scholarly journals Application of the capillary method in micro X-ray diffractometry (µ-XRD): A useful technique for the characterization of small amounts of clay minerals

Author(s):  
Ivett Kovács ◽  
Tibor Németh ◽  
Gabriella B. Kiss ◽  
Zsolt Benkó

AbstractThe laboratory micro X-ray diffraction (μ-XRD) technique is a suitable method to study minerals in-situ in whole-rock specimens without any sample preparation or in polished thin sections, and even in small amounts in powdered form. The micro X-ray diffraction method uses the conventional, closed-tube X-ray generator, but modifications were needed in the diffraction column, sample holder and detector in order to achieve μ-XRD capability.In this paper, we present a case study of the capillary method used in µ-XRD on hydrothermal clay mineral assemblages that formed in the Velence Mts (Hungary). The capillary method in µ-XRD has many advantages in the investigation of small amounts of clay minerals: (1) easy and rapid preparation of randomly oriented, powdered samples; (2) rapid measurements; (3) accurate diffraction patterns. By using the capillary method, the formation of preferred orientation can be eliminated; thus the (hkl) reflection of the clay minerals can be precisely measured. Illite polytype quantification and the investigation of (060) reflection of clay minerals can be used satisfactorily in µ-XRD.Hydrothermal clay mineral assemblages are indicative of temperature and pH. Their examination can determine the physicochemical parameters of the hydrothermal fluids that interacted with the host granite in the Velence Mts. The analyzed hydrothermal clay minerals from the western part of the mountains suggest lower temperatures (150–200 °C) and intermediate pH conditions. In contrast, the clay mineral assemblages' characteristics for the eastern part of the mountains indicate more intense argillization and higher temperatures (∼220 °C) and intermediate pH conditions.

Clay Minerals ◽  
2010 ◽  
Vol 45 (2) ◽  
pp. 209-224 ◽  
Author(s):  
J. C. Martínez ◽  
J. A. Dristas ◽  
H.-J. Massonne ◽  
T. Theye

AbstractA general alteration pattern of two transitional clay mineral assemblages was determined by petrography and X-ray diffractometry studies at the Tandilia Late Proterozoic unconformity zone, around the Barker locality: (1) K-white mica + chlorite + calcite ± anatase-rutile ± secondary quartz (farther from the unconformity) and (2) pyrophyllite + K-white mica + Ti-rich hematite ± aluminium phosphate-sulphate minerals ± tourmaline ± anatase-rutile (closer to the unconformity). The local occurrence of Na in K-white micas and K-Na in pyrophyllite is described for the first time. Possible interlayering with intermediate K-Na mica and paragonite is indicated by detailed X-ray diffraction analyses. A negative Eu anomaly (Eu/Eu* = 0.24), strongly positive Eu anomaly (Eu/Eu* =11.7) and positive Ce anomaly characterized rapid changes from an unaltered basement to the most altered basement and sedimentary rocks at the unconformity. Aluminium phosphate-sulphate minerals dominate patterns of LREE. A model of hydrothermal alteration comparable to that of unconformity-related uranium deposits is presented.


Clay Minerals ◽  
1967 ◽  
Vol 7 (1) ◽  
pp. 79-90 ◽  
Author(s):  
Ronald J. Gibbs

AbstractIn the quantitative X-ray diffraction analysis of a series of samples, the problems arising from the variable compositions and degrees of crystallinity of clay minerals were overcome to a great extent by the use of standards extracted from the samples. Procedures are given for separation of the montmorillonite standard by differential settling of Na-montmorillonite solvated in an ethanol solution and for isolation of the kaolinite, mica, and chlorite standards by density separation of their Na-forms in thallous formate.Calibration curves were prepared from the X-ray diffractograms obtained for series of known mixtures of Ca-forms of the standards and the internal standard boehmite using both powder and smear-oriented mounting techniques.


