• Title/Summary/Keyword: MDL

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Analysis of Volatile Organic Compounds in Sediments Using HS-GC/MS - Confirmation of Matrix Effects in External and Internal Standard Methods - (HS-GC/MS를 이용한 퇴적물 중 휘발성유기화합물 분석 - 외부 및 내부표준방법에서 매질영향 확인 -)

  • Shin, Myoung-Chul;Jung, Da-som;Noh, Hye-ran;Yu, Soon-ju;Seo, Yong-Chan;Lee, Bo-Mi
    • Journal of Korean Society on Water Environment
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    • v.37 no.6
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    • pp.510-519
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    • 2021
  • Volatile Organic Compounds (VOCs) in sediments, which can cause human health problems, have been monitored in Korea since 2014. Measured VOC concentrations can be affected by matrix type and the volatility of target substances. In this study, (1) VOCs volatility and the influence of matrix interference were confirmed, and (2) internal standards (IS) method was applied to improve analytical method. For these purposes, method detection limit (MDL), calibration linearity, precision and accuracy of VOCs were compared in various matrices using the IS. Some of VOCs in sediments showed different peak areas and reduced rates compared to water matrix. It was suggested that adsorption properties of sediments hindered the migration to vapor during heat pretreatment in headspace method. A calibration curve was created in clean sand. Recovery rates for the calibration curve method and IS applying method were 64.1~83.1% and 99.1~119.3%, respectively. Relative standard deviations ranged from 11.1% to 21.6% for the calibration curve method and those for IS ranged 4.7% to 13.7%. In case of real sediment, calibration curve and 1,2-Dichlorobenzene-d4 (ODCB) among IS were not suitable. The average recovery rate of Fluorobenzene (FBZ) increased by 56.4% and Relative Standard Deviation (RSD) by 4.7%. However, the recovery rate was increased in the samples with large values of igniting intensity. This study confirmed that influence of the matrix of VOCs in sediment, and addition of IS materials improved precision and accuracy. Although IS corrects volatilization and adsorption, it is recommended that more than two types of IS should be added rather than single.

Study on establishment of emission cell test method for liquid phase building materials (방출셀을 이용한 액상건축자재 오염물질 방출시험방법 정립에 관한 연구)

  • Lim, Jungyun;Jang, Seongki;Seo, Sooyun
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.191-200
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    • 2009
  • The aim of this study was to evaluate and establish of emission test method for liquid phase building materials such as paint, adhesive, sealant by emission cell. A small-scale emission chamber and emission cell were used to evaluate emission of TVOC from paint, adhesive, sealant. The quantity of TVOC emission were measured by a gas chromatography/mass spectrometry (GC/MS). Background concentration of TVOC was below $10{\mu}g/m^3$ in the emission chamber and cell. Air tightness and recovery in chamber and cell showed good results. The recovery of thermal desorber for toluene and n-dodecane were about 120%. The repeatability of response factor and retention time in GC/MS below 30%. The method detection limit of VOCs ranged 0.04~8.82 ng. The concentration of TVOC emission using emission cell was 1.35~1.41 times higher than emission chamber. The correlation of TVOC emission using chamber and cell method was significantly high (r=0.91~0.97).

Analysis of mercury and methylmercury in river sediment samples (하천퇴적물 중의 수은 및 메틸수은 분석 연구)

  • Lee, Jung-Sub;Park, Jae-Sung;Kang, Hak-Gu;Cho, Jae-Seok;Hong, Eun-Jin;Jeong, Gi-Taeg;Cha, Jun-Seok;Jung, Kwang-Yong;Kim, Young-Hee
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.44-50
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    • 2009
  • In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

Development of an analytical method of organochlorine pesticides in human bloods using head space-solid phase microextraction coupled with gas chromatography/mass spectrometry (HS SPME-GC/MS를 이용한 혈액 중 유기염소계 농약의 분석법 개발)

  • Kang, Tae-Woo;Pyo, Hee-Soo;Hong, Jong-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.259-271
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    • 2008
  • The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with $85{\mu}m$, adsorption time was for 5 min, adsorption optimum temperature was at $280^{\circ}C$, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs.

