• Title/Summary/Keyword: 크로마토그래피

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A Study of Conservation and Desalination Methods for an Iron Stele of the Joseon Dynasty (조선시대 철비(鐵碑)의 보존처리와 탈염방법 비교 연구)

  • Lee, Hye-Youn;Cho, Nam-Chul
    • Journal of Conservation Science
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    • v.25 no.4
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    • pp.399-409
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    • 2009
  • Outdoor iron artefacts are easily corroded by affection of environmental pollutants directly. Especially they need to be removed $Cl^-$ ions, but outdoor iron artefacts are excluded for desalination owing to their special features. Therefore this study contains the conservation processes of an iron stele of the Joseon Dynasty as the sample as well as desalination experiments that were carried out the desalting method using spill pads and the immersion desalting method together in order to compare. Desalting methods were compared by analyses such as an optical and metallurgical microscope, SEM-EDS, pH meter, Ion Chromatography and X-ray diffraction. As a result of the analysis, the optical and metallurgical microscopy show that the corrosion products are constituted by the layers and the metallurgical microstructure is a white cast iron. The SEM-EDS results of corrosion products detected mainly Fe, O, and especially Cl upto 2.48wt%. The results of pH and anion analysis for the washing solution, the desalting method using spill pads shows the similar effect to the immersion desalting method. As a result of XRD analysis before and after desalting corrosion products, goethite, magnetite, lepidocrocite and akaganeite are detected before desalting, but akaganeite is not detected after desalting at the desalting methode using spill pads, which indicates to have an effect on desalination. Therefore the results show that the desalting method using spill pads has an effect on desalination similar to the immersing desalting method.

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Material Analysis and Conservation Treatment of Sangryangmun in Jinnamgwan, Yeosu (여수 진남관 상량문의 재질분석 및 보존처리)

  • Imn, Se Yeon;Yu, Ji A;Lee, Jae Sung;Jeong, Hee Won
    • Journal of Conservation Science
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    • v.36 no.3
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    • pp.213-224
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    • 2020
  • This research conducted a component analysis and conservation treatment of "Sangryangmun," a material which had been written in 1965 and was discovered during the repair project for "Jinnamgwan" in Yeosu. The "Sangryangmun" has been stored in a cylindrical metal storage; however, defects, discolorations, hardening, and damages caused by pollutants were found. Based on the XRF analysis, rust in the cylindrical metal storage, which was made of Cu, was stuck on the surface of the "Sangryangmun". Using FT-IR and Pyrolysis-GC/MS analyses, carbonyl and compounds of fatty acids were detected; the organic material on the surface of the "Sangryangmun" was identified to have belonged to oil-based components. Therefore, it was presumed that the bast fibers of a mulberry was used in the paper. To determine the conservation materials, component analysis, condition survey, and preliminary test on adhesives were conducted. Moreover, the missing parts and partial linings were filled using mulberry-fiber paper, methyl cellulose, etc.

Pesticide-Originated Persistent Organic Pollutants in Agricultural Waterways in Chungcheong Province, Korea (충청지역 농업용수 중 농약 유래 POPs의 모니터링 연구)

  • Lee, Hwa-Sung;Jeon, Hwang-Ju;Lee, Hoi-Seon;Lee, Sung-Eun
    • Journal of Applied Biological Chemistry
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    • v.58 no.4
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    • pp.291-294
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    • 2015
  • Persistent organic pollutants (POPs) including banned organochlorine pesticides, are found in Korean agricultural environments. Their translocation from agricultural environment to major crops has been reported. In this study, the POPs in 15 different agricultural waters of the Chungchung Province were monitored and all samples were prepared, followed by liquid-liquid fractionation and column chromatography prior to analysis using gas chromatography. Among pesticide-originated persistent organic pollutants, ${\alpha}$-endosulfan was determined in the range of 0.01 to 1.13 ng/mL. ${\beta}$-Endosulfan was determined in the range of 0.01 to 0.55 ng/mL, and endosulfan sulfate was ranged from 0.13 to 1.13 ng/mL. The total sum of endosulfans reached the range of 0.38 to 1.18 ng/mL. Three pesticides being used currently were also found in samples as 2.03-2.05 ng/mL for triadimefon, 0.26-0.33 ng/mL for tolyfluanid, and 1.34-3.85 ng/mL for chlorpyrifos. Taken together, endosulfans were introduced in the agricultural waters and their fates need continuous monitoring.

