Chemical and X-ray diffraction analyses in tills of southern Ontario

1981 ◽  
Vol 18 (3) ◽  
pp. 584-590
Author(s):  
Q. H. J. Gwyn ◽  
B. J. Fryer ◽  
A. Dreimanis ◽  
A. M. Reid

The ratio of red to purple garnets found in tills in the eastern Great Lakes area has been very useful in stratigraphic and provenance studies of the tills. In an attempt to determine the basis of the color difference, and to supplement the colour differences by more objective criteria in till studies, X-ray diffraction and fluorescence, atomic absorption, and microprobe analyses were made. X-ray diffraction analyses show a consistent difference in the cell parameter of 0.05 Å (0.005 nm) or more between the two groups. Microprobe analyses of major elements indicate that the calcium and calculated ferric iron contents are higher and magnesium is lower in dark red garnets than in purple garnets. Bulk analyses of minor and trace elements by X-ray fluorescence and atomic absorption of different colour groups show distinct differences in rare-earth element patterns and manganese, which is eight times more abundant in the dark red garnets.

Coatings ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 37
Author(s):  
Yan Liu ◽  
Taoling Dong ◽  
Kun Zhang ◽  
Fuwei Yang ◽  
Liqin Wang

Targeting cleaning of the artificial gypsum layer on white marble was studied. It was conducted by means of the specific depletion of the calcium and sulfate ions by the barium carbonate scavenger, which led to the continuous dissolution and clearance of gypsum layer. The cleaning effect was evaluated by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), capillary suction, and color difference measurement. By this method, only the gypsum layer was cleared away and the carbonate substrate of marble was left intact at the same time. This method will be highly useful for the conservation of marble relics from surface weathering.


2020 ◽  
Vol 849 ◽  
pp. 113-118
Author(s):  
Yayat Iman Supriyatna ◽  
Slamet Sumardi ◽  
Widi Astuti ◽  
Athessia N. Nainggolan ◽  
Ajeng W. Ismail ◽  
...  

The purpose of this study is to characterize Lampung iron sand and to conduct preliminary experiments on the TiO2 synthesis which can be used for the manufacturing of functional food packaging. The iron sand from South Lampung Regency, Lampung Province that will be utilized as raw material. The experiment was initiated by sieving the iron sand on 80, 100, 150, 200 and 325 mesh sieves. Analysis using X-Ray Fluorescence (XRF) to determine the element content and X-Ray Diffraction (XRD) to observe the mineralization of the iron sand was conducted. The experiment was carried out through the stages of leaching, precipitation, and calcination. Roasting was applied firstly by putting the iron sand into the muffle furnace for 5 hours at a temperature of 700°C. Followed by leaching using HCl for 48 hours and heated at 105°C with a stirring speed of 300 rpm. The leaching solution was filtered with filtrate and solid residue as products. The solid residue was then leached using 10% H2O2 solution. The leached filtrate was heated at 105°C for 40 minutes resulting TiO2 precipitates (powder). Further, the powder was calcined and characterized. Characterization of raw material using XRF shows the major elements of Fe, Ti, Mg, Si, Al and Ca. The highest Ti content is found in mesh 200 with 9.6%, while iron content is about 80.7%. While from the XRD analysis, it shows five mineral types namely magnetite (Fe3O4), Rhodonite (Mn, Fe, Mg, Ca) SiO3, Quart (SiO2), Ilmenite (FeOTiO2) and Rutile (TiO2). The preliminary experiment showed that the Ti content in the synthesized TiO2 powder is 21.2%. The purity of TiO2 is low due to the presence of Fe metal which is dissolved during leaching, so that prior to precipitation purification is needed to remove impurities such as iron and other metals.


2016 ◽  
Vol 49 (1) ◽  
pp. 110-119 ◽  
Author(s):  
Nanna Wahlberg ◽  
Niels Bindzus ◽  
Sebastian Christensen ◽  
Jacob Becker ◽  
Ann-Christin Dippel ◽  
...  

