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

• Mass Spectrometry Letters
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• v.5 no.2
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• pp.42-48
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• 2014

A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

• Korean Journal of Materials Research
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• v.29 no.7
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• pp.437-442
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• 2019

Green $BaSi_2O_2N_2:0.02Eu^{2+}$ phosphor is synthesized through a two-step solid state reaction method. The first firing is for crystallization, and the second firing is for reduction of $Eu^{3+}$ into $Eu^{2+}$ and growth of crystal grains. By thermal analysis, the three-time endothermic reaction is confirmed: pyrolysis reaction of $BaCO_3$ at $900^{\circ}C$ and phase transitions at $1,300^{\circ}C$ and $1,400^{\circ}C$. By structural analysis, it is confirmed that single phase [$BaSi_2O_2N_2$] is obtained with Cmcm space group of orthorhombic structure. After the first firing the morphology is rod-like type and, after the second firing, the morphology becomes round. Our phosphor shows a green emission with a peak position of 495 nm and a peak width of 32 nm due to the $4f^65d^1{\rightarrow}4f^7$ transition of $Eu^{2+}$ ion. An LED package (chip size $5.6{\times}3.0mm$) is fabricated with a mixture of our green $BaSi_2O_2N_2$, and yellow $Y_3Al_5O_{12}$ and red $Sr_2Si_5N_8$ phosphors. The color rendering index (90) is higher than that of the mixture without our green phosphor (82), which indicates that this is an excellent green candidate for white LEDs with a deluxe color rendering index.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.30 no.2
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• pp.47-54
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• 2020

To develop the bright-vivid red- and yellow-inorganic fluorescent pigments with high luminescence properties, A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments were synthesized by a water assisted solid state reaction (WASSR) method and a conventional solid state reaction method. Although impurity peaks corresponding to the AVO₃ and AV₃O₈ (A = K, Rb, and Cs) were observed in all samples prepared, the trigonal structure A₃V₅O₁₄ (A = K and Rb) and orthorhombic structure Cs₂V₄O₁₁ were successfully obtained as a main phase. These inorganic pigments showed the broad absorption band (under 550 nm) originated from CT transitions of VO₄ polyhedron, and the strong broad red- and green-emission bands due to ³T₂ → ¹A₁ and ³T₁ → ¹A₁ transitions of the [VO₄]^3- group. The A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ pigments showed a bright-vivid red- and yellow-body color, where the a* values of the A₃V₅O₁₄ (A = K and Rb) were +35.5 and +45.9, respectively, and b* value of Cs₂V₄O₁₁ pigments was +50.3. The L* values of the A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments were over +45. These results indicate that the A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments could be an attractive candidate as a bright-vivid red- and yellow inorganic pigments.

• Journal of the Korean Vacuum Society
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• v.15 no.5
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• pp.527-533
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• 2006

Spinel $LiNi_xMn_{2-x}O_4$ thin films were synthesized up to x = 0.9 by a sol-gel method employing spin-coating. The Ni-substituted films were found to maintain cubic structure at low x but to exhibit tetragonal structure for $x{\geq}0.6$. Such cubic-tetragonal phase transition indicates that $Ni^{3+}(d7)$ ions with low-spin $(t_{2g}^6,e_g^1)$ state occupy the octahedral sites of the compound, thus being subject to the Jahn-Teller distortion. By x-ray photoelectron spectroscopy both $Ni^{2+}$ and $Ni^{3+}$ ions were detected. Optical properties of the $LiNi_xMn_{2-x}O_4$ films were investigated by spectroscopic ellipsometry (SE) in the visible?ultraviolet range. The measured dielectric function spectra by SE mainly consist of broad absorption structures attributed to charge-transfer (CT) transitions, $O^{2-}(2p){\rightarrow}Mn^{4+}(3d)$ for 1.9 $(t_{2g})$ and $2.8{\sim}3.0$ eV $(e_g)$ structures and $O^{2-}(2p){\rightarrow}Mn^{3+}(3d)$ for 2.3 $(t_{2g})$ and $3.4{\sim}3.6$ eV $(e_g)$ structures. Also, sharp absorption structures were observed at about 1.6, 1.7, and 1.9 eV, interpreted as due to d-d crystal-field transitions within the octahedral $Mn^{3+}$ ion. The strengths of these absorption structures are reduced by the Ni substitution. Rapid reduction of the CT transition strength involving the eg states for x = 0.6 is attributed to the reduced wavefunction overlap between the $e_g$ and the $O^{2-}(2p)$ states due to the tetragonal extension of the lattice constant by the Jahn-Teller effect.

• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1684-1688
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• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

• Economic and Environmental Geology
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• v.47 no.5
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• pp.507-515
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• 2014

Asbestos is designated as carcinogen minerals. Detoxification of asbestos is being conducted by physical and chemical treatments that lead the formation of non-fibrous mineral particles or phase transitions. Major researches have been performed on mineralogical properties of asbestos and possibilities of detoxification in Korea. More specific studies are needed to prove the form and crystal structure changes during the detoxification of asbestos via heat treatment. Therefore, we studied thermal effects on mineralogical characteristics of chrysotile and asbestiform tremolite using electron microscopy investigation. Electron microscopy investigation showed chrysotile fibers were fully transformed into rod-shaped forsterite at $850^{\circ}C$ in 2 hours, and asbestiform tremolite fibers were converted into non-fibrous diopside at $1050^{\circ}C$ in 2 hours. Fibrous asbestos were converted into rod-shaped minerals, which are non-asbestiform. However, compositions of both minerals were not changed before and after heat treatment. These results indicate that thermal treatment of asbestos completely broke down asbestos structure due to dehydroxylation and recrystallization. Thus, electron microscopy investigation can provide the useful information of shapes, crystal structure, and chemistries of the asbestos for the detoxification.

