Rapid chemical analysis of the <2 μm clay fraction using an SEM/EDS technique

Clay Minerals ◽  
2007 ◽  
Vol 42 (4) ◽  
pp. 549-562 ◽  
Author(s):  
T. Clayton ◽  
R. B. Pearce
Keyword(s):  
Chemical Analysis ◽  
Clay Mineral ◽  
Clay Fraction ◽  
Additional Treatment ◽  
Chemical Data ◽  
X Ray Diffraction ◽  
Analytical Technique ◽  
Conductive Surface ◽  
Mineral Mixtures ◽  
Analytical Errors

AbstractScanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) analysis of smear slides of oriented <2 mm clay fractions is shown to be a reliable and rapid analytical technique for providing chemical data on clay mineral mixtures. Such smear slides are routinely prepared for clay mineral analysis by X-ray diffraction and the only additional treatment required for chemical analysis by EDS is carbon-coating to form an electronically conductive surface. Using standard clays, mixtures of standard clays, and sediment samples, it is shown that sample thickness, sample heterogeneity and surface roughness do not introduce significant analytical errors, although the presence of non-clay mineral phases such as calcite, dolomite, quartz and pyrite may introduce minor discrepancies. Chemical data complement the XRD analyses and increase their accuracy and reliability.

Mineralogical and chemical heterogeneity of three standard clay mineral samples

Clay Minerals ◽  
1996 ◽  
Vol 31 (3) ◽  
pp. 417-422 ◽  
Author(s):  
H. M. Köster
Keyword(s):  
Particle Size ◽  
Chemical Analysis ◽  
Clay Mineral ◽  
Chemical Heterogeneity ◽  
X Ray Diffraction ◽  
Accessory Minerals ◽  
Size Fractions ◽  
X Ray ◽  
Compositional Variations

AbstractMineralogical and chemical heterogeneity within three standard clay mineral samples have been identified by X-ray diffraction and chemical analysis of various size-fractions. This heterogeneity is partly attributed to accessory minerals, but mostly to structural and compositional variations in the 2:1 layer minerals of different particle size in the same specimen.

Quantitative Analysis of Clay Mineral Mixtures by X-ray Diffraction

Nature ◽  
1964 ◽  
Vol 204 (4964) ◽  
pp. 1228-1230 ◽  
Author(s):  
A. A. THEISEN ◽  
E. BELLIS
Keyword(s):  
Quantitative Analysis ◽  
Clay Mineral ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mineral Mixtures

A method to eliminate the background in X-ray diffraction patterns of oriented clay mineral samples

Clay Minerals ◽  
1981 ◽  
Vol 16 (4) ◽  
pp. 383-393 ◽  
Author(s):  
S. J. Van Der Gaast ◽  
A. J. Vaars
Keyword(s):  
Clay Mineral ◽  
Quantitative Estimate ◽  
Considerable Increase ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Two Samples ◽  
Diffraction Patterns ◽  
Mineral Mixtures

AbstractA method is described for calculating, and then subtracting, the background from X-ray diffraction patterns of oriented clay mineral samples. Ti-Kα radiation is used and, to minimize the absorption of this radiation by air, a vacuum and helium-flushed device has been developed. This device can be used with other X-ray sources, offering a considerable increase of intensity—e.g. Co-Kα radiation is increased by 125%. With the background-eliminated patterns a better semi-quantitative estimate of the composition of clay mineral mixtures is possible. Small differences in composition of two samples can be identified by subtracting one of the background-eliminated patterns from the other. Using this method, peak maxima of smectite-group minerals can also be accurately determined.

Quantitative Determination of Clay Mineral Mixtures by X-Ray Diffraction

1957 ◽  
Vol 21 (3) ◽  
pp. 257-260 ◽  
Author(s):  
N. Lynn Jarvis ◽  
R. Dean Dragsdorf ◽  
Roscoe Ellis
Keyword(s):  
Quantitative Determination ◽  
Clay Mineral ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mineral Mixtures

High Resolution Replication of Organoclay Surfaces

1982 ◽  
Vol 40 ◽  
pp. 576-577
Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys
Keyword(s):  
Clay Mineral ◽  
Organic Molecule ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Naturally Occurring ◽  
Silicate Layers ◽  
Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

Microdomains in BaFeO3-y (0.35 < y < 0.50)

1990 ◽  
Vol 48 (4) ◽  
pp. 780-781
Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier
Keyword(s):  
Electron Diffraction ◽  
Chemical Analysis ◽  
Monoclinic Phase ◽  
Orthorhombic Phase ◽  
Total Iron ◽  
Zone Axis ◽  
Electron Micrograph ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compositional Variations

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.

