• Title/Summary/Keyword: Chemical Ionization

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Analysis of Polymer Characteristics Using Matrix-assisted Laser Desorption/Ionization Time-of-flight Mass Spectrometry (말디토프 질량분석을 이용한 고분자의 특성분석)

  • Kang, Min-Jung;Seong, Yunseo;Kim, Moon-Ju;Kim, Myung Soo;Pyun, Jae-Chul
    • Applied Chemistry for Engineering
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    • v.28 no.3
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    • pp.263-271
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    • 2017
  • The application of mass spectrometry to polymer science has rapidly increased since the development of MALDI-TOF MS. This review summarizes current polymer analysis methods using MALDI-TOF MS, which has been extensively applied to analyze the average molecular weight of biopolymers and synthetic polymers. Polymer sequences have also been analyzed to reveal the structures and composition of monomers. In addition, the analysis of unknown end-groups and the determination of polymer concentrations are very important applications. Hyphenated techniques using MALDI-tandem MS have been used for the analysis of fragmentation patterns and end-groups, and also the combination of SEC and MALDI-TOF MS techniques is recommended for the analysis of complex polymers. Moreover, MALDI-TOF MS has been utilized for the observation of polymer degradation. Ion mobility MS, TOF-SIMS, and MALDI-TOF-imaging are also emerging technologies for polymer characterization because of their ability to automatically fractionate and localize polymer samples. The determination of polymer characteristics and their relation to the material properties is one of the most important demands for polymer scientists; the development of software and instrument for higher molecular mass range (> 100 kD) will increase the applications of MALDI-TOF MS for polymer scientists.

Mineralogical Characteristics and Provenance of Cu-bearing Green Minerals Used as Traditional Pigments (전통 안료로 사용된 구리함유 녹색광물의 광물학적 특성과 산지추정)

  • Do, Jin-Young;Jung, Jongmee
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.2
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    • pp.123-135
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    • 2018
  • This study tried to find the clue to Seokrok province by comparing Seokrok used in painting culture properties with Seokrok ore from domestic occurrence and imported Seokrok ore. To this end, chemical and mineralogical characteristics of painting cultural properties were identified with portable X-ray Florescence (p-XRF), micro X-ray diffraction (micro XRD) and SEM/EDS Analysis. To obtain Pb isotopic ratio, the Pb contained in Seokrok has been analyzed with Thermal Ionization Mass Spectrometer. Atacamite (or botallackite) and small quantity of brochantite were identified from Seokrok in Dancheong, and malachite was also identified from Buddhist painting besides those two ingredients. Without distinction of type, most Seokrok used in painting cultural properties is atacamite composed of Cu and Cl. From Pb isotope analysis, it was found that Seokrok in painting cultural properties was closer to that of north Korea, north China and Japan than south Korea as in regional division for East North Asia suggested by Mabuchi. The Pb isotopic ratio of domestic green mineral belongs to the distribution of Seokrok inside the painting cultural properties but imported malachite showed considerably difference. Considering the fact that atacamite, the main mineral of Seokrok in painting cultural properties is rarely produced from southern mine of the Korean Peninsula and the result of Pb isotope analysis.

Catalytic decomposition of HDPE over Al-MCM-48 using TGA and Py-GC/FID (TGA와 Py-GC/FID를 이용한 Al-MCM-48상에서 HDPE의 촉매(觸媒) 열분해(熱分解))

  • Kim, Young-Min;Kim, Seung-Do;Park, Young-Kwon;Kim, Ji-Man;Jeon, Jong-Ki
    • Resources Recycling
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    • v.15 no.5 s.73
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    • pp.17-25
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    • 2006
  • Al-MCM-48 was used as a catalyst to decompose high density polyethylene(HDPE). Catalytic activity of Al-MCM-48 was compared with those of Al-MCM-41, Beta, and ZSM-5. Catalytic decomposition rate over Al-MCM-48 was much higher than at of non-catalytic pyrolysis only. Compared to other catalysts, Al-MCM-48 revealed the little higher activation energy value. The progressive deactivation behavior of the catalysts has also studied. ZSM-5 and Al-MCM-48 showed slower deactivation rates than Al-MCM-41 and Beta. Pyrolysis coupled with gas chromatographic separation and flame ionization detection (Py-GC/ FID) was also performed to assess the characteristics of pyrolysis products. ZSM-5 gave a higher fraction of gaseous products ($C_1-C_4$). Al-MCM-41 and Beta produced mainly $C_5-C_{12}$ products. The selectivity to oil product ($C_5-C_{22}$) obtained with Al- MCM-48 is higher an that with the other catalysts employed in this study.

