• Title/Summary/Keyword: liquid-liquid-solid

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Quantitative Elemental Analysis in Soils by using Laser Induced Breakdown Spectroscopy(LIBS) (레이저유도붕괴분광법을 활용한 토양의 정량분석)

  • Zhang, Yong-Seon;Lee, Gye-Jun;Lee, Jeong-Tae;Hwang, Seon-Woong;Jin, Yong-Ik;Park, Chan-Won;Moon, Yong-Hee
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.5
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    • pp.399-407
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    • 2009
  • Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.

A Study on Optimization of Nitric Acid Leaching and Roasting Process for Selective Lithium Leaching of Spent Batreries Cell Powder (폐 배터리 셀 분말의 선택적 리튬 침출을 위한 질산염화 공정 최적화 연구)

  • Jung, Yeon Jae;Park, Sung Cheol;Kim, Yong Hwan;Yoo, Bong Young;Lee, Man Seung;Son, Seong Ho
    • Resources Recycling
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    • v.30 no.6
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    • pp.43-52
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    • 2021
  • In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNixCoyMnzO2, LiCoO2) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L16(44) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO3 from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Effects of Hydrothermal Pretreatment on the Nutritional Values and In Vitro Fermentation Characteristics of Tall Fescue (Festuca arundinacea) and Corn Silage (열수 전처리에 따른 톨페스큐와 옥수수 사일리지의 영양적 가치와 in vitro 발효특성에 미치는 영향)

  • Kim, Dong Hyeon;Son, Jun Kyu;Lee, Ji Hwan;Kim, Sang Bum;Park, Beom Young;Kim, Doo San;Jang, Gul Won;Lim, Hyun Joo;Hur, Tai Young;Kim, Eun Tae
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.1
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    • pp.468-476
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    • 2021
  • This study examined the effects of a hydrothermal pretreatment (HP) on the nutritional values and in vitro fermentation characteristics of tall fescue and corn silage. This study was conducted through a factorial design of 2 (control or HP) × 2 (hay; tall fescue or silage; corn). For the HP, forage was placed into a glass bottle with 20% w/v of water, and the glass bottle was sealed and heated to reach a temperature of 121℃ (0.12 MPa). The solid residue and liquid were collected and oven-dried at 65℃ for three days. The dried materials were tested for in vitro fermentation at 39℃ for 24 and 48 h. The content of ADF increased significantly regardless of the forage type. After in vitro incubation for 24 h, the total VFA content was significantly lower after HP, regardless of the forage type (p ≤ 0.05), and the propionate concentration was increased in corn silage with HP (p ≤ 0.05). After 48 hours of in vitro incubation, the propionate content increased significantly (p ≤ 0.03) in corn silage with HP (p ≤ 0.05), but the butyrate content decreased significantly (p ≤ 0.05). There was no change in the in vitro dry matter and neutral detergent fiber digestibility by HP regardless of the forage type. Therefore, the use of hydrothermally pretreated corn silage could be advantageous for the supply of energy for ruminants.

Development of Method using LC-ESI-MS/MS and KASP for Identification of Gymnema sylvestre in Food (식품에서 당살초 판별을 위한 LC-ESI-MS/MS 분석법과 KASP 마커 개발)

  • Park, Boreum;Lee, Sun Hee;Eom, Kwonyong;Noh, Eunyoung;Moon Han, Kyoung;Hwang, Jinwoo;Kim, Hyungil;Baek, Sun Young
    • Journal of Food Hygiene and Safety
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    • v.37 no.2
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    • pp.46-54
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    • 2022
  • Known for its effectiveness in weight loss and diabetes prevention, Gymnema sylvestre products can be found in the US, Japanese, and Indian markets. However, the recommended dosage or safety of these products has not yet been proven. Therefore, development of an analytical method for detecting the content of Gymnema sylvestre in food products is required. Accordingly, this study proposes an analysis method that can examine Gymnema sylvestre in food using LC-ESI-MS/MS and KASP (Kompetitive Allele-Specific PCR) markers. In LC-ESI-MS/MS, a simultaneous analysis method for gymnemic acid and deacylgymnemic acid was optimized using negative ionization mode, and its validation test was completed for solid and liquid samples. In addition, KASP markers were prepared by finding the specific SNP of G. sylvestre in ITS2 and matK through DNA barcodes. The two KASP markers returned positive FAM fluorescence result when combined with G. sylvestre, and this aspect was confirmed in raw G. sylvestre as well. The applicability of the method was tested on 21 different food and healthy functional products containing G. sylvestre purchased on the internet. As a result, although there was a difference in the ratios of gymnemic acid and deacylgymnemic acid in LC-ESI-MS/MS, the index component was detected in all 21 products samples. In the KASP analysis, 9 products returned positive FAM result, and the rest of the products were found to be containing G. sylvestre extract. This study is the first study to use the dual system of LC-ESI-MS/MS and KASP for the analysis of G. sylvestre. The study has confirmed that these two methods are applicable to the examine G. sylvestre content in food products.

