A PRACTICAL GUIDE FOR THE PREPARATION OF SPECIMENS FOR X-RAY FLUORESCENCE AND X-RAY DIFFRACTION ANALYSIS EDITED BY VICTOR E. BUHRKE The Buhrke Company RON JENKINS International Centre for Diffraction Data OEANE K. SMITH Pennsylvania State University WI LEY-VCH . New York / Chichester / Weinheim / Brisbane / Singapore / Toronto
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A PRACTICAL GUIDE FOR THE PREPARATION OF SPECIMENS FOR X-RAY FLUORESCENCE AND X-RAY DIFFRACTION ANALYSIS
EDITED BY
VICTOR E. BUHRKE The Buhrke Company
RON JENKINS International Centre for Diffraction Data
OEANE K. SMITH Pennsylvania State University
~ WI LEY-VCH . New York / Chichester / Weinheim / Brisbane / Singapore / Toronto
CONTENTS
PREFACE xxi
INTRODUCTION xxlli
1 GENERAL INTRODUCTION 1
1.1 Sampling / 1
1.1.1 What Is Sampling? / 1
1.1.2 Kinds of Materials Sampled / 3
1.1.3 Record Keeping / 3
1.1.4 Meaningful Sampling / 3
1.1.5 Sampling for Scientific Investigation / 4
1.1.6 Sampling for Analytical Truth / 4
1.1.7 Matching Sampling Methodology with Analytical Goals-Heterogeneity / 5
1.2 Basic Statistical Definitions / 7
1.2.1 Introduction / 7
1.2.2 The Representative Sample / 7
1.2.3 Mean / 8
1.2.4 Dispersion / 9
1.2.5 Sampling Errors / 11
1.2.6 Replication / 13
1.2.7 Practicalities and Compromises / 14
1.3 Obtaining a Representative Sample from the Bulle / 15
1.4 Sampling Procedures / 16
1.4.1 Cone and Quartering / 17
1.4.2 Alternate Sh~veling / 18
lx
X CONTENTS
1.4.3 Linear Japan Cake / 18 1.4.4 Riffle Splitting / 19 1.4.5 Sectorial Splitting / 19
1.4.6 The Holistic Approach to Sampling / 20 1.5 Methods of Comminuting Powders for X-ray Diffraction / 21
1.5.1 Requirements for an Ideal Specimen / 21 1.5.2 Ideal Particle Size for X-Ray Diffraction Applications / 22
1.6 Grinding for X-Ray Diffraction Applications / 22
1.6.1 Mechanical Grinding: Precautions and Considerations / 22
1.6.2 Dry Grinding for X-Ray Diffraction Applications / 23 1.6.3 Wet Grinding for X-Ray Diffraction Applications / 23 1.6.4 Types of Grinding / 25
3.11 Steel / 95 3.11.1 Evaluation of Grinding Materials / 96 3.11.2 Special Problems and Hints / 98_
3.12 Aluminum-Bearing Materials / 100 3.12.1 General Discussion of the Problem / 100 3.12.2 Specimen Preparation Procedure / 101 3.12.3 Special Problemsand Hints / 101
3.13 Alumina / 102 3.13.1 General Discussion / 102 3.13.2 Specimen Preparation Procedure for Aluminas / 102
CONTENTS XIII
3.13.3 Fusion Specimen Preparation for Aluminas / 103 3.13.4 Special Problemsand Hints / 103
3.14 Bath Electrolyte / 103 3.14.1 General Discussion ofthe Problem / 103 3.14.2 Specimen Preparation Procedure for Bath Samples / 104 3.14.3 Special Problemsand Hints / 104
3.15 Surface Waters / 105 3.15.1 Use oflon-exchange Resins / 105 3.15.2 Coprecipitation Methods for Surface Waters / 106 3.15.3 Surface Adsorption / 106 3.15.4 Other Concentration Methods / 106
3.16 Oil Analyses / 106 3.16.1 General Discussion ofthe Problem / 106 3.16.2 Special Problemsand Hints for Oil Analyses / 107
3.17 Coal Derivatives-Pitch and Asphalts / 108 3.17.1 General Discussion ofthe Problem / 108 3.17 .2 Selection of a Representative Sample of Pitch or
Asphalt / 108 J. 17 .3 Preparation of Pitch Specimens / 109 3.17.4 Special Problemsand Hints / 112 3.17 .5 Particle Size Effect in the Analysis of Silicon in
Pitch / 112 3.17 .6 General Discussion / 114
3.18 Leaves and Vegetation / 115 3.18.1 General Discussion / 115 3.18.2 Selection of a Representative Sample of Leaves or
Vegetation / 116 3.18.3 Collection of Leaves from a Tree / 116 3.18.4 Specimen Preparation / 117 3.18.5 Discussion / 118
4 SPECIMEN PREPARATION IN X-RAY DIFFRACTION
4.1 Common Problems in Preparing and Presenting Specimens for X-ray Diffraction / 123
4.2 Geometries of Diffraction Equipment / 125 4.3 Properties of Materials and Samples / 128
4.6 Preparing Specimens for Reference Patterns / 152 4.6.1 Preliminary Pattern / 152 4.6.2 Preparing Specimens for Accurate d-spacing
Measurements: Background Information / 153 4.6.3 Thin Specimen on Fiat Support / 154 4.6.4 Interna! Standard Pattern / 155 4.6.5 Intensity Patterns / 156 4.6.6 Long Duration Pattern / 156 4.6.7 Reference-Intensity-Ratio Pattern / 157
4.7 Processing Small Samples for Diffractometry / 157 4.7.1 Collecting or Concentrating Material for Analysis / 158 4.7.2 Preparing the Specimen / 160 4.7.3 Concentrating Phases in Large Bulle Samples / 161 4.7.4 Preparation ofMounts for Diffractometry / 161
4.8 Procedures for Specimen Preparation by Aerosol Suspensions / 162 4.8.1 lntroduction / 162