• Title/Summary/Keyword: Analytical mode

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The Effect of the Oxygen Flow Rate on the Electronic Properties and the Local Structure of Amorphous Tantalum Oxide Thin Films

  • Denny, Yus Rama;Lee, Sunyoung;Lee, Kangil;Kang, Hee Jae;Yang, Dong-Seok;Heo, Sung;Chung, Jae Gwan;Lee, Jae Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.398-398
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    • 2013
  • The electronic properties and the local structure of tantalum oxide thin film with variation of oxygen flow rate ranging from 9.5 to 16 sccm (standard cubic centimeters per minute) have been investigated by X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), and X-ray absorption spectroscopy (XAS). The XPS results show that the Ta4f spectrum for all films consist of the strong spin-orbit doublet $Ta4f_{7/2}$ and $Ta4f_{5/2}$ with splitting of 1.9 eV. The oxygen flow rate of the film results in the appearance of new features in the Ta4f at binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV, these peaks attribute to $Ta^{1+}$, $Ta^{2+}$, $Ta^{4+}$/$Ta^{2+}$, and $Ta^{5+}$, respectively. Thus, the presence of non-stoichiometric state from tantalum oxide ($TaO_x$) thin films could be generated by the oxygen vacancies. The REELS spectra suggest the decrease of band gap for tantalum oxide thin films with increasing the oxygen flow rate. The absorption coefficient ${\mu}$ and its fine structure were extracted from the fluorescence mode of extended X-ray absorption fine structure (EXAFS) spectra. In addition, bond distances (r), coordination numbers (N) and Debye-Waller factors (${\sigma}^2$) each film were determined by a detailed of EXAFS data analysis. EXAFS spectrapresent both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the increase of oxygen flow rate.

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Development and validation of a qualitative GC-MS method for methamphetamine and amphetamine in human urine using aqueous-phase ethyl chloroformate derivatization

  • Kim, Jiwoo;Sim, Yeong Eun;Kim, Jin Young
    • Analytical Science and Technology
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    • v.33 no.1
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    • pp.23-32
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    • 2020
  • Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

Analytical Evaluation of FFR-aided Heterogeneous Cellular Networks with Optimal Double Threshold

  • Abdullahi, Sani Umar;Liu, Jian;Mohadeskasaei, Seyed Alireza
    • KSII Transactions on Internet and Information Systems (TIIS)
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    • v.11 no.7
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    • pp.3370-3392
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    • 2017
  • Next Generation Beyond 4G/5G systems will rely on the deployment of small cells over conventional macrocells for achieving high spectral efficiency and improved coverage performance, especially for indoor and hotspot environments. In such heterogeneous networks, the expected performance gains can only be derived with the use of efficient interference coordination schemes, such as Fractional Frequency Reuse (FFR), which is very attractive for its simplicity and effectiveness. In this work, femtocells are deployed according to a spatial Poisson Point Process (PPP) over hexagonally shaped, 6-sector macro base stations (MeNBs) in an uncoordinated manner, operating in hybrid mode. A newly introduced intermediary region prevents cross-tier, cross-boundary interference and improves user equipment (UE) performance at the boundary of cell center and cell edge. With tools of stochastic geometry, an analytical framework for the signal-to-interference-plus-noise-ratio (SINR) distribution is developed to evaluate the performance of all UEs in different spatial locations, with consideration to both co-tier and cross-tier interference. Using the SINR distribution framework, average network throughput per tier is derived together with a newly proposed harmonic mean, which ensures fairness in resource allocation amongst all UEs. Finally, the FFR network parameters are optimized for maximizing average network throughput, and the harmonic mean using a fair resource assignment constraint. Numerical results verify the proposed analytical framework, and provide insights into design trade-offs between maximizing throughput and user fairness by appropriately adjusting the spatial partitioning thresholds, the spectrum allocation factor, and the femtocell density.

Validation of urinary N-methylacetamide reference material for proficiency test (숙련도시험을 위한 소변 중 N-메틸아세트아미드 표준시료 검증)

  • Lee, Mi-Young
    • Analytical Science and Technology
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    • v.27 no.6
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    • pp.339-346
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    • 2014
  • The author assessed the availability of urine reference material for proficiency test provided for laboratories in occupational health. N-methylacetamide is the biomarker of exposure to N,N-dimethyl acetamide, which was used as the substitute for hepatotoxic N,N-dimethylformamide (DMF). N-methylacetamide (NMAC) urine samples of 3 different levels covering the 0.2~2 times of the exposure limit were tested. Stability test up to 180 days (0, 7, 30, 60, 180 days) at 4 different temperatures (-60, -20, 5, $25^{\circ}C$) and homogeneity test were performed for these samples. New analytical condition by GC/MSD using SIM mode (m/z 58, 59) and DB-624 column was investigated for better selectivity, sensitivity and resolution. Urinary NMAC samples showed good homogeneity for 3 levels. These samples also showed good stability up to 180 days. The data of stability and homogeneity of urinary DMAC confirmed the basis of including this item into Korean proficiency test for occupational health laboratories since 2008.

