• Title/Summary/Keyword: Peak tailing

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A Correction Method for the Peak Tailing Backgrounds for Accurate Isotope Ratio Measurements of Uranium in Ultra Trace Levels using Thermal Ionization Mass Spectrometry

  • Park, Jong-Ho;Choi, In-Hee;Park, Su-Jin;Lee, Myung-Ho;Song, Kyu-Seok
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4327-4331
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    • 2011
  • A new method in thermal ionization mass spectrometry (TIMS) was developed to correct peak tailing backgrounds in the isotope ratio measurements of uranium in ultra trace levels for higher accuracy. Two different uranium standard reference materials (U005 and U030) were used to construct databases of signal intensities at mass 234 u and mass 236 u, which correspond to the two uranium minor isotopes, and signal intensity of $^{238}U$. Correlations between peak tailing backgrounds and $^{238}U$ were obtained by least-squares regression on calculated backgrounds at mass 234 u and mass 236 u with respect to the signal intensity of $^{238}U$ followed by separation of the peak tails of the two major isotopes of uranium ($^{235}U$ and $^{238}U$), which enables us to obtain a master equation for peak tailing background correction on all kinds of samples. Verification of the correction method was carried out using U010 and IRMM-040a.

Feasibility study of membrane interface for gas chromatograph-mass spectrometry (기체크로마토그래프-질량분석기의 실리콘 분리막 인터페이스의 유용성 연구)

  • Kang, Gil Seon;Lee, Dong Soo;Lee, Hwa Sim;Park, Chang Joon
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.495-501
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    • 2008
  • Agilent 5973 GC-MS instrument was modified so that the capillary direct interface was removed and that a silicone membrane was installed between GC and MS. Feasibility study of the membrane interface GC-MS has been carried out. Vacuum of the mass spectrometer was not affected by the carrier gas flow rate up to $4.7m{\ell}/min$. As the carrier flow rate was increased, peak tailing was reduced and chromatogram peaks appeared earlier. Chromatogram peaks showed better separation and higher sensitivity as the membrane thickness was reduced from $127{\mu}m$ to $75{\mu}m$, and also as the interface temperature was increased. However, the membrane interface GC-MS had drawbacks such as background ions at 73 and 147 m/z and poor peak separation due to peak tailing.

Development of Signal Process Circuit for PSAPD Detector (위치민감형 광다이오드 검출기의 신호처리회로 개발과 적용)

  • Yoon, Do-Kun;Lee, Won-Ho
    • Journal of radiological science and technology
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    • v.35 no.4
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    • pp.315-319
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    • 2012
  • The aim of this study was to develop a signal process circuit for a position sensitive avalanche photodiode detector. The circuit parts consisted of amplification, differential and peak/hold circuit. This research was the baseline to develop highly compact radiation detector. The signal was amplified by an amplification chip and its shape was changed in a differential circuit to minimize the pulse tailing. The peak/hold circuit detect the peak of the signal from the differential circuit and hold the amplitude of the peak for data acquisition. In order to test the intrinsic function of the circuit, the input signal was transmitted from a commercial pulse generator.

Soil Samples in 134Cs of the 604, 795 keV Spectrum Analysis (토양시료 속 134Cs의 604, 795 keV 에너지 스펙트럼 분석)

  • Jang, Eunsung
    • Journal of the Korean Society of Radiology
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    • v.8 no.7
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    • pp.443-447
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    • 2014
  • $^{134}Cs$ radioactive concentration among soil samples is difficult to classify due to the background impact on crust originated natural radioactive nuclide, and overlapping and interfering between peaks. The ways to identify true peaks in gamma-ray spectroscopy are as follows to reduce statistical fluctuation by smoothing based on the fact that the shapes of peak are mostly Gaussian, to inspect the levels of width and height of peaks, to add functions on low-energy trailing phenomena, or 4) to check the peaks after modifying Gaussian function itself. Therefore, it is considered that information and knowledge for spectrum analysis are necessary.

