• Title/Summary/Keyword: Sampling and analytical method

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The Analysis of VOCs by GC/MS with Whole Column Coldtrapping on a Fused Silica Capillary Column in Indoor Environment

  • Dai, Shugui;Zhang, Lin;Bai, Zhipeng
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.829-834
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    • 1995
  • Whole column coldtrapping(WCC) on a fused silica capillary (FSCC)combined with GC/MS analysis was evaluated for use in the investigation of volatile organic compounds(VOCs) in indoor air. Research had indicated that a temperature of $-80^{\circ}C$ is optimal for WCC. Samples were analyzed on a $50m{\times}0.2mm$ cross-linked 5% phenylmethylsilicone fused silica column. Liquid nitrogen was used as the coolant for the peak resolution significantly. The analysis can be performed quickly and conveniently. More than 112 of VOCs were determined in the samples from three typical indoor environment including: (1) a room which had just been decorated involving building materials and paints; (2)a kitchen used for Chinese cooking, and (3) a room had tobacco smoke. The method is could be readily applied to rapid sample screening for VOCs contamination surveys or initial investigations with its valid and simple sampling and analytical technique.

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Analytical method for analyzing formaldehyde using 2, 4-DNPH and gas chromatography/FID, NPD (2,4-DNPH와 가스크로마토그래프를 이용한 포름알데히드 분석방법)

  • Jeong, Jee Yeon;Park, Seung Hyun;Yi, Gwang Yong;Oh, Se Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.10 no.1
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    • pp.126-146
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    • 2000
  • To develop and evaluate formaldehyde measurement method using 2,4-dinitro-phenylhydrazine (2,4-DNPH) coated sampler and gas chromatography, laboratory test and field test were conducted. Results of this study are as follows. Limit of detection(LOD) of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is $0.008{\mu}g/m{\ell}$ $0.060{\mu}g/m{\ell}$, $0.472{\mu}g/m{\ell}$ respectively. Coefficiency of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is 0.008, 0.009, 0.020 respectively. Desorption efficiency of sep-pak xposure aldehyde sampler and sorbent sample tube is 1.05(range : 0.99 - 1.12), 1.02(range : 0.99 - 1.06) respectively. Samples of sorbent sample tube and sep-pak xposure aldehyde sampler turned out to be stored at refrigerator, according to storage test results. Measurement methods of HPLC-UVD, GC-NPD, GC-FID, according to results of precision for the combined sampling and analytical procedure, became acceptable to OSHA evaluation standard. Field test using exposure chamber met the NIOSH overall uncertainty recommendation(less than 25%). Overall uncertainty of Sepak-HPLC(UVD), Tube-GC(NPD), Tube-GC(FID) is 11.0% - 17.0%. Consequently gas chromatography(GC-NPD, GC-FID) and high performance liquid chromatography(EPA TO-11) using 2,4-DNPH coated sampler for formaldehyde measurement turned out to be suitable to measure personal formaldehyde exposure at workplaces.

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Field Validation of an IC/Visible Spectrophotometry Method for the Determination of Cr(VI) in Mist (미스트중 6가 크롬 측정을 위한 IC/Visible Spectrophotometry 방법 (Shin & Paik′s Method)의 현장 평가)

  • 신용철;백남원;김상우;김선자;이유미
    • Proceedings of the Korean Environmental Health Society Conference
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    • 2002.04a
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    • pp.40.1-43
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    • 2002
  • The purpose of this study was to evaluate a new sampling and analytical method for the determination of hexavalent chromium, Cr(VI) in mist from 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 for Occupational Safety and Health (NIOSH) Method 7600, and the filter 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 screw-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 MN/sub a/Hco₃ 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, four 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 (r/sup 2/=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 Significantly different form 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. We concluded that the Shin & Paik's Method could prevent Cr(VI) losses caused by reduction and give more reliable results of airborne Cr(VI) concentrations in work environments.

