• Title/Summary/Keyword: Thermal desorption spectrometry

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Rapid Surface Heating Promotes Laser Desorption Ionization of Thermally Labile Molecules from Surfaces

  • Han, Sang Yun
    • Mass Spectrometry Letters
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    • v.7 no.4
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    • pp.91-95
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    • 2016
  • In recent years, matrix-free laser desorption ionization (LDI) for mass spectrometry of thermally labile molecules has been an important research subject in the pursuit of new ionization methods to serve as alternatives to the conventional matrix-assisted laser desorption ionization (MALDI) method. While many recent studies have reported successful LDI of thermally labile molecules from various surfaces, mostly from surfaces with nanostructures, understanding of what drives the LDI process still requires further study. This article briefly reviews the thermal aspects involved in the LDI mechanism, which can be characterized as rapid surface heating. The thermal mechanism was supported by observed LDI and postsource decay (PSD) of peptide ions produced from flat surfaces with special thermal properties including amorphous Si (a-Si) and tungsten silicide ($WSi_x$). In addition, the concept of rapid surface heating further suggests a practical strategy for the preparation of LDI sample plates, which allows us to choose various surface materials including crystalline Si (c-Si) and Au tailorable to specific applications.

Observation of Peptide-Ion Generation by Laser-Induced Surface Heating from Tungsten Silicide Surfaces

  • Kim, Shin-Hye;Park, Sun-Hwa;Song, Jae-Yong;Han, Sang-Yun
    • Mass Spectrometry Letters
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    • v.3 no.1
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    • pp.18-20
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    • 2012
  • We report observation of laser desorption/ionization (LDI) of peptides from flat surfaces of tungsten silicide ($WSi_2$). In contrast to MALDI (matrix-assisted laser desorption/ionization) and SALDI (surface-assisted laser desorption/ionization) mass spectrometry, this study did not utilize any matrices and surface nanostructures. In this work, LDI on $WSi_2$ surfaces is demonstrated to cover a mass range up to 1,600 Da (somatostatin; monoisotopic mass = 1637.9 Da). In addition, it exhibited a high sensitivity, which could detect peptides, which could detect peptides of low femtomole levels (20 fmol for angiotensin II). The observed LDI process was discussed to be largely thermal, more specifically, due to laser-induced surface heating that is most likely promoted by the low thermal diffusivity (${\kappa}$) of $WSi_2$ substrate.

Adsorption properties of MgO protective layer in AC PDP

  • Manakhov, Anton;Nikishin, Nikolay;Hur, Min;Heo, Eun--Gi
    • 한국정보디스플레이학회:학술대회논문집
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    • 2008.10a
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    • pp.384-387
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    • 2008
  • We have studied the adsorption of contaminations on the MgO protective layer by Thermal Desorption Spectrometry (TDS). The result shows that the increase in exposure time, MgO thickness and humidity multiply the quantity of adsorbed contaminations. It is also found that the desorption activation energy and contamination quantity is decreased by the additional firing process of MgO layer under oxygen environment.

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Analysis of Organic Compounds in Ambient PM2.5 over Seoul using Thermal Desorption-comprehensive Two Dimensional Gas Chromatography-time of Flight Mass Spectrometry (TD-GCxGC-TOFMS) (Thermal Desorption-comprehensive Two Dimensional Gas Chromatography-time of Flight Mass Spectrometry (TD-GCxGC-TOFMS)을 이용한 서울 대기 중 PM2.5 유기성분 분석)

  • Lee, Ji-Yi;Lane, Douglas A.;Huh, Jong-Bae;Yi, Sung-Muk;Kim, Yong-Pyo
    • Journal of Korean Society for Atmospheric Environment
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    • v.25 no.5
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    • pp.420-431
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    • 2009
  • Characteristics and advantages of the thermal desorption-comprehensive two dimensional gas chromatography-time of flight mass spectrometry (TD-GCxGC-TOFMS) were discussed and the organic compound's analysis result was shown for the ambient $PM_{2.5}$ sample collected in Seoul, Korea. Over 10,000 individual organic compounds were separated from about $70{\mu}g$ of aerosols in a single procedure with no sample pre-treatment. Among them, around 300 compounds were identified and classified based on the mass fragmentation patterns and GCxGC retention times. Several aliphatic compounds groups such as alkanes, alkenes, cycloalkanes, alkanoic acids, and alkan-2-ones were identified as well as 72 PAH compounds including alkyl substituted compounds and 8 hopanes. In Seoul aerosol, numerous oxidized aromatic compounds including major components of secondary organic aerosols were observed. The inventory of organic compounds in $PM_{2.5}$ of Seoul, Korea suggested that organic aerosol were constituted by the compounds of primary source emission as well as the formation of secondary organic aerosols.