Synthesis of o-Xylene-Organosilicon Hybrid Polymer and Its Optical Properties

  • Choi, Jin-Kyu;Jeong, Hyun-Dam
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.515-518
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    • 2013
  • We present synthesis of a new kind of organic-inorganic hybrid polymer, poly xylene-hexamethyltrisiloxane hybrid (PXS) by a new synthetic way from o-xylene and 1,1,3,3,5,5-hexamethyltrisiloxane. The merged molecular structure of the two monomeric components for the PXS polymer was confirmed by $^{13}C$- and $^1H$-NMR, and FT-IR. Its optical absorption and emission properties were investigated by UV-vis absorption and photoluminescence (PL) spectroscopy. The PXS exhibits absorption at 265 nm which is the same with the o-xylene but tailing up to nearly 400 nm, which is maybe related the polymeric structure of the PXS. For the PL investigation, the PXS shows red-shift of the peak from 288 nm (o-xylene) to 372 nm in the case of excitation at 265 nm, at which both PXS and o-xylene have sufficiently high absorption for excitation. When 325-nm laser is used for excitation, the PXS shows a broader peak at 395 nm compared to the excitation at 265 nm and the o-xylene shows no luminescence probably due to the lack of absorption at 325 nm.

Fabrication of Virtual Frisch-Grid CdZnTe ${\gamma}$-Ray Detector (가상 Frisch-그리드를 이용한 CdZnTe 감마선 소자 제작)

  • Park, Chansun;Kim, Pilsu;Cho, PyongKon;Choi, Jonghak;Kim, Jungmin;Kim, KiHyun
    • Journal of radiological science and technology
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    • v.37 no.4
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    • pp.253-259
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    • 2014
  • Large volume of $6{\times}6{\times}12mm^3$ CdZnTe ${\gamma}$-ray detector was fabricated with CdZnTe single crystals grown by Traveling Heater Method (THM) to evaluate the energy resolution of 662 keV in $^{137}Cs$. Hole tailing effect which originated from the large mobility difference in electron and hole degrade energy resolution of radiation detector and its effects become more severe for a large volume detectors. Generally, single carrier collection technique is very useful method to remove/minimize hole tailing effect and thereby improvement in energy resolution. Virtual Frisch-grid technique is also one of single charge collection method through weighting potential engineering and it is very simple and easily applicable one. In this paper, we characterized CZT detector grown by THM and evaluated the effectiveness of virtual Frisch-grid technique for a high energy gamma-ray detector. The proper position and width of virtual Frisch-grid was determined from electric field simulation using ANSYS Maxwell ver. 14.0. Energy resolution of 2.2% was achieved for the 662 keV ${\gamma}$-peak of $^{137}Cs$ with virtual Frisch-grid CdZnTe detector.

Spatial correlation of aerodynamic forces on 5:1 rectangular cylinder in different VIV stages

  • Lei, Yongfu;Sun, Yanguo;Zhang, Tianyi;Yang, Xiongwei;Li, Mingshui
    • Wind and Structures
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    • v.34 no.1
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    • pp.81-90
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    • 2022
  • To better understand the vortex-induced vibration (VIV) characteristics of a 5:1 rectangular cylinder, the distribution of aerodynamic force and the non-dimensional power spectral density (PSD) of fluctuating pressure on the side surface were studied in different VIV development stages, and their differences in the stationary state and vibration stages were analyzed. The spanwise and streamwise correlations of surface pressures were studied, and the flow field structure partitions on the side surface were defined based on the streamwise correlation analysis. The results show that the variation tendencies of mean and root mean square (RMS) pressure coefficients are similar in different VIV development stages. The RMS values during amplitude growth are larger than those at peak amplitude, and the smallest RMS values are observed in the stationary state. The spanwise correlation coefficients of aerodynamic lifts increase with increase of the peak amplitude. However, for the lock-in region, the maximum spanwise correlation coefficient for aerodynamic lifts occurs in the VIV rising stage rather than in the peak amplitude stage, probably due to the interaction of vortex shedding force (VSF) and self-excited force (SEF). The streamwise correlation results show that the demarcation point positions between the recirculation region and the main vortex region remain almost constant in different VIV development stages, and the reattachment points gradually move to the tailing edge with increasing amplitude. This study provides a reference to estimate the demarcation point and reattachment point positions through streamwise correlation and phase angle analysis from wind tunnel tests.