A serious limitation of the all-in-vacuum diffractometer reported by Straasø, Dippel, Becker & Als-Nielsen [J. Synchrotron Rad.(2014),21, 119–126] has so far been the inability to cool samples to near-cryogenic temperatures during measurement. The problem is solved by placing the sample in a jet of helium gas cooled by liquid nitrogen. The resulting temperature change is quantified by determining the change in unit-cell parameter and atomic displacement parameter of copper. The cooling proved successful, with a resulting temperature of ∼95 (3) K. The measured powder X-ray diffraction data are of superb quality and high resolution [up to sinθ/λ = 2.2 Å−1], permitting an extensive modelling of the thermal displacement. The anharmonic displacement of copper was modelled by a Gram–Charlier expansion of the temperature factor. As expected, the corresponding probability distribution function shows an increased probability away from neighbouring atoms and a decreased probability towards them.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 325
Author(s):  
Sytle Antao

Synchrotron high-resolution powder X-ray diffraction (HRPXRD) and Rietveld structure refinements were used to examine the crystal structure of single phases and intergrowths (either two or three phases) in 13 samples of the helvine-group minerals, (Zn,Fe,Mn)8[Be6Si6O24]S2. The helvine structure was refined in the cubic space group P4¯3n. For the intergrowths, simultaneous refinements were carried out for each phase. The structural parameters for each phase in an intergrowth are only slightly different from each other. Each phase in an intergrowth has well-defined unit-cell and structural parameters that are significantly different from the three endmembers and these do not represent exsolution or immiscibility gaps in the ternary solid-solution series. The reason for the intergrowths in the helvine-group minerals is not clear considering the similar radii, identical charge, and diffusion among the interstitial M cations (Zn2+, Fe2+, and Mn2+) that are characteristic of elongated tetrahedral coordination. The difference between the radii of Zn2+ and Mn2+ cations is 10%. Depending on the availability of the M cations, intergrowths may occur as the temperature, pressure, fugacity fS2, and fluid composition change on crystallization. The Be–Si atoms are fully ordered. The Be–O and Si–O distances are nearly constant. Several structural parameters (Be–O–Si bridging angle, M–O, M–S, average <M–O/S>[4] distances, and TO4 rotational angles) vary linearly with the a unit-cell parameter across the series because of the size of the M cation.


1987 ◽  
Vol 2 (4) ◽  
pp. 225-226
Author(s):  
Peter Bayliss ◽  
Slade St. J. Warne

AbstractMagnesium-chlorophoenicite may be differentiated from the Mn-analogue chlorophoenicite, because for magnesium-chlorophoenicite at 7Å, whereas for chlorophoenicite.In a review of the literature for the Mineral Powder Diffraction File by Bayliss et al. (1980), powder X-ray diffraction data could not be found of the mineral species magnesium-chlorophoenicite, (Mg,Mn)3Zn2(AsO4)(OH,O)6. Dunn (1981) states that the powder X-ray diffraction data of magnesium-chlorophoenicite is essentially identical to that of chlorophoenicite (Mn analogue) and confirms that the minerals are isostructural.With the crystal structure parameters determined by Moore (1968) for a Harvard University specimen from New Jersey of chlorophoenicite, a powder X-ray diffraction pattern was calculated with the programme of Langhof, Physikalische Chemie Institute, Darmstadt. The calculated pattern was used to correct and complete the indexing of the powder X-ray diffraction data of chlorophoenicite specimen ROM M15667 from Franklin, Sussex County, New Jersey, U.S.A. by the Royal Ontario Museum (PDF 25-1159). With the correctly indexed data of ROM M15667, the unitcell parameters were refined by least-squares analysis and are listed in Table 1.The most magnesium-rich magnesium-chlorophoenicite found in the literature is a description of Harvard University specimen 92803 from Franklin, Sussex County, New Jersey, U.S.A. by Dunn (1981), where Mg is slightly greater than Mn. A 114.6 mm Debye-Schemer film taken of HU92803 with Cu radiation and a Ni filter (CuKα = 1.5418Å) was obtained from Dr. P. Dunn and measured visually. The unit-cell parameters, which were refined by least-squares analysis starting from the unit-cell parameters of PDF 25-1159 in space group C2/m(#12), are listed in Table 1, and give F28 = 4.1(0.050,136) by the method of Smith & Snyder (1979).The hkl, dcalulated, dobserved and relative intensities (I/I1) of HU92803 are presented in Table 2. With the atomic positions and temperature factors of chlorophoenicite determined by Moore (1968), the Mn atomic positions occupied by 50% Mg and 50% Mn, and the unit-cell parameters of HU92803, a powder X-ray diffraction pattern was calculated and Icalculated is recorded in Table 2. A third powder X-ray diffraction pattern was calculated with the Mn atomic positions fully occupied by Mg. Because the atomic scattering factor of Mn is more than twice greater than Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the calculated intensities of the first three reflections given in Table 3.Although the a, c and β unit-cell parameters of chlorphoenicite are similar to those of magnesium-chlorphoenicite, the b unit-cell parameter of chlorophoenicite is significantly greater than that of magnesium-chlorophoenicite (Table 1). The b unit-cell parameter represents the 0–0 distance of the Mn octahedra (Moore, 1968). Since the size of Mn is greater than that of Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the b unit-cell parameter given in Table 1.American Museum of Natural History (New York, N.Y., U.S.A.) specimen 28942 from Sterling Hill, Ogdensburg, New Jersey is composed of willemite, haidingerite and magnesian chlorophoenicite. A spectrographic analysis of the magnesian chlorophoenicite shows As, Mg, Mn and Zn. Powder X-ray diffraction data (PDF 34-190) of the magnesian chlorophoenicite was collected by diffractometer with Cu radiation and a graphite 0002 monochromator (Kα1 = 1.5405) at a scanning speed of 0.125° 2θ per minute. The unit-cell parameters, which were refined by leastsquares analysis starting from the unit-cell parameters of PDF 25-1159, are given in Table 1. Specimen AM 28942 is called chlorophoenicite, because of its large b unit-cell parameter (Table 1), and the I/I1 of 25 for reflection 001 and of 50 for reflection 201 compared to the Icalculated in Table 3.