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Analysis Methods for Measurement of Ammonia Concentration (가스상 암모니아 측정을 위한 분석방법별 특성 연구)

  • Sa, Jae-Hwan;Yoon, Seok-Kyung;Roh, Gi-Hwan;Jeon, Eui-Chan
    • Journal of Korean Society for Atmospheric Environment
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    • v.24 no.1
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    • pp.43-54
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    • 2008
  • Management and control of ammonia at the sources and ambient largely depend on sampling and measurement techniques. Good sampling and measurement techniques provide high quality data. The main purpose of the study is compare the analytical characteristics of the Indolphenol method which is one of the standard method in Korea with automatic analyzers for continued measuring gaseous ammonia. For comparison with other analytical methods, the verification test was designed to evaluate performance parameters; linearity, absorption efficiency, reproducibility and repeatability test, accuracy, and response time test. $R^2$ of calibration curve using IPM and CLM was very high (value is 1.000), but for EcSM $R^2$ value was estimated to be lower than IPM and CLM (as 0.991). The RSD of the CLM ranged from 0.1 to 2.3% over the nine concentration levels measured, %Ds was 0.1 to 10.7%, and average RA over all the measurements was 3.3%. The RSD of IPM and EcSM was ranged from 1.0 to 8.1, 3.9 to 14.0 respectively, and average RA were 8.71, 4.9% respectively. Rise in response times of EcSM was estimated to be 1 minute. It is found to be more sensitive than response time (which ranged from 2 to 9 minute) of CLM. For ammonia concentration measured using the IPM and the CLM from the same ammonia source, linear regression of IPM versus CLM show a slope of 0.805, an intercept of 637 ppb, and $R^2$ of 0.868.

Improvement of Verification Method for Remedial Works through the Suggestion of Indicative Parameters and Sampling Method (정화 보조지표와 시료 채취 방법 제안을 통한 토양정화검증 제도 개선 연구)

  • Kwon, Ji Cheol;Lee, Goontaek;Kim, Tae Seung;Yoon, Jeong-Ki;Kim, Ji-in;Kim, Yonghoon;Kim, Joonyoung;Choi, Jeongmin
    • Journal of Soil and Groundwater Environment
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    • v.21 no.6
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    • pp.179-191
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    • 2016
  • In addition to the measurement of the concentration of soil contaminants, the new idea of indicative parameters was proposed to validate the remedial works through the monitoring for the changes of soil characteristics after applying the clean up technologies. The parameters like CFU (colony forming unit), pH and soil texture were recommended as indicative parameters for land farming. In case of soil washing, water content and the particle size distribution of the sludge were recommended as indicative parameters. The sludge is produced through the particle separation process in soil washing and it is usually treated as a waste. The parameters like water content, organic matter content, CEC (cation exchange capacity) and CFU were recommended as indicative parameters for the low temperature thermal desorption method. Besides the indicative parameter, sampling methods in stock pile and the optimal minimum amount of composite soil sample were proposed. The rates of sampling error in regular grid, zigzag, four bearing, random grid methods were 17.3%, 17.6%, 17.2% and 16.5% respectively. The random grid method showed the minimum sampling error among the 4 kinds of sampling methods although the differences in sampling errors were very little. Therefore the random grid method was recommended as an appropriate sampling method in stock pile. It was not possible to propose a value of optimal minimum amount of composite soil sample based on the real analytical data due to the dynamic variation of $CV_{fund{\cdot}error}$. Instead of this, 355 g of soil was recommended for the optimal minimum amount of composite soil sample under the assumption of ISO 10381-8.

Fluorimetric Determination of Phosphate in Sea Water by Flow Injection Analysis

  • Motomizu, Shoji;Oshima, Mitsuko;Katsumura, Naoya
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.843-848
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    • 1995
  • A sensitive method for the determination of trace amounts of phosphate by fluorescence-quenching detection / FIA is proposed. The fluorescence of Rhodamine B(RB) was quenched with the formation of the ion associate of molybdophosphate with RB;${\lambda}_{ex}$ and ${\lambda}_{em}$ were 560nm and 580nm, respectively. A calibration graph was linear over the ranges from $10^{-8}$ to $3{\times}10^{-6}M$ of phosphate (~0.3~93ppb of phosphorus). The relative standard deviation was 1.2% with $8{\times}10^{-7}M$ phosphate solution and sampling rate was 15 samples / h. The proposed method was applied to the determination of phosphate in sea and river water samples.

