Reach of pollution and sediment correlation with the tailings in Šibenik Bay (Croatia)

<p>To determine the influence of the historic factory of electrodes and ferroalloys on the Šibenik bay sediments, XRPD analysis were carried out. The factory was established in the city of Šibenik, on the coast of the Krka River estuary, and produced calcium carbide, and later electrodes and ferroalloys. It was active from 1900 until 1995 [1]. During that time, a large amount of produced tailings were stored nearby and on the shore of the estuary. Due to the presence of the strong winds (bora and sirocco), which can reach up to 130 km/h, the tailings material could be transported to long distances [2].</p><p>Samples of tailing were collected at the location of the former factory, which is a tailing hill today, samples of dust were collected from the rooftop of the factory in the 1980s. Other samples were taken on a 1 km distant beach in the Šibenik bay  (Beach A) and a 19 km distant beach on the island in the outer Šibenik archipelago (Beach B). Both beaches are located south-west of the factory. The samples from the beaches were taken with a corer at different depths: 0 – 3 cm, 3 – 5 cm, around 5 cm. The sample from 3 – 5 cm depth was not analysed.</p><p>Bulk sample and a fraction <63 µm were analysed on X-Ray Diffractometer. The XRPD analysis of the sediments from Beach B in the outer Šibenik archipelago shows that calcite and quartz are the most abundant phases. This mineral composition shows that distant islands were not affected by aeolian transportation of the factory dust and tailing. In the bulk samples from Beach A, in the uppermost part (0 – 3 cm depth) mineral components are calcite, aragonite, calcium manganite, bustamite ferroan and carbon, while calcite, quartz, aragonite, calcium manganite and manganosite are present in the fraction <63 µm. The sample from the depth of 5 cm at the same beach, shows calcite, aragonite and Mn-oxide, while fraction <63 µm lacks in Mn-oxide.</p><p>A bulk sample of tailings shows mineral components: calcite, quartz, calcium manganite, bustamite ferroan and gypsum which corresponds to the previous research [3], and there is also manganese silicon, manganese silicide, carbon and amorphous phase [4]. A fraction <63 µm of the tailing, shows the following mineral phases: calcite, quartz, calcium manganite and bustamite ferroan, as presented in previous research [3]. Analysis of the rooftop dust shows three phases: carbon, bustamite ferroan and manganosite, which does not correspond to the data given from the factory [3].</p><p>From the presented results, it could be concluded that the historic factory influenced sediments in the Šibenik bay, however, its influence was not detected on the Beach B 19 km to the SW, which opens the question of reach and distance to which tailings can be transported by sea and/or wind.</p><p>This work has been supported in part (samples collection) by Croatian Science Foundation under the project lP-2019-04-5832.</p>

Quantitative Analysis of Asbestos-Containing Materials Using Various Test Methods

The advantages of X-ray powder diffraction (XRPD) analysis are its non-destructive nature, reliability, fast and easy sample preparation, and low costs. XRPD analysis has been used for mineral identification and the quantitative/qualitative determination of various types of fibrous minerals in asbestos-containing materials (ACMs). In order to test the detection limit of ACMs by XRPDD, standard samples with various concentrations of ACMs (0.1%, 1%, and 3%) were fabricated using three matrix materials (talc, vermiculite, and sepiolite). Asbestiform tremolite and chrysotile were identified in the XRPD profiles of the samples with 1% and 3% ACMs. Their integral intensities were positively correlated with the concentrations. However, the XRPD peak of asbestos was not found in the samples with 0.1% ACMs. Therefore, scanning and transmission electron microscopy were utilized to investigate the samples with a very low concentration of ACMs. Although the ACM concentration (0.1%) was negligible and its direct observation was time-consuming, electron microscopy allowed for the detection of asbestos in several matrix materials. Thus, a combination of XRPD and electron microscopy improve analytical performance and data reliability.

Archaeometric study of the historic terrazzo pavement of Prince Mohamed Ali Museum, Cairo, Egypt

This research will shed light on studying a terrazzo pavement in Prince Mohamed Ali Museum (the case study). The authors used visual inspection, stereo microscope, USB microscope, XRPD analysis, and SEM.EDX to identify its components, deterioration aspects and execution techniques. The XRPD and SEM.EDX results revealed that Portland cement was used in the three layers of terrazzo because of the detection of Hatrurite, Alite, Anorthite, Albite, Aragonite, etc. Many pigments were used in the topping terrazzo layer as; Goethite, Greenalite, Hematite, Azurite and Magnetite. The divider strips were made of brass alloy and the topping layer chips were prepared from basalt, marble and sea shells.

