• Title/Summary/Keyword: Stability Limit

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Improvement of an Analytical Method for Fluoroimide Residue in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Fluoroimide의 잔류농약 분석법 개선)

  • Kim, Nam Young;Park, Eun-Ji;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.220-227
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    • 2021
  • Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO4 and NaCl were used with acetonitrile. C18 (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

Effects of Neutral Particle Beam on Nano-Crystalline Silicon Thin Film Deposited by Using Neutral Beam Assisted Chemical Vapor Deposition at Room Temperature

  • Lee, Dong-Hyeok;Jang, Jin-Nyoung;So, Hyun-Wook;Yoo, Suk-Jae;Lee, Bon-Ju;Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.254-255
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    • 2012
  • Interest in nano-crystalline silicon (nc-Si) thin films has been growing because of their favorable processing conditions for certain electronic devices. In particular, there has been an increase in the use of nc-Si thin films in photovoltaics for large solar cell panels and in thin film transistors for large flat panel displays. One of the most important material properties for these device applications is the macroscopic charge-carrier mobility. Hydrogenated amorphous silicon (a-Si:H) or nc-Si is a basic material in thin film transistors (TFTs). However, a-Si:H based devices have low carrier mobility and bias instability due to their metastable properties. The large number of trap sites and incomplete hydrogen passivation of a-Si:H film produce limited carrier transport. The basic electrical properties, including the carrier mobility and stability, of nc-Si TFTs might be superior to those of a-Si:H thin film. However, typical nc-Si thin films tend to have mobilities similar to a-Si films, although changes in the processing conditions can enhance the mobility. In polycrystalline silicon (poly-Si) thin films, the performance of the devices is strongly influenced by the boundaries between neighboring crystalline grains. These grain boundaries limit the conductance of macroscopic regions comprised of multiple grains. In much of the work on poly-Si thin films, it was shown that the performance of TFTs was largely determined by the number and location of the grain boundaries within the channel. Hence, efforts were made to reduce the total number of grain boundaries by increasing the average grain size. However, even a small number of grain boundaries can significantly reduce the macroscopic charge carrier mobility. The nano-crystalline or polymorphous-Si development for TFT and solar cells have been employed to compensate for disadvantage inherent to a-Si and micro-crystalline silicon (${\mu}$-Si). Recently, a novel process for deposition of nano-crystralline silicon (nc-Si) thin films at room temperature was developed using neutral beam assisted chemical vapor deposition (NBaCVD) with a neutral particle beam (NPB) source, which controls the energy of incident neutral particles in the range of 1~300 eV in order to enhance the atomic activation and crystalline of thin films at room temperature. In previous our experiments, we verified favorable properties of nc-Si thin films for certain electronic devices. During the formation of the nc-Si thin films by the NBaCVD with various process conditions, NPB energy directly controlled by the reflector bias and effectively increased crystal fraction (~80%) by uniformly distributed nc grains with 3~10 nm size. The more resent work on nc-Si thin film transistors (TFT) was done. We identified the performance of nc-Si TFT active channeal layers. The dependence of the performance of nc-Si TFT on the primary process parameters is explored. Raman, FT-IR and transmission electron microscope (TEM) were used to study the microstructures and the crystalline volume fraction of nc-Si films. The electric properties were investigated on Cr/SiO2/nc-Si metal-oxide-semiconductor (MOS) capacitors.

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Assessment of Equivalent Heights of Soil for the Lateral Earth Pressure Against Retaining Walls Due to Design Truck Load by 3D Numerical Analysis (3차원 수치해석에 의한 표준트럭하중에 의해 옹벽에 작용하는 수평토압의 등가높이 산정)

  • Seo, Seunghwan;Jin, Hyunsik;Kim, Dongwook;Chung, Moonkyung
    • Journal of the Korean Geosynthetics Society
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    • v.18 no.4
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    • pp.75-85
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    • 2019
  • The lateral load from traffic depends on standard truck's axle loads and locations, loading distance from the inner wall. The method of limit state design has been adopted and used for design of roads in the Republic of Korea since 2015. The concept of equivalent height of soil accounting for traffic loading is often used for design of retaining walls to quantify the traffic loads transmitted to the inner wall faces. Due to the different characteristics of the standard design trucks between Korea and US (AASHTO), the direct use of the guidelines from AASHTO LRFD leads to incorrect estimation of traffic load effects on retaining walls. This paper presents the results of evaluation of equivalent height of soil to reflect the standard truck of the nation, based on the findings from analytical solutions using 3D finite element method. Compare to US, the standard truck loading has a structure where the axle load is concentrated so that the equivalent load height is estimated to be slightly larger than AASHTO for lower retaining wall height. It would be reasonable to present the equivalent load height in Korea more conservatively than AASHTO in terms of securing long term stability of the retaining wall structure.

