• Title/Summary/Keyword: 크로마토 그래피 추출

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Analysis and risk assessment of polycyclic aromatic hydrocarbons (PAHs) in seafood from oil contaminated bay (유류 오염지역의 수산물 중 다환방향족탄화수소류 (PAHs) 분석 및 위해평가)

  • Jeong, Ji-Yoon;Choi, Chan-Woong;Ryeom, Tai-Kyung;Cho, Kyoung-Hee;Park, Se-Ryung;Shin, Ho-Sang;Lee, Kwang-Ho;Lee, Hyo-Min
    • Analytical Science and Technology
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    • v.23 no.2
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    • pp.187-195
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    • 2010
  • To assess health risk for the intake among residents after the Hebei Spirit oil spill, 16 Polycyclic Aromatic Hydrocarbons (PAHs) in seafood samples from oil contaminated bay were determined by Gas Chromatography-Mass Spectrometry (GC-MSD) and samples were personally collected and purchased by residents. Samples were hydrolyzed with KOH and extracted with methylene chloride. The extracted solution were cleaned up using silica/florisil column and 16 PAHs were eluted by methylene chloride : n-hexane (1:9) mixture and determined by GC-MSD in Selected Ion Monitoring (SIM) mode. The mean recoveries for 16 PAHs ranged from 79% to 85%. The 16 PAHs levels in 126 samples ranged from 0.17 to $6.04\;{\mu}g$/kg and the TEQBaP (Toxic EQuivalents) levels in 126 samples were calculated using benzo(a)pyrene toxic equivalency factor for individual 16 PAHs and ranged from 0 to $0.91\;{\mu}gTEQ$/kg. The average Benzo(a)pyrene dietary exposure of residents was $5.5{\times}10^{-8}\;mg/kg$ bw/day and the average PAHs chronic dietary exposure was $1.3{\times}10^{-5}\;mg$ TEQ/kg bw/day. The margin of exposure (MOE) and the excess cancer risk and were $1.8{\times}10^6$ and $9.8{\times}10^{-8}$, respectively. Therefore, the assessment result was considered as low concern for health risk.

Anti-hepatotoxic Activity of Chrysanthemum coronarium L. var. spatiosum Extract (쑥갓의 간독성 보호작용)

  • Kang, Hyun-Jung;Lee, Eun-Ju;Sung, Sang-Hyun;Kim, Young-Choong;Song, Eun-Sook;Park, Mi-Jung;Lee, Heum-Sook
    • Korean Journal of Food Science and Technology
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    • v.35 no.1
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    • pp.138-143
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    • 2003
  • Total methanolic extract of Chrysanthemum coronarium L. var. spatiosum (Compositae) was revealed to have anti-hepatotoxic activity against galactosamine-induced toxicity on primary cultured rat hepatocytes. After successive partitioning with chloroform, n-butanol, and water, the chloroform fraction showed a significant inhibition activity of 51% at 50 ppm, compared with that of silybin, 45.9% at $100\;{\mu}M$. The chloroform fraction was subjected to silica gel column chromatography and yielded active CH-II, CH-V and CH-VI subfractions, and the anti-hepatotoxic activity of these subfractions were 47.6, 56.3, and 23.2%, respectively, at 50 ppm. Total glutathione contents of CH-II, CH-V, and CH-VI increased by 49.8, 43.9, and 47.5% of the control, respectively at 50 ppm, whereas that of silymarin was, 59.7% at $100\;{\mu}M$ after challenged with galactosamine. The ratio of (reduced glutathione) / (total glutathione) in CH-II, CH-V and CH-VI subfraction showed similar values of $0.86{\sim}0.87$ at 50 ppm, whereas that of silymarin was, 0.85 at $100\;{\mu}M$. The incorporation of $[^3H]-uridine$ uptake into RNA was not affected by these active subfractions.

Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Development and Validation of an Official Analytical Method for Determination of Ipfencarbazone in Agricultural Products using GC-ECD (GC-ECD를 이용한 농산물 중 Ipfencarbazone의 신규분석법 개발 및 검증)

  • Jang, Jin;Kim, Heejung;Lee, Eun-Hyang;Ko, Ah-Young;Ju, Yunji;Kim, Sooyeon;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.210-217
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    • 2015
  • Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

Determination of Fomesafen Residue in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 fomesafen의 분석)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Nam, Mi-Young;Hong, Seung-Beom;Yun, Won-Kap;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.14 no.2
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    • pp.95-103
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    • 2010
  • Fomesafen is a selective herbicide, and used to control annual and perennial broad-leaf grass on soybean and fruit fields in USA and China, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of fomesafen were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for fomesafen residue in crops using HPLC-UVD/MS. Fomesafen residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover fomesafen from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The fomesafen was quantitated by HPLC with UVD, using a Shiseido CAPCELL-PAK UG C18 column. The crops were fortified with fomesafen at 3 levels per crop. Mean recovery ratio were ranged from 87.5% for a 0.4 ppm in hulled rice to 102.5% for a 0.4 ppm in apple. The coefficients of variation were ranged from 0.6% for a 2.0 ppm in hulled rice to 7.7% for a 0.04 ppm in green pepper. Quantitative limit of fomesafen was 0.04 mg/kg in representative 5 crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fomesafen in agricultural commodities.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

Characterization of Anti-Advanced Glycation End Products (AGEs) and Radical Scavenging Constituents from Ainsliaea acerifolia (단풍취의 최종당화산물 생성 저해 및 라디칼 소거 물질의 동정)

  • Jeong, Gyeng Han;Kim, Tae Hoon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.6
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    • pp.759-764
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    • 2017
  • Reactive oxygen species (ROS) and advanced glycation end products (AGEs) are valuable therapeutic targets for the regulation of diabetic complications. Activity-guided isolation of the ethylacetate (EtOAc)-soluble portion of 70% ethanolic extract from aerial parts of Ainsliaea acerifolia was performed, followed by AGE formation inhibition assay for the characterization of four dicaffeoylquinic acid derivatives of a previously known structure, methyl 3,5-di-O-caffeoyl-epi-quinate (1), 3,5-di-O-caffeoyl-epi-quinic acid (2), 4,5-di-O-caffeoyl-quinic acid (3), and methyl 4,5-di-O-caffeoyl-quinate (4). The structures of these compounds were confirmed by interpretation of nuclear magnetic resonance (NMR, $^1H-$, $^{13}C-NMR$, two-dimensional NMR) and mass spectroscopic data. Among the isolates, the major secondary metabolites, 3,5-di-O-caffeoyl-epi-quinic acid (2) and 4,5-di-O-caffeoyl-quinic acid (3) showed the most potent inhibitory effects against AGE formation with $IC_{50}$ values of $0.6{\pm}0.1{\mu}M$ and $0.4{\pm}0.1{\mu}M$, respectively. Furthermore, all isolated dicaffeoylquinic acid derivatives were evaluated for their radical scavenging activities using 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) radical, and compound 3 exhibited the most potent inhibitory effect in a concentration-dependent manner. This result suggests that the caffeoylquinic acid dimers isolated from A. acerifolia might be beneficial for the prevention of diabetic complications and related diseases.

Silicon thin films and solar cells by HWCVD (열선 화학 기상 증착법에 의한 실리콘 박막 및 태양전지 특성)