A comparative analysis of volatile organic compound levels in field samples between different gas chromatographic approaches (분석기법의 차이에 따른 현장시료의 VOC 분석결과 비교연구: 분석오차의 발생 양상과 원인)

  • Ahn, Ji-Won;Pandey, Sudhir Kumar;Kim, Ki-Hyun
    • Analytical Science and Technology
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    • v.23 no.5
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    • pp.465-476
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    • 2010
  • In this study, a number of volatile organic compounds (VOCs) including benzene, toluene, p-xylene, styrene, and methyl ethyl ketone were analyzed from samples collected in ambient air and under the field conditions. These samples were analyzed independently by two different set-ups for VOC analyses, i.e., between [1] gas chromatography/flame ionization detector with tube sampling - (F-T system) and [2] gas chromatography/mass spectrometer with bag sampling (M-B system). The analytical results derived by both systems showed fairly similar patterns in relative sense but with moderately large differences in absolute sense. The results of M-B system were high relative to F-T system with the F-T/M-B ratio below 1. If the relative biases of the two measurement techniques are derived in terms of percent difference (PD) in concentration values, the results were generally above 35% on average. A student t-test was applied to investigate the statistical significance of those differences between the systems. The results of both analytical systems were different at 95% confidence level for toluene, p-xylene, styrene, and methyl ethyl ketone (P < 0.043). However, F-T and M-B systems showed strong correlations for toluene and p-xylene. The observed bias is explained in large part by such factors as the differences in standard phases used for each system and the chemical loss inside the bag sampler.

Pervaporation Separation of Ethanol Aqueous Solution through Carbonate-type Polyurethane Membrane III. The Effect of Zwitterionic Group (카보네이트형 폴리우레탄막을 이용한 에탄올 수용액의 투과증발분리 III. 양쪽이온성기에 의한 영향)

  • Oh, Boo Keun;Lee, Young Moo;Noh, Si Tae
    • Applied Chemistry for Engineering
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    • v.3 no.4
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    • pp.605-613
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    • 1992
  • NCO-terminated prepolymers were synthesized by reacting carbonate-type polyol(PTMCG)($M_w=1,000$ and 2,000) with MDI and N-methyldiethanolamine, as a chain extender. Carbonate-type polyurethane containg zwitterionic group was prepared by reacting the prepolymer with 1,3-propane sultone. From the IR and NMR spectra of model reactions, it was known that the ionization occurred under the same condition. The structure of zwitterionic carbonate-type polyurethane(ZPU) therefore could be confirmed from the model reactions. Glass transition temperature(Tg) ranged between $-15{\sim}-30^{\circ}C$ from the thermal data. Tg was between $-15{\sim}-18^{\circ}C$ for a series of ZPU10 samples and between $-25{\sim}-26^{\circ}C$ for a series of ZPU20 polymers. Tensile strength increased with mole ratio of ionic content. On the contrary, elongation was rather dropped with mole ratio of ionic content. ZPU10-30 having better tensile strength and less elongation was selected as a membrane for the concentration of ethanol aqueous solution through pervaporation. To obtain the better selectivity, it was crosslinked with HMDI. In the swelling test, it showed the higher swelling degree at around 50wt% ethanol concentration due to the plastization effect of ethanol. To optimize the separation capacity, two operating factors-feed concentration and temperature-were considered. The overall separation capacity was as follows : separation factor, 2~83.2 ; the flux, $25.4{\sim}58.8g/m^2hr$.

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Establishment of a library of fragments for the rapid and reliable determination of anabolic steroids by liquid chromatography-quadrupole time of flight-mass spectrometry

  • Do, Jung-Ah;Noh, Eunyoung;Yoon, Soon-Byung;Choi, Hojune;Baek, Sun-Young;Park, Sung-Kwan;Lee, Sang-Gyeong
    • Analytical Science and Technology
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    • v.30 no.1
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    • pp.10-19
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    • 2017
  • Anabolic steroids have similar structures to testosterone, both of which promote the growth of muscle mass and increase strength. However, the side effects of anabolic steroid use may lead to heart attacks or strokes. Additionally, the excessive use of steroids inhibits the production of the sex hormones in the body via a negative feedback loop, which results in testicular atrophy in males and amenorrhea in females. Currently, the method of choice used to test for the presence of anabolic steroids is GC-MS. However, GC-MS methods require chemical derivatization of the steroid sample to ensure compatibility with the analytical method; therefore, analysis of many different samples is difficult and time consuming. Unlike GC-MS, the liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) method is suitable for many samples. Twenty-two different anabolic steroids were analyzed by LC-Q-TOF-MS with various collision energies (CE). Accurate mass spectral data were obtained using a Q-TOF-MS equipped with an electro-spray ionization source and operated in the positive MS/MS mode for several classes of steroids that are often the targets of testing. Based on the collected data, fragmentation pathways were carefully elucidated. The high selectivity and sensitivity of the LC-Q-TOF-MS instrument combined with these fragmentation pathways offers a new approach for the rapid and accurate screening of anabolic steroids. The obtained data from the 22 different anabolic steroids will be shared with the scientific community in order to establish a library to aid in the screening of illegal anabolic steroids.

