A Practical Guide for the Preparation of Specimens for X-Ray Fluorescence and X-Ray Diffraction Analysis

, by Buhrke, Victor E.; Jenkins, Ron; Smith, Deane K.

$A Practical Guide for the Preparation of Specimens for X-Ray Fluorescence and X-Ray Diffraction Analysis by Buhrke, Victor E.; Jenkins, Ron; Smith, Deane K., 9780471194583$

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ISBN: 9780471194583 | 0471194581
Cover: Hardcover
Copyright: 11/19/1997

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Summary

Author Biography

Supplemental Materials

* Contains useful bibliography and helpful references.

PREFACE

xxi

(2)

INTRODUCTION

xxiii

1 GENERAL INTRODUCTION

(34)

1.1 Sampling

(6)

1.1.1 What Is Sampling?

(2)

1.1.2 Kinds of Materials Sampled

(1)

1.1.3 Record Keeping

(1)

1.1.4 Meaningful Sampling

(1)

1.1.5 Sampling for Scientific Investigation

(1)

1.1.6 Sampling for Analytical Truth

(1)

1.1.7 Matching Sampling Methodology with Analytical Goals--Heterogeneity

(2)

1.2 Basic Statistical Definitions

(8)

1.2.1 Introduction

(1)

1.2.2 The Representative Sample

(1)

1.2.3 Mean

(1)

1.2.4 Dispersion

(2)

1.2.5 Sampling Errors

(2)

1.2.6 Replication

(1)

1.2.7 Practicalities and Compromises

(1)

1.3 Obtaining a Representative Sample from the Bulk

(1)

1.4 Sampling Procedures

(5)

1.4.1 Cone and Quartering

(1)

1.4.2 Alternate Shoveling

(1)

1.4.3 Linear Japan Cake

(1)

1.4.4 Riffle Splitting

(1)

1.4.5 Sectorial Splitting

(1)

1.4.6 The Holistic Approach to Sampling

(1)

1.5 Methods of Comminuting Powders for X-ray Diffraction

(1)

1.5.1 Requirements for an Ideal Specimen

(1)

1.5.2 Ideal Particle Size for X-Ray Diffraction Applications

(1)

1.6 Grinding for X-Ray Diffraction Applications

(4)

1.6.1 Mechanical Grinding: Precautions and Considerations

(1)

1.6.2 Dry Grinding for X-Ray Diffraction Applications

(1)

1.6.3 Wet Grinding for X-Ray Diffraction Applications

(2)

1.6.4 Types of Grinding

(1)

1.6.5 Effects of Grinding

(1)

1.7 Absorption Problems

(5)

1.7.1 Absorption of X-rays

(2)

1.7.2 Scattering and Diffraction of X-rays

(2)

1.7.3 Absorption in X-ray Fluorescence

(1)

1.7.4 Absorption in X-ray Diffraction

(1)

1.8 Crystallinity and Particle Effects in X-ray Diffraction Applications

(4)

2 SPECIMEN PREPARATION PROCEDURES IN X-RAY FLUORESCENCE ANALYSIS

(24)

2.1 Common Problems in Preparing and Presenting Specimens for X-ray Fluorescence

(1)

2.1.1 General

(1)

2.1.2 Types of Samples Analyzed

(1)

2.2 Presenting the Specimen to the Spectrometer

(3)

2.2.1 Physical Form of the Specimen in X-ray Fluorescence Analysis

(1)

2.2.2 Specimen Placement

(1)

2.2.3 Photochemical Decomposition

(1)

2.3 Handling Samples Without Pretreatment

(1)

2.4 Use of Pressed Powder Pellets

(1)

2.4.1 General

(1)

2.4.2 Direct Pelletizing of the Specimen

(1)

2.5 Lithium and Sodium Tetraborate Fusion Methods

(3)

2.5.1 Advantages of Fusion

(1)

2.5.2 Choice of Fusion Mixture

(1)

2.5.3 Choice of Reaction Crucible

(2)

2.5.4 Controlling the Fusion Reaction

(1)

2.6 Liquids and Solutions

(3)

2.6.1 General

(1)

2.6.2 Preconcentration Methods

(1)

2.6.3 Direct Methods

(1)

2.6.4 Concentration by Evaporation

(1)

2.6.5 Use of Ion-Exchange Resins

(1)

2.7 Handing Very Small Samples

(4)

2.7.1 Size of the Specimen in X-ray Fluorescence Analysis

(2)

2.7.2 Direct Analysis of Limited Quantities of Sample

(2)

2.8 Radioactive Samples

(1)

2.9 Special Problems with Low Atomic Number Elements

(8)