Minerals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 522
Author(s):  
David Cruset ◽  
Jordi Ibáñez-Insa ◽  
Irene Cantarero ◽  
Cédric M. John ◽  
Anna Travé

Fracture-filling rose-like clusters of bladed calcite crystals are found in the northern sector of the Cadí thrust sheet (SE Pyrenees). This unusual calcite crystal morphology has been characterized by using optical and electron microscope, X-ray diffraction, Raman spectroscopy, δ18O, δ13C, 87Sr/86Sr, clumped isotopes, and major and rare earth elements + yttrium (REEs + Y) analysis. Petrographic observations and powder X-ray diffraction measurements indicate that these bladed crystals are mainly made of massive rhombic crystals with the conventional (104) faces, as well as of possibly younger, less abundant, and smaller laminar crystals displaying (108) and/or ( 1 ¯ 08) rhombic faces. Raman analysis of liquid fluid inclusions indicates the presence of aromatic hydrocarbons and occasionally alkanes. Clumped isotopes thermometry reflects that bladed calcite precipitated from meteoric fluids at ~60–65 °C. The 87Sr/86Sr ratios and major elements and REEs content of calcite indicate that these fluids interacted with Eocene marine carbonates. The presence of younger ‘nailhead’ calcite indicates later migration of shallow fresh groundwater. The results reveal that rose-like calcite clusters precipitated, at least in the studied area, due to a CO2 release by boiling of meteoric waters that mixed with benzene and aromatic hydrocarbons. This mixing decreased the boiling temperature at ~60–65 °C. The results also suggest that the high Sr content in calcite, and probably the presence of proteins within hydrocarbons trapped in fluid inclusions, controlled the precipitation of bladed crystals with (104) rhombohedral faces.


2013 ◽  
Vol 29 (1) ◽  
pp. 20-27 ◽  
Author(s):  
Sytle M. Antao ◽  
Allison M. Klincker