1954 ◽  
Vol 5 (1) ◽  
pp. 98
Author(s):  
JA Ferguson

The development in the Toowoomba area, Queensland, of red, black, and transitional soil types from basalt is typical of similar processes in many parts of eastern Australia. Systematic samples from this area have been investigated mineralogically by differential thermal analysis, X-ray diffraction, and other methods. Montmorillonite appears to be the clay mineral first formed under present weathering conditions. The further transition to red soils in certain situations is due to partial decomposition of montmorillonite to minerals of the kaolin group by loss of alkalis and iron, the latter being stabilized in the upper horizons as hydrated oxides. Further decomposition of kaolin minerals produces gibbsite. Changes in the nature and amount of clay minerals are thought to correspond with stages in the evolution of basalt soil types.


1954 ◽  
Vol 5 (1) ◽  
pp. 98
Author(s):  
JA Ferguson

The development in the Toowoomba area, Queensland, of red, black, and transitional soil types from basalt is typical of similar processes in many parts of eastern Australia. Systematic samples from this area have been investigated mineralogically by differential thermal analysis, X-ray diffraction, and other methods. Montmorillonite appears to be the clay mineral first formed under present weathering conditions. The further transition to red soils in certain situations is due to partial decomposition of montmorillonite to minerals of the kaolin group by loss of alkalis and iron, the latter being stabilized in the upper horizons as hydrated oxides. Further decomposition of kaolin minerals produces gibbsite. Changes in the nature and amount of clay minerals are thought to correspond with stages in the evolution of basalt soil types.


Clay Minerals ◽  
2015 ◽  
Vol 50 (2) ◽  
pp. 249-272 ◽  
Author(s):  
E. Zeelmaekers ◽  
M. Honty ◽  
A. Derkowski ◽  
J. Środoń ◽  
M. De Craen ◽  
...  

AbstractThe Boom Clay Formation of early Oligocene age, which occurs underground in northern Belgium, has been studied intensively for decades as a potential host rock for the disposal of nuclear waste. The goal of the present study is to determine a reference composition for the Boom Clay using both literature methods and methods developed during this work. The study was carried out on 20 samples, representative of the lithological variability of the formation. The bulk-rock composition was obtained by X-ray diffraction using a combined full-pattern summation and singlepeak quantification method. Siliciclastics vary from 27 to 72 wt.%, clay minerals with 25–71 wt.% micas, 0–4 wt.% carbonates, 2–4 wt.% accessory minerals (mainly pyrite and anatase) and 0.5–3.5 wt.% organic matter. This bulk-rock composition was validated independently by majorelement chemical analysis. The detailed composition of the clay-sized fraction was determined by modelling of the oriented X-ray diffraction patterns, using a larger sigma star (σ*) value for discrete smectite than for the other clay minerals. The <2 μm clay mineralogy of the Boom Clay is qualitatively homogeneous; it contains 14–25 wt.% illite, 19–39 wt.% smectite, 19–42 wt.% randomly interstratified illite-smectite with about 65% illite layers, 5–12 wt.% kaolinite, 4–17 wt.% randomly interstratified kaolinite-smectite and 2–7 wt.% chloritic minerals (chlorite, “defective” chlorite and interstratified chlorite-smectite). All modelled clay mineral proportions were verified independently using major-element chemistry and cation exchange capacity measurements. Bulkrock and clay mineral analysis results were combined to obtain the overall detailed quantitative composition of the Boom Clay Formation.


