The hydrogen reduction behavior of molybdenum oxides was studied using a horizontal-tube reactor. Reduction was carried out in two stages: MoO3 → MoO2 and MoO2 → Mo. In the first stage, a mixed gas composed of 30 vol% H2 and 70 vol% Ar was selected for the MoO3 reduction because of its highly exothermic reaction. The temperature ranged from 550 to 600 ℃, and the residence time ranged from 30 to 150 min. In the second step, pure H2 gas was used for the MoO2 reduction, and the temperature and residence time ranges were 700-750 ℃ and 30-150 min, respectively. The hydrogen reduction behavior of molybdenum oxides was found to be somewhat different between the two stages. For the first stage, a temperature dependence of the reaction rate was observed, and the best curve fittings were obtained with a surface reaction control mechanism, despite the presence of intermediate oxides under the conditions of this study. Based on this mechanism, the activation energy and pre-exponential were calculated as 85.0 kJ/mol and 9.18 × 107, respectively. In addition, the pore size within a particle increases with the temperature and residence time. In the second stage, a temperature dependence of the reaction rate was also observed; however, the surface reaction control mechanism fit only the early part, which can be ascribed to the degradation of the oxide crystals by a volume change as the MoO2 → Mo phase transformation proceeded in the later part.
The effect of the soil-structure interaction (SSI) on has been recently evaluated in shaking table tests. However, most of these tests were conducted on single-degree-of-freedom (SDOF) superstructures and a single-pile. This study investigates the inertial interaction effect of a multi-degree-of-freedom (MDOF) superstructure system with a group piles on a large-scale shaking table test. Whereas the SDOF superstructure system shows a single-frequency amplification tendency, the MDOF superstructure system exhibited amplification tendencies of the acceleration phase and frequency responses for multiple frequencies. In addition, the amplification phenomenon between the footing and the column-type superstructure exceeded that between the footing and the wall-type superstructure, indicating a greater inertial interaction effect of the column-type superstructure. The relationship between shear force and inertial force, the relative vertical and horizontal displacements on the footing was figured out. Also, the ananlysis of dynamic p-y curve at each depth was conducted. In summary, the MDOF and SDOP superstructure systems exhibited different behaviors and the column-type superstructure exerted a higher interaction effect than the wall-type superstructure.
A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH2) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r2) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.
Kim, Jin Hee;Park, Ah Yeon;Jung, Eun Ha;Lee, Cheol Woo;Lee, Tae Ho;Youm, Jeong-Rok
Analytical Science and Technology
/
v.20
no.4
/
pp.323-330
/
2007
A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.
Asteroids have undergone various processes such as impacts, space weathering, and thermal evolution. Because they expose their surfaces to space without atmosphere, these evolutional processes have been recorded directly on their surfaces. The remote-sensing observations have been conducted to reveal these evolutional histories of the target asteroids. For example, crater and boulder distributions are unambiguous evidence for past nondestructive impacts with other celestial bodies. Multiband and spectroscopic observations have revealed space-weathering history (as well as compositions). Whereas most physical quantities have been examined intensively using spacecraft and telescopes, only a little has been studied on "the grain size". It is one of the fundamental physical quantities for diagnosing the collisional and thermal history of asteroids. Our group has conducted polarimetric research of asteroids (as well as Moon [1]) to determine the particle size and further investigate the evolutional histories of target asteroids [2],[3]. For example, the existence of regolith on an S-type asteroid, Toutatis, was suggested almost twenty years before space exploration [4]. Moreover, we reported that near-Sun asteroids indicate a signature of submillimeter grains, which could be created by a thermal sintering process by solar radiation [5]. However, it is important to note that in-situ polarimetry has not been reported on the asteroid surface, although the Korean Lunar Exploration Program aims to do polarimetry on the lunar surface [6]. Therefore, it is expected that the polarizer mounted on the Korean Apophis spacecraft can make the first estimate of the grain size and its regional variation over the Apophis surface. In this presentation, we outline research of S-type asteroid surfaces through remote-sensing observations and consider the role of polarimetry. Based on this review, we consider the purpose, potentiality, and strategy of the polarimetry using the onboard device for the Apophis spacecraft. We will report a possible polarization phase curve of Apophis estimated from ordinary chondrites and past observational data of S-type asteroids, taking account of the space weathering effect. Based on this estimation, we will consider the strategy of how to determine the particle size (and space weathering degree) of the Apophis surface. We will also mention the detectability of dust hovering on the surface.
Journal of the Society of Cosmetic Scientists of Korea
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v.49
no.4
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pp.291-298
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2023
In this study, a quantitative analysis method was developed using high-performance liquid chromatography (HPLC) to analyze the content of ceramide NP in lotion, cream, and cleanser formulations in cosmetics. The analysis was performed using a C18 column, and the mobile phase was set at a ratio of 70 : 30 for acetonitrile and methanol, the flow rate was set to 0.8 mL/min, and the column temperature was set to 20 ℃. The method was verified by analyzing specificity, linearity, limit of detection, limit of quantitation, accuracy, and precision in accordance with the ICH guidelines. As a result of validating the method, the linearity of the calibration curve was excellent (R2 = 0.99984). The accuracy of the lotion, cream, and cleanser formulations was confirmed with a recovery rate ranging from 95.11% to 100.48%. The precision analysis showed a low relative standard deviation (RSD) of less than 0.26%. The limit of detection was 0.902 ㎍/mL, and the limit of quantitation was 2.733 ㎍/mL. Through this quantitative analysis method of ceramide NP applied in cosmetics, it is expected to assist in the quality control of products by enabling measurement even when it is difficult to separate the main peak due to the influence of interfering substances.
