A new method in estimation of total hexavalent chromium in Portland pozzolan cement

Variamine blue was used first time for the detection of hexavalent chromium from cement samples. In present method, cement was treated sequentially with water, sulphate and carbonate buffer to extract soluble, sparingly soluble and insoluble hexavalent chromium respectively. Extracted Cr (VI) was determined using variamine blue as chromogenic reagent. The determination is based on the reaction of hexavalent chromium with potassium iodide in an acid medium to liberate iodine. This oxidizes variamine blue to form a violet coloured species having an absorption to maximum at 556 nm. Energy-dispersive X-ray spectroscopy (EDX) and Infrared Spectroscopy (IR) confirmed the complete extraction of hexavalent chromium by sequential extraction process. SRM 2701 (Reference material from NIST, USA) was used for revalidating the results. The percentage of recovery for proposed and reference method (diphelycarbazide method) varied from 98.5 to 101 and 97.5 to 100.5. Whereas, their relative error percentage varied from -1.5 to 0.33 and -2.5 to 0.5.

Download Full-text

Diphosphinoazine Rhodium(I) and Iridium(I) Complexes

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc20060197 ◽

2006 ◽

Vol 71 (2) ◽

pp. 197-206 ◽

Cited By ~ 1

Author(s):

Martin Pošta ◽

Jan Čermák ◽

Pavel Vojtíšek ◽

Ivana Císařová

Keyword(s):

Rhodium Complexes ◽

Iridium Complexes ◽

X Ray ◽

First Time

The first rhodium complexes of diphosphinoazines [{RhCl(1,2-η:5,6-η-CH=CHCH2CH2CH=CHCH2CH2)}2 {μ-R2PCH2C(But)=NN=C(But)CH2PR2] (R = Ph, Cy, Pri) were prepared by cleavage of the bridge in chloro(cycloocta-1,5-diene)rhodium(I) dimer, the analogous iridium(I) complexes were also prepared for the first time. The X-ray structures of isostructural rhodium and iridium complexes with bis(dicyclohexylphosphino)pinacoloneazine were determined. Diphosphinoazine ligands in the complexes remained in (Z,Z) configuration bridging two RhCl(C8H12) units.

Download Full-text

Quartz Crystallite Size and Moganite Content as Indicators of the Mineralogical Maturity of the Carboniferous Chert: The Case of Cherts from Eastern Asturias (Spain)

Minerals ◽

10.3390/min11060611 ◽

2021 ◽

Vol 11 (6) ◽

pp. 611

Author(s):

Celia Marcos ◽

María de Uribe-Zorita ◽

Pedro Álvarez-Lloret ◽

Alaa Adawy ◽

Patricia Fernández ◽

...

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Crystallite Size ◽

Archaeological Sites ◽

X Ray Diffraction ◽

X Ray ◽

Transmission Electron ◽

Infrared And Raman Spectroscopy ◽

First Time ◽

Geological Formations

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.

Download Full-text

First Report on the Geologic Occurrence of Natural Na–A Zeolite and Associated Minerals in Cretaceous Mudstones of the Paja Formation of Vélez (Santander), Colombia

Crystals ◽

10.3390/cryst11020218 ◽

2021 ◽

Vol 11 (2) ◽

pp. 218

Author(s):

Carlos Alberto Ríos-Reyes ◽

German Alfonso Reyes-Mendoza ◽

José Antonio Henao-Martínez ◽

Craig Williams ◽

Alan Dyer

Keyword(s):

