• Title/Summary/Keyword: 잔류분 분석

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A Study on Removal Effect of Residual Pesticide on Adsorbent (흡착제에 의한 잔류농약 제거효과에 관한 연구)

  • An, Jung-hyeok;Kim, Joon-bum;Kwon, Young-du;Jeon, Choong;Park, Kwang-ha
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.537-544
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    • 2007
  • This study was carried out to investigate adsorption characteristics of residual pesticides on an adsorbent. $Bauxsol^{TM}$ and mackban-stone as adsorbent were used. Analytical method for residual pesticides was established by GC/NPD and $GC/{\mu}ECD$. Pesticides used in this study were ${\alpha}$-endosulfan, ${\beta}$-endosulfan, pendimethalin and chlorpyrifos-methyl, fenitrothion, and recovery rates were more than 97%. Adsorption rate on an adsorbent was decreased in order of endosulfan, chlorpyrifos-methyl, pendimethalin, fenitrothion. Organochlorine pesticides showed higher removal rate than the other pesticides. $Bauxsol^{TM}$ gave both chemical decomposition and physical adsorption. Mackban-stone gave only physical adsorption on the other hand. The high pH and chloric ions structure of eluted solution have greatly affected at chemical resolution. The removal rate of pesticides was increased due to the physical property of adsorbent, i.e. high porosity. The above adsorbent is to be a candidate to remove residual pesticides in water and pond of links.

Gas desorption species and quantity from the hot cathode ionization gauges (열음극 전리 진공게이지의 기체이탈 특성)

  • ;;;I. Arakawa
    • Journal of the Korean Vacuum Society
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    • v.12 no.4
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    • pp.201-206
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    • 2003
  • A residual gas analyzer was used to study the outgassing behavior of stainless steel 304 chamber as a function of bake-out temperature up to $235 ^{\circ}C$ and to identify the gas species evolved during turn on and degassing of the three different types of hot cathode ionization gauges. It was found that $H_2O$, CO, and $H_2O$ were the dominent outgassing species in the vacuum chamber during bake-out but finally $H_2$ and CO(mass 28) persisted at room temperature. Dominant outgassing species were also $H_2$ and $H_2O$ while fuming on the ionizations and then $H_2$,$H_2O$ and CO were found to be the main species degassed gauges. It was appeared that the outgassing species and quantity were not agreed to the three different types of hot cathode ionization gauges.

Determination of Ethylenethiourea in Fruits (과실류에 잔류하는 Ethylenethiourea 분석)

  • Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
    • Korean Journal of Food Science and Technology
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    • v.43 no.3
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    • pp.277-281
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    • 2011
  • A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.

Monitoring and Risk Assessment of Pesticide Residues for Circulated Agricultural Commodities in Korea-2013 (국내 유통 농산물의 잔류농약 모니터링 및 위해평가-2013년)

  • Kim, Jae-Young;Lee, Sang-Mok;Lee, Han-Jin;Chang, Moon-Ik;Kang, Nam-Sook;Kim, Nam-Sun;Kim, Heejung;Cho, Yoon-Jae;Jeong, Jiyoon;Kim, Mee Kyung;Rhee, Gyu-Seek
    • Journal of Applied Biological Chemistry
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    • v.57 no.3
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    • pp.235-242
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    • 2014
  • The purpose of this study is the establishment of scientific processes for making food safety policies. Thus, we investigated pesticide residue level of the agricultural commodities from market, and performed risk assessment. Fifteen agricultural items are chosen based on the frequency of Korean consumption. The samples were collected from 9 cities where populations are more than one million. Total 283 active ingredients were monitoring ( total sample number =232). Single-analysis of target pesticides was for three kinds of possible growth regulators and the multicomponent analysis was for 280 kinds of pesticides, a total of 283 species were selected to perform the pesticide residues. Before monitoring the analytes, the improvements of the analytical methods were done by method validations under the CODEX analytical method development guidelines and can produce metrics that represent the international standards applied in accordance with the guidelines. In addition to residual pesticides detected during monitoring we compare the ADI to EDI values using detected result and dietary consumption data which is extracted from annual market basket survey. The 163 samples were non-detected in the total 232 samples so it means that every agricultural commodity will residual pesticides-free in 70.3%. The detected residual pesticides showed for a total of 69 cases (29.7%). Two of samples violate Korean MRL (0.9%). The ratio of EDI compared to ADI resulted in only from 0.00087 to 0.902%. In result, we can assume that all detected residual pesticides are very safe level and current policies of Korean pesticides control may be working.

Determination of Methoxyfenozide, Chromafenozide and Tebufenozide Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 작물 중 methoxyfenozide, chromafenozide 및 tebufenozide의 분석법 확립)

  • Lee, Su-Jin;Kim, Young-Hak;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jeong-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.14 no.1
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    • pp.37-48
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    • 2010
  • The diacylhydrazine insecticides, methoxyfenozide, chromafenozide and tebufenozide are new-generation insecticides. These insecticides induce premature molting and cause the death of insects by mimicking their hormone. Also, these insecticides have already been widely used for vegetables planting in worldwide. Highperformance liquid chromatography (HPLC) is the most widely used procedure for determination of each compound residues in crops. However, simultaneous analysis method of these diacylhydrazine insecticides was not reported. The purpose of this study is to develop a simultaneous determination procedure of methoxyfenozide, chromafenozide and tebufenozide residue in crops using HPLC-UVD/MS method. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were quantitated by HPLCUVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at two levels per crop. Mean recoveries ranged from 89.0 to 104.8% in five representative agricultural commodities. The coefficients of variation were less than 3.9%. Quantitative limits of methoxyfenozide, chromafenozide and tebufenozide were 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of methoxyfenozide, chromafenozide and tebufenozide in agricultural commodities.