3 SPECIMEN PREPARATION IN X-RAY FLUORESCENCE

(64)

3.1 Whole Rock Analysis

(6)

3.1.1 General

(1)

3.1.2 Specimen Preparation Procedures

(4)

3.1.3 Special Problems and Hints

(1)

3.2 Limes, Dolomitic Limes, and Ferrolimes

(3)

3.2.1 General Discussion

(1)

3.2.2 Sampling

(1)

3.2.3 Specimen Preparation--Fused Glass Disk

(1)

3.2.4 Results

(1)

3.2.5 Discussion

(1)

3.3 Limestones, Dolomites, and Magnesites

(3)

3.3.1 General Discussion

(1)

3.3.2 The Pressed Powder Method

(2)

3.3.3 Determination of Carbon Dioxide, CO(2)

(1)

3.3.4 Calibration Standards

(1)

3.3.5 Results

(1)

3.4 Natural and By-product Gypsum

(5)

3.4.1 General Discussion

(1)

3.4.2 Remarks

(1)

3.4.3 Elements Determined

(1)

3.4.4 Dehydration of Gypsum

(1)

3.4.5 Drying of Gypsum

(1)

3.4.6 Grinding

(3)

3.4.7 Results

(1)

3.4.8 Reference Materials

(1)

3.4.9 Discussion

(1)

3.5 Glass Sands

(3)

3.5.1 General Discussion

(1)

3.5.2 Selection of a Representative Sample

(1)

3.5.3 Fusion with Lithium Tetraborate and Lithium Fluoride

(1)

3.5.4 Discussion

(1)

3.6 Cements, Clinker, and Raw Materials

(4)

3.6.1 Types and Compositions of Cements

(1)

3.6.2 Pressed Powder Briquet Preparation

(1)

3.6.3 Fused Bead Preparation

(1)

3.6.4 ASTM C 114 Qualification

(1)

3.7 Preparation of Metals

(5)

3.7.1 Sampling

(1)

3.7.2 Solubility of Elements

(2)

3.7.3 Alloy Metallographic Structure

(1)

3.7.4 Parameters Affecting the Analytical Surface Finish

(1)

3.7.5 Effective Thickness and Volume

(1)

3.7.6 Hardness

(1)

3.8 Aluminum and Its Alloys

(4)

3.8.1 Surface Preparation Techniques

(1)

3.8.2 X-ray Fluorescence Tests

(1)

3.8.3 Discussion of Selected Surface Preparation Techniques

(2)

3.9 Titanium

(1)

3.10 Cast Iron

(2)

3.10.1 General Discussion

(1)

3.10.2 Specimen Preparation Procedure

(1)

3.11 Steel

(5)

3.11.1 Evaluation of Grinding Materials

(2)

3.11.2 Special Problems and Hints

(2)

3.12 Aluminum-Bearing Materials

100

(2)

3.12.1 General Discussion of the Problem

100

(1)

3.12.2 Specimen Preparation Procedure

101

(1)

3.12.3 Special Problems and Hints

101

(1)

3.13 Alumina

102

(1)

3.13.1 General Discussion

102

(1)

3.13.2 Specimen Preparation Procedure for Aluminas

102

(1)

3.13.3 Fusion Specimen Preparation for Aluminas

103

(1)

3.13.4 Special Problems and Hints

103

(1)

3.14 Bath Electrolyte

103

(2)

3.14.1 General Discussion of the Problem

103

(1)

3.14.2 Specimen Preparation Procedure for Bath Samples

104

(1)

3.14.3 Special Problems and Hints

104

(1)

3.15 Surface Waters

105

(1)

3.15.1 Use of Ion-exchange Resins

105

(1)

3.15.2 Coprecipitation Methods for Surface Waters

106

(1)

3.15.3 Surface Adsorption

106

(1)

3.15.4 Other Concentration Methods

106

(1)

3.16 Oil Analyses

106

(2)

3.16.1 General Discussion of the Problem

106

(1)

3.16.2 Special Problems and Hints for Oil Analyses

107

(1)

3.17 Coal Derivatives--Pitch and Asphalts

108

(7)

3.17.1 General Discussion of the Problem

108

(1)

3.17.2 Selection of a Representative Sample of Pitch or Asphalt

108

(1)

3.17.3 Preparation of Pitch Specimens

109

(3)

3.17.4 Special Problems and Hints

112

(1)

3.17.5 Particle Size Effect in the Analysis of Silicon in Pitch

112

(2)

3.17.6 General Discussion

114

(1)

3.18 Leaves and Vegetation

115

(8)

3.18.1 General Discussion

115

(1)