Structures and properties of three new homobinuclear nanosized supramolecular copper coordination polymers derived from carboxylate type ligands and benzimidazole

Three new homobinuclear nanosized supramolecular copper coordination polymers are hydrothermally synthesized by self-assembly reaction of L-tyrosine (Tyr), terephthalic acid (H2bdc), pyromellitic acid (H4btec) and benzimidazole (Hbzim) with copper chloride salt to generate with formula [[Cu2(tyr)2(bzim)2(Cl)2(H2O)2]]n 1, [[Cu2(bdc)2(bzim)2(H2O)6].3H2O]n 2 and [Cu2(H2btec)(bzim)(H2O)6].2H2O]n 3, which have been investigated by elemental analysis, molar conductivity and magnetic measurements, FT-IR and UV-Vis spectroscopy, (TGA/DTA) thermal analysis and X-ray powder diffraction(XRPD) analysis as well as MM2 theoretical calculations. The magnetic moment and electronic spectra of the complexes are certainly indicating the octahedral geometries. Thermal analysis of the complexes confirms the suggested structures and thermal stability. The results of the XRPD analysis and the average nanosized values of the complexes have nanosized supramolecular polymers in the triclinic system. The MM2 theoretical calculations are supported by the proposed structures.

COMPARATIVE FOURIER TRANSFORM INFRARED AND X-RAY POWDER DIFFRACTION ANALYSIS OF NATURALLY OCCURRED K-FELDSPARS

Natural K-feldspars from igneous rocks have been examined by means of X-ray powder diffraction(XRPD) and Fourier transform infrared (FTIR) spectroscopy in the spectral range 400-1400 cm-1,where the Si-Al-O bonds exhibit the dominant vibrations. From the XRPD analysis three specieshave been distinguished, i.e. microclines (3 samples), orthoclases (4 samples) and sanidines (3 samples);their unit cell parameters were calculated. The FTIR transmittance spectra of all sampleshave common bands at 426, 463, 584, 604, 726 and 772 cm-1 and some additional features. The spectraof sanidine and orthoclase exhibit fewer and broader bands than the microclines’, especially inthe area 1000-1200 cm-1. The differences in their spectra are located in four bands. The bands ataround 536-538 and 646-648 cm-1 in the spectrum of microcline, are shifted at around 542-544 and640-642 cm-1 in the spectrum of orthoclase and at around 546 and 636 cm-1 in the spectrum of sanidine.Four bands at 1010, 1050, 1090 and 1136 cm-1 in the spectra of microcline are substitutedwith two quite broad bands at about 1030 and 1125 cm-1 in the spectra of orthoclase and sanidine.These differences are attributed to different degree of Al-Si ordering in the structure of K-feldspars.

Removal of Cs ions from aqueous solutions by using matrices of natural clinoptilolite and its safe disposal

The possibility to use natural zeolite - clinoptilolite as a host material for radioactive Cs immobilization has been investigated. Cs-exchanged form of clinoptilolite which was prepared by treatment of clinoptilolite powder with 0.25 M CsCl solution was compacted. Both, powder and powder compact of exchanged clinoptilolite were thermally treated at 1200?C. The XRPD analysis showed that Cs was successfully immobilized after heat treatment by formation of stable cesium dodecaoxo-alumopentasilicate in both, powder sample and compact. The newly formed compound showed satisfactory Cs ions retention during leaching test. The sintered compact showed somewhat better resistance to Cs leaching than the thermally treated powder. The compressive strength of sintered compact was close to 200 MPa which is more than enough for easy handling and safe storage.

Quality of zeolit from Vranjska banja deposit according to size classes

This paper presents results of investigations of the quality of the natural zeolite as well as the quality of particular particle size classes of the natural zeolite. The aim of the investigations was to determine if the different classes possess different qualitys. The starting material used in experiements was the natural zeolite from Zlatokop deposit (Vranjska Banja, Serbia).. The classes -0.2+0.8 mm; -0.8+0.6 mm; -0.6+0.4 mm; -0.4+0.1 mm were obtained by wet sieving of the natural zeolite. Grinding processes of the natural zeolite gave classes -0.3+0.63 mm; -0.63+0 mm; -0,43+0 mm. Chemical composition , mineralogical XRPD analysis and cation exchange capacity (CEC) were performed on the starting sample and the obtained particle size classes. It was determined that all particle size classes possess similar quality. The highest cation exchange capacity was observed in classes -0,043+0mm (166,5 meq/100g) and -0,063+0mm (158, 8 meq/100g).

A sample holder for in-house X-ray powder diffraction studies of protein powders

A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 µl of sample, corresponding to approximately 2–3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the ZnK-edge were tested with hexameric Zn insulin.