K–Ar age determinations on the fine fractions of clay mineral ‘Crystallinity Index Standards’ from the Palaeozoic mudrocks of southwest England

Clay Minerals ◽  
2019 ◽  
Vol 54 (1) ◽  
pp. 15-26 ◽  
Author(s):  
Anna C. Schomberg ◽  
Klaus Wemmer ◽  
Laurence N. Warr ◽  
Georg H. Grathoff

AbstractClay mineral ‘Crystallinity Index Standards’ (CIS) composed of Palaeozoic mudrocks from southwest England were investigated systematically in five sub-fractions per sample for the first time. X-ray diffraction was used to determine mineral assemblages, calibrated 001 illite full-width-at-half-maximum (FWHM) values and illite polytype compositions, in addition to K–Ar isotopic analyses of all fine fractions. The FWHM results of the <2 µm fraction are consistent with previous studies and reflect the range of diagenetic to epizonal grades covered by the sample set SW1 to SW7 (~0.61–0.26°2θ). Diagenetic and lower anchizone samples also show significant broadening of 001 illite reflections in the finer fractions and contain mixtures of authigenic 1M + 1Md illite and detrital 2M1 white mica polytypes suitable for illite age analysis. The estimated end-member ages of the Bude (SW1-1992) and younger Crackington (SW3-2000) mudstones yield detrital ages of Late Cambrian to Middle Ordovician (493–457 Ma) and a broad range of 1M + 1Md illite ages between Middle Permian and Early Jurassic (271–190 Ma). The detrital age of the stratigraphically older Crackington Formation mudrock (SW2-1992) is Late Devonian (384–364 Ma) with 1M + 1Md illite ages between Late Triassic and Early Jurassic (219–176 Ma). The origin of Mesozoic 1M + 1Md illite ages may represent neocrystallized illite associated with Mesozoic hydrothermal events or similar events that thermally reset older authigenic illite with partial loss of radiogenic argon and no renewed crystal growth. In contrast, upper anchizonal and epizonal Devonian slates (SW3-2012, SW4-1992, SW6-1992 and SW7-2012) contain only the 2M1 polytype, with K–Ar ages younger than the stratigraphic age. The three finest fractions of SW4-1992 yield consistent Late Carboniferous ages (331–304 ± 7 Ma) that are considered to date the neocrystallized 2M1 mica. Most fractions of epizonal slate (SW6-1992, SW7-2012) yield Early Permian ages (293.6–273 Ma) corresponding to published cooling ages of the Tintagel High-Strain Zone and the intrusion of the Bodmin granite (291.4 ± 0.8 Ma). These first K–Ar age constraints for the fine fractions of the CIS should provide useful reference values for testing analytical procedures of illite age analysis.

Clay Minerals ◽  
2018 ◽  
Vol 53 (3) ◽  
pp. 339-350 ◽  
Author(s):  
Laurence N. Warr

ABSTRACTA new set of clay mineral ‘Crystallinity’ Index Standards (CIS) is available for improved calibration of the half-peak-width values of the X-ray diffraction 001 illite reflection (the Kübler index) and the 002 chlorite reflection (the Árkai index), two widely used indices for determining the state of prograde diagenesis and low-temperature metamorphism. Calibration using mudrock standards removes the numerical differences between laboratories caused by variations in sample preparation, machine settings and measurement methods, thus avoiding erroneous grade determinations. The number of standards available has been increased to nine. These can be used to obtain Kübler index values for each CIS sample and Árkai index values for upper anchizonal and epizonal samples. The diagenetic and lower anchizonal mudrocks are not suitable for Árkai index measurements due to the absence of chlorite or overlap by the 001 kaolinite reflection. Applying the new Kübler-equivalent upper and lower boundary limits of the anchizone placed at 0.32°2θ and 0.52°2θ, respectively (Warr & Ferreiro Mählmann, 2015), the nine standards from the Palaeozoic mudrocks of southwest England now comprise two diagenetic, two lower anchizonal, three upper anchizonal and two epizonal grade samples. These range from weakly cleaved mudstones to strongly foliated slates.


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.


