• The Journal of the Petrological Society of Korea
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• v.20 no.3
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• pp.161-172
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• 2011

Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

• Korean Journal of Materials Research
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• v.5 no.6
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• pp.754-762
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• 1995

Strontium titanate(SrTiO$_3$) thin film was prepared on Si substrates by RF magnetron sputtering for a high capacitance density required for the next generation of LSTs. The optimum deposition conditions for SrTiO$_3$thin film were investigated by controlling the deposition parameters. The crystallinity of films and the interface reactions between SrTO$_3$film and Si substrate were characterized by XRD and AES respectively. High quality films were obtained by using the mixed gas of Ar and $O_2$for sputtering. The films were deposited at various bias voltages to obtain the optimum conditions for a high quality file. The best crystallinity was obtained at film thickness of 300nm with the sputtering gas of Ar+20% $O_2$and the bias voltage of 100V. The barrier layer of Pt(100nm)/Ti(50nm) was very effective in avoiding the formation of SiO$_2$layer at the interface between SrTiO$_3$film and Si substrate. The capacitor with Au/SrTiO$_3$/Pt/Ti/SiO$_2$/Si structure was prepared to measure the electric and the dielectric properties. The highest capacitance and the lowest leakage current density were obtained by annealing at $600^{\circ}C$ for 2hrs. The typical specific capacitance was 6.4fF/$\textrm{cm}^2$, the relative dielectric constant was 217, and the leakage current density was about 2.0$\times$10$^{-8}$ A/$\textrm{cm}^2$ at the SrTiO$_3$film with the thickness of 300nm.

• Journal of the Korean Wood Science and Technology
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• v.35 no.1
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• pp.73-80
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• 2007

This study was carried out to separate the heavy toxic metals in eco-building materials by low-temperature pyrolysis, especially arsenic (As) compounds in CCA wood preservative as a solid in char. The pyrolysis was carried out to heat the CCA-treated Hemlock at $280^{\circ}C$, $300^{\circ}C$, $320^{\circ}C$, and $340^{\circ}C$ for 60 mins. Laboratory scale pyrolyzer composed of [preheater$\rightarrow$pyrolyzer$\rightarrow$1st water scrubber$\rightarrow$2nd bubbling flask with 1% $HNO_3$ solution$\rightarrow$vent], and was operated to absorb the volatile metal compound particulates at the primary water scrubber and the secondary nitric acid bubbling flask with cooling condenser of $4^{\circ}C$ under nitrogen stream of 20 mL/min flow rate. And the contents of copper, chromium and arsenic compounds in its pyrolysis such as carbonized CCA treated wood, 1st washing and 2nd washing liquors as well as its raw materials, were determined using ICP-AES. The results are as follows : 1. The yield of char in low-temperature pyrolysis reached about 50 percentage similar to the result of common pyrolytic process. 2. The higher the pyrolytic temperature was, the more the volatiles of CCA, and in particular, the arsenic compounds were to be further more volatile above $320^{\circ}C$, even though the more repetitive and sequential monitorings were necessary. 3. More than 85 percentage of CCA in CCA-treated wood was left in char in such low-temperature pyrolytic condition at $300^{\circ}C$. 4. Washing system for absorption of volatile CCA in this experiment required much more contacting time between volatile gases and water to prevent the loss of CCA compounds, especially the loss of arsenic compound. 5. Therefore, more complete recovery of CCA components in CCA-treated wood required the lower temperature than $320^{\circ}C$, and the longer contacting time of volatile gases and water needed the special washing and recovery system to separate the toxic and volatile arsenic compounds in vent gases.

• Korean Journal of Soil Science and Fertilizer
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• v.42 no.5
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• pp.399-407
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• 2009

Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.

• Journal of Food Hygiene and Safety
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• v.21 no.4
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• pp.231-237
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• 2006

Nowadays the teabag is worldwide used for various products including green tea, tea, coffee, etc. since it is convenient for use. In case of outer packaging printed, however, there is a possibility that the plasticizers which is used for improvement in adhesiveness of printing ink may shift to inner tea bag. In this study, in order to monitor residual levels of plasticizers in teabags, we have established the simultaneous analysis method of 9 phthalates and 7 adipates plasticizers using gas chromatography (GC). These compounds were also confirmed using gas chromatography-mass spectrometry (GC-MSD). The recoveries of plasticizers analyzed by GC ranged from 82.7% to 104.6% with coefficient of variation of $0.6\sim2.7%$ and the correlation coefficients of each plasticizer was $0.9991\sim0.9999$. Therefore this simultaneous analysis method was showed excellent reproducibility and linearity. And limit of detection (LOD) and limit of quantitation (LOQ) on individual plasticizer were $0.1\sim3.5\;ppm\;and\;0.3\sim11.5\;ppm$ respectively. When 143 commercial products of teabag were monitored, no plasticizers analysed were detected in filter of teabag products. The migration into $95^{\circ}C$ water as food was also examined and the 16 plasticizers are not detected. In addition we carried out analysis of heavy metals, lead (Pb), cadmium (Cd), arsenic (As) and aluminum (Al) in teabag filters using ICP/AES. $Trace\sim23{\mu}g$ Pb per teabag and $0.6\sim1718{\mu}g$ Al per teabag were detected in materials of samples and Cd and As are detected less than LOQ (0.05 ppm). The migration levels of Pb and Al from teabag filter to $95^{\circ}C$ water were upto $11.5{\mu}g\;and\;20.8{\mu}g$ per teabag, respectively and Cd and As were not detected in exudate water of all samples. Collectively, these results suggest that there is no safety concern from using teabag filter.