Feasibility study of the beating cancellation during the satellite vibration test

  • Bettacchioli, Alain
    • Advances in aircraft and spacecraft science
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    • v.5 no.2
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    • pp.225-237
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    • 2018
  • The difficulties of satellite vibration testing are due to the commonly expressed qualification requirements being incompatible with the limited performance of the entire controlled system (satellite + interface + shaker + controller). Two features cause the problem: firstly, the main satellite modes (i.e., the first structural mode and the high and low tank modes) are very weakly damped; secondly, the controller is just too basic to achieve the expected performance in such cases. The combination of these two issues results in oscillations around the notching levels and high amplitude beating immediately after the mode. The beating overshoots are a major risk source because they can result in the test being aborted if the qualification upper limit is exceeded. Although the abort is, in itself, a safety measure protecting the tested satellite, it increases the risk of structural fatigue, firstly because the abort threshold has been already reached, and secondly, because the test must restart at the same close-resonance frequency and remain there until the qualification level is reached and the sweep frequency can continue. The beat minimum relates only to small successive frequency ranges in which the qualification level is not reached. Although they are less problematic because they do not cause an inadvertent test shutdown, such situations inevitably result in waiver requests from the client. A controlled-system analysis indicates an operating principle that cannot provide sufficient stability: the drive calculation (which controls the process) simply multiplies the frequency reference (usually called cola) and a function of the following setpoint, the ratio between the amplitude already reached and the previous setpoint, and the compression factor. This function value changes at each cola interval, but it never takes into account the sensor signal phase. Because of these limitations, we firstly examined whether it was possible to empirically determine, using a series of tests with a very simple dummy, a controller setting process that significantly improves the results. As the attempt failed, we have performed simulations seeking an optimum adjustment by finding the Least Mean Square of the difference between the reference and response signal. The simulations showed a significant improvement during the notch beat and a small reduction in the beat amplitude. However, the small improvement in this process was not useful because it highlighted the need to change the reference at each cola interval, sometimes with instructions almost twice the qualification level. Another uncertainty regarding the consequences of such an approach involves the impact of differences between the estimated model (used in the simulation) and the actual system. As limitations in the current controller were identified in different approaches, we considered the feasibility of a new controller that takes into account an estimated single-input multi-output (SIMO) model. Its parameters were estimated from a very low-level throughput. Against this backdrop, we analyzed the feasibility of an LQG control in cancelling beating, and this article highlights the relevance of such an approach.

Improvement in Mechanical Properties of Cast Magnesium Alloy through Solid-solution Hardening and Grain Refinement (고용 강화 및 결정립 미세화를 통한 마그네슘 합금 주조재의 기계적 물성 향상)

  • Kim, Sang-Hoon;Moon, Byoung-Gi;You, Bong-Sun;Park, Sung-Hyuk
    • Journal of Korea Foundry Society
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    • v.37 no.6
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    • pp.207-216
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    • 2017
  • This study investigated the effects of the addition of Zn, Ca, and SiC on the microstructure and mechanical properties of Mg-Al alloys. The tensile properties of homogenized Mg-xAl (x = 6, 7, 8, and 9 wt.%) alloys increased with increasing Zn content by the solid-solution strengthening effect. However, when the added Zn content exceeded the solubility limit, the strength and ductility of the alloys decreased greatly owing to premature fracture caused by undissolved coarse particles or local melting. Among the Mg-xAl-yZn alloys tested in this study, the AZ74 alloy showed the best tensile properties. However, from the viewpoints of the thermal stability, castability, and tensile properties, the AZ92 alloy was deemed to be the most suitable cast alloy. Moreover, the addition of a small amount (0.17 wt.%) of SiC reduced the average grain size of the AZ91 alloy significantly, from $430{\mu}m$ to $73{\mu}m$. As a result, both the strength and the elongation of the AZ91 alloy increased considerably by the grain-boundary hardening effect and the suppression of twinning behavior, respectively. On the other hand, the addition of Ca (0.5-1.5 wt.%) and a combined addition of Ca (0.5-1.5 wt.%) and SiC (0.17 wt.%) increased the average grain size of the AZ91 alloy, which resulted in a decrease in its tensile properties. The SiC-added AZ92 alloy exhibited excellent tensile properties (YS 125 MPa, UTS 282 MPa, and EL 12.3%), which were much higher than those of commercial AZ91 alloy (YS 93 MPa, UTS 192 MPa, and EL 7.0%). The fluidity of the SiC-added AZ92 alloy was slightly lower than that of the AZ91 alloy because of the expansion of the solid-liquid coexistence region in the former. However, the SiC-added AZ92 alloy showed better hot-tearing resistance than the AZ91 alloy owing to its refined grain structure.

