• Title/Summary/Keyword: 잔류분석

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Residue Analysis of Quinclorac in Soil by Supercritical Fluid Extraction and Fluorogenic Derivatization Coupled with High Performance Liquid Chromatography (초임계추출과 형광유도체를 이용한 HPLC 에서의 Quinclorac 의 토양중 잔류분석)

  • Kim, Yong-Whan
    • Applied Biological Chemistry
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    • v.40 no.5
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    • pp.442-446
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    • 1997
  • A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

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A Study on the Neoasozine Residues in Rice Grain by Neutron Activation Method (방사화(放射化) 분석법(分析法)에 의한 미곡(米穀)중 네오아소진 잔류분(殘留分)에 관한 연구(硏究))

  • Kim, Yong-Hwa;Lee, Koon-Ja;Lee, Su-Rae
    • Korean Journal of Food Science and Technology
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    • v.13 no.1
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    • pp.20-24
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    • 1981
  • Residues of neoasozine in rice grain were determined by neutron activation and colorimetric techniques. Twice application of the chemical before flowering did not lead to any increased residue level while 4-times application resulted in significant increase in the residue level up to 0.54-0.75 mg $As_2O_3/kg$. The partition ratio of arsenic residues into polished rice grain and bran was 73 : 27 in 100% polishing while most of the residues in the bran was transferred to oil cake fraction during solvent extraction, reaching up to 2.9 mg $As_2O_3/kg$. The neutron activation technique was advantageous because of its high sensitivity and the smaller sample amounts required for analysis.

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Residual stress control in sputter-deposited molybdenum and tungsten thin films (스퍼터링법으로 증착된 몰리브네늄 박막 및 텅스텐 박막의 잔류 응력 제어)

  • Choe, Du-Ho
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.49.2-49.2
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    • 2018
  • 스퍼터링에 의해 증착된 박막 내 기계적 응력 발생 현상을 규명하기 위하여 활발한 이론적, 실험적 접근이 있었으나, 복잡한 플라즈마 증착환경 내에서 다양한 증착 파라미터로 인해 정확한 응력 발생 메커니즘에 대해 아직도 완벽한 규명이 되지 않은 상황이다. 본 연구에서는 몰리브데늄 (Mo)과 텅스텐 (W) 박막을 마그네트론 스퍼터링법을 이용하여 증착 시 발생하는 잔류응력 발생 현상에 대해 논의하겠다. Mo 박막의 경우 증착압력을 2.5 mTorr와 4.1 mTorr로 고정시킨 채 기판 바이어스를 0-250 V 간격으로 변화시킨 결과, 2.5 mTorr에서는 기판바이어스가 증가할수록 압축응력이 증가하는 반면 4.1 mTorr에서는 기판바이어스가 증가할수록 인장응력이 증가하는 것이 확인되었다. 이러한 반대 경향의 잔류응력을 발생시키는 기판 바이어스 효과를 확인하기 위하여 증착 파라미터 변경에 따른 박막 성장 거동 모델을 제시한다. W 박막은 준안정상인 ${\beta}$-상이 증착 초기(2.5 nm)에 형성이 되고, 증착 과정에서 열역학적 안정상인 ${\alpha}$-상으로 상변태 하였다. 상변태에 의한 부피 변화에 따른 잔류응력 발생의 분석을 위하여 X-ray 회절피크의 비대칭성을 분석한 결과 압축응력과 인장응력이 공존하고 있는 것으로 확인되었다. 본 연구결과는 스퍼터링 공정 시 높은 에너지를 가지는 중성화된 Ar과 스퍼터된 원자가 기판과 충돌 시 atomic peening effect에 의해 압축응력이 발생한다는 일반적인 이론과 상충되는 결과로서, Mo 및 W 박막 내 잔류응력 제어를 위한 방안을 제시한다.

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Establishment of Analytical Method for Carpropamid in Agricultural Commodities using HPLC-DAD/MS (HPLC-DAD/MS를 이용한 농산물 중 살균제 Carpropamid의 정밀 잔류분석법 확립)

  • Lee, Hyeri;Choi, Hoon;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.185-194
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    • 2015
  • This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

Analysis of Recent Four Years Situation for Pesticide Residues in the GAP Certified Agricultural Products Analyzed by National Agricultural Cooperative Federation (농협에서 실시한 농산물우수관리인증 농산물 대상 농약 잔류량 조사결과의 최근 4년간 현황 분석)

  • Kim, Hyeong-Kook;Choi, Dong-Seon;Kim, Sung-Gu
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.271-282
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    • 2013
  • This is the result of pesticide residue monitoring certified Good Agricultural Practice (GAP) by national agricultural cooperative federation (NACF) from 2009 to 2012. NACF evaluated simultaneously 283 pesticide multi-analysis method with GC (ECD, NPD) and HPLC. 6,590 agricultural products were analyzed in this period. As the results 1) detected 20.27% in 2009, 23.42% in 2010, 28.07% in 2011 and finally 31.75% in 2012, respectively. There was the total detected pesticide residue in the agricultural products. The violated ratio of agricultural products were 2.25% in 2009, 1.82% in 2010, 1.67% in 2011 and 3.47% in 2012, respectively. 13 pesticides went over the maximum residue limits (MRLs); carbendazim was the predominant violation. 40 pesticides; endosulfan was the predominant detected pesticide did not registered respectively crops in Korea. Most agricultural products that were under the MRLs met the safety standard, however agricultural products that contain neither registered nor set up MRL any level for example endosulfan in strawberry. Agricultural products that go over the MRLs with permitted pesticides, for example carbendazim in apple, are rejected. Because of these intricacies continual observation and evaluation will be need during GAP agricultural cultivation.

