• Title/Summary/Keyword: Quadrupole mass spectrometer

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Diagnosis of uhv Application System by Quadrupole Mass Spectrometer (사중극 질량분석기에 의한 초고진공 응용시스템 진단)

  • 임재영;이철로;정광화;노삼규;이연환
    • Journal of the Korean Vacuum Society
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    • v.3 no.2
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    • pp.173-178
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    • 1994
  • 박막성장을 위한 초고진공 응용시스템을 제작하고 이것의 특성을 사중극질량분석계로 측정하였 다. 초고진공 시스템을 박막성장에 활용하기 위해서는 챔버 뿐만 아니라 펌프, 이온게이지, 전자총 등도 베이킹이 요구되었다. 또한 이온게이지와 전자총은 적어도 박막성장 20분전에 탈가스를 하여야함을 알 았다. 이 시스템으로 달성된 진공도는 7x10-11 torr이었다.

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Outgassing and thermal desorption measurement system for parts of CRT (CRT 부품용 탈가스 및 Thermal Desorption 측정장치 개발)

  • Sin, Yong Hyeon;Hong, Seung Su;Mun, Seong Ju;Seo, Il Hwan;Jeong, Gwang Hwa
    • Journal of the Korean Vacuum Society
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    • v.6 no.4
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    • pp.298-307
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    • 1997
  • TDS(Thermal Desorption Spectroscopy)system, for diagnosis of CRT manufacturing process, was designed and constructed. Outgassings and thermal desorptions from the part or materials of CRT can be measured and analysed with this system at various temperatures. The system is consisted of 3 parts, vacuum chamber and pumping system with variable conductance, sample heating stages & their controller, and outgassing measurement devices, like as ion gauge or quadrupole mass spectrometer. The ultimate pressure of the system was under $1{\times}10^{-7}$ Pa. With the variable conductance system, the effective pumping speed of the chamber could be controlled from sub l/s to 100 l/s. The effective pumping speed values were determined by dynamic flow measurement principle. The temperatures and ramp rate of sample were controlled by tungsten heater and PID controller up to 600℃ within ±1℃ difference to setting value. Ion gauge & QMS were calibrated for quantitative measurements. Some examples of TDS measurement data and application on the CRT process analysis were shown.

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이온 에너지 분석을 통한 저손상 그래핀 클리닝 연구

  • Kim, Gi-Seok;Min, Gyeong-Seok;Yeom, Geun-Yeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.218.2-218.2
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    • 2014
  • 그래핀은 높은 전기 전도도와 열전도도, 기계적 강도를 가지고 있고 동시에 높은 전자이동도($200,000cm^2{\cdot}V{\cdot}^1{\cdot}s{\cdot}^1$) 특성을 갖는 물질로써 차세대 소재로 각광받고 있다. 하지만 그래핀을 소자에 응용하기 위해서는 전사공정과 lithography 공정 과정에서 발생되는 PMMA(Poly methyl methacrylate) residue를 완벽하게 제거해야 하는 문제점이 있다. 특히, lithography 공정 중 완벽하게 PMMA residue 가 제거되지 않고 잔류해 있을 경우에 소자의 life time, performance에 악영향을 준다는 보고가 있다. 이와같은 문제를 해결하기 위해 화학적 cleaning, 열처리를 통한 cleaning, 전류 인가에 의한 cleaning과 같은 방법들을 이용하여 그래핀의 PMMA residue를 제거하는 공정들이 보고되고 있지만, 화학적 cleaning 방법의 경우 chloroform 이라는 독성물질 사용으로 인해 산업적으로 응용이 어렵고, 열처리 방법은 전극 등의 금속이 $200^{\circ}C$ 이상의 높은 온도에서 장시간 노출될 경우 쉽게 손상을 입으며, 전류 인가에 의한 cleaning 방법은 국부적으로만 효과를 볼 수 있기 때문에 lithography 공정 후 PMMA residue를 효과적으로 제거하기에는 한계를 보이고 있다. 본 연구에서는 Ar을 이용하는 Ion beam 시스템을 통해 beam energy를 제어함으로써 PMMA residue를 효과적으로 제거하는 연구를 진행하였다. 최적화된 플라즈마 발생 조건을 찾기 위해 QMS(Quadrupole Mass Spectrometer)를 이용하여 입사하는 ion energy와 flux 양을 컨트롤 하였고, 250 W에서 최적화된 ion energy distribution 영역이 존재한다는 것을 확인할 수 있었다. 또한, 25 Gauss 정도의 electro-magnetic field를 이용하여 Ar의 ion energy를 10 eV 이하로 낮추어 damage를 최소화함으로써 효과적으로 그래핀을 cleaning 할 수 있었다. Cleaning과정에서 ion bombardment에 의해 발생한 damage는 $250^{\circ}C$에서 6시간 동안 annealing 공정을 거치면서 회복되는 것을 Raman spectroscopy의 D peak ($1335cm{\cdot}^1$) / G peak ($1572cm{\cdot}^1$) ratio 로 확인할 수 있었고, PMMA residue의 cleaning 여부는 G peak ($1580cm{\cdot}^1$)의 blue shift와 2D peak ($2670cm{\cdot}^1$)의 red shift를 통해 확인하였다. 그리고 AFM (Atomic Force Microscopy)을 이용하여 cleaning 공정과정에서 RMS roughness가 4.99 nm에서 2.01 nm로 감소하는 것을 관찰하였다. 마지막으로, PMMA residue의 cleaning 정도를 정량적으로 분석하기 위해 XPS (X-ray Photoelectron Spectroscopy)를 이용하여 sp2 C-C bonding이 74.96%에서 87.66%로 증가함을 확인을 할 수 있었다.