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Quality Control(QC) Analysis of Ambient VOCs in Canisters Using GC/MSD Method (Canister와 GC/MSD를 이용한 대기 중 VOCs 분석시스템의 정도관리(QC))

  • Jeon, Jun-Min;Hur, Dang;Kim, Dong-Sool
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.6
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    • pp.527-538
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    • 2002
  • In this study, the performance of sampling and of analytical methodology was examined against a number of selected volatile organic compounds (VOCs) in the ambient air. The canister-based sampling method for VOCs has been a viable and widely used approach that is based on research and evaluation performed over the past several years. VOCs were determined using canisters by GCMSD analysis. A total of target analyses in this study included approximately 30 VOCs designated in TO-l4A categories including BTEX. The methodology for QC(quality control) was intensively investigated with a wide range of performance criteria such as; (1) cleanliness of canisters, (2) reproducibility of diluter, (3) instrumental detection limits of preconcentrator and GCMSD, and (4) precision and accuracy of GCMSD. For most of the compounds tested, precision was less than $\pm$5%, IDL was 0.2 ppbv, accuracy was $\pm$5%, respectively. This study demonstrated that the combination of canister sampling and GC/MSD analysis could be reliably applied to the measurements of BTEX in ppbv levels that are typically observed in/outdoor air environment.

A solid-state NMR study on the activity of an antimicrobial peptide, magainin 2 (항균성 펩타이드인 magainin 2의 활성에 대한 고체 핵자기 공명 분광 연구)

  • Kim, Chul
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.460-466
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    • 2011
  • The activity of an antimicrobial peptide, magainin 2, on lipid membranes was investigated using solid-state NMR and a new sampling method that employed mechanically aligned bilayers between thin glass plates. The experiments were performed at two hydration levels. At 95% hydration about 15% of the lipid bilayers were disrupted and at full hydration 20% were disrupted. From the comparison of two equilibrium states established by two sampling methods the importance of peptide binding to the lipid bilayer for whole membrane disruption was demonstrated.

Measurement Uncertainty of Methane Concentrations from a Rice Paddy Measured by a Closed Automated Chamber System (벼논에서 폐쇄형 자동 챔버 시스템으로 측정한 메탄 농도에 대한 요인별 측정 불확도 비교)

  • Ju, Ok Jung;Kang, Namgoo;Lim, Gap June
    • Korean Journal of Environmental Agriculture
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    • v.39 no.3
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    • pp.228-236
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    • 2020
  • BACKGROUND: The closed chamber method is the most commonly used for measuring greenhouse gas emissions from rice fields. This method has the advantages of being simple, easily available and economical. However, a measurement result using the chamber method is an estimated value and is complete when the uncertainty is estimated. The methane emissions from a rice paddy account for the largest portion of the greenhouse gas emissions in the agriculture sectors. Although assessment of uncertainty components affecting methane emission from a rice paddy is necessary to take account of dispersion characteristics, research on these uncertainty components is very rare to date. The goal of this study was to elucidate influencing factors on measurement uncertainty of methane concentrations measured by a closed automated chamber system from a rice paddy. METHODS AND RESULTS: The methane sampling system is located in the rice paddy in Gyeonggi-do Agricultural Research and Extension Services (37°13'15"N, 127°02'22"E). The primary measurement uncertainty components influencing methane concentrations (influencing factors) investigated in this research were repeatability, reproducibility and calibration in the aspects of methane sampling and analytical instrumentation. The magnitudes of the relative standard uncertainty of each influencing factor were quantified and compared. CONCLUSION: Results of this study showed what influencing factors were more important in determination of methane concentrations measured using the chamber system and analytical instrumentation located in the monitoring site. Quantifying the measurement uncertainty of the methane concentrations in this study would contribute to improving measurement quality of methane fluxes.

A Study of Sap Analysis for the Establishment of Nutrient Diagnosis Method (온실멜론의 양액재배에 있어서 영양진단법 확립을 위한 즙액분석)

  • 장홍기;정순주
    • Journal of Bio-Environment Control
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    • v.6 no.4
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    • pp.310-316
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    • 1997
  • This experiments comparisons were conducted to establish the effective sap analytical method including quantitative analysis of nitrate and phosphorous, sap extraction method, extraction rate, macerating time and sampling position. Earl's Favorite muskmelon was sown on February 11th, 1993 and transplanted to rockwool slab when three to fourth true leaf appeared. Non-circulating system was employed in this experiment. Sap testing using a sample provides an immediate analysis of nutritional status of the crop and potential problems can be recognized and corrective measures taken. Some methods were recommended UV-spectroscopy for the analysis of nitrate nitrogen, Vanad molybdenium acid method for phosphorous. Optimal extraction rate of sample to water was determined as one to four and the best result observed at 60seconds in macerating duration. Further trials would be requested about sampling time due to the difference according to the sampling time. Given sampling position was favorable for the sap analysis.

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