Natural Zeolite ◽

Scanning Electron Micrographs ◽

Total Sulfur ◽

Zeolite A ◽

X Ray Diffraction ◽

X Ray ◽

Mineral Phases ◽

The World ◽

Porosity And Permeability ◽

First Time

This study reports for the first time the geologic occurrence of natural zeolite A and associated minerals in mudstones from the Cretaceous Paja Formation in the urban area of the municipality of Vélez (Santander), Colombia. These rocks are mainly composed of quartz, muscovite, pyrophyllite, kaolinite and chlorite group minerals, framboidal and cubic pyrite, as well as marcasite, with minor feldspar, sulphates, and phosphates. Total organic carbon (TOC), total sulfur (TS), and millimeter fragments of algae are high, whereas few centimeters and not biodiverse small ammonite fossils, and other allochemical components are subordinated. Na–A zeolite and associated mineral phases as sodalite occur just beside the interparticle micropores (honeycomb from framboidal, cube molds, and amorphous cavities). It is facilitated by petrophysical properties alterations, due to processes of high diagenesis, temperatures up to 80–100 °C, with weathering contributions, which increase the porosity and permeability, as well as the transmissivity (fluid flow), allowing the geochemistry remobilization and/or recrystallization of pre-existing silica, muscovite, kaolinite minerals group, salts, carbonates, oxides and peroxides. X-ray diffraction analyses reveal the mineral composition of the mudstones and scanning electron micrographs show the typical cubic morphology of Na–A zeolite of approximately 0.45 mμ in particle size. Our data show that the sequence of the transformation of phases is: Poorly crystalline aluminosilicate → sodalite → Na–A zeolite. A literature review shows that this is an unusual example of the occurrence of natural zeolites in sedimentary marine rocks recognized around the world.

Download Full-text

The Effect of Surfactant-Modified Montmorillonite on the Cross-Linking Efficiency of Polysiloxanes

Materials ◽

10.3390/ma14102623 ◽

2021 ◽

Vol 14 (10) ◽

pp. 2623

Author(s):

Monika Wójcik-Bania ◽

Jakub Matusik

Keyword(s):

Total Pore Volume ◽

Cross Linking ◽

X Ray Diffraction ◽

X Ray ◽

Transmission Electron ◽

The Cross ◽

Chain Lengths ◽

First Time ◽

Substituent Influence ◽

Benzyl Substituent

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.

Download Full-text

Homopiperazine (Hexahydro-1,4-diazepine)

Molbank ◽

10.3390/m1200 ◽

2021 ◽

Vol 2021 (2) ◽

pp. M1200

Author(s):

R. Alan Aitken ◽

Dheirya K. Sonecha ◽

Alexandra M. Z. Slawin

Keyword(s):

13C Nmr ◽

Title Compound ◽

Coupling Constants ◽

15N Nmr ◽

Time Data ◽

Nmr Spectrum ◽

X Ray ◽

First Time

The X-ray structure of the title compound has been determined for the first time. Data on its 1H–13C-NMR coupling constants and 15N-NMR spectrum are also given.

Download Full-text

Removal of hexavalent chromium from wastewater by Cu/Fe bimetallic nanoparticles

Scientific Reports ◽

10.1038/s41598-021-90414-0 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Jien Ye ◽

Yi Wang ◽

Qiao Xu ◽

Hanxin Wu ◽

Jianhao Tong ◽

...

Keyword(s):

Hexavalent Chromium ◽

Removal Efficiency ◽

Photoelectron Spectroscopy ◽

Bimetallic Nanoparticles ◽

Chemical Reduction ◽

Particle Surface ◽

Zerovalent Iron ◽

Order Model ◽

X Ray ◽

Nanoscale Zerovalent Iron

AbstractPassivation of nanoscale zerovalent iron hinders its efficiency in water treatment, and loading another catalytic metal has been found to improve the efficiency significantly. In this study, Cu/Fe bimetallic nanoparticles were prepared by liquid-phase chemical reduction for removal of hexavalent chromium (Cr(VI)) from wastewater. Synthesized bimetallic nanoparticles were characterized by transmission electron microscopy, Brunauer–Emmet–Teller isotherm, and X-ray diffraction. The results showed that Cu loading can significantly enhance the removal efficiency of Cr(VI) by 29.3% to 84.0%, and the optimal Cu loading rate was 3% (wt%). The removal efficiency decreased with increasing initial pH and Cr(VI) concentration. The removal of Cr(VI) was better fitted by pseudo-second-order model than pseudo-first-order model. Thermodynamic analysis revealed that the Cr(VI) removal was spontaneous and endothermic, and the increase of reaction temperature facilitated the process. X-ray photoelectron spectroscopy (XPS) analysis indicated that Cr(VI) was completely reduced to Cr(III) and precipitated on the particle surface as hydroxylated Cr(OH)3 and CrxFe1−x(OH)3 coprecipitation. Our work could be beneficial for the application of iron-based nanomaterials in remediation of wastewater.

