• Title/Summary/Keyword: Sampling and analytical method

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Measurement of Carbonyl Compounds in Ambient Air using a DNPH Cartridge coupled with HPLC Method (DNPH 카트리지와 HPLC를 이용한 대기 중 카르보닐화합물의 농도측정)

  • 황윤정;박상곤;백성옥
    • Journal of Korean Society for Atmospheric Environment
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    • v.12 no.2
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    • pp.199-209
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    • 1996
  • The purpose of this study is to evaluate analytical method for the measurement of carbonyl compounds and to apply method to the measurement of indoor and outdoor concentrations of these compounds at public facilities. For sampling, 2.4-dinitrophenylhydrazine (DNPH) coated DNPH-Silica cartridges were uwed in this study. DNPH reacts with carbonyl compounds and forms carbonyl hydrazone, The carbonyl hydarzone was eluted from the cartridge with acetonitrile and analyzed by reverse-phase HPLC with UV detection. Possible interference caused by ozone during sampling was eliminated by using KI trap commected in series with the DNPH-Silica cartridge. A number of experimental studies were undertaken to evaluate and validate the analytical method, including collection efficiency, recovery, repeatability, lower limits of detection, and effect of ozone. Indoor and outdoor measurements of carbonyl compounds were simultaneously carried out at 14 public facilities located in Taegu city and Kyungsan city from June to July, 1995. Except for one or two sites, the indoor concentrations were found to be higher than the outdoor concentrations for carbonyl compounds. And the concentrations of carbonyl compounds measured in the morning and afternoon were showed higher than the concentrations measured in the evening.

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Evaluation of Sampling and Analytical Methods for the Determination of Polycyclic Aromatic Hydrocarbons in the Ambient Atmosphere (환경대기중 다환방향족탄화수소의 포집과 분석방법에 관한 연구)

  • 백성옥
    • Journal of Korean Society for Atmospheric Environment
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    • v.7 no.1
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    • pp.1-16
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    • 1991
  • In this study, sampling and analytical procedures were evaluated for the determination of ambient levels of atmospheric PAH, both in gaseous and particulate phase. The method involves low-volume sampling and Soxhlet extraction of the filters and Tenax absorbent, followed by a clean-up stage using a silica column prior to analysis by reversed-phase HPLC with wavelength programmable fluorescence and UV detection. A total of 18 PAH were identified and quantified, all of which have been of environmental concern. In order to validate the methodology and to ensure compatibility of the results, the analytical method used for the determination of PAH was evaluated with respect to the efficiencies of extraction and clean-up procedure, HPLC separation, and lower limits of detection. In addition, substrate dependency of PAH recovery was investigated for the two types of fiters, i.e. glass fiber and PTFE filters.

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Reduced sulfur gas loss in the bag sampling procedure - Comparison by calibration slope values (악취황 성분의 채취와 샘플백 내부의 시료 유실율 비교: 검량선의 기울기를 이용한 평가)

  • Kim, K.H.;Choi, Y.J.;Ahn, J.W.
    • Analytical Science and Technology
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    • v.18 no.4
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    • pp.338-343
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    • 2005
  • In this work, sample loss of reduced sulfur compounds (RSC) was investigated with respect to bag sampling techniques. For comparison purpose, calibration slopes were obtained by analyzing standards prepared by 'within syringe dilution' (WSD) method against those made either by 'Tedlar bag dilution' (TBD) or by 'polyester aluminum bag dilution' (PBD) method. The results indicated that the recovery rate of TBD showed the mean values of about 87%, while those of PBD about 77%. Despite the fact that sample loss is inevitable, precise sampling of reduced sulfur compounds may still be possible, if one acknowledges and be prepared for such loss rates of bag sampling methods.

Analysis of Volatiles in Sesame Oil Collected by Simultaneous Distillation/Extraction(SDE) and Dynamic Headspace Sampling (DHS) (연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)에 의한 참기름 중의 향기성분의 분석)

  • Ha, Jaeho
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.399-405
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    • 1996
  • The flavor compounds of the oil from roasted sesame seeds were collected by simultaneous steam distillation/ extraction(SDE) and dynamic headspace sampling(DHS) and were analyzed using a gas chromatograph equipped with a flame ionization detector and connected into a mass spectrometer. Among the flavor compounds collected by the SDE method, 46 compounds were identified. They consisted of 6 alcohols, 6 aldehydes, 5 ketones or acids, 4 furans or phenols, 12 pyrazines, 4 pyridines or thiazoles, and others. Thirty six compounds were identified by DHS and many of them were the same as those identified by the SDE method. However, some compounds such as 1-hexanol, pentanal, and dimethylsulfide were identified only by the DHS method.