Evaluation of the Potential of Nitrogen Plasma to Cosmetics (질소 플라즈마의 화장품 가능성 평가)

  • Lee, So Min;Jung, So Young;Brito, Sofia;Heo, Hyojin;Cha, Byungsun;Lei, Lei;Lee, Sang Hun;Lee, Mi-Gi;Bin, Bum-Ho;Kwak, Byeong-Mun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.3
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    • pp.189-196
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    • 2022
  • Plasma refers to an ionized gas that is often referred to as "the fourth phase of matter", following solid, liquid, and gas. Plasma has traditionally been utilized for industrial applications such as welding and neon signs, but its promise in biomedical fields such as cancer treatment and dermatology has lately been recognized. Indeed, due to its beneficial effects in promoting collagen production, improving skin tone, and eliminating harmful bacteria in the skin, plasma treatment constitutes an important target for dermatological research. In this study, a plasma device for cosmetic manufacturing based on nitrogen, the main component of the atmosphere, was designed and assembled. Moreover, nitric oxide (NO) was selected since is easier to follow and evaluate than other nitrogen plasma active species, and its contents were measured to perform a quantitative and qualitative evaluation of plasma. First, an injection method, using different proximities labeled "sinking" and "non sinking" treatments, was performed to test the most efficient plasma treatment method. As a result, it was observed that the formulation obtained by a non sinking treatment was more effective. Furthermore, toner and ampoule were selected as cosmetics formulations, and the characteristics of the formulation and changes in the injected plasma state were observed. In both formulations, the successful injection of NO plasma was 2 times higher in toner formulation than ampoule formulation, and it gradually decreased with time, having dissipated after a week. It was confirmed that the nitrogen plasma used did not affect the stability of the toner and ampoule formulations at low temperature (4 ℃), room temperature (25 ℃), and high temperature (37 ℃ and 50 ℃) conditions. The results of this study demonstrate the potential of plasma cosmetics and highlight the importance of securing the stability of the injected plasma.

A Study on the Recovery of Lithium from Secondary Resources of Ceramic Glass Containing Li-Al-Si by Ca-based Salt Roasting and Water Leaching Process (Li-Al-Si 함유 유리세라믹 순환자원으로부터 Ca계열 염배소법 및 이에 따른 수침출 공정에 의한 리튬의 회수 연구)

  • Sung-Ho Joo;Dong Ju Shin;Dongseok Lee;Shun Myung Shin
    • Resources Recycling
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    • v.32 no.1
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    • pp.42-49
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    • 2023
  • The glass ceramic secondary resource containing Li-Al-Si is used in inductor, fireproof glass, and transparent cookware and accounts for 14% of the total consumption of Li, which is the second most widely used after Li-ion batteries. Therefore, new Li resources should be explored when the demand for Li is exploding, and extensive research on Li recovery is needed. Herein, we recovered Li from fireproof Li-Al-Si glass ceramic, which is a new secondary resource containing Li. The fireproof glass among all Li-Al-Si glass ceramics was used as raw material that contained 1.5% Li, 9.4% Al, and 28.9% Si. The process for recovering Li from the fireproof glass was divided into two parts: (1) calcium salt roasting and (2) water leaching. In calcium salt roasting, a sample of fireproof glass was crushed and ground below 325 mesh. The leaching efficiency was compared based on the presence or absence of heat treatment of the fireproof glass. Moreover, the leaching rates based on the input ratios of calcium salt, Li-Al-Si glass, and ceramics and the leaching process based on calcium salt roasting temperatures were compared. In water leaching, the leaching and recovery rates of Li based on different temperatures, times, solid-liquid ratios, and number of continuous leaching stages were compared. The results revealed that fireproof glass ceramics containing Li-Al-Si should be heat treated to change phase to beta-type spodumene. CaCO3 salt should be added at a ratio of 6:1 with glass ceramics containing Li-Al-Si, and then leached 4 times or more to achieve a recovery efficiency of Li over 98% from a solution containing 200 mg/L of Li.