3.18.2 Selection of a Representative Sample of Leaves or Vegetation

116

(1)

3.18.3 Collection of Leaves from a Tree

116

(1)

3.18.4 Specimen Preparation

117

(1)

3.18.5 Discussion

118

(5)

4 SPECIMEN PREPARATION IN X-RAY DIFFRACTION

123

(48)

4.1 Common Problems in Preparing and Presenting Specimens for X-ray Diffraction

123

(2)

4.2 Geometries of Diffraction Equipment

125

(3)

4.3 Properties of Materials and Samples

128

(6)

4.3.1 Crystallite Statistics

128

(4)

4.3.2 Specimen Configurations

132

(2)

4.4 Effects of Crystal Properties on Specimens

134

(7)

4.4.1 Crystallite Size and Particle Size

134

(1)

4.4.2 Specimen and Sample Homogeneity

134

(1)

4.4.3 Crystallite Perfection and Peak Shapes

135

(1)

4.4.4 Peak Resolution in Complex Patterns

136

(1)

4.4.5 Particle Shapes and Preferred Orientation

136

(1)

4.4.6 Absorption Effects and Depth of Penetration

137

(1)

4.4.7 Microabsorption

138

(1)

4.4.8 Background

139

(1)

4.4.9 Surface Roughness

140

(1)

4.4.10 Crystal Perfection and Extinction

140

(1)

4.5 Preparing Specimens for Simple Routine Analysis

141

(11)

4.5.1 Goal of Specimen Preparation

141

(1)

4.5.2 Flat Specimen Supports

141

(1)

4.5.3 The Cavity Mount

142

(1)

4.5.4 Slurry Mounts

143

(2)

4.5.5 Alternative Cavity Mounting Techniques, Back-loading Cavity Mounts

145

(3)

4.5.6 Alternative Cavity Mounting Techniques, Side-Drifted Specimens

148

(1)

4.5.7 Alternative Flat Surface Techniques, Top Dusted Mounts

149

(2)

4.5.8 Creating Spheroidal Particle Aggregates

151

(1)

4.5.9 Bonded Specimens

151

(1)

4.6 Preparing Specimens for Reference Patterns

152

(5)

4.6.1 Preliminary Pattern

152

(1)

4.6.2 Preparing Specimens for Accurate d-spacing Measurements: Background Information

153

(1)

4.6.3 Thin Specimen on Flat Support

154

(1)

4.6.4 Internal Standard Pattern

155

(1)

4.6.5 Intensity Patterns

156

(1)

4.6.6 Long Duration Pattern

156

(1)

4.6.7 Reference-Intensity-Ratio Pattern

157

(1)

4.7 Processing Small Samples for Diffractometry

157

(5)

4.7.1 Collecting or Concentrating Material for Analysis

158

(2)

4.7.2 Preparing the Specimen

160

(1)

4.7.3 Concentrating Phases in Large Bulk Samples

161

(1)

4.7.4 Preparation of Mounts for Diffractometry

161

(1)

4.8 Procedures for Specimen Preparation by Aerosol Suspensions

162

(9)

4.8.1 Introduction

162

(1)

4.8.2 Simple Aspirator Bottles

163

(2)

4.8.3 Tubular Aerosol Suspension Chamber (TASC)

165

(4)

4.8.4 Microhood for Special Materials

169

(2)

5 SPECIFIC AREAS OF SPECIMEN PREPARATION IN X-RAY POWDER DIFFRACTION

171

(46)

5.1 Ceramics

171

(4)

5.1.1 Powders of Stable and Common Ceramics

171

(1)

5.1.2 Specimen Mounting of Ceramic Materials

172

(1)

5.1.3 Atmospheric-sensitive or Toxic Ceramics

172

(2)

5.1.4 Ceramic Compacts or Ceramic Thin Films

174

(1)

5.2 Preparation of Bulk Metals and Alloys

175

(4)

5.2.1 General Discussion of the Problem

175

(1)

5.2.2 Specimen Preparation Procedures for Metals

175

(2)

5.2.3 Special Problems and Hints

177

(1)

5.2.4 Step-by-step Procedure for Metals

178

(1)

5.3 Minerals

179

(6)

5.3.1 Analysis of Minerals

180

(1)

5.3.2 Beneficiation of Minerals

180

(3)

5.3.3 Identification of Sedimentary Minerals

183

(1)

5.3.4 Determination of Crystalline Silica

183

(2)

5.4 Aluminum Ores

185

(2)

5.4.1 Grinding Samples of Aluminum Ores

186

(1)

5.4.2 Packing of the Specimen

187

(1)

