X-Ray Diffraction and the Identification and Analysis of Clay Minerals

by Moore, Duane M.; Reynolds, Robert C.

• ISBN13: 9780195087130
• ISBN10: 0195087135
• Edition: 2nd
• Format: Spiral Bound
• Copyright: 1997-02-13
• Publisher: Oxford University Press

Summary

This successful text/reference, now in a new edition, explores the applications and limitations of data produced by the interaction of X-rays with clay minerals. This edition pays particular attention to integrating the mineralogy of soils and features a new chapter on disorder and polytypes.Chapter Four, from the first edition, has been expanded and split into two chapters, "Structure and Properties: General Treatment" and "Structure, Nonmenclature, and Occurrences of Clay Minerals." Essential in agriculture, geology, and in making informed engineering decisions, this text offers thenecessary information on the properties of these minerals, combining theoretical discussion with recipe-like directions for laboratory procedures. Ideal for students who have completed introductory geology, chemistry, and mineralogy courses, this text can also be used as a reference for researchersand workers in industry.

Table of Contents

Preface to the Second Edition	xiii
Preface to the First Edition	xv
Introduction and Historical Background	3	(25)
History	5	(12)
The Discovery of X-Rays	6	(4)
The Discovery of X-Ray Diffraction	10	(4)
History of Clay Mineralogy	14	(3)
The Importance of Clay Mineralogy	17	(1)
Clay Minerals as Catalysts	18	(4)
The Literature of Clay Mineralogy	22	(1)
Summary	23	(1)
References	24	(4)
Nature and Production of X-Rays	28	(33)
Other Methods	28	(3)
Safety and Protection	31	(1)
Defining a Dose of Radiation	31	(2)
The Nature or X-Rays	33	(9)
Continuous or White Radiation	33	(2)
Characteristic Radiation	35	(3)
General Absorption of X-Rays	38	(2)
Characteristic Absorption	40	(2)
Equipment for Producing and Recording X-Rays	42	(16)
Stabilizing the Voltage	42	(1)
Generating X-Rays	43	(1)
The Diffractometer	44	(5)
Step-Scanning with Automated Diffractometers	49	(3)
The Single-Crystal Monochromator	52	(1)
The Detector	52	(2)
Signal Processing Circuitry	54	(1)
The Strip-Chart Recorder	55	(1)
An Example of a Checklist for Operating XRD Equipment	56	(2)
Summary	58	(1)
References	59	(2)
X-Ray Diffraction	61	(43)
Scattering	62	(2)
Interference	64	(8)
Scattering from a Row of Atoms	64	(3)
Scattering from a Three-Dimensional Array of Atoms	67	(2)
Bragg's Law	69	(1)
Diffraction and Reflection	70	(2)
The Arithmetic of Scattering	72	(12)
The Summation of Scattering Amplitudes	72	(5)
The Structure Factor F	77	(2)
Information from Intensity	79	(1)
The Reciprocal Lattice	80	(4)
Real versus Idealized Peaks on XRD Tracings	84	(19)
The Interference Function F: Diffraction from a Crystal Whose Unit Cell Has a Unitary Scattering Factor	88	(2)
The Lorentz-Polarization Factors	90	(2)
Putting It All Together---Building an 001 Diffraction Pattern	92	(5)
Exercise: Calculation of the Intensity from d(001) for Illite	97	(6)
Points to Remember	103	(1)
References	103	(1)
Structure and Properties: General Treatment	104	(34)
General Structural Features	104	(13)
Tetrahedral Sheets	104	(1)
Octahedral Sheets	105	(1)
Dioctahedral and Trioctahedral	106	(1)
Joining the Sheets	107	(5)
Stacking the Layers	112	(5)
Properties	117	(13)
Total Charge, Layer or Permanent Charge, and Variable Charge	118	(2)
Electric Double Layer	120	(1)
Exchangeable Ions or Cation-Exchange Capacity	121	(2)
Interaction of Water with Clay Mineral Surfaces	123	(3)
Interaction with Organic Compounds	126	(4)
Classification	130	(4)
Nomenclature	132	(2)
References	134	(4)
Structure, Nomenclature, and Occurrences of Clay Minerals	138	(66)
The Individual Clay Minerals	138	(29)
The 1:1 Layer Type	138	(1)
Serpentine minerals	139	(1)
Berthierine	139	(1)
Odinite	139	(1)
Kaolin minerals	140	(4)
Uses of Kaolinite	144	(1)
Allophane and imogolite	145	(1)
The 2:1 Layer Type, x = 0	146	(1)
The 2:1 Layer Type, x ∼ 1	146	(1)
The trioctahedral subgroup	147	(1)
The dioctahedral subgroup	147	(1)
The 2:1 Layer Types with x < 1	148	(1)
Illite	149	(4)
Glauconite	153	(2)
Smectite	155	(3)
Alteration of Ash-Fall Layers	158	(1)
Vermiculite	158	(4)
Chlorite	162	(5)
