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9780471194583

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

by ; ;
  • ISBN13:

    9780471194583

  • ISBN10:

    0471194581

  • Edition: 1st
  • Format: Hardcover
  • Copyright: 1997-11-19
  • Publisher: Wiley-VCH
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Summary

* Contains useful bibliography and helpful references.

Author Biography

VICTOR E. BUHRKE heads The Buhrke Company in Redwood City, California.<br> <br> RON JENKINS is the general manager of the International Center for Diffraction Data in Newton Square, Pennsylvania.<br> <br> K. SMITH is a professor emeritus in the Department of Geosciences at Pennsylvania State University.

Table of Contents

PREFACE xxi(2)
INTRODUCTION xxiii
1 GENERAL INTRODUCTION
1(34)
1.1 Sampling
1(6)
1.1.1 What Is Sampling?
1(2)
1.1.2 Kinds of Materials Sampled
3(1)
1.1.3 Record Keeping
3(1)
1.1.4 Meaningful Sampling
3(1)
1.1.5 Sampling for Scientific Investigation
4(1)
1.1.6 Sampling for Analytical Truth
4(1)
1.1.7 Matching Sampling Methodology with Analytical Goals--Heterogeneity
5(2)
1.2 Basic Statistical Definitions
7(8)
1.2.1 Introduction
7(1)
1.2.2 The Representative Sample
7(1)
1.2.3 Mean
8(1)
1.2.4 Dispersion
9(2)
1.2.5 Sampling Errors
11(2)
1.2.6 Replication
13(1)
1.2.7 Practicalities and Compromises
14(1)
1.3 Obtaining a Representative Sample from the Bulk
15(1)
1.4 Sampling Procedures
16(5)
1.4.1 Cone and Quartering
17(1)
1.4.2 Alternate Shoveling
18(1)
1.4.3 Linear Japan Cake
18(1)
1.4.4 Riffle Splitting
19(1)
1.4.5 Sectorial Splitting
19(1)
1.4.6 The Holistic Approach to Sampling
20(1)
1.5 Methods of Comminuting Powders for X-ray Diffraction
21(1)
1.5.1 Requirements for an Ideal Specimen
21(1)
1.5.2 Ideal Particle Size for X-Ray Diffraction Applications
22(1)
1.6 Grinding for X-Ray Diffraction Applications
22(4)
1.6.1 Mechanical Grinding: Precautions and Considerations
22(1)
1.6.2 Dry Grinding for X-Ray Diffraction Applications
23(1)
1.6.3 Wet Grinding for X-Ray Diffraction Applications
23(2)
1.6.4 Types of Grinding
25(1)
1.6.5 Effects of Grinding
26(1)
1.7 Absorption Problems
26(5)
1.7.1 Absorption of X-rays
26(2)
1.7.2 Scattering and Diffraction of X-rays
28(2)
1.7.3 Absorption in X-ray Fluorescence
30(1)
1.7.4 Absorption in X-ray Diffraction
30(1)
1.8 Crystallinity and Particle Effects in X-ray Diffraction Applications
31(4)
2 SPECIMEN PREPARATION PROCEDURES IN X-RAY FLUORESCENCE ANALYSIS
35(24)
2.1 Common Problems in Preparing and Presenting Specimens for X-ray Fluorescence
35(1)
2.1.1 General
35(1)
2.1.2 Types of Samples Analyzed
35(1)
2.2 Presenting the Specimen to the Spectrometer
36(3)
2.2.1 Physical Form of the Specimen in X-ray Fluorescence Analysis
36(1)
2.2.2 Specimen Placement
37(1)
2.2.3 Photochemical Decomposition
38(1)
2.3 Handling Samples Without Pretreatment
39(1)
2.4 Use of Pressed Powder Pellets
40(1)
2.4.1 General
40(1)
2.4.2 Direct Pelletizing of the Specimen
40(1)
2.5 Lithium and Sodium Tetraborate Fusion Methods
41(3)
2.5.1 Advantages of Fusion
41(1)
2.5.2 Choice of Fusion Mixture
42(1)
2.5.3 Choice of Reaction Crucible
42(2)
2.5.4 Controlling the Fusion Reaction
44(1)
2.6 Liquids and Solutions
44(3)
2.6.1 General
44(1)
2.6.2 Preconcentration Methods
45(1)
2.6.3 Direct Methods
46(1)
2.6.4 Concentration by Evaporation
46(1)
2.6.5 Use of Ion-Exchange Resins
47(1)
2.7 Handing Very Small Samples
47(4)
2.7.1 Size of the Specimen in X-ray Fluorescence Analysis
47(2)
2.7.2 Direct Analysis of Limited Quantities of Sample
49(2)
2.8 Radioactive Samples
51(1)
2.9 Special Problems with Low Atomic Number Elements
51(8)
3 SPECIMEN PREPARATION IN X-RAY FLUORESCENCE
59(64)
3.1 Whole Rock Analysis
59(6)
3.1.1 General
59(1)
3.1.2 Specimen Preparation Procedures
60(4)
3.1.3 Special Problems and Hints
64(1)
3.2 Limes, Dolomitic Limes, and Ferrolimes
65(3)
3.2.1 General Discussion
65(1)
3.2.2 Sampling
66(1)
3.2.3 Specimen Preparation--Fused Glass Disk
66(1)
3.2.4 Results
67(1)
3.2.5 Discussion
68(1)
3.3 Limestones, Dolomites, and Magnesites
68(3)
3.3.1 General Discussion
68(1)
3.3.2 The Pressed Powder Method
68(2)
3.3.3 Determination of Carbon Dioxide, CO(2)
70(1)
3.3.4 Calibration Standards
70(1)
3.3.5 Results
71(1)
3.4 Natural and By-product Gypsum
71(5)
3.4.1 General Discussion
71(1)
3.4.2 Remarks
71(1)
3.4.3 Elements Determined
72(1)
3.4.4 Dehydration of Gypsum
72(1)
3.4.5 Drying of Gypsum
72(1)
3.4.6 Grinding
72(3)
3.4.7 Results
75(1)
3.4.8 Reference Materials
75(1)
3.4.9 Discussion
75(1)
3.5 Glass Sands
76(3)
3.5.1 General Discussion
76(1)
3.5.2 Selection of a Representative Sample
76(1)
3.5.3 Fusion with Lithium Tetraborate and Lithium Fluoride
77(1)
3.5.4 Discussion
78(1)
3.6 Cements, Clinker, and Raw Materials
79(4)
3.6.1 Types and Compositions of Cements
79(1)
3.6.2 Pressed Powder Briquet Preparation
80(1)
3.6.3 Fused Bead Preparation
81(1)
3.6.4 ASTM C 114 Qualification
82(1)
3.7 Preparation of Metals
83(5)
3.7.1 Sampling
83(1)
3.7.2 Solubility of Elements
83(2)
3.7.3 Alloy Metallographic Structure
85(1)
3.7.4 Parameters Affecting the Analytical Surface Finish
86(1)
3.7.5 Effective Thickness and Volume
87(1)
3.7.6 Hardness
88(1)
3.8 Aluminum and Its Alloys
88(4)
3.8.1 Surface Preparation Techniques
88(1)
3.8.2 X-ray Fluorescence Tests
89(1)
3.8.3 Discussion of Selected Surface Preparation Techniques
90(2)
3.9 Titanium
92(1)
3.10 Cast Iron
93(2)
3.10.1 General Discussion
93(1)
3.10.2 Specimen Preparation Procedure
94(1)
3.11 Steel
95(5)
3.11.1 Evaluation of Grinding Materials
96(2)
3.11.2 Special Problems and Hints
98(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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