Separation Characteristics of Alkali and Alkaline Earth Metal Ions Using Novel HDBPDA Ion Exchanger (새로운 HDBPDA 이온교환체를 사용한 알칼리 및 알칼리 토금속 이온들의 분리특성)

  • Kim, Dong Won;Kim, Chang Suk;Choi, Ki Young;Jeon, Young Shin;Hong, Choon Pyo
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.471-477
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    • 1993
  • The novel macrocylic ligand {(4, 5):(13, 14)-dibenzo-6, 9, 12-trioxa-3, 15, 21, -triazabicyclo [15. 3. 1]heneicosa-(1, 17, 19)(18, 20, 21) triene: HDBPDA} was synthesized, and protonable constants of the ligand and the complex stability constants with alkali metals alkaline earth metals were determined. We evaluated the resolution factor(${\Delta}$) from equation that inducing from stability constants(pK). Also, this ligand was grafted on chloromethylated styrene-divinyl benzene(Merrifield resin) for HDBPDA, ion exchanger. Alkali and alkaline earth metal ions were separated using water by the column chromatography with this ion exchanger. Selectivity(${\alpha}$) and resolution(Rs) of alkali and alkaline earth metal ions were measured from the elution curves chromatogram. The selectivity and resolution values of the various ions calculated from the elution curves were compared with those abtained from pK values. The results were in a good agreement between tow methods. Ion exchange capacity of the resin were determined using the alkali and alkaline earth metal ions and pH dependence of capacity was also discussed.

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Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation (QuEChERS 전처리법과 GC-TOF/MS, ECD, NPD를 이용한 잔류농약 다성분분석)

  • Park, Jungwook;Kim, Aekyung;Kim, Jongpil;Lee, Hyanghee;Park, Duckwoong;Moon, Sujin;Ha, Dongryong;Kim, Eunsun;Seo, Kyewon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.278-295
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    • 2014
  • Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

Determination of Amisulbrom Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.321-329
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    • 2014
  • This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% 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 amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

The Study on the Migration of Sulfite in Commercial Wooden Chopsticks (국내 유통 나무젓가락 중 이산화황 이행량에 관한 연구)

  • Park, Na-Young;Yun, Hae-Jung;Jeon, Dae-Hoon;Choi, Hyun-Cheol;Eom, Mi-Ok;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Hyun-Rock;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.23 no.3
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    • pp.218-221
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    • 2008
  • The levels of sulfites in wooden chopsticks were analyzed using two different methods, distillation-alkali titration and ion chromatography. According to the two methods, Sulfur dioxide($SO_2$) was validated by 0.6 and 0.2 ${\mu}ml$ of limit of detection(LOD), 1.8 and 0.5 ${\mu}ml$ of limit of quantification, (LOQ) and a $R^2>0.998$ for linearity, respectively. The recoveries of $SO_2$ from food simulants spiked ar levels of 100 ppm were 70.2-100.2%. 158 samples of wooden chopsticks were monitored the migrated amounts of sulfites. Sulfites were detected in 30 samples in ranged of 0.6 to 15.5 ppm. Maximum migration level, 15.5 ppm of sulfites was considered giving no harmful effect to human since it was reached 5.5% of estimated SML.

