• Journal of the Korean Ceramic Society
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• v.40 no.8
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• pp.739-745
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• 2003

In $N_{x}$ films were deposited on soda-lime glass without substrate heating by reactive dc magnetron sputtering using indium (In) metal target. Depositions were carried out under various total gas pressures ( $P_{tot}$) of mixture gases (Ar+$N_2$ or He+$N_2$). He gas was introduced to $N_2$ gas in order to enhance the reactivity of nitrogen on film surface by the "penning ionization". Plasma impedance decreased greatly when 20% or more introduced the $N_2$ gas. This is due to the In $N_{x}$ layers formed on target surface because a secondary electron emission rate of InN is small compared with In metal. XRD patterns of the films revealed that <001> preferred oriented polycrystalline In $N_{x}$ films, where the crystallinity of the films was improved with decrease of $P_{tot}$ and with increase of $N_2$ flow ratio. The improvement of the crystallinity and stoichimetry of the In $N_{x}$ films were considered to be caused by an increase in the activated nitrogen radicals and also by an increase in the kinetic energy of sputtered In atoms arriving at growing film surface, which should enhance the chemical reaction and surface migration on the growing film surface, respectively. Furthermore, the films deposited using mixture gases of He+$N_2$ showed higher crystallinity compared with the film deposited by the mixture gases of Ar+$N_2$.$.EX>.

• Safety and Health at Work
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• v.8 no.2
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• pp.220-225
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• 2017

Background: Benzene is a known occupational and environmental pollutant. Its urinary metabolite trans, trans-muconic acid (tt-MA) has been introduced by some environmental and occupational health regulatory associations as a biological index for the assessment of benzene exposure; however, recently, doubts have been raised about the specificity of tt-MA for low-level benzene exposures. In the present study, we investigated the association between urinary levels of tt-MA and inhalational exposure to benzene in different exposure groups. Methods: Benzene exposure was assessed by personal air sampling. Collected benzene on charcoal tube was extracted by carbon disulfide and determined by a gas chromatograph (gas chromatography with a flame ionization detector). Urinary tt-MA was extracted by a strong anion-exchange column and determined with high-performance liquid chromatography-UV. Results: Urinary levels of tt-MA in intensive benzene exposure groups (chemical workers and police officers) were significantly higher than other groups (urban and rural residents), but its levels in the last two groups with significant different exposure levels (mean = 0.081 ppm and 0.019 ppm, respectively) showed no significant difference (mean = $388{\mu}g/g$ creatinine and $282{\mu}g/g$, respectively; p < 0.05). Before work shift, urine samples of workers and police officers showed a high amount of tt-MA and its levels in rural residents' samples were not zero. Conclusion: Our results suggest that tt-MA may not be a reliable biomarker for monitoring low-level (below 0.5 ppm) benzene exposures.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.18 no.1
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• pp.32-40
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• 2008

Methyl bromide has been used as a representative fumigant for quarantine, and several poisoning cases have occurred recently by this chemical in Korea. The purpose of this study is to evaluate workers' exposures to airborne methyl bromide in the importing and exporting plant products quarantine companies. Air samples were collected 400/200 mg Anasorb 747TM and were analyzed by gas chromatograph /flame ionization detector according to the Occupational Safety and Health Agency (OSHA) Method PV2040. Geometric mean (GM) and arithmetic mean (AM) of total 27 workers' exposure concentrations to airborne methyl bromide were 1.12 ppm and 0.24 ppm, respectively. Two exposures(12.1 ppm and 12 ppm as 8hr-TWA) of total 27 workers' exposures exceeded the Korean standard (5 ppm) of Ministry Labor, while 4 exposures (15%) exceeded the Threshold Limit Value (TLV) (1 ppm) of American Conference of Governmental Industrial Hygienists (ACGIH). Seven samples (11%) of total 63 short-term air samples exceeded the OSHA Permissible Exposure Limit (PEL) 20 ppm (Ceiling). The opening (management) task in wood fumigation by tent showed the highest short-term exposure concentrations (AM: 18.6 ppm, GM: 0.58 ppm, maximum: 340.7 ppm). The maximum level in treatment task of the same process was 2.01 ppm. Methyl bromide concentrations in opening operation was significantly higher than that in treatment operation (p<0.05). In conclusion, the GM of workers' 8hr-TWA exposures to airborne methyl chloride in the importing/exporting plant quarantine industry was estimated below the ACGIH TLV (1 ppm). However, opening task in the fumigation of wood being covered with tent or fumigation of pant products in container showed the levels exceeding ACGIH TLV (1 ppm), and opening task in the fumigation of wood being covered with tent showed the level exceeding the Korean standard of Ministry of Labor (5 ppm).