Hydrolytic products of Fe(III) after oxidation of Fe(II) by chlorate

1982 ◽  
Vol 47 (4) ◽  
pp. 1069-1077 ◽  
Author(s):  
Karel Mádlo ◽  
František Hanousek ◽  
Antonín Petřina ◽  
Jaroslav Tláskal
Keyword(s):  
Electron Microscopy ◽  
Ir Spectroscopy ◽  
Chemical Analysis ◽  
Ferrous Sulphate ◽  
Reaction Medium ◽  
Potassium Chlorate ◽  
X Ray Diffraction ◽  
X Ray

Ferrous sulphate was oxidized by potassium chlorate in the pH region 2-7 and at temperatures ranging from 298.1 to 323.1 K and various hydrolytic products of Fe(III) were separated and indentified. The separated solid ferric products were analyzed using a combination of the chemical analysis, IR spectroscopy, X-ray diffraction, and electron microscopy. The following substances were found as major components of the products: Fe2O3.n H2O ("ferric gel"), Fe2O3.n H2O with bound SO2-4 ions ("sulphogel"), α-FeO(OH), γ-FeO(OH) and Fe3O4. Their amount depends particularly on the pH temperature of the reaction medium.

scholarly journals Provenance and Sedimentary Context of Clay Mineralogy in an Evolving Forearc Basin, Upper Cretaceous-Paleogene and Eocene Mudstones, San Joaquin Valley, California

Minerals ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 71
Author(s):  
Andrew Hurst ◽  
Michael Wilson ◽  
Antonio Grippa ◽  
Lyudmyla Wilson ◽  
Giuseppe Palladino ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Upper Cretaceous ◽  
Clay Fraction ◽  
Clay Mineralogy ◽  
Bulk Rock ◽  
X Ray Diffraction ◽  
Arc Volcanism ◽  
X Ray ◽  
Magmatic Arc ◽  
Tropical Weathering

Mudstone samples from the Moreno (Upper Cretaceous-Paleocene) and Kreyenhagen (Eocene) formations are analysed using X-ray diffraction (XRD) and X-ray fluorescence (XRF) to determine their mineralogy. Smectite (Reichweite R0) is the predominant phyllosilicate present, 48% to 71.7% bulk rock mineralogy (excluding carbonate cemented and highly bio siliceous samples) and 70% to 98% of the <2 μm clay fraction. Opal CT and less so cristobalite concentrations cause the main deviations from smectite dominance. Opal A is common only in the Upper Kreyenhagen. In the <2 μm fraction, the Moreno Fm is significantly more smectite-rich than the Kreyenhagen Fm. Smectite in the Moreno Fm was derived from the alteration of volcaniclastic debris from contemporaneous rhyolitic-dacitic magmatic arc volcanism. No tuff is preserved. Smectite in the Kreyenhagen Fm was derived from intense sub-tropical weathering of granitoid-dioritic terrane during the hypothermal period in the early to mid-Eocene; the derivation from local volcanism is unlikely. All samples had chemical indices of alteration (CIA) indicative of intense weathering of source terrane. Ferriferous enrichment and the occurrence of locally common kaolinite are contributory evidence for the intensity of weathering. Low concentration (max. 7.5%) of clinoptilolite in the Lower Kreyenhagen is possibly indicative of more open marine conditions than in the Upper Kreyenhagen. There is no evidence of volumetrically significant silicate diagenesis. The main diagenetic mineralisation is restricted to low-temperature silica phase transitions.

Geochemistry of halloysite-7Å formation from plagioclase in trachyandesite rocks from Limnos Island, Greece

Clay Minerals ◽  
2014 ◽  
Vol 49 (1) ◽  
pp. 75-89 ◽  
Author(s):  
D. Papoulis ◽  
S. Komarneni ◽  
D. Panagiotaras
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Chemical Analysis ◽  
Geochemical Data ◽  
X Ray Diffraction ◽  
Polarizing Microscopy ◽  
X Ray ◽  
Geochemical Evaluation ◽  
Scanning Electron ◽  
Southwest Part

AbstractTrachyandesite rocks, occurring over an area of about 1 km2in the southwest part of Limnos Island, Greece, are altered mainly to halloysite. The samples were collected and analysed by polarizing microscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and chemical analysis. The alteration of plagioclase to halloysite follows seven discrete stages that are described in detail. The geochemical evaluation of the data shows enrichment of the lightREE(LREE) over heavyREE(HREE) as expressed by the (La/Yb)n ratio. TheΣLREErange from 206.44 to 272.30, while the sum ofHREEvaries from 11.01 to 26.26. The (La/Yb)n ratio ranges from 9.72 to 27.64. Fractionation amongLREEexpressed as (La/Sm)n and between middleREE(MREE) andHREEis shown as (Tb/Yb)n ratios. The most altered rocks close to the fault zone have high (Tb/Yb)n ratios and low (La/Sm)n and Eu/Eu* ratios. Although mineralogy and clay mineral textures indicate hydrothermal genesis of halloysite, the geochemical data are not conclusive due to a secondary weathering effect.

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