Effects of Climatic Condition on Stability and Efficiency of Crop Production (농업 기상특성과 작물생산의 효율 및 안전성)

  • Robert H. Shaw
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.27 no.4
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    • pp.296-313
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    • 1982
  • At a time when world population and food supply are in a delicate balance, it is essential that we look at factors to improve this balance. We can alter the environment to better fit the plant's needs, or we can alter the plant to better fit the environment. Improved technology has allowed us to increase the yield level. For moderately detrimental weather events technology has generally decreased the yield variation, yet for major weather disasters the variation has increased. We have raised the upper level, but zero is still the bottom level. As we concentrate the production of particular crops into limited areas where the environment is closest to optimum, we may be increasing the risk of a major weather related disaster. We need to evaluate the degree of variability of different crops, and how weather and technology can interact to affect it. The natural limits of crop production are imposed by important ecological factors. Production is a function of the climate, the soil, and the crop and all activities related to them. In looking at the environment of a crop we must recognize these are individuals, populations and ecosystems. Under intensive agriculture we try to limit the competition to one desired species. The environment is made up of a complex of factors; radiation, moisture, temperature and wind, among others. Plant response to the environment is due to the interaction of all of these factors, yet in attempting to understand them we often examine each factor individually. Variation in crop yields is primarily a function of limiting environmental parameters. Various weather parameters will be discussed, with emphasis placed on how they impact on crop production. Although solar radiation is a driving force in crop production, it often shows little relationship to yield variation. Water may enter into crop production as both a limiting and excessive factor. The effects of moisture deficiency have received much more attention than moisture excess. In many areas of the world, a very significant portion of yield variation is due to variation in the moisture factor. Temperature imposes limits on where crops can be grown, and the type of crop that can be grown in an area. High temperature effects are often combined with deficient moisture effects. Cool temperatures determine the limits in which crops can be grown. Growing degree units, or heat accumulations, have often been used as a means of explaining many temperature effects. Methods for explaining chilling effects are more limited.

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Unguided Rocket Trajectory Analysis under Rotor Wake and External Wind (로터 후류와 외풍에 따른 무유도 로켓 궤적 변화 해석)

  • Kim, Hyeongseok;Chae, Sanghyun;Yee, Kwanjung
    • Journal of the Korean Society for Aeronautical & Space Sciences
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    • v.46 no.1
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    • pp.41-51
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    • 2018
  • Downwash from helicopter rotor blades and external winds from various maneuvering make an unguided rocket change its trajectory and range. For the prediction of the trajectory and range, it is essential to consider the downwash effect. In this study, an algorithm was developed to calculate 6-Degree-Of-Freedom(6 DOF) forces and moments exerting on the rocket, and total flight trajectory of a 2.75-inch unguided rocket in a helicopter downwash flow field. Using Actuator Disk Model(ADM) analysis result, the algorithm could analyze the entire trajectory in various initial launch condition such as launch angle, launch velocity, and external wind. The algorithm that considered the interference between a fuselage and external winds could predict the trajectory change more precisely than inflow model analysis. Using the developed algorithm, the attitude and trajectory change mechanism by the downwash effect were investigated analyzing the effective angle of attack change and characteristics of pitching stability of the unguided rocket. Also, the trajectory and range changes were analyzed by considering the downwash effect with external winds. As a result, it was concluded that the key factors of the rocket range change were downwash area and magnitude which effect on the rocket, and the secondary factors were the dynamic pressure of the rocket and the interference between a fuselage and external winds. In tailwind case which was much influential on the range characteristics than other wind cases, the range of the rocket rose as increasing the tailwind velocity. However, there was a limit that the range of the rocket did not increase more than the specific tailwind velocity.

Validation of an HPLC Method for the Pharmacokinetic Study of Glipizide in Human (글리피짓 체내동태 연구를 위한 혈청 중 글리피짓의 HPLC 정량법 검증)

  • Cho, Hea-Young;Lee, Hwa-Jeong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.3
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    • pp.137-142
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fexofenadine in Human (테르페나딘 체내동태 연구를 위한 혈청 중 펙소페나딘의 HPLC 정량법 개발 및 검증)

  • Cho, Hye-Young;Kang, Hyun-Ah;Kim, Yoon-Gyoon;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.6
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    • pp.437-443
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Etodolac in Human (에토돌락 체내동태 연구를 위한 혈청 중 에토돌락의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Moon, Jai-Dong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.4
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    • pp.265-271
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.