Download Full-text

A novel and potentially scalable CVD-based route towards SnO2:Mo thin films as transparent conducting oxides

Journal of Materials Science ◽

10.1007/s10853-021-06269-3 ◽

2021 ◽

Author(s):

Tianlei Ma ◽

Marek Nikiel ◽

Andrew G. Thomas ◽

Mohamed Missous ◽

David J. Lewis

Keyword(s):

Thin Films ◽

Photoelectron Spectroscopy ◽

Mixed Valence ◽

Chemical Vapour ◽

X Ray Diffraction ◽

X Ray ◽

Conducting Oxides ◽

Valence States ◽

3 Omega ◽

First Time

AbstractIn this report, we prepared transparent and conducting undoped and molybdenum-doped tin oxide (Mo–SnO2) thin films by aerosol-assisted chemical vapour deposition (AACVD). The relationship between the precursor concentration in the feed and in the resulting films was studied by energy-dispersive X-ray spectroscopy, suggesting that the efficiency of doping is quantitative and that this method could potentially impart exquisite control over dopant levels. All SnO2 films were in tetragonal structure as confirmed by powder X-ray diffraction measurements. X-ray photoelectron spectroscopy characterisation indicated for the first time that Mo ions were in mixed valence states of Mo(VI) and Mo(V) on the surface. Incorporation of Mo6+ resulted in the lowest resistivity of $$7.3 \times 10^{{ - 3}} \Omega \,{\text{cm}}$$ 7.3 × 10 - 3 Ω cm , compared to pure SnO2 films with resistivities of $$4.3\left( 0 \right) \times 10^{{ - 2}} \Omega \,{\text{cm}}$$ 4.3 0 × 10 - 2 Ω cm . Meanwhile, a high transmittance of 83% in the visible light range was also acquired. This work presents a comprehensive investigation into impact of Mo doping on SnO2 films synthesised by AACVD for the first time and establishes the potential for scalable deposition of SnO2:Mo thin films in TCO manufacturing. Graphical abstract

Download Full-text

Incorporation of silver stearate nanoparticles in methacrylate polymeric monoliths for hemeprotein isolation

Open Chemistry ◽

10.1515/chem-2020-0051 ◽

2020 ◽

Vol 18 (1) ◽

pp. 399-411

Author(s):

Eman Alzahrani

Keyword(s):

Noble Metals ◽

Extraction Process ◽

Sem Analysis ◽

X Ray ◽

Polymeric Scaffold ◽

Extended Surface ◽

Unique Method ◽

Unique Approach ◽

Ft Ir ◽

Ft Ir Spectroscopy

AbstractA unique method was used to synthesize extremely stable silver stearate nanoparticles (AgStNPs) incorporated in an organic-based monolith. The facile strategy was then used to selectively isolate hemeproteins, myoglobin (Myo) and hemoglobin (Hb). Ethyl alcohol, silver nitrate, and stearic acid were, respectively, utilized as reducing agents, silver precursors, and capping agents. The color changed to cloudy from transparent, indicating that AgStNPs had been formed. AgStNP nanostructures were then distinctly integrated into the natural polymeric scaffold. To characterize the AgStNP–methacrylate polymeric monolith and the silver nanoparticles, energy-dispersive X-ray (EDX), scanning electron microscopy (SEM), and Fourier-transform infrared (FT-IR) spectroscopy were used. The results of the SEM analysis indicated that the AgStNP–methacrylate polymeric monolith’s texture was so rough in comparison with that of the methacrylate polymeric monolith, indicating that the extraction process of the monolith materials would be more efficient because of the extended surface area of the absorbent. The comparison between the FT-IR spectra of AgStNPs, the bare organic monolith, and AgStNP–methacrylate polymeric monolith confirms that the AgStNPs were immobilized on the surface of the organic monolith. The EDX profile of the built materials indicated an advanced peak of the Ag sequence which represented an Ag atom of 3.27%. The results therefore established that the AgStNPs had been successfully integrated into the monolithic materials. Extraction efficiencies of 92% and 97% were used to, respectively, recover preconcentrated Myo and Hb. An uncomplicated method is a unique approach of both fabrication and utilization of the nanosorbent to selectively isolate hemeproteins. The process can further be implemented by using other noble metals.