Studies of the Organic Molecules Dissociative Surface Ionization in the Mass-Spectrometric Surface Ionization Method

  • Ilkhomjan Saydumarov;Dilshadbek Usmanov
    • Mass Spectrometry Letters
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    • v.15 no.1
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    • pp.54-61
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    • 2024
  • An improved voltage modulation method (VMM) was used to control the heat release and adsorption properties of the adsorbent. In this work, the voltage and flux modulation methods were considered under unified experimental conditions of dissociative surface ionization (SI) of polyatomic organic molecules, the criteria were found when under VMM conditions the current relaxation of SI carries information about the kinetic properties of thermal desorption of ionizable dissociation particles arriving on the surface of polyatomic molecules. Conditions were found under which the relaxation of the ionic current in the flux modulation method is determined by the kinetics of the heterogeneous dissociation reaction of the original polyatomic molecules. The values of the thermal desorption rate constant K+ and the activation energy E+ obtained with VMM for desorption of (CH3)2NCH+2 ions with m/z 58 by adsorption of imipramine and amitriptyline molecules agree well with each other and with the results for the desorption of the same ions by adsorption of other molecules. This confirms one of the basic conditions for the equilibrium process SI - the a degree (β coefficient) of the same particles SI on the same emitter surface is the same and does not depend on the way these particles are formed on the emitter surface.

The Interaction of CO and W(111) Surface

  • Lee, S. Y.;Kim, Y. D.;Seo, S. N.;Park, C. Y.;Kwak, H. T.;Boo, J. H.;Lee, S. B.
    • Bulletin of the Korean Chemical Society
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    • v.20 no.9
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    • pp.1061-1066
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    • 1999
  • The adsorption of CO on W(111) surface in the range of adsorption temperature between 300 K and 1000 K has been studied using AES, LEED, and TDS in an UHV system. After CO saturation at 300 K, four desorption peaks are observed at temperatures (K) of about 400, 850, 1000, and 1100 in thermal desorption spectra, called as α, β1, β2, and β3 state, respectively. The state was attributed to molecular species of CO, which is well known. Because the CO in βstates (especially the β3 state) is still debated as to whether it is dissociative or non-dissociative, the β3 state is mainly discussed. By using the variation method of heating rate in the thermal desorption spectrometry, the desorption energy and pre-exponential factor for the β3 state are evaluated to be 280 kJ/mol and 1.5×10 12 s-1 , respectively. A lateral interaction energy of 5.7 kJ/mol can also be estimated by Bragg-Williams approximation. To interpret the thermal desorption spectra for the β3 state, moreover, those for the model of a first order and a second order desorption are simulated using quasi-chemical approximation. In this study, a model of lying-down CO species is proposed for the β3 state of CO adsorption.

Application of Thermal Vapor Deposition Method for MALDI-MS : Molecular Weight Determination of Insoluble Sorbitol Derivatives (열증착 시료 제작법이 적용된 MALDI 질량분석법에 의한 불용성 Sorbitol 유도체의 분자량 결정)

  • 신철민;남해선;김성호
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.4 no.3
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    • pp.260-262
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    • 2003
  • A thermal vapor deposition method for crystallization of insoluble analytes with matrix is established as a new sample preparation method for matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). A mixture of mono, bis and tris(p-ethyl benzylidene) sorbitols was incorporated into microcrystals of ferulic acid, which was confirmed by confocal micrographs. Molecular masses of sorbitol derivatives were determined in this way by MALDI-MS without thermal decomposition.

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Application of Thermal Vapor Deposition Method for MALDI-MS : Molecular Weight Determination of Insoluble Sorbitol Derivatives (열증착 시료 제작법이 적용된 MALDI 질량분석법 에 의한 불용성 Sorbitol 유도체의 분자량 결정)

  • 신철민;남해선;김성호
    • Proceedings of the KAIS Fall Conference
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    • 2003.06a
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    • pp.311-313
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    • 2003
  • A thermal vapor deposition method for crystallization of insoluble analysis with matrix is established as a new sample preparation method for matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). A mixture of mono, bis and tris(p-ethyl benzylidene) sorbitols was incorporated into microcrystals of ferulic acid, which was confirmed by confocal micrographs. Molecular masses of sorbitol derivatives were determined in this way by MALDI-MS without thermal decomposition.

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS

  • Min, Hye-Jeong;Lee, Jeong-Min;Shin, Han-Jae;Lee, Moon-Yong;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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    • pp.26-33
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    • 2014
  • Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

Thermal Decomposition of Octanethiolate Self-Assembled Monolayers on Cu(111) in UHV

  • Sung, Myung-M.;Yun, Won-J.;Lee, Sun-S.;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.610-612
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    • 2003
  • Octanethiol ($CH_3(CH_2)_7SH$) based self-assembled monolayer on Cu(111) in ultra-high vacuum has been examined using x-ray photoelectron spectroscopy (XPS), temperature programmed desorption (TPD), intergrated desorption mass spectrometry (IDMS), and contact angle analysis. The results show that the octanethiolate monolayers similar to those on gold are formed on Cu(111). The monolayers are stable up to temperatures of about 480 K. Above 495 K the monolayers decompose via the γ-hydrogen elimination mechanism to yield 1-octene in the gas phase. The thiolate head groups on the copper surface change to Cu₂S following the decomposition of hydrocarbon fragments in the monolayers at about 605 K.