• Korean Journal of Mineralogy and Petrology
• /
• v.35 no.1
• /
• pp.65-73
• /
• 2022

The proper estimation of physical and chemical properties of Earth materials and their structures at high pressure and high temperature conditions is key to the full understanding of diverse geological processes in Earth and planetary interiors. Multi-anvil press - high-pressure generating device - provides unique information of Earth materials under compression, mainly relevant to Earth's upper mantle. The quantitative estimation of the relationship between the oil load within press and the actual pressure conditions within the sample needs to be established to infer the planetary processes. Such pressure-load calibration has often been based on the phase transitions of crystalline earth materials with known pressure conditions; however, unlike at high temperature conditions, phase transitions at low (or room) temperatures can be sluggish, making the calibration at such conditions challenging. In this study, we explored the changes in Al coordination environments of permanently densified pyrope glasses upon the cold compression using the high-resolution ²⁷Al MAS and 3QMAS NMR. The fractions of highly coordinated Al in the cold compressed pyrope glasses increase with increasing oil load and thus, the peak pressure condition. Based on known relationship between the peak pressure and the Al coordination environment in the compressed pyrope glasses at room temperature, we established a room temperature pressure-load calibration of the 14/8 HT assembly in 1,100-ton multi-anvil press. The current results highlight the first pressure-load calibration of any high pressure device using high-resolution NMR. Irreversible structural densification upon cold compression observed for the pyrope glasses provides insights into the deformation and densification mechanisms of amorphous earth materials at low temperature and high pressure conditions within the subducting slabs.

• Journal of the Mineralogical Society of Korea
• /
• v.29 no.3
• /
• pp.155-165
• /
• 2016

Understanding the effect of boron content on atomic structures of boron-bearing multicomponent silicate melts is essential to reveal the atomistic origins of diverse geochemical processes involving silica-rich magmas, such as explosive volcanic eruption. The detailed atomic environments around B and Al in boron-bearing complex aluminosilicate glasses yield atomistic insights into reactivity of nuclear waste glasses in contact with aqueous solutions. We report experimental results on the effect of boron content on the atomic structures of sodium borate glasses and boron-bearing multicomponent silicate melts [malinkoite ($NaBSiO_4$)-nepheline ($NaAlSiO_4$) pseudo-binary glasses] using the high-resolution solid-state NMR ($^{11}B$ and $^{27}Al$). The $^{11}B$ MAS NMR spectra of sodium borate glasses show that three-coodrinated boron ($^{[3]}B$) increases with increasing $B_2O_3$ content. While the spectra imply that the fraction of non-ring species decreases with decreasing boron content, peak position of the species is expected to vary with Na content. Therefore, the quantitative estimation of the fractions of the ring/non-ring species remains to be explored. The $^{11}B$ MAS NMR spectra of the glasses in the malinkoite-nepheline join show that four-coordinated boron ($^{[4]}B$) increases as $X_{Ma}$ [$=NaBSiO_4/(NaBSiO_4+NaAlSiO_4)$] increases while $^{[3]}B$ decreases. $^{27}Al$ MAS NMR spectra of the multicomponent glasses confirm that four-coordinated aluminum ($^{[4]}Al$) is dominant. It is also observed that a drastic decrease in the peak widths (full-width at half-maximum, FWHM) of $^{[4]}Al$ with an addition of boron ($X_{Ma}=0.25$) in nepheline glasses. This indicates a decrease in structural and topological disorder around $^{[4]}Al$ in the glasses with increasing boron content. The quantitative atomic environments around boron of both binary and multicomponent glasses were estimated from the simulation results of $^{11}B$ MAS NMR spectra, revealing complex-nonlinear variation of boron topology with varying composition. The current results can be potentially used to account for the structural origins of the change in macroscopic properties of boron-bearing oxide melts with varying boron content.

• Journal of the Korean Chemical Society
• /
• v.39 no.8
• /
• pp.627-634
• /
• 1995

Layered double hydroxides ($Mg-Al-CO_3$ systems, LDH), which are hydrotalcite-like anionic clay minerals, having different $Mg^{2+}\;to\;Al^{3+}$ ratio were synthesized by coprecipitation method. The subsequent products were characterized by the following methods; elemental analysis, X-ray powder diffraction, thermal analysis (DSC and TGA), FT-IR and $^{27}$Al-MAS NMR. X-ray powder patterns showed that the products formed were layered structure materials. Two heat absorption peaks were observed around 20 ∼280$^{\circ}C$ (surface water and interlayer water) and 280∼500$^{\circ}C$ (water from lattice hydroxide and carbon dioxide from interlayer carbonate) in DSC diagrams, and they were quantitatively analyzed by TGA diagrams (in case LDH4 16.2% and 28.6% respectively). FT-IR spectra indicate that the interlayer carbonate ions occupied symmetrical sites between two adjacent layers in a parallel direction. $^{27}$Al-MAS NMR spectra show only single resonance (8.6 ppm) of the octahedrally coordinated aluminum similar magnesium. When LDH4 was calcined at 560$^{\circ}C$ for 3 hours in air, its layered structure was destroyed giving a mixed metal oxide. However it readily became rehydrated in aqueous chromate solution to its original structure.

• Journal of Korean Society of Environmental Engineers
• /
• v.31 no.3
• /
• pp.179-185
• /
• 2009

In this research, the removal capacity of Cr(VI) by the reused powdered wastes (RPW) containing aluminium oxides was studied. As a pre-treatment process for the preparation of calcined wastes, calcination was conducted at $550^{\circ}C$ to remove organic fraction in the raw wastes. In order to study the adsorption trend of Cr(VI) ions from aqueous solutions, the pH-edge adsorption, adsorption kinetic and adsorption isotherm were investigated using a batch reactor in the presence of four different background electrolytes($NO_3\;^-,\;CO_3\;^{2-},\;SO_4\;^{2-},\;PO_4\;^{3-}$). Cr(VI) adsorption was greatly reduced in the presence of $SO_4\;^{2-}$ and $PO_4\;^{3-}$ over the entire pH range. Meanwhile the inhibition effect by $NO_3\;^-$ and $CO_3\;^{2-}$ was relatively lower than that by $SO_4\;^{2-}$ and $PO_4\;^{3-}$. Cr(VI) adsorption was maximum around pH 4.5 in the presence of $NO_3\;^-$ and $CO_3\;^{2-}$. As the concentration of background electrolytes increased, Cr(VI) adsorption decreased. This result mightly suggests that adsorption between the surface of RPW and Cr(VI) occurs through outer-sphere complex. Cr(VI) adsorption onto the RPW was well described by second-order kinetics. From the Langmuir isotherm at initial pH 3, the maximum adsorbed amount of Cr(VI) onto the RPW was 11.1, 10, 3.3, 5 mg/g in the presence of $NO_3\;^-,\;CO_3\;^{2-},\;SO_4\;^{2-}$, and $PO_4\;^{3-}$, respectively.