Determination of Ethylenethiourea in Fruits (과실류에 잔류하는 Ethylenethiourea 분석)

  • Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
    • Korean Journal of Food Science and Technology
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    • v.43 no.3
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    • pp.277-281
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    • 2011
  • A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.

Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

LATEST RESULTS OF THE MAXI MISSION

  • MIHARA, TATEHIRO
    • Publications of The Korean Astronomical Society
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    • v.30 no.2
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    • pp.559-563
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    • 2015
  • Monitor of All-sky X-ray Image (MAXI) is a Japanese X-ray all-sky surveyer mounted on the International Space Station (ISS). It has been scanning the whole sky since 2009 during every 92-minute ISS rotation. X-ray transients are quickly found by the real-time nova-search program. As a result, MAXI has issued 133 Astronomer's Telegrams and 44 Gamma-ray burst Coordinated Networks so far. MAXI has discovered six new black holes (BH) in 4.5 years. Long-term behaviors of the MAXI BHs can be classified into two types by their outbursts; a fast-rise exponential-decay type and a fast-rise flat-top one. The slit camera is suitable for accumulating data over a long time. MAXI issued a 37-month catalog containing 500 sources above a ~0.6 mCrab detection limit at 4-10 keV in the region ${\mid}{b}{\mid}$ > $10^{\circ}$. The SSC instrument utilizing an X-ray CCD has detected diffuse soft X-rays extending over a large solid angle, such as the Cygnus super bubble. MAXI/SSC has also detcted a Ne emission line from the rapid soft X-ray nova MAXI J0158-744. The overall shapes of outbursts in Be X-ray binaries (BeXRB) are precisely observed with MAXI/GSC. BeXRB have two kinds of outbursts, a normal outburst and a giant one. The peak dates of the subsequent giant outbursts of A0535+26 repeated with a different period than the orbital one. The Be stellar disk is considered to either have a precession motion or a distorted shape. The long-term behaviors of low-mass X-ray binaries (LMXB) containing weakly magnetized neutron stars are investigated. Transient LMXBs (Aql X-1 and 4U 1608-52) repeated outbursts every 200-1000 days, which is understood by the limit-cycle of hydrogen ionization states in the outer accretion disk. A third state (very dim state) in Aql X-1 and 4U 1608-52 was interpreted as the propeller effect in the unified picture of LMXB. Cir X-1 is a peculiar source in the sense that its long-term behavior is not like typical LMXBs. The luminosity sometimes decreases suddenly at periastron. It might be explained by the stripping of the outer accretion disk by a clumpy stellar wind. MAXI observed 64 large flares from 22 active stars (RS CVns, dMe stars, Argol types, young stellar objects) over 4 years. The total energies are $10^{34}-10^{36}$ erg $s^{-1}$. Since MAXI can measure the spectrum (temperature and emission measure), we can estimate the size of the plasma and the magnetic fields. The size sometimes exceeds the size of the star. The magnetic field is in the range of 10-100 gauss, which is a typical value for solar flares.

Study on Characteristics and Features of Re-corrosion on Archaeological Iron Nails after Conservation Treatments (철제관정의 보존처리 후 재부식 양상 및 특성 연구)

  • Lee, Hyeyoun;Park, Hyungho;Kim, Sujung;Yu, Jaeeun
    • Journal of Conservation Science
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    • v.28 no.4
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    • pp.343-351
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    • 2012
  • Excavated archaeological iron objects are prevented from being corroded going through desalination which slow down being corroded. However archaeological iron objects are liable to be corroded due to the high ionization tendency even though they are stored in environment restricted from corrosion factors. Iron objects could be deteriorated more than just excavated. Therefore this study investigated about the characteristic of re-corrosion and the effect on objects. In study, archaeological iron nails in storage for 4 years after conservation treatments were tested. Optical microscopy and X-ray photography for appearance, XRD, SEM-EDS, Raman spectroscopy for chemical composition, IC for chloride ions concentration inside iron nails were used. As results, iron nails carried out conservation treatments measured a high concentration of chloride ions after the long storage period. The form of objects were not in good condition such as broken or destroyed when the high chloride ions concentration was detected. In addition, the yellow and red powdery corrosion product were detected on the boundary between corrosion products and substrates and they were identified as akaganeite which is symptom of active corrosion.