The structure of a birefringent andradite–grossular sample was refined using single-crystal X-ray diffraction (SCD) and synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. Electron-microprobe results indicate a homogeneous composition of {Ca2.88Mn2+0.06Mg0.04Fe2+0.03}Σ3[Fe3+1.29Al0.49Ti4+0.17Fe2+0.06]Σ2(Si2.89Al0.11)Σ3O12. The Rietveld refinement reducedχ2 = 1.384 and overallR(F2) = 0.0315. The HRPXRD data show that the sample contains three phases. For phase-1, the weight %, unit-cell parameter (Å), distances (Å), and site occupancy factor (sof) are 62.85(7)%,a = 12.000 06(2), average <Ca–O> = 2.4196, Fe–O = 1.9882(5), Si–O = 1.6542(6) Å, Ca(sof) = 0.970(2), Fe(sof) = 0.763(1), and Si(sof) = 0.954(2). The corresponding data for phase-2 are 19.14(9)%,a = 12.049 51(2), average <Ca–O> = 2.427, Fe–O = 1.999(1), Si–O = 1.665(1) Å, Ca(sof) = 0.928(4), Fe(sof) = 0.825(3), and Si(sof) = 0.964(4). The corresponding data for phase-3 are 18.01(9)%,a = 12.019 68(3), average <Ca–O> = 2.424, Fe–O = 1.992(2), Si–O = 1.658(2) Å, Ca(sof) = 0.896(5), Fe(sof) = 0.754(4), and Si(sof) = 0.936(5). The fine-scale coexistence of the three phases causes strain that arises from the unit-cell and bond distances differences, and gives rise to strain-induced birefringence. The results from the SCD are similar to the dominant phase-1 obtained by the HRPXRD, but the SCD misses the minor phases.


1996 ◽  
Vol 11 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Nicole M. L. N. P. Closset ◽  
René H. E. van Doorn ◽  
Henk Kruidhof ◽  
Jaap Boeijsma

The crystal structure of La1−xSrxCoO3−δ (0≤x≤0.6) has been studied, using powder X-Ray diffraction. The crystal structure shows a transition from rhombohedral distorted perovskite for LaCoO3−δ into cubic perovskite for La0.4Sr0.6CoO3−δ. The cubic unit cell parameter is ac=3.8342(1) Å for La0.4Sr0.6CoO3−δ, the space group probably being Pm3m. Using a hexagonal setting, the cell parameters for La0.5Sr0.5CoO3−δ, are a=5.4300(3) Å, c=13.2516(10) Å; a=5.4375(1) Å, c=13.2313(4) Å for La0.6Sr0.4CoO3−δ; a=5.4437(1) Å, c=13.2085(5) Å for La0.7Sr0.3CoO3−δ; a=5.4497(2) Å, c=13.1781(6) Å for La0.8Sr0.2CoO3−δ and a=5.4445(2) Å, c=13.0936(6) Å for LaCoO3−δ with the space group probably being R3c.


1978 ◽  
Vol 58 (3) ◽  
pp. 391-395 ◽  
Author(s):  
L. J. EVANS ◽  
J. G. ROWSELL ◽  
J. D. ASPINALL

Massive, but very localized, iron formations have been noted in some Humic Gleysols in southern Ontario. Some of these formations weigh up to 9 kg, and invariably occur at the contact zone between sandy loam to loam surface horizons and underlying clay-rich subsoils. The contents of Fe2O3 and MnO2 of 16 samples varied from 19.6 to 49.9% and 0.8 to 11.1%, respectively, although no crystalline oxides or hydroxides of Fe or Mn could be detected by X-ray diffraction. The localized occurence of these formations suggests that Fe2+ and Mn2+ are moving laterally through the subsoil and oxidizing at some seepage point downslope in the more aerated surface horizons.


1996 ◽  
Vol 11 (4) ◽  
pp. 268-275 ◽  
Author(s):  
Winnie Wong-Ng ◽  
F. Jiang ◽  
Bryan R. Jarabek ◽  
Gregory J. McCarthy

Powder X-ray diffraction was used to investigate the solid solution range of the Bi14SrxCa12−xO33 series in the Bi–Sr–Ca–O system. Solid solution forms over the range 1≤x≤7 in Bi14SrxCa12−xO33. Experimental X-ray reference patterns of selected members with x=1, 3, 5, and 7 have been prepared for the powder diffraction file (PDF). These phases are monoclinic, C2/m, with cell parameter a ranging from 21.473(4) to 21.868(4) Å, b from 4.3564(9) to 4.3898(9) Å, c from 12.753(2) to 12.962(2) Å, β from 102.91(2)° to 102.79(1)°, and V from 1162.9(3) to 1213.5(3) Å3, respectively. These parameters increase monotonically as Ca is continuously replaced by the larger Sr.


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