5.5 Clays

187

(9)

5.5.1 Introduction

187

(1)

5.5.2 Specimen Preparation of Clays

188

(1)

5.5.3 Pretreatment of Clays

188

(2)

5.5.4 Size Separation of Clays

190

(3)

5.5.5 Slide Preparation and Analysis of Clays

193

(3)

5.6 Preparation of Zeolites for X-ray Diffraction

196

(3)

5.6.1 Introduction

196

(1)

5.6.2 Dehydrated Zeolites

196

(1)

5.6.3 Zeolite Equilibration

196

(1)

5.6.4 Effect of Cations in Zeolites

197

(1)

5.6.5 Particle Size and Preferred Orientation in Zeolites

198

(1)

5.7 Air-sensitive Samples

199

(1)

5.7.1 Alkali and Alkaline-earth Metals

199

(1)

5.7.2 Samples Stored under Water

199

(1)

5.7.3 Other Samples

199

(1)

5.8 Thin Films

200

(5)

5.8.1 Introduction

200

(1)

5.8.2 Specimen Holders

201

(1)

5.8.3 Specimen Preparation Methods for Thin Films

201

(4)

5.9 Microsamples

205

(2)

5.10 Forensic Samples

207

(3)

5.10.1 Preparation of Debye-Scherrer Specimens for Forensic Work

208

(2)

5.10.2 Preparation of Gandolfi Specimens

210

(1)

5.11 Paper and Plastics

210

(1)

5.11.1 Small Samples

210

(1)

5.11.2 Intermediate Sized Samples

210

(1)

5.11.3 Large Samples

211

(1)

5.12 Gemstones

211

(1)

5.13 Energetic Materials

212

(5)

5.13.1 Preparation of Specimens from Energetic Materials

213

(1)

5.13.2 Special Precautions in Dealing with Energetic Materials

213

(1)

5.13.3 Reducing the Size of Larger Energetic Specimens

214

(3)

6 SPECIAL PROBLEMS IN THE PREPARATION OF X-RAY DIFFRACTION SPECIMENS

217

(36)

6.1 High Pressure Studies

217

(7)

6.1.1 Diamond Anvil Cells

217

(2)

6.1.2 Specimen Preparation for the Diamond Anvil Cell

219

(1)

6.1.3 Large Volume High Pressure-Temperature Devices

220

(1)

6.1.4 Pressure Medium

220

(3)

6.1.5 X-ray Diffraction Pressure Calibrants

223

(1)

6.1.6 High Pressure Work with Synchrotron Sources

223

(1)

6.2 Specimen Preparation and Laboratory Procedures for Residual Stress and Strain Determination by X-ray Diffraction

224

(13)

6.2.1 Specimen Preparation for Stress Measurements

225

(1)

6.2.2 Mounting Procedures

226

(2)

6.2.3 Specimen Displacement Errors

228

(2)

6.2.4 Parallel-beam Optics

230

(4)

6.2.5 Sequence of Procedures in Conducting Stress Measurements

234

(3)

6.3 Measurements on Single Crystals

237

(5)

6.3.1 Identification of Crystal Faces

238

(1)

6.3.2 Orientation of Single Crystal Specimens

239

(1)

6.3.3 Example of an Orientation Experiment

240

(1)

6.3.4 Final Comments

241

(1)

6.4 Unusual Tricks with Unusual Samples

242

(4)

6.4.1 Isolation of Material

242

(1)

6.4.2 Reactive Materials

242

(1)

6.4.3 Toxic Materials

243

(1)

6.4.4 Radioactive Materials

243

(1)

6.4.5 Flowing Materials

244

(1)

6.4.6 High Temperature Diffraction

244

(1)

6.4.7 Low Temperature Diffraction

245

(1)

6.4.8 Organic Materials

245

(1)

6.4.9 Bulk Specimens for the Diffractometer

245

(1)

6.5 Preparing Specimens for the Synchrotron

246

(7)

6.5.1 Effects of Data Recording

246

(1)

6.5.2 Intensity Values

246

(1)

6.5.3 Importance of Proper Alignment

246

(1)

6.5.4 Statistics Applied to Samples and Sampling

247

(1)

6.5.5 Methods for Commuting Powders

247

(1)

6.5.6 Preparing Specimens for Simple Routine Analysis

247

(1)

6.5.7 Use of Standards in X-ray Diffraction Analysis

247

(1)

6.5.8 Preparing Specimens for Accurate d-spacing Measurements

248

(1)

6.5.9 Preparing Specimens for Accurate Intensities

248

(5)

7 SPECIMEN PREPARATION FOR CAMERA METHODS

253

(12)