  • Kim Sang-Kyun;Lee Jeong Chul;Jeon Sang Won;Lim Chung Hyun;Ahn Sae Jin;Yun Jae Ho;Kim Seok Ki;Song Jinsoo;Park S-J;Yoon Kyung Hoon
    • 한국신재생에너지학회:학술대회논문집
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    • 2005.06a
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    • pp.205-208
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    • 2005
  • 최근 열선 화학 기상 증착법(HWCVD)은 낮은 온도에서 TFT용 Poly Si 중착을 할 수 있다는 점과 실리콘 박막을 빠른 속도로 증착할 수 있다는 점에서 각광을 받고 있다. 본 연구에서는 HWCVD를 이용하여 태양전지를 제조하고 그 특성을 평가하였다. 조건에 따른 실리콘 박막의 특성 변화를 알기 위해 corning glass 및 실리콘 wafer에 다양한 조건에서 단위 박막(intrinsic layer)을 증착하였고 이 결과를 바탕으로 p/i/n 구조의 태양전지를 제조하였다. Ta 열선 온도는 1700-2000도였고 가스 원료인 $SiH_4$와 수소의 비율을 조절하면서 그 영향을 관찰하였다. 태양전지의 경우 p충과 n충은 PECVD로 증착하였으며 단위박막 및 태양전지 i충 증착시 기판과 열선간의 거리는 7cm, 기판 온도는 $200^{\circ}C$$250^{\circ}C$로 고정하였고 작업압력은 30mTorr였다. 단위 박막 특성 평가를 위해 암/광 전도도, SEM, Raman Scattering, FT-IR등을 사용하였으며 태양전지 특성 평가를 위해 I-V 및 Spectral response를 측정하였다. 열선 온도가 증가함에 따라 증착속도 및 결정화 분율은 증가하였다. 특히 비정질에서 결정질로 전이되는 구간은 매우 좁았으며 여러 분석 방법에서 일치되는 결과를 보였다. $SiH_4$ 유량이 늘어날수록 비정질이 결정질로 바뀌는 열선 온도가 증가하였으며 기판 온도가 낮을 경우 또한 결정으로 바뀌는 열선 온도가 증가하였다. 태양전지의 경우 열선 온도가 증가함에 따라 $V_{oc}$ 및 W가 낮아졌으며 $J_{sc}$, 는 증가하는 경향을 보였으며 결정질 비율이 증가하는 것을 관찰할 수 있었다. 이러한 경향은 quantum efficiency 결과에서도 확인할 수 있었다.용을 반복하면서 석재 내부와 외부의 암석 및 결정에 균열과 미세열극 등이 생성되어 석재 자체의 구조적 안정성에 영향을 주고 있다. 따라서 감은사지 석탑은 지리적 환경 차이로 인해 일반적인 환경의 석조물들과는 다른 형태의 풍화양상을 보이고 있어서 풍화양상 및 풍화형태에 대한 정확한 연구와 이해를 바탕으로 보존대책이 마련되어야 한다.되었다. 이런 모든 시편들을 각 탈염방법에 따라 탈염처리한 후 XRD와 SEM-EDS으로 분석한 결과 인철광과 침철광은 어떠한 변화도 보이지 않았고, 다만 적금광으로 동정된 시편만이 잔존하지 않았다. 철기 제작별 $Cl^-$ 이온 추출량과 탈염효과에 대한 비교 실험은 이온 크로마토그래피 분석 결과와 마찬가지로 단조 철제유물이 주조 철제보다 $Cl^-$ 이온을 많이 가지고 있었으며, 탈염 처리 후에는 $Cl^-$ 이온은 전혀 발견되지 않았다. 이상의 결과 $K_2CO_3$와 Sodium 용액은 탈염처리에서 가장 적합한 탈염처리 용액으로 알수가 있었으며 특히 어떠한 탈염 용액으로 유물을 처리한다 해도 철제유물에 생성된 부식물은 제거되지 않는다는 것을 알게 되었다. 따라서 보존처리자는 유물 표면의 부식 상태만을 보고 처리하기 보다는 철기제작물로 고려하여 처리하는 것이 필요하다. 또한 금속에 부식을 야기시키는 $Cl^-$ 이온과 부식물을 완전하게 제거하여 탈염처리를 하는 것이 유물 부식을 최대한 지연시킬 수 있는 것이라 생각된다.TEX>$88\%$)였다.(P=0.063). 결론: 본 연구에서는 MTHFR C/T & T/T 유전자 다형성이 위암의 발생과 그 위치에 대해 관련이 있는 것으로 여겨지고, 흡연력, 음주력과는 관련이 없는 것으로 여겨진다.험이 커지는 경향을 보였으나, 나이 및 병기, 종양의 크기, MD-BED $Gy_{10}$ 등의 예후 인자를 보정한 다변

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Comparison of In Vitro Lipid Deposition and Change of Optical Characteristics on Daily Disposable Lenses (1-day) and 3-days Lenses Over 3 days (3-days lenses와 daily disposable lenses(1-day)의 착용 시간 별 지방 침착량 및 광학적 특성 변화의 비교)