Profiling of Urinary Environmental Estrogens by Gas Chromatography/Mass Spectrometry (GC/MS를 이용한 뇨 중 환경 에스트로겐들의 동시 프로필)

  • Yang, Yoon-Jung;Lee, Seon-Hwa;Chung, Bong-Chul
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.265-272
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    • 1999
  • A simultaneous profile analysis of 19 environmental estrogens, which act like estrogen and may effect the endocrine system by binding to hormone receptors or influencing cell signaling pathways, was attempted. The present method was based on the selected ion monitoring (SIM) mode of gas chromatography/mass spectrometry (GC/MS). It involves solid-liquid extraction, enzyme hydrolysis, liquid-liquid extraction and quantitative conversion into trimethylsilyl (TMS)-ether derivatives. Analytical recovery range was 47.6 ~ 99.5% and the RSD values of within-a-day and day-to-day test were 0.66 ~ 9.33%, 1.66 ~ 16.14%, respectively. The Korean reference values for the evaluation of environmental estrogen effects were established by this method.

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Nonlinear Analytical Model for RC Flat Plate Frames (RC 플랫 플레이트 골조의 비선형 해석모델)

  • Park, Young-Mi;HwangBo, Jin;Han, Sang-Whan
    • Proceedings of the Korea Concrete Institute Conference
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    • 2008.04a
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    • pp.241-244
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    • 2008
  • In general, RC flat plate frames have been used as a gravity load resisting system(GLRS) in building. This system should be constructed with lateral force resisting system(LFRS) such as shear walls and brace frames. When lateral loads such as earthquakes occur, LFRS undergo displacement by which connected gravity systems experience lateral displacement. Thus, flat plate system designed as GLRS should be predict unbalanced moments and punching failure due to lateral deformation. This study developed an analytical mode for predicting nonlinear behavior of RC slab column connection for the seismic performance evaluation of RC flat plate frames. For verifying the analytical model, the test results of two flat plate specimens having two continous spans with the difference gravity shear ratio($V_g/{\phi}V_c$) were compared with the results of analysis. The developed model can predict the failure modes and punching failures.

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Experimental, numerical and analytical studies on a novel external prestressing technique for concrete structural components

  • Lakshmanan, N.;Saibabu, S.;Murthy, A. Rama Chandra;Ganapathi, S. Chitra;Jayaraman, R.;Senthil, R.
    • Computers and Concrete
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    • v.6 no.1
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    • pp.41-57
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    • 2009
  • This paper presents the details of a novel external prestressing technique for strengthening of concrete members. In the proposed technique, transfer of external force is in shear mode on the end block thus creating a complex stress distribution and the required transverse prestressing force is lesser compared to conventional techniques. Steel brackets are provided on either side of the end block for transferring external prestressing force and these are connected to the anchor blocks by expansion type anchor bolts. In order to validate the technique, an experimental investigation has been carried out on post-tensioned end blocks. Performance of the end blocks have been studied for design, cracking and ultimate loads. Slip and slope of steel bracket have been recorded at various stages during the experiment. Finite element analysis has been carried out by simulating the test conditions and the responses have been compared. From the analysis, it has been observed that the computed slope and slip of the steel bracket are in good agreement with the corresponding experimental observations. A simplified analytical model has been proposed to compute load-deformation of the loaded steel bracket with respect to the end block. Yield and ultimate loads have been arrived at based on force/moment equilibrium equations at critical sections. Deformation analysis has been carried out based on the assumption that the ratio of axial deformation to vertical deformation of anchor bolt would follow the same ratio at the corresponding forces such as yield and ultimate. It is observed that the computed forces, slip and slopes are in good agreement with the corresponding experimental observations.

Free vibration of axially loaded Reddy-Bickford beam on elastic soil using the differential transform method

  • Yesilce, Yusuf;Catal, Seval
    • Structural Engineering and Mechanics
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    • v.31 no.4
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    • pp.453-475
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    • 2009
  • The literature regarding the free vibration analysis of Bernoulli-Euler and Timoshenko beams on elastic soil is plenty, but the free vibration analysis of Reddy-Bickford beams on elastic soil with/without axial force effect using the Differential Transform Method (DTM) has not been investigated by any of the studies in open literature so far. In this study, the free vibration analysis of axially loaded Reddy-Bickford beam on elastic soil is carried out by using DTM. The model has six degrees of freedom at the two ends, one transverse displacement and two rotations, and the end forces are a shear force and two end moments in this study. The governing differential equations of motion of the rectangular beam in free vibration are derived using Hamilton's principle and considering rotatory inertia. Parameters for the relative stiffness, stiffness ratio and nondimensionalized multiplication factor for the axial compressive force are incorporated into the equations of motion in order to investigate their effects on the natural frequencies. At first, the terms are found directly from the analytical solutions of the differential equations that describe the deformations of the cross-section according to the high-order theory. After the analytical solution, an efficient and easy mathematical technique called DTM is used to solve the governing differential equations of the motion. The calculated natural frequencies of one end fixed and the other end simply supported Reddy-Bickford beam on elastic soil using DTM are tabulated in several tables and figures and are compared with the results of the analytical solution where a very good agreement is observed and the mode shapes are presented in graphs.

Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry (기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법)

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.29-36
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    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.