7.1 The Debye-Scherrer Camera

253

(4)

7.1.1 Geometry of the Debye-Scherrer Camera

253

(1)

7.1.2 Preparing Mounts for the Debye-Scherrer Camera

253

(1)

7.1.3 Self-supporting Specimens

254

(1)

7.1.4 Rod Mounted Specimens

254

(2)

7.1.5 Capillary Mounts for the Debye-Scherrer Camera

256

(1)

7.1.6 Preparing Debye-Scherrer Specimens for Nonambient Measurements

257

(1)

7.2 The Gandolfi Camera

257

(3)

7.2.1 Gandolfi Mounts

258

(1)

7.2.2 Handling Very Small Specimens in the Gandolfi Camera

258

(2)

7.3 The Guinier Camera

260

(5)

7.3.1 Mounting the Specimen in the Guinier Camera

261

(1)

7.3.2 Foils and Glues

261

(1)

7.3.3 Moving the Specimen in the Guinier Camera

262

(1)

7.3.4 Capillary Techniques with the Guinier Camera

262

(1)

7.3.5 Nonambient Temperatures--High Temperatures

263

(1)

7.3.6 Nonambient Temperatures--Low Temperatures

264

(1)

8 SPECIMEN PREPARATION EQUIPMENT

265

(20)

8.1 Introduction

265

(1)

8.2 Grinding and Pulverizing Equipment

265

(4)

8.2.1 Large Crushing and Pulverizing Equipment

266

(2)

8.2.2 Splitters

268

(1)

8.2.3 Mills

268

(1)

8.2.4 Mortars

268

(1)

8.3 Special Equipment

269

(3)

8.3.1 Presses

269

(1)

8.3.2 Fluxers

270

(1)

8.3.3 Aerosol Suspension Devices

270

(1)

8.3.4 Liquid Specimen Holders

271

(1)

8.3.5 Metallic Specimens

271

(1)

8.4 Preparing X-ray Diffraction Specimen Holders

272

(1)

8.4.1 Specimen Holders for Large Specimens

273

(1)

8.4.2 Specimen Holders for Small Specimens

273

(1)

8.5 Recovering Damaged Platinum Ware

273

(3)

8.5.1 General Hints on the Use of Platinum Crucibles

273

(1)

8.5.2 Discussion of the Problem

274

(1)

8.5.3 Repair Procedure

274

(1)

8.5.4 Special Problems and Hints

275

(1)

8.6 Specimen Preparation Kit for X-ray Diffraction

276

(3)

8.6.1 Kit for Preparing Specimens

276

(2)

8.6.2 Sources for Kit Items

278

(1)

8.7 Equipment for Preparation of Zeolite Specimens

279

(1)

8.7.1 Equipment Suppliers, Zeolite Preparation

279

(1)

8.8 Vendor Addresses

280

(5)

9 USE OF STANDARDS IN X-RAY FLUORESCENCE ANALYSIS

285

(28)

9.1 Standards--An Overview

285

(20)

9.1.1 Introduction

285

(1)

9.1.2 Definitions

286

(1)

9.1.3 Catalogues

287

(1)

9.1.4 Origin and Types

287

(1)

9.1.5 Preparation Procedure

288

(1)

9.1.6 Certificate Evaluation

288

(1)

9.1.7 Applications

289

(7)

9.1.8 Conclusion

296

(1)

9.1.9 Monitor Samples

296

(4)

9.1.10 Procedure

300

(2)

9.1.11 Frequency of Monitor Measurement

302

(3)

9.2 Recalibration

305

(1)

9.2.1 Introduction

305

(1)

9.2.2 Quality Standard Programs

305

(1)

9.3 Instrumental Short- and Long-term Drift

306

(2)

9.3.1 Overview

306

(1)

9.3.2 Recalibration

307

(1)

9.3.3 Specimens Used for Drift Correction and Recalibration

308

(1)

9.4 Sources for Reference Materials for X-ray Diffusion and X-ray Fluorescence

308

(5)

9.4.1 Office of Standard Reference Data

308

(1)

9.4.2 Alternate Sources of Standard Materials

309

(1)

9.4.3 Sources for X-ray Fluorescence Standards

309

(1)

9.4.4 Addresses for Sources of X-ray Fluorescence and X-ray Diffraction Standards

310

(3)

GLOSSARY

313

(8)

BIBLIOGRAPHY

321

(6)

INDEX

327

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A Practical Guide for the Preparation of Specimens for X-Ray Fluorescence and X-Ray Diffraction Analysis

Summary

Author Biography

Table of Contents

Supplemental Materials