• Environmental Analysis Health and Toxicology
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• v.17 no.2
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• pp.95-107
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• 2002

This study was designed to investigate the characteristics of atmospheric concentrations of toxic volatile organic compounds (VOCs) in Korea. Target compounds included 1,3-butadiene, aromatics such as BTEX, and a number of carbonyl compounds. In this paper, as the first part of the study, the performance of sampling and analytical methods was evaluated for the measurement of selected VOCs and carbonyl compounds in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/MSD analysis, while carbonyls by the DNPH-silica cartridge sampling with HPLC analysis. The methodology was investigated with a wide range of performance criteria such as repeatability, linearity. lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal standards. In addition, the sampling and analytical methods established in this study were applied to real field samples duplicately collected in various ambient environments. Precisions for the duplicate samples appeared to be comparable with the performance criteria recommended by USEPA TO-17. The overall precision of the sampling and analytical methods was estimated to be within 20 ∼ 30% for major aromatic VOCs such as BTEX, whereas the precision for major carbonyl compounds such as formaldehyde and acetaldehyde was within 10 ∼ 20% for field samples. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

• Journal of Korean Society for Atmospheric Environment
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• v.18 no.1
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• pp.39-49
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• 2002

In this study, limits of detection (LOD), accuracy and precision of four sampling/ analytical methods were evaluated and compared for the determination of airborne hexavalent chromium, Cr (VI). The methods include : (1) a combination of the National Institute for Occupational Safety and Health (NIOSH) Method 7600/U. S. Environmental Protection Agency (EPA) Method 218.6 (NIOSH/EPA Method) proposed by Shin and Paik, 2) two impinger methods using 2% NaOH/3% Na$_2$CO$_3$. (3) same as (2) but with 0.02 N NaHCO$_3$absorbing solution, and (4) the Occupational Safety and Health (OSHA) Method ID-215. An ion chromatograph/visible absorbance detector was used for the analysis of Cr (VI) in sample solution. Limit of detection (LOD) , analytical accuracy, and precision were also tested using Cr (VI) spike samples. Recoveries (as index of accuracy) and coefficient of variation (CV) (as a index of precision) were determined. Two-way ANOVA and Turkey's test were performed to test the significance in differences among recoveries and CVs of the methods. In all the methods, the peaks of Cr (VI) were separated sharply on chromatograms and exhibited a strong linearity with Cr (VI) concentrations in solution. The correlation coefficients of calibration curves typically ranged from 0.9997 to 0.9999, and the analytical LODs from 0.025 to 0.1$\mu\textrm{g}$/sample. All the method had good sensitivities and linearities between Cr (VI) levels and peak areas. The accuracies (% mean recoveries) of the methods ranged from 80.1 to 104.2%, while the precisions (pooled coefficient of variation) ranged from 3.16 to 4.43%. The impinger methods showed higher recoveries ( > 95%) than those of the PVC filter methods (the OSHA Method and the NIOSH/EPA Method). It was assumed that Cr (VI) on PVC filter was exposed to air and reduced to trivalent chromium, Cr (III), whereas it was stabilized in alkali solution contained in impinger. Thus, a special treatment of Cr (VI) samples collected on PVC filters may be required.

• Analytical Science and Technology
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• v.8 no.4
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

• Journal of Korean Society for Atmospheric Environment
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• v.14 no.5
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• pp.507-518
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• 1998

A field comparison study was carried out to quantify differences among various sampling and analytical methods for volatile organic compounds (VOCs) at a site in Vlsan in June 1997. Air sampling containers (SUMMA canisters) were used by the Korea Institute of Science and Technology (KIST) and adsorption tubes (carbotrap) were used by Yeungnam University (YN Univ.) for sampling ambient air. Duplicate samples obtained by KIST were analyzed by KIST with a GC-MS system for aromatics and halogenated hydrocarbons and by Atm AA with a GC -FID system for C2∼C9 hydrocarbons, respectively. The adsorption tube samples were analyzed by YN Univ. with a GC-FID system for aromatics. VOC levels for the duplicate canister sampls analyzed by KIST and Atm AA were in good agreement. Concentrations of aromatics by the adsroption tube method were generally higher than those by the canister sampling method by factor of 1.5 to 2.0. Differences between the two sampling methods were discussed.