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Radioactive waste sampling for characterisation - A Bayesian upgrade

  • Pyke, Caroline K.;Hiller, Peter J.;Koma, Yoshikazu;Ohki, Keiichi
    • Nuclear Engineering and Technology
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    • v.54 no.1
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    • pp.414-422
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    • 2022
  • Presented in this paper is a methodology for combining a Bayesian statistical approach with Data Quality Objectives (a structured decision-making method) to provide increased levels of confidence in analytical data when approaching a waste boundary. Development of sampling and analysis plans for the characterisation of radioactive waste often use a simple, one pass statistical approach as underpinning for the sampling schedule. Using a Bayesian statistical approach introduces the concept of Prior information giving an adaptive sample strategy based on previous knowledge. This aligns more closely with the iterative approach demanded of the most commonly used structured decision-making tool in this area (Data Quality Objectives) and the potential to provide a more fully underpinned justification than the more traditional statistical approach. The approach described has been developed in a UK regulatory context but is translated to a waste stream from the Fukushima Daiichi Nuclear Power Station to demonstrate how the methodology can be applied in this context to support decision making regarding the ultimate disposal option for radioactive waste in a more global context.

Comparison of Sampling Methods for On-Farm Use Quick Test Procedure of Soil Nitrate (토양의 질산태질소 현장검정을 위한 시료 채취방법 비교)

  • Kang, Seong-Soo;Kim, Ki-In;Chung, Keun-Yook;Hong, Soon-Dal
    • Korean Journal of Soil Science and Fertilizer
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    • v.38 no.1
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    • pp.32-37
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    • 2005
  • The procedure of soil sampling for on-farm quick test of soil nitrate is very important to improve practical application without weighing or drying soil. To improve application of test strip reflectometer as a quick on-farm analytical procedure for the estimation of soil nitrate concentration, three sampling methods such as gravimetric sampling (GS), particle density sampling (PDS) and bulk density sampling (BDS) for on-farm analytical procedure were investigated with twelve soils of 45 to $281mg\;kg^{-1}$ nitrate nitrogen concentration. The nitrate nitrogen concentrations measured from different soils were compared with two analytical methods, ion electrode method as a standard laboratory analysis (SLA) and test strip reflectometer at three moisture conditions, viz. air dried soil, 20 and 40% of maximum water holding capacity (MWHC). Nitrate nitrogen concentration measured by test strip reflectometer was significantly correlated with that of SLA, and the coefficients of variation (CV) were in the range of 3.5 to 10.9%. These CV values less than 10.9% were thought to be acceptable for the measurement of soil nitrate as an on-farm real time analytical procedure. The nitrate nitrogen concentration by BDS for test strip reflectometer as well as ion electrode method was more similar to that of SLA compared with those by GS and PDS especially in case of moist soils. This result suggests that the BDS is more useful than GS and PDS in case of on-farm analytical procedure of soil nitrate for moist soils. Further the practical measurement by BDS could be improved by substituting the bottle cap with a larger container.

Application of Adsorption Sampling and Thermal Desorption with GC/MS Analysis for the Measurement of Low-Molecular Weight PAHs in Ambient Air (환경대기 중 저분자 PAHs 측정을 위한 흡착-열탈착-GC/MS 방법의 적용)

  • Seo, Seok-Jun;Seo, Young-Kyo;Hwang, Yoon-Jung;Jung, Dong-Hee;Baek, Sung-Ok
    • 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.

Comparison of USEPA Digestion Methods for Trace Metal Analysis Using SRM

  • Shin, Mi-Young;Yoon, Hyeon;Kim, Youn-Tae;Yoon, Cheol-Ho;Woo, Nam-Chil
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2004.09a
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    • pp.223-226
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    • 2004
  • The importance of a proper sample preparation and analysis technique has getting attention due to the complicity of toxic elements of interest from environmental samples depend on analytical purposes. It is critical to use proper analytical method to evaluate trace elements concentration in many environmental samples especially for making remediation decisions. Therefore, it is critical to apply a proper sampling and analytical method such as EPA publication SW-846 (Test Methods for Evaluating Solid Waste, Physical/chemical Methods). The objective of this study was to compare the USEPA Methods 3050B, modified 3050B, 305 la, and KBSI method (modified EPA 3052 Method) in term of recovery rate of metals. The NIST SRM (Montana soil) was used to compare the extraction and digestion efficiency. After sample has been collected the analysis were achieved by ICP-MS (Elan 6100, Perkin Elmer) as well as ICP-AES (Ultima 2C, JY) for trace elements and major elements.

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A Simple Proposition for Improving Industrial Hygiene Air Sampling Methods

  • Paik, Samuel Y.;Zalk, David M.
    • Safety and Health at Work
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    • v.10 no.3
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    • pp.389-392
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    • 2019
  • When conducting an exposure assessment, the primary goal of the industrial hygienist is to fully characterize the worker's exposure during a work shift to compare it with an occupational exposure limit. This applies regardless of the duration of the work activity as an activity that is relatively short in duration can still present exposure in excess of the occupational exposure limit even when normalized over an 8-hr shift. This goal, however, is often impeded by the specification of a minimum sample volume in the published sampling method, which may prevent the sample from being collected or submitted for analysis. Removing the specification of minimum sample volume (or adjusting it from a requirement to a recommendation), in contrast, allows for a broader assessment of jobs that consist of short-duration and high-exposure activities and also eliminates the unnecessary practice of running sampling pumps in clean air to collect a specified, minimum volume.

Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.