• Journal of Pharmaceutical Investigation
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• v.41 no.4
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• pp.255-262
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• 2011

Method using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of pregabalin in plasma samples. Acquisition was performed by monitoring the transitions: m/z 160.1${\rightarrow}$142.2 for pregabalin and m/z 423.2${\rightarrow}$207.1 for losartan (as an internal standard). After cold acetonitrileinduced protein precipitation of the plasma samples, separation was performed with C18 column by isocratic mobile phase consisted of 10 mM ammonium acetate and acetonitrile (15:85, v/v). Results were linear over the concentration ranged from 0.1 to $10{\mu}g$/mL and the correlation coefficients (r) were $\geq0.99$. Intra- and inter-day precisions were $\leq6.02$ and $\leq11.04%$, respectively, and intra- and inter-day accuracies were 96.60-101.09 and 98.10-102.60%, respectively. This validated method was successfully applied to a bioequivalence study of two formulations of pregabalin, Daewoong pregabalin capsule (Daewoong Pharm. Co., Ltd.) and Lyrica$^{(R)}$ capsule (Pfizer Korea Ltd.) in twenty eight healthy Korean volunteers. The subjects received a single oral dose of each formulation (150 mg as pregabalin) in a randomized $2{\times}2$ crossover study and plasma samples were obtained from each subject at predetermined time intervals. Then, the pharmacokinetic parameters ($AUC_{0-t}$, $C_{max}$ and $T_{max}$) were calculated and statistically analyzed to assess the differences between two formulations. The 90% confidence intervals for the log-transformed data were acceptable range of log 0.8-log 1.25 (e.g., log 1.0048-log 1.0692 for AUC0-t, log 0.9142-log 1.0421 for $C_{max}$). Thus, $AUC_{0-t}$ and $C_{max}$ met the criteria of the Korea Food and Drug Administration (KFDA) for bioequivalence test indicating that Daewoong pregabalin capsule was bioequivalent to Lyrica$^{(R)}$ capsule.

• Journal of Pharmaceutical Investigation
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• v.39 no.1
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• pp.65-71
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• 2009

The aim of the present study was to evaluate the bioequivalence of two domperidone maleate tablets, Motilium-$M^{(R)}$ Tablet (Janssen Korea Ltd., reference product) and $Toriem^{(R)}$ Tablet (Daewon Pharm. Co., Ltd., test product). Domperidone was extracted by liquid-liquid extraction using tert-butyl methyl ether and separated in less than 3 min on $C_{18}$ reverse-phase column using an isocratic elution. A tandem mass spectrometer, as detector, was used for quantitative analysis in positive mode by a multiple reaction monitoring mode to monitor the m/z $426.1{\rightarrow}119.1$ and the m/z $837.4{\rightarrow}158.2$ transitions for domperidone and the internal standard (roxithromycin), respectively. Calibration curves, from $0.05{\sim}50$ ng/mL of domperidone, showed correlation coefficients (r) higher than 0.9941. Intra day and inter day precision (C.V. %) for quality control were ranged from 10.04 to 16.09% and from 10.87 to 18.69%, respectively. The lower limit of quantification (LLOQ) of domperidone was 0.05 ng/mL. The method described is precise and sensitive and has been successfully applied to the study of bioequivalence of domperidone in 24 healthy Korean volunteers. Twenty-four healthy male Korean volunteers received a single dose of each medicine ($2{\times}12.72\;mg$ domperidone maleate) in a $2{\times}2$ crossover study. There was a one-week washout period between the doses. Plasma concentrations of domperidone were monitored for over a period of 24 hr after the administration. $AUC_{0-t}$ (the area under the plasma concentration-time curve) was calculated by the linear trapezoidal rule. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. The 90% confidence intervals for the log transformed data were within acceptable range of log 0.8 to log 1.25 (e.g., $log\;0.92{\sim}log\;1.05$ for $AUC_{0-t}$, $log\;0.81{\sim}log\;1.05$ for $C_{max}$). The major parameters, $AUC_{0-t}$ and $C_{max}$ met the criteria of KFDA for bioequivalence indicating that $Toriem^{(R)}$ tablet is bioequivalent to Motilium-$M^{(R)}$ tablet.

• Korean Journal of Mineralogy and Petrology
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• v.33 no.1
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• pp.11-18
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• 2020

High-pressure synchrotron X-ray powder diffraction experiments were performed on natural illite (K_0.65Al₂(Al_0.65Si_3.35)O₁₀(OH)₂) using diamond anvil cell (DAC) under two different pressure transmitting media (PTM), i.e., water and ME41 (methanol:ethanol = 4:1 by volume). When using water as PTM, occasional heating was applied up to about 250℃ while reaching pressure up to 2.7 GPa in order to promote both hydrostatic conditions and intercalation of water molecules into the layer. When using ME41, pressure was reached up to 6.9 GPa at room temperature. Under these conditions, illite did not show any expansion of interlayer distance or phase transitions. Pressure-volume data were used to derive bulk moduli (K₀) of 45(3) GPa under water and 51(3) GPa under ME41 PTM. indicating no difference in compressibility within the analytical error. Linear compressibilities were then calculated to be β^a = 0.0025, β^b = 0.0029, β^c = 0.0144 under ME41 PTM showing the c-axis is ca. six times more compressible than a- and b-axes. These elastic behaviors of illite were compared to muscovite, one of its structural analogues.