Trends and Prospects of N. Korea Military Provocations After the Sinking of ROKS Cheon-an (천안함 폭침 이후 북한의 군사도발 양상과 전망)

  • Kim, Sung-Man
    • Strategy21
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    • s.34
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    • pp.58-92
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    • 2014
  • Even after S. Korea took 5.24 Measure(24 May 2014), N. Korea has not stopped raising provocations such as the shelling of Yeonpyeong Island, electronic and cyber attacks. To make matters worse, the communist country lunched long-range missiles(twice) and conducted 3rd nuclear test, escalating tensions which could possibly lead to an all-out war. Korean Government failed to respond properly. However, escalation into an all-out war was deterred by the CFC immediately carrying out its peacetime duty(CODA). The US made a rapid dispatch of its augmentation forces(Aircraft carrier, nuclear-powered submarine, strategic bomber, F-22) to the Korean Peninsula. In recognition of the importance of the Combined Forces Command, since May 2013 the Park Geun-Hye Administration has been pushing ahead with re-postponement of Wartime Operational Control Transfer(which initially meant the disassembling of the CFC as of 1 December 2015) More recently, there has been a series of unusual indicators from the North. Judging from its inventory of 20 nuclear weapons, 1,000 ballistic missiles and biochemical weapons, it is safe to say that N. Korea has gained at least war deterrence against S. Korea. Normally a nation with nuclear weapons shrink its size of conventional forces, but the North is pursuing the opposite, rather increasing them. In addition, there was a change of war plan by N. Korea in 2010, changing 'Conquering the Korean Peninsula' to 'Negotiation after the seizure of the Greater Seoul Metropolitan Area(GSMA)' and establishing detailed plans for wartime projects. The change reflects the chain reaction in which requests from pro-north groups within the South will lead to the proclamation of war. Kim, Jeong-Un, leader of N. Korean regime, sent threatening messages using words such as 'exercising a nuclear preemptive strike right' and 'burning of Seoul'. Nam, Jae-June, Director of National Intelligence Service, stated that Kim, Jung-Un is throwing big talks, saying communization of the entire Korean Peninsula will come within the time frame of 3 years. Kim, Gwan-Jin, Defense Minister, shared an alarming message that there is a high possibility that the North will raise local provocations or a full-fledged war whenever while putting much emphasis on defense posture. As for the response concept of the Korean Government, it has been decided that 'ROK·US Combined Local Provocation Counter-Measure' will be adopted to act against local provocations from the North. Major provocation types include ▲ violation of the Northern Limit Line(NLL) with mobilization of military ships ▲ artillery provocations on Northwestern Islands ▲ low altitude airborne intrusion ▲ rear infiltration of SOF ▲ local conflicts within the Military Demarcation Line(MDL) ▲ attacking friendly ships by submarines. Counter-measures currently established by the US involves the support from USFK and USFJ. In order to keep the sworn promise, the US is reinforcing both USFK and USFJ. An all-out war situation will be met by 'CFC OPLAN5027' and 'Tailored Expansion Deterrence Forces' with the CFC playing a central role. The US augmentation forces stands at 690,000 troops, some 160 ships, 2,000 aircraft and this comprise 50% of US total forces, which is estimated to be ninefold of Korean forces. The CFC needs to be in center in handling both local provocations and an all-out war situation. However, the combat power of S. Korean conventional forces is approximately around 80% of that of N. Korea, which has been confirmed from comments made by Kim, Gwan-Jin, Defense Minister, during an interpellation session at the National Assembly. This means that S. Korean forces are not much growing. In particular, asymmetric capabilities of the North is posing a serious threat to the South including WMD, cyber warfare forces, SOF, forces targeting 5 Northwestern Islands, sub-surface and amphibious assault forces. The presence of such threats urgently requires immediate complementary efforts. For complementary efforts, the Korean Government should consider ① reinforcement of Korean forces; putting a stoppage to shrinking military, acquisition of adequate defense budget, building a missile defense and military leadership structure validity review, ② implementation of military tasks against the North; disciplinary measures on the sinking of ROKS Cheon-an/shelling of Yeonpyeong Islands, arrangement of inter-Korean military agreements, drawing lessons from studies on the correlation between aid for N. Korea, execution of inter-Korean Summit and provocations from the North, and ③ bolstering the ROK·US alliance; disregarding wartime operational control transfer plan(disassembling of CFC) and creation of a combined division.

