorine as silver chloride, AgCl

Zirconium

Decomposition of samples

Silica determination in zirconium-bearing materials

Zirconium as phosphate

Zirconium as mandelate

Chromium

Decomposition of samples

Boron

Decomposition of the sample

Titrimetric procedure

Gravimetric method

Lead

Decomposition of samples

Titrimetric method

Titration of the lead Chromate by ferrous ammonium sulfate

Nickel

Decomposition of samples

Copper

Electro-gravimetric procedure

Zinc

Gravimetric procedure for zinc in silicates

Titrimetric methods

Chapter 8. Classical Volumetric Methods

Normality and molarity

Procedure for total iron

Acid-base titrations

The silver reductor

The Jones reductor

Chapter 9. Emission Flame Spectrophotometry

Introduction

Instrumentation

Preparation of sample

Removal of interfering anions

Determination of sodium, potassium, calcium (and magnesium)

Beer's law

Chapter 10. Atomic Absorption Spectroscopy

Introduction

Instrumentation and methods

Methods

Determination of magnesium

Standards for atomic absorption

Chapter 11. Instrumental Nondestructive Analysis

Introduction

Electromagnetic radiation

Atom as a source of electromagnetic radiation

Separation, detection, and measurement of the electromagnetic radiation

Scintillation counters

Semiconductor detectors

Chapter 12. X-ray Emission Analysis

Introduction

Precision in X-ray emission analysis

Methods in X-ray spectrochemistry

Procedure for pelletizing

Chapter 13. Fast-Neutron Activation Analysis

Introduction

Fast-neutron generators

Laboratories shielded for fast-neutron activation analysis

Determination of oxygen by fast-neutron activation

Procedure

Determination of silicon by fast-neutron activation

Procedure

Appendix 1. Gravimetric Factors

Appendix 2. Analytical Quality Reagents for Stock Solutions in Atomic-Absorption and Emission-Flame Analysis

Bibliography

Index

Elemental Analysis in Geochemistry: A. Major Elements provides an introduction to basic classical and modern instrumental ""macro"" methods for geochemical research. The intention is to acquaint the beginning analyst or geochemist with the minimum of analytical methods required to satisfactorily perform a complex silicate or similar analysis. By combining classical and modern instrumental methods in one book, strong emphasis is put on the importance of the analyst's ability to grasp the general structure and relation of some of the most frequently used analytical techniques.
The book begins with basic concepts such as the preparation and decomposition of samples; statistical evaluation; and methods of separation and analysis. It outlines the classical qualitative separation scheme, which is very useful in understanding the analytical problems of complex mixtures, especially when hydrogen sulfide group metals are present. It discusses analytical techniques such as the detection and quantitative gravimetric analysis of silicon; volumetric or titrimetric methods; emission photometric analysis; atomic absorption spectroscopy; nondestructive instrumental methods; methods in X-ray spectrochemistry; and developments in neutron activation analysis.