A new collection of clay mineral ‘Crystallinity’ Index Standards and revised guidelines for the calibration of Kübler and Árkai indices

Clay Minerals ◽  
2018 ◽  
Vol 53 (3) ◽  
pp. 339-350 ◽  
Author(s):  
Laurence N. Warr
Keyword(s):  
Clay Mineral ◽  
Lower Boundary ◽  
Crystallinity Index ◽  
Measurement Methods ◽  
Peak Width ◽  
X Ray Diffraction ◽  
X Ray ◽  
Kübler Index ◽  
Boundary Limits ◽  
Mineral Crystallinity

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.

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
Keyword(s):  
Clay Mineral ◽  
Crystallinity Index ◽  
White Mica ◽  
Early Jurassic ◽  
Late Triassic ◽  
X Ray Diffraction ◽  
Middle Ordovician ◽  
Late Cambrian ◽  
Isotopic Analyses ◽  
Mineral Crystallinity

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.

Recommendations for Kübler Index standardization

Clay Minerals ◽  
2015 ◽  
Vol 50 (3) ◽  
pp. 283-286 ◽  
Author(s):  
L.N. Warr ◽  
R. Ferreiro Mählmann
Keyword(s):  
Lower Boundary ◽  
Crystallinity Index ◽  
Round Table ◽  
Rock Fragment ◽  
Round Table Discussion ◽  
Working Definition ◽  
Kübler Index ◽  
Definition Of ◽  
Boundary Limits ◽  
Index Standardization

AbstractFollowing a round-table discussion at the Mid-European Clay Conference in Dresden 2014, new recommendations for illite ‘crystallinity’ Kübler index standardization have been agreed upon. The use of Crystallinity Index standards in the form of rock-fragment samples will be continued, along with the same numerical scale of measurement presented by Warr & Rice (1994). However, in order to be compatible with the original working definition of Kübler's (1967) anchizone, the upper and lower boundary limits of the Crystallinity Index Standard (CIS) scale are adjusted appropriately from 0.25°2θ and 0.42°2θ to 0.32°2θ and 0.52°2θ. This adjustment is based on an inter-laboratory correlation between the laboratories of Basel, Neuchâtel and the CIS scale. The details of this correction are presented in this first note, as discussed at the round-table meeting and will be further substantiated by a correlation program between CIS and former Kübler–Frey–Kisch standards.

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.

scholarly journals Valorization of Byproducts of Hemp Multipurpose Crop: Short Non-Aligned Bast Fibers as a Source of Nanocellulose

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4723
Author(s):  
Sara Dalle Vacche ◽  
Vijayaletchumy Karunakaran ◽  
Alessia Patrucco ◽  
Marina Zoccola ◽  
Loreleï Douard ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Cannabis Sativa ◽  
Crystallinity Index ◽  
Residual Lignin ◽  
Chemical Pretreatment ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bast Fibers ◽  
Seed Maturity

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.

Clay Mineral Alteration in Oil and Gas Fields: Integrated Analyses of Surface Expression, Soil Spectra, and X-Ray Diffraction Data

2020 ◽  
Vol 46 (2) ◽  
pp. 237-251
Author(s):  
Tri Muji Susantoro ◽  
Asep Saepuloh ◽  
Fitriani Agustin ◽  
Ketut Wikantika ◽  
Agus Handoyo Harsolumakso
Keyword(s):  
Clay Mineral ◽  
Diffraction Data ◽  
Oil And Gas ◽  
Surface Expression ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oil And Gas Fields ◽  
Mineral Alteration ◽  
Gas Fields

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.

scholarly journals Preparation and Properties of Nanocellulose from Miscanthus x giganteus

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Valerii A. Barbash ◽  
Olha V. Yashchenko ◽  
Olesia A. Vasylieva
Keyword(s):  
Structural Changes ◽  
Thermochemical Treatment ◽  
Crystallinity Index ◽  
Alkaline Treatment ◽  
X Ray Diffraction ◽  
Miscanthus X Giganteus ◽  
X Ray ◽  
Second Stage ◽  
20 Nm ◽  
Hydrolysis Of

Miscanthus x giganteus stalks were used to make organosolvent pulp and nanocellulose. The organosolvent miscanthus pulp (OMP) was obtained through thermal treatment in the mixture of glacial acetic acid and hydrogen peroxide at the first stage and the alkaline treatment at the second stage. Hydrolysis of the never-dried OМP was carried out by a solution of sulfuric acid with concentrations of 43% and 50% and followed by ultrasound treatment. Structural changes and the crystallinity index of OMP and nanocellulose were studied by SEM and FTIR methods. X-ray diffraction analysis confirmed an increase in the crystallinity of OMP and nanocellulose as a result of thermochemical treatment. We show that nanocellulose has a density of up to 1.6 g/cm3, transparency up to 82%, and a crystallinity index of 76.5%. The AFM method showed that the particles of nanocellulose have a diameter in the range from 10 to 20 nm. A thermogravimetric analysis confirmed that nanocellulose films have a denser structure and lower mass loss in the temperature range of 320–440°C compared to OMP. The obtained nanocellulose films have high tensile strength up to 195 MPa. The nanocellulose obtained from OMP exhibits the improved properties for the preparation of new nanocomposite materials.

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