Simultaneous determinations of anthracycline antibiotics by high performance liquid chromatography coupled with radial-flow electrochemical cell (고성능 액체 크로마토그래피/방사흐름 전기화학전지를 이용한 안트라사이클린계 항생제의 동시 정량)

  • Cho, Yonghee;Hahn, Younghee
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.308-314
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    • 2007
  • The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.

Nutritional quality evaluation of complementary baby food products in Korea according to food composition (국내 시판 간편 이유식의 식품 구성에 따른 영양적 질 평가)

  • Eun-Ju Lee;Jee-Young Yeon;Mi-Hyun Kim
    • Journal of Nutrition and Health
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    • v.56 no.5
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    • pp.537-553
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    • 2023
  • Purpose: The purpose of this study was to evaluate the nutritional quality of complementary baby food products sold in Korea according to the baby food stages and food composition. Methods: A total of 1,587 complementary food products sold online and offline between March and December 2021 were investigated. They ranged from liquid meals to solid rice for babies aged 5 to 36 months. Results: The number of intakes per packaged volume was 2.8 in Stage 1, 1.9 in Stage 2, 1.4 in Stage 3, and 1.1 in Stage 4 (p < 0.0001). The dietary variety scores (DVS) of the complementary baby food products were 3.4 in Stage 1, 5.5 in Stage 2, 7.1 in Stage 3, and 9.7 in Stage 4 (p < 0.0001) and showed a significant increase in the later stages. The Korean dietary diversity score (KDDS) significantly increased from 2.3 in Stage 1, to 2.8 in Stage 2, 3.0 in Stage 3, and 3.4 in Stage 4 (p < 0.0001). The higher the baby food stage, the higher the proportion of grains/meat/vegetable ingredients. The ratio of protein intake to Adequate Intake (AI) or Recommended Nutrition Intake (RNI) was higher in products with a KDDS of 3 points or more, or in products with 2 points or fewer in Stages 1 and 2 (p < 0.0001, respectively). The ratio of protein intake to RNI increased as the KDDS score increased in Stages 3 and 4 (p < 0.0001, respectively). For all stages of baby foods, the ratio of protein intake to AI or RNI was high in products that included the meat group (beans, nuts, meat, eggs, fish, and shellfish) (p < 0.0001, respectively). Conclusion: Continuous research and nutritional evaluation are required for establishing nutrient content standards for commercially available baby foods, considering breast milk intake.

A Rheological Study on Creep Behavior of Clays (점토(粘土)의 Creep 거동(擧動)에 관한 유변학적(流變學的) 연구(研究))

  • Lee, Chong Kue;Chung, In Joon
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.1 no.1
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    • pp.53-68
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    • 1981
  • Most clays under sustained load exhibit time-dependent deformation because of creep movement of soil particles and many investigators have attempted to relate their findings to the creep behavior of natural ground and to the long-term stability of slopes. Since the creep behavior of clays may assume a variety of forms depending on such factors as soil plasticity, activity and water content, it is difficult and complicated to analyse the creep behavior of clays. Rheological models composed of linear springs in combination with linear or nonlinear dashpots and sliders, are generally used for the mathematical description of the time-dependent behavior of soils. Most rheological models, however, have been proposed to simulate the behavior of secondary compression for saturated clays and few definitive data exist that can evaluate the behavior of non-saturated clays under the action of sustained stress. The clays change gradually from a solid state through plastic state to a liquid state with increasing water content, therefore, the rheological models also change. On the other hand, creep is time-dependent, and also the effect of thixotropy is time-function. Consequently, there may be certain correlations between creep behavior and the effects of thixotropy in compacted clays. In addition, the states of clay depend on water content and hence the height of the specimen under drained conditions. Futhermore, based on present and past studies, because immediate elastic deformation occurs instantly after the pressure increment without time-delayed behavior, the factor representing immediate elastic deformations in the rheological model is necessary. The investigation described in this paper, based on rheological model, is designed to identify the immediate elastic deformations and the effects of thixotropy and height of clay specimens with varing water content and stress level on creep deformations. For these purposes, the uniaxial drain-type creep tests were performed. Test results and data for three compacted clays have shown that a linear top spring is needed to account for immediate elastic deformations in the rheological model, and at lower water content below the visco-plastic limit, the effects of thixotropy and height of clay specimens can be represented by the proposed rheological model not considering the effects. Therefore, the rheological model does not necessitate the other factors representing these effects. On the other hand, at water content higher than the visco-plastic limit, although the state behavior of clays is visco-plastic or viscous flow at the beginning of the test, the state behavior, in the case of the lower height sample, does not represent the same behavior during the process of the test, because of rapid drainage. In these cases, the rheological model does not coincide with the model in the case of the higher specimens.

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