Iron Oxides in the Laboratory Preparation and Characterization

Udo Schwertmann, Rochelle M. Cornell9783527296699, 9783527613236, 3527296697

Iron Oxides play an important role in numerous disciplines. Since the publication of the first edition, there has been a surge of interest in synthetic fine to ultrafine iron oxides in a wide range of scientific and technological disciplines, especially in mineralogy, geosciences and environmental science and in various branches of technology. As before, the main aim of the second edition is to present reliable, well-tested, up-to-date methods of synthesizing pure iron oxides. The section on monodispersed particles, presently of great interest to industry, has been expanded. Furthermore the methods of characterization have been focused on their relevance to iron oxides. The well tried syntheses have been retained and some new ones have been incorporated.

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Table of contents :
Iron Oxides in the Laboratory……Page 2
Contents……Page 10
Introduction……Page 22
1 The Iron Oxides……Page 26
1.1 The Major Iron Oxides……Page 27
1.2 Less Conmon or Rare Iron Oxides……Page 31
1.3 Iron Oxides in the Environment……Page 34
2.2.1 Washing……Page 40
2.2.3 Storage……Page 42
2.3.1 Total Analysis……Page 43
2.3.3 Impurities……Page 44
2.4 Removal of Iron Oxides from Reaction Vessels……Page 45
2.5 Purity of Reagents……Page 46
3.2 Color (A. Scheinost)……Page 48
3.2.1 Origin of Color……Page 50
3.2.2 Color Measurement……Page 53
3.2.3 Color Systems……Page 54
3.2.4 Identification of Iron Oxides by Color and Crystal-Field Bands……Page 58
3.3 X-Ray Powder Diffraction……Page 63
3.4 Microscopy……Page 68
3.5 Surface Area, Porosity and Fractal Dimensions……Page 70
3.6 Acid Oxalate Extraction……Page 71
3.7 Infrared Spectroscopy……Page 72
3.9 Mössbauer Spectroscopy……Page 74
4.1.1 Nucleation……Page 76
4.1.3 Production of Monodispersed Particles……Page 78
4.1.4 Production of Nanoparticles……Page 80
4.2.1 Hydrolysis of Acidic Solutions of FeIII Salts……Page 81
4.2.2 Transformation of Ferrihydrite……Page 82
4.2.3 Oxidative Hydrolysis of FeII Salts……Page 83
4.2.5 The Gel-Sol Method……Page 84
4.2.7 Decomposition of Metal Chelates……Page 85
5.1 Introductions……Page 88
5.2.1 Preparation from an Alkaline System (acc. to Böhm. 1925)……Page 94
5.2.2 Preparation fiom an Acid System (acc. to Mørup et al., 1983)……Page 95
5.2.3 Preparation From a Cysteine/2-line Ferrihydrite System……Page 97
5.3 Pure Goethite from an FeII System……Page 99
5.4 General Comments……Page 104
5.5.1.1 Preparation from an Alkaline FeIII System……Page 107
5.5.1.2 Preparation from an FeII-System……Page 109
5.5.2 Cr-Substituted Goethite Fe1–xCrxOOH……Page 110
5.5.3 Mn-Substituted Goethite Fe1–xMnxOOH……Page 111
5.5.4 V-Substituted Goethite Fe1–xVxOOH……Page 112
6.1 Introduction……Page 114
6.2 Preparation……Page 115
6.3 Other Methods……Page 118
7.2 Preparation……Page 120
8.1 Introduction……Page 124
8.2 6-Line Ferrihydrite……Page 125
8.3 2-Line Ferrihydrite……Page 126
8.4 Ferrihydrites with a Range of Crystallinities (acc. to D. G. Lewis)……Page 131
9.2 Preparation by Hydrolysis of Acidic FeCI3 Solutions (Somatoids)……Page 134
9.4 Si-containing Akaganéite……Page 139
10.1 Introduction……Page 142
10.2 Preparation by Forced Hydrolysis of FeIII Salt Solutions……Page 143
10.3 Preparation by Transformation of 2-Line Ferrihydrite……Page 147
10.4 Monodisperse Hematites of Different Crystal Shapes……Page 151
10.5 Other Methods……Page 153
10.6 Al-substituted Hematite……Page 154
10.7 Coated Hematite……Page 155
11.2 Preparation by Oxidation of a FeII Solution……Page 156
11.3 Cation-substituted Magnetites……Page 161
12.2 Preparation……Page 162
13.2 Preparation……Page 164
14.1 Introduction……Page 168
14.2 Preparation……Page 169
15.1 Introduction……Page 174
15.2 Preparation……Page 175
16.1 Introduction……Page 178
16.2 Demonstration: Synthesis of Fe Oxides……Page 179
16.3 Lecture: Processes by which Fe Oxides Form……Page 180
16.4 Video : Iron in a Landscape……Page 183
References……Page 186
Acknowledgement……Page 202
Index……Page 204