• YAKHAK HOEJI
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• v.51 no.3
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• pp.206-213
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• 2007

Recently estimating the uncertainty of an analytical result has become an essential part of quantitative analysis. This study describes the uncertainty of the measurement for the determination of methamphetamine and its major metabolite amphetamine in human hair, The method consists of washing, drying, weighing, incubation and extraction with methanolic HCI solution, clean-up, trifluoroacetyl derivatization, and qualification/quantification of residues by gas chromatography/mass spectrometry (GC/MS). Traceability of measurement was established through traceable standards and calibrated volumetric equipment and measuring instruments. Measurement uncertainty associated with each analyte in real samples was estimated using quality control (QC) data. The main source of combined standard uncertainty comprised two components, which are uncertainties associated with calibration linearity and variations in QC, while those associated with preparation of analytical standards and sample weighing were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method ranged for individual analytes from 4.99 to5.03%.

• Analytical Science and Technology
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• v.14 no.6
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• pp.471-475
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• 2001

Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

• Analytical Science and Technology
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• v.7 no.4
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• pp.441-453
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• 1994

Two extraction methods, liquid-liquid extraction(LLE) and solid-phase extraction(SPE), coupled with GC/MS were compared as preconcentration procedures for priority pollutants in water. Among the semi-volatile priority pollutants, 11 acid and 44 base/neutral compounds were spiked in reagent water. With LLE, which is a modification of EPA Method 625, the overall mean recovery of the 54 compounds was 91% with a mean relative standard deviation(RSD) of 4.6%. With SPE, the overall mean recovery of the 52 compounds was 53% with a mean RSD of 8.9%. The detection limits of both methods were in the range of $1{\sim}5{\mu}g/l$.

• Bulletin of the Korean Chemical Society
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• v.29 no.12
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• pp.2482-2486
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• 2008

• Proceedings of the PSK Conference
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• 2000.04a
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• pp.201.2-202
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• 2000

• Journal of Korean Society for Atmospheric Environment
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• v.30 no.4
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• pp.362-377
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• 2014

Polycyclic aromatic hydrocarbons (PAHs) have been of particular concern since they are present both in the vapor and particulate phases in ambient air. In this study, a simple method was applied to determine the vapor phase PAHs, and the performance of the new method was evaluated with a conventional method. The simple method was based on adsorption sampling and thermal desorption with GC/MS analysis, which is generally applied to the determination of volatile organic compounds (VOCs) in the air. A combination of Carbotrap (300 mg) and Carbotrap-C (100 mg) sorbents was used as the adsorbent. Target compounds included two rings PAHs such as naphthalene, acenaphthylene, and acenaphthene. Among them, naphthalene was listed as one of the main HAPs together with a number of VOCs in petroleum refining industries in the USA. For comparison purposes, a method based on adsorption sampling and solvent extraction with GC/MS analysis was adopted, which is in principle same as the NIOSH 5515 method. The performance of the adsorption sampling and thermal desorption method was evaluated with respect to repeatabilities, detection limits, linearities, and storage stabilities for target compounds. The analytical repeatabilities of standard samples are all within 20%. Lower detection limits was estimated to be less than 0.1 ppbv. In the results from comparison studies between two methods for real air samples. Although the correlation coefficients were more than 0.9, a systematic difference between the two groups was revealed by the paired t-test (${\alpha}$=0.05). Concentrations of two-rings PAHs determined by adsorption and thermal desorption method consistently higher than those by solvent extraction method. The difference was caused by not only the poor sampling efficiencies of XAD-2 for target PAHs and but also sample losses during the solvent extraction and concentration procedure. This implies that the levels of lower molecular PAHs tend to be underestimated when determined by a conventional PAH method utilizing XAD-2 (and/or PUF) sampling and solvent extraction method. The adsorption sampling and thermal desorption with GC analysis is very simple, rapid, and reliable for lower-molecular weight PAHs. In addition, the method can be used for the measurement of VOCs in the air simultaneously. Therefore, we recommend that the determination of naphthalene, the most volatile PAH, will be better when it is measured by a VOC method instead of a conventional PAH method from a viewpoint of accuracy.

• Analytical Science and Technology
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• v.24 no.3
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• pp.183-192
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• 2011

This study was done for the determination and excretion profile of superdrol and its metabolites in human urine using both liquid chromatography with electrospray ionization mass spectrometry and gas chromatography with mass spectrometry after trimethylsilylation. Superdrol and its two metabolites were detected in human urine after administration of superdrol to healthy volunteers. The intra-day recovery ranged 89.7-113.2%, accuracy ranged 91.8-113.8% and reproducibility ranged 0.2-6.8% and inter-day recovery ranged 89.3-104.1%, accuracy ranged 95.2-103.0%, reproducibility ranged 0.7-7.8%. We found that superdrol M1 was a hydration at C-3 and superdrol M2 was a hydroxylation at D-ring. Superdrol and two metabolites were excreted as their glucuronided fractions. The glucuro-/sulfa-conjugated ratio of superdrol, superdrol M1 and superdrol M2 were 0.02, 0.02, 0.01, respectively. The excretion studies showed that superdrol and two metabolites were reached 4.3 h after oral administration and superdrol and superdrol M1 were detected until 48 h in human urine.

• Analytical Science and Technology
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• v.16 no.5
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• pp.339-348
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• 2003

Determination of some PAHs in used engine oils have been carried out by extraction of the components into acetonitrile followed by GC/FID and synchronous spectrofluorimetric technique. 7 PAHs, such as acenaphthene (Ace), anthracene (Anth), benzo(a)pyrene (BaP), chrysene (Chry), phenanthrene (Phen), fluoranthene (Ft), and perlyrene (Per) in used engine oil sample were able to determine separately by synchronous spectrofluorimetry. Calibration curves for those components were linear for the concentration range of 0.4~166 ppb PAHs with the corelation factor of 0.9985~0.9999. The peak areas produced by GC/FID split ratio program were used for the calibration curves of the other 8 PAHs. Detection sensitivity of the synchronous spectrofluorimetry seems to be 100 times more sensitive than GC/FID method. The total amount of PAHs in the used engine oil were 5.5 ng/g for LNG (bus), 10.5 ng/g for LPG(taxi), 92.2 ng/g for gasoline-passenger car, and 130 ng/g for diesel trailer, respectively.

• Analytical Science and Technology
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• v.16 no.6
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• pp.483-487
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• 2003

Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

• Analytical Science and Technology
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• v.21 no.1
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• pp.41-47
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• 2008

Although liquid-liquid extraction (LLE) method has been used routinely for the analysis of amphetamine-like drugs (amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA), a solid-phase extraction (SPE) method, which can be automated, was applied for the simultaneous determination by GC/MS in human urine. Urine samples (3 mL) and 0.1 M phosphate buffer (1 mL, pH 7.0) were extracted by an automated SPE system. The eluent was evaporated, derivatized with trifluoroacetic anhydride (TFAA), and analyzed by GC/MS. The calibration curves was linear with correlation coefficient ($r^2$) above 0.994 in the ranges of 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL for AP, MDA, and 50.0~2000.0 ng/mL for MA, MDMA, and MDEA. The limits of detection ranged from 4.0 to 10.0 ng/mL, and the limits of quantitation ranged from 12.0 to 34.0 ng/mL. The relative recoveries were 93.5~107.7 %. The precisions and accuracies were 1.9~14.8 % and -8.7~14.8 %, respectively. The present method was successfully applied to identify the MA or Ecstasy (MDMA) abusers in exact as well as rapid.