Purification and Characterization of Carotenoprotein from the Muscle of Ascidian, Halocynthia roretzi (우렁쉥이 육으로부터 Carotenoprotein의 분리.정제 및 특성)

  • Kang, Ok-Ju;Byun, Hee-Guk;Jeon, You-Jin;Kim, Jong-Bae;Kim, Se-Kwon
    • Applied Biological Chemistry
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    • v.41 no.1
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    • pp.31-41
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    • 1998
  • A carotenoprotein from the muscle of Ascidian (Halocynthia roretzi) was purified by ion exchange chromatography and gel filtration chromatography, and analyzed molecular weight, stability of pH and heat, effect of denaturing agents, amino acids and fatty acids composition. The purified carotenoprotein had absorption maxima of 463 nm and 439 nm. The carotenoprotein had an approxmimate molecular weight of 64.4 kDa in polyacrylamide gel electrophoresis. The amino acid compositions of carotenoprotein were mainly Gly (15.39%), Asn (11.31%), Gln (10.62%) and Ser (13.35%). The major fatty acids composition of carotenoprotein were $C_{16:1(n-7)}\;(15.4%)$, $C_{22:1(n-9)}\;(14.5%)$ and $C_{20:1(n-11)}\;(11.4%)$. The monounsaturated fatty acids (45.2%) contained abundant content compared to other saturated (38.1%) and polyunsaturated (11.7%) fatty acids.

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A case study on the fire victim in the vehicle by GC/MS through derivatization of cyanide with pentafluorobenzyl bromide (PFBBr) (시안화이온의 pentafluorobenzyl bromide (PFBBr)에 의한 유도체화 후 GC/MS 분석에 의한 차량화재 변사체 사인규명에 관한 사례연구)

  • Lee, Joon-Bae;Shon, Sung Kun;Woo, Sang Hee;Park, Se Yeon;Hwang, Jung Ho;Kwon, O-Seong;Kim, Nam Yi;Paeng, Ki Jung
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.73-78
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    • 2016
  • Hydrogen cyanide (HCN) is an extremely toxic gas frequently produced during the incineration of plastics, such as acrylonitrile-butadiene-styrene (ABS). A victim of a fire who has inhaled smoke could have cyanide in the blood. Therefore, cyanide could be a good marker for a post-mortem examination of a fire as well as carboxyhemoglobine (COHb) test of blood samples. For a particular fire case, a burned body with a suicide note was found inside a burned vehicle. Even though the COHb value is conclusive evidence, measuring the COHb for denatured blood might be difficult due to severe thermal denaturation or the formation of methemoglobin (MetHb). To overcome this difficulty, cyanide could be used as an indicator when investigating the death of a fire victim. In this study, gas chromatography/mass spectrometry (GC/MS) was adopted to measure the levels of cyanide in the blood through derivatization with pentafluorobenzyl bromide (PFBBr) under cation surfactant by scan and SIM mode. The concentration of cyanide in the blood of heart blood and brain of the victim was found to be 0.36 µg/mL and 1.20 µg/mL respectively, which was higher than the average value (0.041 µg/mL) found in the blood of 14 people who smoked.

Effects of reaction conditions on composition of the organic liquid product during the deoxygenation process of palm oil (팜유(Plam Oil)의 탈산소 공정 중 운전 조건이 생성물의 조성에 미치는 영향)

  • Kim, Sungtak;Jang, Jeong Hee;Ahn, Minhwei;Kwak, Yeonsu;Han, Gi Bo;Jeong, Byung Hun;Han, Jeong Sik;Kim, Jae-Kon
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.3
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    • pp.865-875
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    • 2018
  • Selection of optimum reaction conditions during deoxygenation process of palm oil is essential factor to obtain the maximum yield of bio-jet fuel. In this context, the deoxygenation of palm oil was carried out in a fixed bed reactor with an internal diameter of 1 inch loaded with a 1 wt.% $Pt/Al_2O_3$ catalyst. The composition of the organic liquid product(OLP), which can be utilized as a transportation fuel through the upgrading process, was analyzed by a gas chromatography method. The palm oil/hydrogen ratio and hydrogen pressure in the feed affected the decarboxylation(DCB) and hydrodeoxygenation(HDO) reactions, resulting in a change in the composition of the OLP. As the reaction temperature increased, the continuous cracking reaction of the deoxygenation product was promoted and the product composition in the $C_5{\sim}C_{14}$ region was increased. Thus, the results can help to understand the characteristics of deoxidation reaction of palm oil as well as the subsequent process, hydro-upgrading, to obtain the maximum yield of bio-jet fuel.