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Scattering of Noble Gas Ions from a Si(100) Surface at Hyperthermal Energies (20-300 eV)

  • 이현우;Kang, H.
    • Bulletin of the Korean Chemical Society
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    • v.16 no.2
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    • pp.101-104
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    • 1995
  • In an attempt to understand the nature of hyperthermal ion-surface collisions, noble gas ion beams (He+, Ne+, Ar+, and Xe+) are scattered from a Si(100) surface for collision energies of 20-300 eV and for 45°incidence angle. The scattered ions are mass-analyzed using a quadrupole mass spectrometer and their kinetic energy is measured in a time-of-flight mode. The scattering event for He+ and Ne+ can be approximated as a sequence of quasi-binary collisions with individual Si atoms for high collision energies (Ei > 100 eV), but it becomes of a many-body nature for lower energies, Ar+ and Xe+ ions undergo mutliple large impact parameter collisions with the surface atoms. The effective mass of a surface that these heavy ions experience during the collision increases drastically for low beam energies.

Identification of Pitfalls Related to the Analysis of Liquid Chromatography-Tandem Mass Spectrometry and Liquid Chromatography-Time of Flight Mass Spectrometry (액체크로마토그래프-질량분석기를 이용한 정성 및 정량 오류의 확인)

  • Kwon, Jin-Wook;Cho, Yoon-Jae;Rhee, Gyu-Seek
    • Korean Journal of Environmental Agriculture
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    • v.34 no.3
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    • pp.230-237
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    • 2015
  • BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

Simultaneous Determination of the Seven Phenylpropanoids in Xanthii Fructus Using a HPLC-PDA and LC-MS

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.24 no.3
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    • pp.206-212
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    • 2018
  • Xanthii Fructus has been traditionally used for the treatment of rhinitis, rheumatoid arthritis, and eczema. In this study, a high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and then used for the simultaneous analysis of eight phenylpropanoids in Xanthii Fructus. The analytical column used for this separation was a $SunFire^{TM}$ $C_{18}$ column, maintained at $40^{\circ}C$. The mobile phase used was 1.0% acetic acid in distilled water and 1.0% acetic acid in acetonitrile with gradient elution. For identify of each component, the mass spectrometer (MS) was used a Waters triple quadrupole mass spectrometer requipped with electrospray ionization (ESI) source. The HPLC-PDA method showed good linearity: correlation coefficients were ${\geq}0.9996$. The limits of detection and quantification of the eight compounds were 0.02 - 0.04 and $0.06-0.14{\mu}g/mL$, respectively. The extraction recoveries ranged from 97.51 to 108.67%. The relative standard deviation values of intra- and inter-day precision were 0.06 - 1.55 and 0.09 - 1.68%, respectively. The validated HPLC-PDA method was applied to simultaneously analyse the amounts of eight phenlypropanoids in Xanthii Fructus.

Review on the Analytical Methods and Ambient Concentrations of Organic Nitrogenous Compounds in the Atmosphere (대기 유기질소화합물의 분석방법 및 농도)

  • Choi, Na Rae;Kim, Yong Pyo
    • Journal of Korean Society for Atmospheric Environment
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    • v.34 no.1
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    • pp.120-143
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    • 2018
  • The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

Etching characteristics of PST thin films using quderupole mass spectrometry (QMS를 이용한 PST 박막의 식각 특성)

  • Kim, Jong-Sik;Kim, Gwan-Ha;Kim, Kyoung-Tae;Kim, Dong-Pyo;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.11a
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    • pp.187-190
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    • 2004
  • In this study, PST thin films were etched with inductively coupled $Cl_2/(Cl_2+Ar)$ plasmas. The etch characteristics of PST thin films as a function of $Cl_2/(Cl_2+Ar)$ gasmixtures were analyzed by using quadrupole mass spectrometer (QMS). Systematic studies were carried out as a function of the etching parameters, including the RF power and the working pressure. The maximum PST film etch rate is 56.2 nm/min, because a small addition of $Cl_2$ to the $Cl_2/Ar$ mixture increased the chemical effect. It was proposed that sputter etching is the dominant etching mechanism while the contribution of chemical reaction is relatively low due to low volatility of etching products.

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Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

  • Jang, Haejong;Mai, Xuan-Lan;Lee, Gunhee;Ahn, Jae Hyoung;Rhee, Jongsook;Truong, Quoc-Ky;Vinh, Dinh;Hong, Jongki;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.95-99
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    • 2018
  • An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.