1960 ◽  
Vol 40 (1) ◽  
pp. 1-14 ◽  
Author(s):  
S. Pawluk

Recent exploratory surveys in the northern sections of Alberta revealed many soils morphologically similar to podzols. A laboratory study was carried out to obtain a better understanding of the genesis and morphology of these soils.Chemical analyses showed the percentage base saturation and pH to be higher than for typical podzols.Physical analyses showed slight increases in clay content in the B horizons and decreases in the A horizons when compared to the parent material.From mineralogical studies of the profiles, the following weathering sequences were established: feldspars>quartz; chlorite>biotite>muscovite; [Formula: see text]. X-ray diffraction data showed illite, montmorillonite-illite mixed layering, montmorillonite, and kaolinite as being the principal clay minerals present in the A and C horizons. The clay mineral components of the B horizons were primarily chlorite-like with lesser amounts of kaolinite. Analyses indicated that the chlorite-like mineral lacked properties attributed to well crystallized chlorites and provided strong evidence in favour of authigenic origin.Data obtained in this study showed the genesis of these soils to be somewhat different from that reported for podzols elsewhere although the process of formation evidently was primarily chemical.


Clay Minerals ◽  
1979 ◽  
Vol 14 (1) ◽  
pp. 47-65 ◽  
Author(s):  
F. Sartori ◽  
R. Riffaldi ◽  
R. Levi-Minzi

AbstractClay mineral assemblages from a Quaternary sequence, sampled near the estuary of the Arno River, commonly contain some intergrade minerals, associated with other 14 Å phases and with illite and subordinate amounts of a kaolin mineral. The X-ray diffraction characteristics of such intergrade phases and their thermal modifications (100–600°C) are analysed and described.The effectiveness of some chemical treatments for removal of interlayer material is investigated and the results discussed on the basis of X-ray diffraction pattern and C.E.C. changes. Finally the properties of these intergrades are compared with those of the 14 Å phases present in the sediments carried by the Arno River and its tributary the Era River as well as with those of a soil from the Era watershed. Hypotheses are expressed about the probable relationships between degree of chloritization and characteristics of the depositional environments.


Clay Minerals ◽  
2009 ◽  
Vol 44 (3) ◽  
pp. 339-360 ◽  
Author(s):  
A. Yildiz ◽  
İ. Dumlupunar

AbstractThere are numerous bentonite deposits, formed by the alteration of volcanic rocks, in the Kapıkaya area (Eskişehir, western Turkey). These deposits can be classified into three groups according to their stratigraphical levels. X-ray diffraction (XRD), scanning electron microscope (SEM), major, rare-earth and trace-element analyses of bentonites and their parent rocks from the Kapıkaya area were used to evaluate the mineralogical and geochemical properties of bentonites and their parental affinities. Mineral assemblages resulting from bentonite deposits consist mostly of clay minerals, gypsum, cristobalite/opal-CT, quartz, feldspar, calcite and dolomite. The clay minerals are represented mainly by dioctahedral smectite and lesser amounts of illite and chlorite. The enrichment and depletion of the elements indicates open-system alteration conditions. The enrichments in MgO, Fe2O3, TiO2, Co, Pb, Zn, and Ni are related to the precipitation of hydrothermal solutions channelled throughout ultramafic sources. The main differences in mineralogy and geochemistry of bentonites from the Kapıkaya area are in the smectite composition and the contents of major, rare-earth and other trace elements. The data obtained show that the types of parent rock the influenced the mineralogical and geochemical compositions of the bentonites.


Author(s):  
Amer Al-Rawas ◽  
Hector Sutherland ◽  
A.W. Hago ◽  
Adnan Basma ◽  
Badar Al-Shihi

Qualitative and quantitative analysis of clay minerals are important in the evaluation of the swelling potential of expansive soils A relatively simple method for the quantification of clay minerals of Al-Khod (Northern Oman) using an X-ray diffraction method is described in detail in this paper. The method is based on the additions of known internal standards to the clay sample. The clay investigated in this study contained montmorillonite, palygorskite, illtte and kaolinite. Internal standards of these minerals were mixed with the clay at different proportions and intensities of reflected peak areas were measured. It was found that the peak areas intensities relate linearly with additions of different proportions of standards. From these intensities, the clay minerals present in the clay of Al-khod were estimated.


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