  • Song, Sun Jung;Lee, Su Yeon;Kim, Ki Hong;Chu, Byoung Sun
    • Journal of the Korean Chemical Society
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    • v.64 no.2
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    • pp.67-73
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    • 2020
  • The study aimed to investigate in vitro lipid deposition of oleic acid, oleic acid methyl ester and cholesterol on a daily disposable (1-day lenses) and 3-days lenses over 3 days and changes of optical characteristics is also investigated. Artificial tear solutions were prepared to simulate actual tear compositions. Two types of contact lenses (1-day lenses (Senofilcon A) and 3-days lenses (silicone tripolymer)) were soaked in the artificial tear solutions within an incubator at 37 ℃ with 150 rpm for 8, 16, 24 hours. Lipid deposition (oleic acid, oleic acid methyl ester and cholesterol) were measured using high performance liquid chromatography (HPLC) instrument. In addition, measurements of oxygen transmissibility, light transmittance and observation of lens surface were conducted. The amount of lipid deposition on the 1-day lenses were 127.55 ㎍/lens for Day 1, 302.96 ㎍/lens, for Day 2, and 353.30 ㎍/lens for Day 3. The 3-days lenses were 46.22 ㎍/lens for Day 1, 66.07 ㎍/lens for Day 2, and 67.45 ㎍/lens for Day 3. Oxygen transmissibility were 81×10-9(cm/sec)(ml O2/ml×mmHg)(Baseline) and 48×10-9(cm/sec)(ml O2/ml×mmHg) (Day 3) for the 1-day lenses, it were 13.23×10-9(cm/sec)(ml O2/ml×mmHg)(Baseline) and 9.6×10-9(cm/sec)(ml O2/ml×mmHg) (Day 3) for the 3-days lenses. Transmittance of each lenses were 97.21% (Baseline) and 94.25% (Day 3) for the 1-day lenses, 97.65% (Baseline) and 95.15% (Day 3) for the 3-days lenses. Observation of surface deposition indicated greatest deposition for the 3-days lenses type on Day 3. Lipid deposition for both lens types increased by day and was greater for the 1-day lenses type. Surface deposition appeared to differ as it was greatest for the 3 days lens type, which may suggest other deposits such as protein may be present.

Characterization of Concentrations of Fine Particulate Matter in the Atmosphere of Pohang Area (포항지역 대기 중 초미세먼지(PM$_{2.5}$)의 오염특성평가)

  • Baek, Sung-Ok;Heo, Yoon-Kyeung;Park, Young-Hwa
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.3
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    • pp.302-313
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    • 2008
  • The purposes of this study are to investigate the concentration levels of fine particles, so called PM$_{2.5}$, to identify the affecting sources, and to estimate quantitatively the source contributions of PM$_{2.5}$. Ambient air sampling was seasonally carried out at two sites in Pohang(a residential and an industrial area) during the period of March to December 2003. PM$_{2.5}$ samples were collected by high volume air samplers with a PM$_{10}$ Inlet and an impactor for particle size segregation, and then determined by gravimetric method. The chemical species associated with PM$_{2.5}$ were analyzed by inductively coupled plasma spectrophotometery(ICP) and ion chromatography(IC). The results showed that the most significant season for PM$_{2.5}$ mass concentrations appeared to be spring, followed by winter, fall, and summer. The annual mean concentrations of PM$_{2.5}$ were 36.6 $\mu$g/m$^3$ in the industrial and 30.6 $\mu$g/m$^3$ in the residential area, respectively. The major components associated with PM$_{2.5}$ were the secondary aerosols such as nitrates and sulfates, which were respectively 4.2 and 8.6 $\mu$g/m$^3$ in the industrial area and 3.7 and 6.9 $\mu$g/m$^3$ in the residential area. The concentrations of chemical component in relation to natural emission sources such as Al, Ca, Mg, K were generally higher at both sampling sites than other sources. However, the concentrations of Fe, Mn, Cr in the industrial area were higher than those in the residential area. Based on the principal component analysis and stepwise multiple linear regression analysis for both areas, it was found that soil/road dust and secondary aerosols are the most significant factors affecting the variations of PM$_{2.5}$ in the ambient air of Pohang. The source apportionments of PM$_{2.5}$ were conducted by chemical mass balance(CMB) modeling. The contributions of PM$_{2.5}$ emission sources were estimated using the CMB8.0 receptor model, resulting that soil/road dust was the major contributor to PM$_{2.5}$, followed by secondary aerosols, vehicle emissions, marine aerosols, metallurgy industry. Finally, the application and its limitations of chemical mass balance modeling for PM$_{2.5}$ was discussed.