• Korean Journal of Veterinary Service
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• v.30 no.1
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• pp.13-21
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• 2007

An atmospheric pressure chemical ionization (APcI) LC/MS/MS method was developed for the simultaneous analysis of fluoroquinolones (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin) residues in eggs. The spiked and blank samples were extracted from whole eggs using 50mM phosphate buffer (pH 7.4). The extract was cleaned up by passage though $Oasis^{(R)}$ MAX extraction cartridge for solid-phase extraction followed by elution with 4% formic acid in methanol. The extract of sample was separated on a Waters $Atlantis^{TM}$ $dC_{18}$ reversed-phase column ($4.6{\times}150mm,\;5{\mu}m$) and analyzed by APcI positive mode mass spectrometry. The mobile phase consists of aqueous 0.2% nonafluoropentanoic acid (NFPA) and methanol. Multiple reaction monitoring (MRM) using the precursor to product ion combinations of m/z $320\;{\dashrightarrow}\;302,\;332\;{\dashrightarrow}\;314,\;360\;{\dashrightarrow}\;342$ and m/z $358\;{\dashrightarrow}\;340$ were used to quantify norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR) and danofloxacin (DAN), respectively. The limits of quantification (LOQ) were 7.8ppb for NOR, 8.5ppb for CIP, 8.9ppb for ENR, and 4.8ppb for DAN. Average recoveries of fortified sample at levels of 0.025 to 0.1 ppm were estimated 71.29% for NOR, 75.27% for CIP, 85.51% for ENR and 81.22% for DAN. These results could be applied for the confirmation and quantification in eggs.

• Proceedings of the KIEE Conference
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• 1996.07c
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• pp.1446-1449
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• 1996

Thin films of diamond-like carbon(DLC) have been deposited using a magnetron plasma-enhanced chemical vapor deposition(PECVD) method with an rf(13.56 MHz) plasma of $C_{3}H_{8}$. From the Langmuir probe I-V characteristics, it can be observed that increasing the magnetic field yields an increase of the temperature($T_e$) and density($N_e$) of electron. At a magnetic field of 82 Gauss, the estimated values of $T_e$ and $N_e$ are approximately $1.5\;{\times}\;10^5$ K(13.5 eV) and $1.3\;{\times}\;10^{11}\;cm^{-3}$, respectively. Such a highly dense plasma can be attributed to the enhanced ionization caused by the cyclotron motion of electrons in the presence of a magnetic field. On the other hand, the negative dc self-bias voltage($-V_{sb}$) decreases with an increasing magnetic field, which is irrespective of gas pressure in the range of $1{\sim}7$ mTorr. This result is well explained by a theoretical model considering the variation of $T_e$. Deposition rates of DLC films increases with a magnetic field. This may be due to the increased mean free path of electrons in the magnetron plasma. Structures of DLC films are examined by using various techniques such as FTIR and Raman spectroscopy. Most of hydrocarbon bonds in DLC films prepared consist of $sp^3$ tetrahedral bonds. Increasing the rf power leads to an enhancement of cross-linking of carbon atoms in DLC films. At approximately 140 W, the maximum film density obtained is about 2.4 $g/cm^3$.