1977 ◽  
Vol 114 (4) ◽  
pp. 281-290 ◽  
Author(s):  
K. Amiri-Garroussi

SummaryClay mineral analysis of shales in the early Liassic Lower Broadford Beds of the Hebrides reveals the presence of abundant quantities of montmorillonite whereas the Upper Broadford Beds contain illite, kaolinite and subordinate mixed layer minerals together with chlorite. Montmorillonite enrichment of the Lower Broadford Beds as a consequence of recent weathering contamination by doleritic sills can effectively be ruled out. It is argued that the montmorillonite may have been derived from the weathering of basic igneous rocks exposed in the sediment source area during Late Triassic times. By Upper Broadford Beds times, the igneous source was either eroded away or transgressed by the early Liassic sea.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

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.


Author(s):  
Maria Ricciardi ◽  
Concetta Pironti ◽  
Oriana Motta ◽  
Rosa Fiorillo ◽  
Federica Camin ◽  
...  

AbstractIn this paper, we analysed the efflorescences present in the frescos of a monumental complex named S. Pietro a Corte situated in the historic centre of Salerno (Campania, Italy). The groundwater of the historic centre is fed by two important streams (the Rafastia and the Fusandola) that can be the sources of water penetration. The aims of this work are to (i) identify the stream that reaches the ancient frigidarium of S. Pietro a Corte and (ii) characterize the efflorescences on damaged frescos in terms of chemical nature and sources. In order to accomplish the first aim, the water of the Rafastia river (7 samples) and the water of the Fusandola river (7 samples) were analysed and compared with the water of a well of the Church (7 samples). The ionic chromatography measurements on the water samples allowed us to identify the Rafastia as the river that feeds the ancient frigidarium of S. Pietro a Corte. To investigate the nature and the origin of the efflorescences (our second aim), anionic chromatography analyses, X-ray diffraction measurements, and the isotopic determination of nitrogen were performed on the efflorescences (9 samples) and the salts recovered from the well (6 samples). Results of these analyses show that efflorescences are mainly made of potassium nitrate with a δ15N value of + 9.3 ± 0.2‰. Consequently, a plausible explanation for their formation could be the permeation of sewage water on the walls of the monumental complex.


Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1527
Author(s):  
Magdalena Woźniak ◽  
Izabela Ratajczak ◽  
Dawid Wojcieszak ◽  
Agnieszka Waśkiewicz ◽  
Kinga Szentner ◽  
...  

In the last decade, an increasingly common method of maize stover management is to use it for energy generation, including anaerobic digestion for biogas production. Therefore, the aim of this study was to provide a chemical and structural characterization of maize stover fractions and, based on these parameters, to evaluate the potential application of these fractions, including forbiogas production. In the study, maize stover fractions, including cobs, husks, leaves and stalks, were used. The biomass samples were characterized by infrared spectroscopy (FTIR), X-ray diffraction and analysis of elemental composition. Among all maize stover fractions, stalks showed the highest C:N ratio, degree of crystallinity and cellulose and lignin contents. The high crystallinity index of stalks (38%) is associated with their high cellulose content (44.87%). FTIR analysis showed that the spectrum of maize stalks is characterized by the highest intensity of bands at 1512 cm−1 and 1384 cm−1, which are the characteristic bands of lignin and cellulose. Obtained results indicate that the maize stover fraction has an influence on the chemical and structural parameters. Moreover, presented results indicate that stalks are characterized by the most favorable chemical parameters for biogas production.


Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4723
Author(s):  
Sara Dalle Vacche ◽  
Vijayaletchumy Karunakaran ◽  
Alessia Patrucco ◽  
Marina Zoccola ◽  
Loreleï Douard ◽  
...  

Nanocellulose was extracted from short bast fibers, from hemp (Cannabis sativa L.) plants harvested at seed maturity, non-retted, and mechanically decorticated in a defibering apparatus, giving non-aligned fibers. A chemical pretreatment with NaOH and HCl allowed the removal of most of the non-cellulosic components of the fibers. No bleaching was performed. The chemically pretreated fibers were then refined in a beater and treated with a cellulase enzyme, followed by mechanical defibrillation in an ultrafine friction grinder. The fibers were characterized by microscopy, infrared spectroscopy, thermogravimetric analysis and X-ray diffraction after each step of the process to understand the evolution of their morphology and composition. The obtained nanocellulose suspension was composed of short nanofibrils with widths of 5–12 nm, stacks of nanofibrils with widths of 20–200 nm, and some larger fibers. The crystallinity index was found to increase from 74% for the raw fibers to 80% for the nanocellulose. The nanocellulose retained a yellowish color, indicating the presence of some residual lignin. The properties of the nanopaper prepared with the hemp nanocellulose were similar to those of nanopapers prepared with wood pulp-derived rod-like nanofibrils.


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