A study on removal effect of Endosulfan in soil and aquatic system (수질 및 토양 중 Endosulfan 제거효과에 관한 연구)

  • An, Jung-Hyeok;Lee, Seog-Jong;Lee, Woan;Kim, Joon-Bum;Lee, Gwang-Chun;Kwon, Young-Du;Jeon, Choong;Park, Kwang-Ha
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.155-162
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    • 2006
  • In this study, a series of experiments were conducted using a standard solution containing ${\alpha}$ and ${\beta}$-endosulfan to follow the removal effect of residual pesticides on soil and aqueous solution. An analytical method for residual pesticides was established by a gas chromatography equipped Ultra II[$(30m{\times}0.25mm(ID){\times}0.25{\mu}m$] capillary column and a ${\mu}$-electron capture detector(${\mu}$-ECD). Recovery rates of residual pesticides for soil samples were 96-100%. The amount of ${\alpha}$ and ${\beta}$-endosulfan that was spread in the soil was checked for various period of time. It indicated that the amount was reduced to 73 and 61%, respectively. When the water spread amount increased from 10 to 100 mL, ${\alpha}$-endosulfan was eliminated from 45 to 85% and while ${\beta}$-endosulfan from 44 to 88%. Removal rates of ${\alpha}$-endosulfan and ${\beta}$-endosulfan were 99% and 98% respectively within 30 minutes. It was assumed that the organic salts and strong alkali elements contained in the pesticide degradator hydrolyzed the residual pesticide.

Development of Analytical Method for Fenoxanil in Agricultural Products Using GC-NPD and GC/MS (농산물 중 Fenoxanil 잔류성 시험법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.4
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    • pp.345-353
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    • 2015
  • The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.

Development of Analytical methods for Chinomethionat in Livestock Products (축산물 중 살균제 Chinomethionat의 개별 잔류분석법 확립)

  • Yang, Seung-Hyun;Kim, Jeong-Han;Choi, Hoon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.134-141
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    • 2021
  • BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r2>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

The Effect of the Hydrophobicity of Silicon Surface on the Formation of the Water Marks during HF-last Wet Chemical Processing (반도체 습식 HF 최종 공정 중 실리콘 표면의 소수성이 Water Mark형성에 미치는 영향)

  • Han, Jeong-Hun;Kim, Sung-Hwan;Park, Jin-Gu;Park, Jong-Jin
    • Korean Journal of Materials Research
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    • v.7 no.10
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    • pp.832-837
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    • 1997
  • 본 연구에서는 반도체 소자의 수율을 현저히 저하시키는 반도체 습식 세정 시 건조 후 웨이퍼 표면에 형성된 water mark의생성 원인을 고찰하였다. 이를 위해 초순수수의 물방울을 다른 접촉각의 시편 위에 고의로 잔류시킨 후 질소 및 산소 분위기에서 건조시켰다. 건조 분위기와 상관없이 HF 처리된 소수성의시편 뿐만 아니라 친수성의 시편에서도 water mark이 관찰되었다. 생성된 water mark의 크기는 분위기에 무관하게 접촉각이 증가함에 따라 감소하였다. 그러나 산소 분위기에서 HF처리된 시편은 건조 후 질소 분위기에서 생성된 water mark의 크기보다 2배이상 크게 형성되었다. 이들 산소 및 질소 분위기에서 HF 처리된 실리콘 시편 위에 생성된 water mark의 성분을 AES(Auger Electron Spectroscopy)로 분석한 결과 water mark는 실리콘과 산소의 화합물 형태로 존재함을 확인하였다. AAS(Atomic Absorption Spectroscopy)분석 결과 건조 분위기에 상관 없이 HF처리된 실리콘 시편 위에 물방울을 30분 잔류시 물방울 내의 실리콘 농도가 증가하였다. 또한 물방울내 ozone을 첨가하여 실리콘 표면을 산화 시켰을 때 물방울과 표면의 접촉각 감소와 water mark의크기의 증가를 초래하였다.

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저진공, 고진공, 초고진공 영역에서의 잔류가스질량분석기 설계특성

  • Park, Chang-Jun;An, Jong-Rok;Jo, Bok-Rae;Han, Cheol-Su;An, Sang-Jeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.108.2-108.2
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    • 2014
  • 잔류가스측정 질량분석기(RGA)는 진공챔버 내부의 진공상태 이상유무, 공정상태 확인 및 주입가스 농도제어 등 여러 종류의 작업에 응용되고 있다. 반도체용 박막 제조공정(PVD, CVD)에서 챔버 내의 수분 혹은 불순물 가스의 정확한 모니터링은 반도체 품질향상에 매우 중요하다. 1 Pascal 진공도의 증착용 챔버에 RGA를 직접 장착하여 작동시키기 위해서는 저진공용 RGA가 사용되어야 한다. 10-3 Pascal에서 6m 자유운동거리를 갖는 질소분자는 1 Pascal에서는 6 mm로 짧은 자유운동거리를 갖는다. 따라서 1 Pascal 저진공영역에서 이온을 생성시키고 mass filter를 사용하여 질량분석을 하기 위해서는 이온원과 mass filter 길이가 자유운동거리 수준으로 작아져야한다. 저 진공영역에서는 검출기와 전자방출용 필라멘트가 저진공에서 작동되도록 일반고진공용 RGA와는 완전히 다르게 소형으로 설계 제작되어야 한다. 10-7 Pascal 이상의 초고진공에서 사용되는 RGA는 이온원이 작동할 때 발생하는 outgassing을 낮추도록 설계가 되어야 초고진공의 유지가 가능하다. 한국표준과학연구원에서 현재 개발 중인 일반고진공용 RGA를 소개하고 저진공용과 초고진공용 RGA의 설계특성을 발표한다.

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