Choeum Kang;Hyun Joo Shin;Haesung Yoon;Jung Woo Han;Chuhl Joo Lyu;Mi-Jung Lee
Korean Journal of Radiology
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v.22
no.7
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pp.1185-1193
/
2021
Objective: Clear cell sarcoma of the kidney (CCSK) is the second-most common but extremely rare primary renal malignancy in children after Wilms' tumor. The aims of this study were to evaluate the imaging features that could distinguish between CCSK and Wilms' tumor and to assess the features with diagnostic value for identifying CCSK. Materials and Methods: We reviewed the initial contrast-enhanced abdominal-pelvic CT scans of children with CCSK and Wilms' tumor between 2010 to 2019. Fifty-eight children (32 males and 26 females; age, 0.3-10 years), 7 with CCSK, and 51 with Wilms' tumor, were included. The maximum tumor diameter, presence of engorged perinephric vessels, maximum density of the tumor (Tmax) of the enhancing solid portion, paraspinal muscle, contralateral renal vein density, and density ratios (Tmax/muscle and Tmax/vein) were analyzed on the renal parenchymal phase of contrast-enhanced CT. Fisher's exact tests and Mann-Whitney U tests were conducted to analyze the categorical and continuous variables, respectively. Logistic regression and receiver operating characteristic curve analyses were also performed. Results: The age, sex, and tumor diameter did not differ between the two groups. Engorged perinephric vessels were more common in patients in the CCSK group (71% [5/7] vs. 16% [8/51], p = 0.005). Tmax (median, 148.0 vs. 111.0 Hounsfield unit, p = 0.004), Tmax/muscle (median, 2.64 vs. 1.67, p = 0.002), and Tmax/vein (median, 0.94 vs. 0.59, p = 0.002) were higher in the CCSK compared to the Wilms' group. Multiple logistic regression revealed that engorged vessels (odds ratio 13.615; 95% confidence interval [CI], 1.770-104.730) and Tmax/muscle (odds ratio 5.881; 95% CI, 1.337-25.871) were significant predictors of CCSK. The cutoff values of Tmax/muscle (86% sensitivity, 77% specificity) and Tmax/vein (71% sensitivity, 86% specificity) for the diagnosis of CCSK were 1.97 and 0.76, respectively. Conclusion: Perinephric vessel engorgement and greater tumor enhancement (Tmax/muscle > 1.97 or Tmax/vein > 0.76) are helpful for differentiating between CCSK and Wilms' tumor in children aged below 10 years.
Purpose To define an MRI scoring system for differentiating xanthogranulomatous cholecystitis (XGC) from wall-thickening type gallbladder cancer (GBC) and compare the diagnostic performance of the scoring system with the visual assessment of radiologists. Materials and Methods We retrospectively analyzed 23 and 35 patients who underwent abdominal MRI and were pathologically diagnosed with XGC and wall-thickening-type GBC after surgery, respectively. Three radiologists reviewed all MRI findings. We defined a scoring system using these MRI findings for differentiating XGC from wall-thickening type GBC and compared the area under the curve (AUC) of the scoring system with the visual assessment of radiologists. Results Nine MRI findings showed significant differences in differentiating the two diseases: diffuse gallbladder wall thickening (p < 0.001), mucosal uniformity (p = 0.002), intramural T2-high signal intensity (p < 0.001), mucosal retraction (p = 0.016), gallbladder stones (p < 0.001), T1-intermediate to high-signal intensity (p = 0.033), diffusion restriction (p = 0.005), enhancement pattern (p < 0.001), and phase of peak enhancement (p = 0.008). The MRI scoring system showed excellent diagnostic performance with an AUC of 0.972, which was significantly higher than the visual assessment of the reviewers. Conclusion The MRI scoring system showed better diagnostic performance than the visual assessment of radiologists to differentiate XGC from wall-thickening-type GBC.
The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.
Background: Although there are improvements of clinical symtoms after bronchodilator inhalation in COPD patients, it has been noted that there was no increase of $FEV_1$ in some cases. $FEV_1$ did not reflect precisely the improvement of ventilatory mechanics after bronchodilator inhalation in these COPD patients. The main pathophysiology of COPD is obstruction of airway in expiratory phase but in result, the load of respiratory system is increased in inspiratory phase. Therefore the improvement of clinical symptoms after bronchodilator inhalation may be due to the decrease of inspiratory load. So we performed the study which investigated the effect of bronchodilator on inspiratory response of vetilatory mechanics in COPD patients. Methods: In 17 stable COPD patients, inspiratory and expiratory forced flow-volume curves were measured respectively before bronchodilator inhalation. 10mg of salbutamol solution was inhaled via jet nebulizer for 4 minutes. Forced expiratory and inspiratory flow-volume curves were measured again 15 minutes after bronchodilator inhalation. Results: $FEV_1$, FVC and $FEV_1$/FVC% were $0.92{\pm}0.34L$($38.3{\pm}14.9%$ predicted), $2.5{\pm}0.81L$($71.1{\pm}21.0%$ predicted) and $43.1{\pm}14.5%$ respectively before bronchodilator inhalation. The values of increase of $FEV_1$, FVC and PIF(Peak Inspiratory Flow) were $0.15{\pm}0.13L$(relative increase: 17.0%), $0.58{\pm}0.38\;L$(29.0%) and $1.0{\pm}0.56L$/sec(37.5%) respectively after bronchodilator inhalation. The increase of PIF was twice more than $FEV_1$ in average(p<0.001). The increase of PIF in these patients whose $FEV_1$ was not increased after bronchodilator inhalation were 35.0%, 44.0% and 55.5% respectively. Conclusion: The inspiratory parameter reflected improvement of ventilatory mechanics by inhaled bronchodilater better than expiratory parameters in COPD patients.
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