Mixed-Layered Clay Minerals	167	(19)
Mixed-layering, interlayering, and interstratification	168	(2)
Illite/smectite (I/S)	170	(1)
Reichweite or Ordering	171	(5)
Models for smectite-to-illite transition	176	(1)
MacEwan crystallite model	177	(1)
Fundamental particle model	177	(2)
Two-solid-solution model	179	(2)
Chlorite/smectite (C/S)	181	(2)
Serpentine/chlorite	183	(1)
Kaolinite/expandables (K/E)	184	(1)
Sepiolite and Palygorskite	185	(1)
The Origin of Clay Minerals	186	(2)
Summary	188	(7)
Exercise: Calculating Structural Formulas	189	(3)
Exercise: Making Structural Models of Layer Silicates	192	(3)
References	195	(9)
Sample Preparation Techniques for Clay Minerals	204	(23)
Evaluating the Sample	204	(2)
Disaggregating the Rock	206	(3)
Separating Clay Minerals from Clastic Rocks	206	(1)
Separating Clay Minerals from Carbonate Rocks	207	(1)
Separating Clay Minerals from Sulfate Rocks	207	(1)
Separating Clay Minerals from Unconsolidated Materials	208	(1)
Glacial Deposits, North American Interior	208	(1)
Chemical Pretreatments	209	(2)
Removal of Iron Oxides	209	(1)
Removal of Organic Materials	209	(1)
Saturating the Clay Minerals with Different Cations	210	(1)
Particle-Size Separation	211	(3)
Preparing the Oriented Clay Mineral Aggregates	214	(6)
The Glass Slide Method	214	(1)
The Smear Mount Method	215	(1)
The Millipore® Filter Transfer Method	216	(2)
The Centrifuged Porous Plate Method	218	(1)
Dealing with Curlers or Peelers	219	(1)
Making the Random Powder Mount	220	(4)
Everyday random powder packs	222	(1)
Freeze-dried random powder packs	222	(2)
Ethylene Glycol Solvation	224	(1)
Final Note	225	(1)
References	225	(2)
Identification of Clay Minerals and Associated Minerals	227	(34)
Clay Mineral Identification---General Principles	228	(16)
Illite and Glauconite	233	(1)
Chlorite and Kaolinite	233	(6)
Vermiculite	239	(2)
Smectite	241	(2)
Sepiolite, Palygorskite, and Halloysite	243	(1)
060 Reflections	244	(2)
The Use of hkl Reflections for the Determination of Polytypes	246	(2)
Chlorite Polytypes	246	(1)
The Kaoline Polytypes	247	(1)
The Micas, Illite, and Glauconite	247	(1)
Nonclay Minerals	248	(11)
Silica Minerals	250	(2)
Feldspar	252	(2)
Zeolites	254	(1)
Carbonates	255	(1)
Apatite, Pyrite, and Jarosite	256	(1)
Gypsum, Anhydrite, Celestite, and Barite	257	(1)
Lepidocrocite, Goethite, Gibbsite, and Anatase	258	(1)
Summary	259	(1)
References	259	(2)
Identification of Mixed-Layered Clay Minerals	261	(37)
Mering's Principles and Mixed-Layered Nomenclature	263	(7)
The Q Rule, a Broadening Descriptor	266	(4)
Mixed-Layered Clay Minerals	270	(26)
Illite/Smectite	270	(6)
Chlorite/Smectite and Chlorite/Vermiculite	276	(8)
Kaolinite/Smectite	284	(5)
Serpentine/Chlorite	289	(3)
Mica/Vermiculite	292	(4)
Summary	296	(1)
References	296	(2)
Quantitative Analysis	298	(32)
Required Sample Characteristics	299	(9)
Sample Length	300	(1)
Sample Thickness	301	(5)
Sample Position	306	(1)
Homogeneity of the Sample	307	(1)
Equations for Quantitative Analysis	308	(9)
Basic Quantitative Diffraction Equation	308	(5)
Derivation of a Working Form of the Equation for Analysis	313	(3)
The Method of the Orienting Internal Standard	316	(1)
Mineral Reference Intensities	317	(4)
General Comments	317	(1)
Calculated Mineral Reference Intensities	318	(3)
Practical Examples of the Application of Reference Intensities	321	(1)
Measurement of Peak Intensity	321	(6)
Comments and Summary	327	(2)
References	329	(1)
Disorder in Smectite, Illite/Smectite, and Illite	330	(29)
Small Crystals in Reciprocal Space	331	(4)
Turbostratic Disorder	335	(21)
Theory	335	(4)
Smectite	339	(1)
Illite/Smectite	339	(2)
Rotational Disorder in Illite and Illite/Smectite	341	(8)
Cis-Vacant Illite and Interstratified Cis- and Trans-Vacant Illite/Smectite	349	(7)
Conclusions	356	(1)
References	357	(2)
APPENDIX: MODELING ONE-DIMENSIONAL X-RAY PATTERNS	359	(14)
The Input Variables	360	(2)
Simulating the Instrument	360	(1)
Describing the Clay Mineral	360	(2)
Theory	362	(6)
Structures of the Component Layers	366	(2)
Advanced Techniques	368	(3)
Pure Minerals	369	(1)
Compositional Superstructures	369	(1)
Layer Types Not Specifically Included	369	(1)
Atom Types Not Incorporated in the Model	370	(1)
Defect Broadening	370	(1)
References	371	(2)
Index	373