Analytical Quality by Design Methodology Approach for Simultaneous Quantitation of Paeoniflorin and Decursin in Herbal Medicine by RP-HPLC Analysis

  • Kim, Min Kyoung;Park, Geonha;Hong, Seon-Pyo;Jang, Young Pyo
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.264-273
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    • 2021
  • Simultaneous quantification of multiple marker compounds in herbal medicine by high performance liquid chromatography (HPLC) analysis is still a challenge due to the complexity in various parameters to be considered and co-existing multi-components. As a case study, a reliable HPLC method for simultaneous quantification of paeoniflorin from Paeoniae Radix and decursin from Angelicae Gigantis Radix in various commercial herbal medicine was developed based on analytical quality by design (AQbD) strategy. As a first step, risk assessment was performed to select the critical method parameters (CMPs) which were decided as organic mobile phase ratio and column oven temperature. In order to evaluate the effect of the CMPs on critical method attributes (CMAs) of peak resolution and tailing, central composite design (CCD) was employed. The final chromatographic conditions were optimized as follows: column- C18, 4.6 × 250 mm, 5 ㎛ particle size; mobile phase- A: acetonitrile, B: 0.1% acetic acid water; detection wavelength- 235 nm for paeoniflorin, 325 nm for decursin; column oven temperature- 25℃; flow rate- 1.0 mL/min; gradient mobile phase system as Time (min) : % A, 0:14, 25:14, 30:50, 60:50, 61:100, 65:100, 66:14, 75:14. The method was successfully validated according to the International Conference on Harmonization (ICH) guidelines and piloted for ten commercial herbal medicines.

Optimization of the experimental conditions for determination of roxithromycin in bulk and dosage forms

  • Jeong, Kyung Min;Lee, Cheong Hoon;Kim, Su Hyun;Lee, Jeongmi
    • Analytical Science and Technology
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    • v.30 no.1
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    • pp.39-48
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    • 2017
  • Roxithromycin (RXT), which is an antibiotic used to treat respiratory tract and urinary infections, is official in Korean Pharmacopoeia (KP) and is marketed in various dosage forms including tablet, granule, suspension, and tablet for suspension in Korea. This study presents how a universal and reliable method to quantify RXT in bulk drug and formulations was developed. Effects of factors including column type, buffer concentration, type and concentration of organic solvent, buffer pH, and type and concentration of mobile phase additive, were examined, and some categorical or crucial factors including the types of column, organic solvent, mobile phase additive and the buffer pH were optimized by one-factor-at-a-time approach. Subsequently, concentrations of the buffer and additive and column temperature were optimized by response surface methodology using Box-Behnken design aiming to acquire the RXT peak of good shape. The optimized method employed a Phenomenex Gemini $5{\mu}$ C18 110A ($150{\times}4.60mm$, $5{\mu}m$) maintained at $30^{\circ}C$ with the mobile phase consisting of 25 mM phosphate buffer (pH 6.0) with 0.3 % tetrabutylammonium hydroxide and methanol at a ratio of 37:63 (v/v). Method validation results showed that the developed method was linear, precise, and accurate. Compared to the compendial methods in KP 10 that exhibited a significant tailing of the RXT peak despite using unfavorably high buffer concentrations and were not harmonized among bulk drug and formulations, this method could be universally applied to RXT bulk drug and marketed products in various dosage forms and thus was adopted in KP 11.

Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.