• Journal of the Korea Society for Simulation
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• v.9 no.2
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• pp.75-87
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• 2000

In this paper, nonstationary multiple sampling plans are discussed which are difficult to solve by analytical method when there exists dependency between the sample data. The initial solution is found by the sequential sampling plan using the sequential probability ration test. The number of acceptance and rejection in each step of the multiple sampling plan are found by grouping the sequential sampling plan's solution initially. The optimal multiple sampling plans are found by simulation. Four search methods are developed U and the optimum sampling plans satisfying the Type I and Type ll error probabilities. The performance of the sampling plans is measured and their algorithms are also shown. To consider the nonstationary property of the dependent sampling plan, simulation method is used for finding the lot rejection and acceptance probability function. As a numerical example Markov chain model is inspected. Effects of the dependency factor and search methods are compared to analyze the sampling results by changing their parameters.

• Journal of Korean Society for Atmospheric Environment
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• v.34 no.1
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• pp.120-143
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• 2018

The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

• Journal of Environmental Health Sciences
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• v.28 no.2
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• pp.109-116
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• 2002

The purpose of this study was to evaluate a new sampling and analytical method for the determination of airborne hexavalent chromium, Cr(Ⅵ), in a field plating operation. The procedures of this new method (Shin & Paik's Method) are as the following: Airborne hexavalent chromium is collected on polyvinyl chloride (PVC) filter according to the National Institute iota Occupational Safety and Health (NIOSH) Method 7600, and the filler sample is placed in a screw-capped vial and soaked with 2% NaOH/3% Na₂CO₃ solution immediately after sampling. The Cr(Ⅵ) sample is analyzed by ion chromatography/visible spectrophotometry (IC/VS) according to the U.S. Environmental Protection Agency (EPA) Method 218.6. The airborne Cr(Ⅵ) concentrations measured by this method were compared with those determined by three reference methods: One (NIOSH/EPA Method) consisted of sampling airborne Cr(Ⅵ) on PVC filters and storing the sample filters in strew-capped vials according to the NIOSH method, and analyzing Cr(Ⅵ) in samples using IC/VS according to the EPA method. The second method (Impinger Method/NaHCO₃) consisted of absorbing airborne Cr(Ⅵ) into 0.02 M NaHCO₃ solution in midget impinger, and analyzing the Cr(Ⅵ) in samples using IC/VS. The third method was the OSHA Method ID-215. Using these four different methods, lour replicates of air samples were collected at an electroplating process and analyzed simultaneously. Two-way ANOVA and paired t-test were used to test difference among values determined by the methods. There was no significant difference and a strong correlation (r²:0.99) between Cr(Ⅵ) concentrations measured by the Shin & Paik's Method and an impinger method (p>0.05). However, Cr(Ⅵ) concentrations determined by Shin & Paik's Method were significant1y different from those by the NIOSH/EPA Method (p<0.05) or the OSHA method (p<0.05). The Cr(Ⅵ) concentrations of Shin & Paik's Method were significantly higher than those of the NIOSH/EPA Method or the OSHA method. This result indicated that the Shin & Paik's Method may prevent Cr(Ⅵ) losses caused by reduction and give more reliable results of airborne Cr(Ⅵ) concentrations in work environments.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2005.10a
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• pp.129-130
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• 2005

• Economic and Environmental Geology
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• v.37 no.1
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• pp.49-59
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• 2004

The concectration and distribution of contaminants obtained from a contaminated land investigation or an environmental geochemistry survey constitutes the basis of a decision-making process on environmental policies or of scientific researches. As the quality of data determines the reliability of the result, the investigation plan should be adjusted according to the purpose of the investigation. In general, the effort to improve the data quality had been focused mainly on the QA/QC procedures in laboratories. The rapid progress of analytical instrument has also contributed toward improving the analytical precision to a sacrificable degree. Nevertheless, in many cases, it is not the analytical precision that needs improvement for the better precision of overall measurement process: it is rather during the sampling process in the field that is responsible for the poor precision. To assess the data quality on a measured value, ISO recommends to provide information on "measurement uncertainty" along with the measured value. The measurement uncertainty in an environmental measurement context can be explained as the statistical number that expresses the degree of the uncertainty stemming from the sampling and analytical procedures. There is a cost involved in order to improve the precision of sampling and analytical methods so as to decrease the degree of measurement uncertainty. The economical point of compromise in an investigation planning can be achieved when the allowable degree of uncertainty has been set before-hand. The investigation can then be planned accordingly not to exceed the uncertainty limit. Furthermore, if the measurement uncertainty estimated from the preliminary investigation can be separated into sampling and analytical uncertainties, it can be used as a criterion where the resources for the investigation should be allotted cost-effectively to reinforce the weakest link of the whole investigation process. This paper aims to present a method of estimating the level of measurement uncertainty of a measured contamination concentration at a site used as an example and to show how the estimated uncertainty can be applied to serve the particular purpose of an investigation.

• Proceedings of the Korean Environmental Health Society Conference
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• 2001.04a
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• pp.101-102
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• 2001