Download Full-text

Reactive Dual Magnetron Sputtering: A Fast Method for Preparing Stoichiometric Microcrystalline ZnWO4 Thin Films

Surfaces ◽

10.3390/surfaces4020013 ◽

2021 ◽

Vol 4 (2) ◽

pp. 106-114

Author(s):

Yannick Hermans ◽

Faraz Mehmood ◽

Kerstin Lakus-Wollny ◽

Jan P. Hofmann ◽

Thomas Mayer ◽

...

Keyword(s):

Thin Films ◽

Magnetron Sputtering ◽

Photoelectron Spectroscopy ◽

Fast Method ◽

X Ray Diffraction ◽

X Ray ◽

Glass Substrates ◽

Post Annealing ◽

Rf Signal ◽

First Time

Thin films of ZnWO4, a promising photocatalytic and scintillator material, were deposited for the first time using a reactive dual magnetron sputtering procedure. A ZnO target was operated using an RF signal, and a W target was operated using a DC signal. The power on the ZnO target was changed so that it would match the sputtering rate of the W target operated at 25 W. The effects of the process parameters were characterized using optical spectroscopy, X-ray diffraction, and scanning electron microscopy, including energy dispersive X-ray spectroscopy as well as X-ray photoelectron spectroscopy. It was found that stoichiometric microcrystalline ZnWO4 thin films could be obtained, by operating the ZnO target during the sputtering procedure at a power of 55 W and by post-annealing the resulting thin films for at least 10 h at 600 °C. As FTO coated glass substrates were used, annealing led as well to the incorporation of Na, resulting in n+ doped ZnWO4 thin films.

Download Full-text

Revealing noncollinear magnetic ordering at the atomic scale via XMCD

Scientific Reports ◽

10.1038/s41598-021-82518-4 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Fridtjof Kielgast ◽

Ivan Baev ◽

Torben Beeck ◽

Federico Pressacco ◽

Michael Martins

Keyword(s):

Ground State ◽

Magnetic Circular Dichroism ◽

Magnetic Moments ◽

Magnetic Ordering ◽

Atomic Scale ◽

Angle Of Incidence ◽

X Ray ◽

First Time ◽

X Ray Absorption ◽

Magnetic Sublattices

AbstractMass-selected V and Fe monomers, as well as the heterodimer $${\text{Fe}}_1{\text{V}}_1$$ Fe 1 V 1 , were deposited on a Cu(001) surface. Their electronic and magnetic properties were investigated via X-ray absorption (XAS) and X-ray magnetic circular dichroism (XMCD) spectroscopy. Anisotropies in the magnetic moments of the deposited species could be examined by means of angle resolving XMCD, i.e. changing the X-ray angle of incidence. A weak adatom-substrate-coupling was found for both elements and, using group theoretical arguments, the ground state symmetries of the adatoms were determined. For the dimer, a switching from antiparallel to parallel orientation of the respective magnetic moments was observed. We show that this is due to the existence of a noncollinear spin-flop phase in the deposited dimers, which could be observed for the first time in such a small system. Making use of the two magnetic sublattices model, we were able to find the relative orientations for the dimer magnetic moments for different incidence angles.

Download Full-text