Determination of Benzimidazole Residues in Livestock Products (축산식품 중 벤지미다졸계 구충제 잔류실태 조사)

  • Lee, Kyung-Jin;Kang, Young-Woon;Kang, Eung-Ui;Kim, Mi-Ran;Bahn, Kyeong-Nyeo;Jang, Young-Mi;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.515-520
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    • 2010
  • This research investigated benzimidazole residues (albendazole, fenbendazole, flubendazole, thiabendazole, oxibendazole) in livestock products. A total of 270 samples of livestock products (beef, pork and chicken) were purchased from local markets in Korea. Ethyl acetate was used to extract analytes from the sample, after which ethyl acetate extracts were purified using a MCX cartridge. Analytes were detected using liquid chromatography-tandem mass spectrometry. The limit of detection was 0.01-0.04 ppb, the limit of quantification was 0.03-0.13 ppb, the linearity ($r^2$) was 0.9992-1.0000, and the recovery was 70-85%. Residues of benzimidazoles, except for fenbendazole in pork, were not found in any of the 270 livestock samples. Fenbendazole was detected in the range of 1.2 to 3.1 ppb in 12 samples of pork.

Studies on the Residues of Chlorinated Organic Insecticides - I. Heptachlor Residues in or on Commercial Vegetables - (유기염소계(有機鹽素系) 살충제(殺蟲劑)의 잔류분(殘留分)에 관(關)한 연구(硏究) - 1. 시판채소중(市販菜蔬中) Heptachlor 잔류분(殘留分)에 관(關)하여 -)

  • Park, Chang-Kyu;Yoo, Jai-Yoon
    • Applied Biological Chemistry
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    • v.15 no.1
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    • pp.7-17
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    • 1972
  • Samples of 13 vegetables were collected, between 14 July and 6 August, 1971, from 15 markets located in 12 different cities and analyzed for Heptachlor residues by gas liquid chromatograph. The residue concentrations of Heptachlor and its epoxide were estimated separately, at a sensitivity level of 0.001 p.p.m., to produce Heptachlor residues on the fresh weight basis. The Heptachlor residues in or on the crops analyzed, including three staple vegetables, potatoe, radish and chinese cabbage, were found fairly low and are far lower than the residue tolerences for respective vegetables recommended jointly by FAO and WHO of the United Nations.

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Analysis of Variability Factors in Establishing Pesticide Residue Limits on Food Crops (농산물중 농약잔류 허용기준 설정시의 변이계수 분석)

  • Lee, Mi-Gyung;Lee, Su-Rae
    • Korean Journal of Food Science and Technology
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    • v.37 no.3
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    • pp.492-497
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    • 2005
  • In establishing legal limits of pesticide residues, various default values are employed to compensate for unavoidable variability in data. Because permissible errors in residue analysis reach ${\pm}30-40%$ RSD, maximum residue limits (MRLs) follow geometric progression. According to 5-yr period JMPR reports, variability factor (ratio of highest to median values) in field residue trials was 3.8-fold in 486 crop-pesticide combinations and round-up effort from highest residue to MRL was 1.5-fold, whereas regulatory margin (ratio of MRL to highest residue) used in Korea was 4.8-fold in 822 crop-pesticide combinations; Korean MRLs will be set at higher levels as compared with Codex limits if these margins are employed. Validation studies to compare and harmonize Korean and Codex MRLs of pesticide residues on food crops should be undertaken.

Evaluation of Metaldehyde Residues on Chinese Cabbage (배추중(中) Metaldehyde의 잔류량평가)

  • Lee, Jae-Young;Kim, Sung-Moon;Han, Dae-Sung
    • Korean Journal of Environmental Agriculture
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    • v.9 no.1
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    • pp.47-52
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    • 1990
  • Metaldehyde Granule (6%) was sprayed 7, 15 and 30 days before harvest at the level of 0.3kg AI/l0a to evaluate metaldehyde residues on the inner and outer part of chinese cabbage. Roots of chinese cabbage were also analyzed. Results were as follows : 1. The amount of free acetaldehyde in chinese cabbage was 0.02-0.18ppm. 2. It was shown that metaldehyde residues in the leaf and root of chinese cabbage increased as the number of treatment increased and treatment period decreased. 3. The metaldehyde residue range in the leaf was in the range of 0.11-1.4ppm 4. The difference of metaldehyde residue on the inner and outer part of chinese cabbage was in the range of 0.01-0.6ppm and the residue on inner parts was slightly higher than outer part. 5. The metaldehyde residue in the root was in the range of 0.04-0.63ppm.

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Residual Stress Comparison of Type III Hydrogen Tank by Curing Conditions (Type III 수소탱크 경화조건에 따른 잔류응력 비교)

  • Yong-Chul Shin
    • Composites Research
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    • v.37 no.1
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    • pp.15-20
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    • 2024
  • Since the residual stress of hydrogen tank is directly related to durability, it is very important to reduce it for safety. Type II~IV hydrogen tank are manufactured by the filament winding method, in which the fiber is impregnated with resin and wound around the liner. Residual stress in composite is affected by curing conditions and fiber tension etc. In this study, the effect of curing conditions on residual stress was analyzed when manufacturing a Type III hydrogen tank using carbon fiber filament winding process. First, the curing behavior of the epoxy resin was analyzed using a differential scanning calorimetry. Through this, the curing temperature was set to 140℃. During the same curing time, the specimens were cured under 2-stage curing condition that reached 140℃ earlier and a 4-stage curing condition that reached 140℃ later, respectively. After curing, the residual stress of the composite material was measured by the ring slitting method, and the experimental values were compared with numerical values. It was confirmed that there was a significant difference in residual stress according to the optimization of curing conditions.