Comparative Study of the Efficiency of GC with Large Volume Injector and SPE Clean-up Process Applied in QuEChERS Method (GC-대용량 주입장치와 SPE를 적용한 QuEChERS 잔류농약 분석법의 효율성 비교)

  • Park, Young Jun;Hong, Su Myeong;Kim, Taek Kyum;Kwon, Hye Young;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.19 no.4
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    • pp.370-393
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    • 2015
  • This study was conducted to compare STQ method, multi-residue method in Korean food code and QuEChERS method for validated selected and accuracy, reproducibility and efficiency. A total of 45 selected and targeted pesticides were the analyzed by GC and 5 of them were crops (apple, potato, green pepper, rice, soy bean). $R^2$ values were calculated in the standard calibration curve was over 0.990. Recovery tests were performed by three replications in two levels and the relative standard deviation of the repeated experiments was less than 30%. The average percentage of recoveries in the multi-residue method in Korean food code was 89.13%, QuEChERS method was 92.45% and STQ method was 85.28%. In addition, matrix effects in multi-residue method in Korean food code was 24.61%, QuEChERS method was 23.98% and STQ method showed 11.24%. The STQ method is easy and showed high clean-up effect in extracting the sample solution than the QuEChERS method and clean-up with C18, PLS, PSA cartridge columns. A large volume of the sample was injected in order to compensable for the problem, that occurred due to high detection limit in the analyser. When the STQ method was applied using a large volume injector, the standard calibration curve showed a higher linearity $R^2=0.990$, and method detection limit was 0.01 mg/kg. It showed an average recovery of 91.84% and the relative standard deviations of three replications repeated in two level process was less than 30% and had an average matrix effect of 17.90%.

A comparative analysis of gas and liquid phase standard spiked solid sorbent tubes for the determination of volatile organic compounds in indoor air by TD-GC/MS (열탈착/저온농축-GC/MS에 의한 실내공기 중 휘발성 유기화합물 정량용 기체상 및 액체상 표준물질 첨가한 고체 흡착관의 비교 분석)

  • Lim, Hyun-Woo;Jung, Sung-Won;Kang, Chul-Ho;Park, Jin-Sook;Park, Byeong Moo;Choi, Yong-Wook
    • Analytical Science and Technology
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    • v.26 no.4
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    • pp.287-297
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    • 2013
  • The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

A Study on the Water Quality of Reservoir Tank in the Building Complex on Jeonnam Area (대형건축물 저수조의 수질실태 및 개선방안에 관한 연구)