• Korean Journal of Materials Research
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• v.21 no.9
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• pp.509-514
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• 2011

In this study, optical emission spectroscopy was used to monitor the plasma produced during the RF magnetron sputtering of a $BaTiO_3$ target. The intensities of chemical species were measured by real time monitoring with various discharge parameters such as RF power, pressure, and discharge gas. The emission lines of elemental and ionized species from $BaTiO_3$ and Ti targets were analyzed to evaluate the film composition and the optimized growth conditions for $BaTiO_3$ films. The emissions from Ar(I, II), Ba(I, II) and Ti(I) were found during sputtering of the $BaTiO_3$ target in Ar atmosphere. With increasing RF power, all the line intensities increased because the electron density increased with increasing RF power. When the Ar pressure increased, the Ba(II) and Ti(I) line intensity increased, but the $Ar^+$ line intensity decreased with increasing pressure. This result shows that high pressure is of greater benefit for the ionization of Ba than for that of Ar. Oxygen depressed the intensity of the plasma more than Ar did. When the Ar/$O_2$ ratio decreased, the intensity of Ba decreased more sharply than that of Ti. This result indicates that the plasma composition strongly depends on the discharge gas atmosphere. When the oxygen increased, the Ba/Ti ratio and the thickness of the films decreased. The emission spectra showed consistent variation with applied power to the Ti target during co-sputtering of the $BaTiO_3$ and Ti targets. The co-sputtered films showed a Ba/Ti ratio of 1.05 to 0.73 with applied power to the Ti target. The films with different Ba/Ti ratios showed changes in grain size. Ti excess films annealed at $600^{\circ}C$ did not show the second phase such as $BaTi_2O_5$ and $TiO_2$.

• Analytical Science and Technology
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• v.30 no.6
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• pp.379-389
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• 2017

In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

• Natural Product Sciences
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• v.26 no.1
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• Korean Journal of Materials Research
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• v.14 no.6
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• pp.407-412
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• 2004

Photo decomposition of gas phase benzene by $TiO_2$ thin films chemically deposited on alumina balls were investigated under UV irradiation. Photo decomposition rates were measured in real time during the reaction using a photo ionization detector, which ionizes C-H bonding of benzene molecules and then converts into volatile organic compounds (VOCs) concentrations. From the measuring results, the VOCs concentration increased instantly when IN irradiated because C-H bonds of benzene molecules strongly absorbed on the surface of $TiO_2$ films before the IN irradiation was destroyed by photo decomposition. After that, the VOCs concentration decreased with increasing surface area of $TiO_2$ and reaction time under the IN irradiation. At the optimal conditions for the photo decomposition of gas phase benzene, the reaction rate of the photo decomposition for high concentrations (over 60 ppm) was slow but that of relatively low concentration (under 60 ppm) was fast, due to limited surface area of $TiO_2$ thin films for the reaction. Thus, it is concluded that the photo decomposition rate was mainly affected by the surface area of $TiO_2$ or absorption reaction.

• Analytical Science and Technology
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• v.33 no.2
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• pp.98-107
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• 2020

Methamphetamine (MA) is currently the most abused illicit drug in Korea. MA is produced by chemical synthesis, and the final target drug that is produced contains small amounts of the precursor chemicals, intermediates, and by-products. To identify and quantify these trace compounds in MA seizures, a practical and feasible approach for conducting chromatographic fingerprinting with a suite of traditional chemometric methods and recently introduced machine learning approaches was examined. This was achieved using gas chromatography (GC) coupled with a flame ionization detector (FID) and mass spectrometry (MS). Following appropriate examination of all the peaks in 71 samples, 166 impurities were selected as the characteristic components. Unsupervised (principal component analysis (PCA), hierarchical cluster analysis (HCA), and K-means clustering) and supervised (partial least squares-discriminant analysis (PLS-DA), orthogonal partial least squares-discriminant analysis (OPLS-DA), support vector machines (SVM), and deep neural network (DNN) with Keras) chemometric techniques were employed for classifying the 71 MA seizures. The results of the PCA, HCA, K-means clustering, PLS-DA, OPLS-DA, SVM, and DNN methods for quality evaluation were in good agreement. However, the tested MA seizures possessed distinct features, such as chirality, cutting agents, and boiling points. The study indicated that the established qualitative and semi-quantitative methods will be practical and useful analytical tools for characterizing trace compounds in illicit MA seizures. Moreover, they will provide a statistical basis for identifying the synthesis route, sources of supply, trafficking routes, and connections between seizures, which will support drug law enforcement agencies in their effort to eliminate organized MA crime.