  • Lee, J.H.;Lee, H.H.;Kim, H.B.;Ahn, G.W.;Park, K.N.;Kim, Y.K.;Bae, J.S.;Mun, H.;Park, C.U.;Oh, E.H.;Park, S.I.;Seo, Y.G.
    • Journal of environmental and Sanitary engineering
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    • v.15 no.4
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    • pp.59-77
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    • 2000
  • This study was carried out to investigate on several factors, which contaminative the water quality through the water pipe during feeding water, in 42 largescaled apart-ments(total 84 cases) and assayed the Volatile Organic Compounds(VOCs) and concen-tration of heavy metals that inflow and outflow in reservior water in Jeonnam area(Mokpo, Suncheon, Yeosu) from January 1999 to December 1999. The results obtained were summarized as follows ; 1. The quality of the water pipe composition in the order of frequency in the quality of water pipes were Copper(45.2%)> Zinc(38.9%)> Stainless steel(9.5%)> PVC(4.8%)> PM(2.4%) in observing 42 sites. All of the drain pipes were used the cast iron quality. 2. The result of certification curve from 12 items(17kind) of VOCs was $1.0-4.0{\mu{g}}/{\ell}$ range, a coefficient of correlation was shown 0.99 over. A MDL of each substance range was within $0.1-1.0{\mu{g}}/{\ell}$. 3. The result of the assay, 5 kinds(Viny chloride, Dichloromethane, Ethylbenzene, M,P-xylene, Styrene) of the VOCs of 14 kinds was not detected and the other items were detected slightly. The detection rate of one item and over in total VOCs samples, were 25.9% in inflow and 27.9% in outflow. And frequency of detect in inflow/outflow of THM(Chloroform, Bromodichloro-methane, Dibromochloromethane, Bromoform) were shown higher than 94.1%, 97.0% each stages. It comes to the conclusion that all of the samples were reason able for drinking water standards. 4. The coefficient of correlation were reasonable, it shown 0.999 over in $0.1-1.0{\mu{g}}/{\ell}$ of a measuring range conditions of 4kinds in organic substance(Zn, Cu, Fe, Mn). 5. The results were showed suitability in 78 cases(92.9%) and unsuitability in 6 cases (7.1%), in 84 cases of in organic substances. Compare to inflow stage, mean concentrations of heavy metal, were increased slightly in Zn, Cu, Fe except Mn than outflow stage. The result of the mean concentration in organic substance inflow and outflow in the apartment water tank using Pair-compared T-test, in 95% reliance index, were $0.179mg/{\ell}(0.151-0.307mg/{\ell})$ in Zinc, $0.136mg/{\ell}(0.113-0.230mg/{\ell})$ in Copper, $0.052mg/{\ell}(0.048-0.098mg/{\ell})$ in Fe, and there was a bit growing tendency but there was no differece in Mn. 6. The mean concentration of Copper which used Cu pipe as a water supply pipe in apartment were $0.216mg/{\ell}(0.161-0.338mg/{\ell})$ in case of the Zine pipe were $0.286mg/{\ell}(0.204-0.435mg/{\ell})$. It shows that the detection rate was more higher than the other material used in Cu or Zn as the water supply pipe. We supposed to Cu and Zn substance were gushing out water supply pipe.

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Monitoring of Pesticides in the Yeongsan and Seomjin River Basin (영산강 및 섬진강 수계 중 농약 분포 조사)

  • Lee, Young-Jun;Choi, Jeong-Heui;Kim, Sang Don;Jung, Hee-Jung;Lee, Hyung-Jin;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.274-281
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    • 2015
  • BACKGROUND: A lasting release of low levels of persistence chemicals including pesticides and pharmaceuticals into river has a bad influence on aquatic ecosystems and humans. The present study monitored pesticide residues in the Yeongsan and Seomjin river basins and their tributaries as a fundamental study for water quality standard of pesticides.METHODS AND RESULTS: Nine pesticides(aldicarb, carbaryl, carbofuran, chlorpyrifos, 2,4-D, MCPA, methomyl, metolachlor, and molinate) were determined from water samples using SPE-Oasis HLB(pH 2) and LC/MS/MS. Validation of the method was conducted through matrix-matched internal calibration curve, method detection limit(MDL), limit of quantification(LOQ), accuracy, precision, and recovery. MDLs of all pesticides satisfied the GV/10 values. Linearity(r2) was 0.9965- 0.9999, and a percentage of accuracy, precision, and recovery was 89.4-113.6%, 3.1-14.0%, and 90.8-106.2%, respectively. All pesticides exclusive of aldicarb were determined in the river samples, and there was a connection between the positive monitoring results and agricultural use of the pesticides.CONCLUSION: Monitoring outcomes of the present study implied that pesticides were a possible non-point pollutant source in the Yeongsan and Seomjin river basins and tributaries. Therefore, it is required to produce and accumulate more monitoring results on pesticides in river waters to set water quality standards, finally to preserve aquatic ecosystems.