• Title/Summary/Keyword: 잔류용매

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A comparative study of micro plastic detection among different pretreatment method (하수처리장 유입수 전처리 방식에 따른 미세플라스틱 검출 비교)

  • Gil, Kyung Ik;Kim, Sung ryul;Lee, Ji Won
    • Proceedings of the Korea Water Resources Association Conference
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    • 2021.06a
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    • pp.422-422
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    • 2021
  • 현대사회에서 플라스틱의 요구량은 꾸준히 증가하고 있으며 이에따라 생산량 역시 맞춰 증가하고 있다. 이에 따라 전세계적으로 플라스틱으로 인해 발생하는 폐기물의 양 역시 증가하고 있으며 이로 인해 플라스틱 재질의 폐기물이 많아지고 있다. 이 중 가장 문제가 되는 폐기물이 바로 미세플라스틱이다. 미세플라스틱은 1㎛ ~ 5mm 미만의 플라스틱으로 그 물리 화학적인 특성으로 인해 회수가 어려우며 외부 환경에 잔류시 독성을 유발할 수 있다. 플라스틱의 약한강도와 열악한 내열성 그리고 유기용매에 취약하다는 단점을 보완하기 위해 첨가하는 화학물질로 인해 내분비계교란물질을 발생시켜 생명체의 내분비계를 교란시켜 최종적으로 성기능장애를 유발한다. 또한 미세플라스틱의 표면은 유기염류성 살충제와 같은 잔류성오염물질(POPs persistent organic pollutants)사이의 흡착성이 크기 때문에 미세플라스틱은 POPs 농도를 주변보다 최대 백만배 높게 만들 수 있다. 미세플라스틱의 분석은 표준화된 방식이 없어서 제각각이지만 대체로 미세플라스틱 표면에 응집된 유기물을 처리하는 전처리, 미세플라스틱의 농도를 분석하는 정량분석, 그리고 미세플라스틱의 성분을 분석하는 정성분석의 과정을 거쳐서 진행된다. 이러한 미세플라스틱의 분석법을 기반으로 하수처리장에 유입되는 하수의 미세플라스틱 분석방법을 제안하면 다음과 같다. 우선 유입수로부터 미세플라스틱을 따로 분리하기 위해 체거름을 진행했다. 이후 유입하수의 성상에 맞는 적정 전처리 방법을 알아내기 위해 유기물을 제거하기 위한 산화방식으롷서 과산화수소수, 80℃의 과산화수소수, 그리고 펜톤산화의 서로 다른 3가지 방식을 사용했다. 이후 이어지는 정량분석과 정성분석결과를 비교하여 유입하수에 가장 최적인 미세플라스틱 측정방법을 알아보고자 한다.

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Simultaneous Analysis Method of BPA, BPF, BADGE, BFDGE and Their Degradation Products in Canned Foods and Food Simulants by HPLC (HPLC를 이용한 캔 식품 및 식품 유사용매 중 BPA, BPF, BADGE, BFDGE 및 분해산물의 동시분석법)

  • Choi, Jae-Chun;Kyung, Suk-Hun;Lee, Gun-Tack;Lee, Kwang-Ho
    • Korean Journal of Food Science and Technology
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    • v.34 no.2
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    • pp.174-179
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    • 2002
  • A simple and sensitive analysis method based on reverse phase (RP) HPCL with flourescence detector was developed for simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE), and their degradation products, $BADGE{\cdot}H_2O$, $BADGE{\cdot}2H_2O$, $BFDGE{\cdot}H_2O$, $BFDGE{\cdot}2H_2O$, $BADGE{\cdot}HCl{\cdot}H_2O$, $BADGE{\cdot}HCl$, $BADGE{\cdot}2HCl$, $BFDGE{\cdot}HCl{\cdot}H_2O$, $BFDGE{\cdot}HCl$ and $BFDGE{\cdot}2HCl$, which were hydrolyzed and chlorinated forms of BADGE and BFDGE, in canned foods and food simulants. These compounds were identified by GC/MSD with $MSTFA-NH_4I-DTE$ derivatization. Recovery study was performed at each 100 ng/mL levels of BPA, BPF, BADGE and BFDGE added to canned foods and food simulants. This method was resulted in recovery of $90{\sim}114%$ with relative standard deviation of $4.1{\sim}7.0%$, detection limits of $6{\sim}11$ ng/mL and quantitation limits of $12{\sim}18\;ng/mL$. Calibration curves were linear with correlatin coefficients of 0.997 for BPF, 0.996 for BPA, 0.9987 for BFDGE, and 0.9989 for BADGE.

Behaviour of the Soil Residues of the Acaricide-Insecticide, [$^{14}C$]Acrinathrin;II. Degradation in Soil (살비살충제 [$^{14}C$Acrinathrin 토양 잔류물의 행적 규명;II. 토양중 분해)

  • Lee, Jae-Koo;Kyung, Kee-Sung;Oh, Kyeong-Seok
    • Korean Journal of Environmental Agriculture
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    • v.14 no.2
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    • pp.202-212
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    • 1995
  • In order to elucidate the degrading characteristics of the pyrethroid acaricide-insecticide, acrinathrin in two different types of soils, Soil A(pH, 5.8; organic matter, 3.4%; C.E.C., 115 mmol(+)/kg soil; texture, sandy loam) and Soil B(pH, 5.7; organic matter, 2.0%; C.E.C., 71 mmol(+)/kg soil; texture, sandy loam), residualities of the non-labeled compound under the field and laboratory conditions, extractability with organic solvents and formation of non-extractable bound residues, and degradabilities of [$^{14}C$]acrinathrin as a function of aging temperature and aging period were investigated. The half lives of acrinathrin in Soil A treated once and twice were about 18 and 22 days and in Soil B about 13 and 15 days, respectively, in the field, whereas, in the laboratory, those in Soil A and B were about 36 and 18 days, respectively, suggesting that the compound would be non-persistent in the environment. The amounts of $^{14}CO_2$ evolved from [$^{14}C$]acrinathrin in Soil A and B during the aging period of 24 weeks were 81 and 62%, respectively, of the originally applied $^{14}C$ activity, and those of the non-extractable soil-bound residues of [$^{14}C$]acrinathrin were about 70% of the total $^{14}C$ activity remaining in both soils, increasing gradually with the aging period. Degradation of [$^{14}C$]acrinathrin in both soils increased with the aging temperature. Three degradation products of m/z 198(3-phenoxy benzaldehyde), m/z 214(3-phenoxybenzoic acid), and m/z 228(methyl 3-phenoxybenzoate) as well as an unknown were detected by autoradiography of acetone extracts of both soils treated with [$^{14}C$]acrinathrin and aged for 15, 30, 60, 90, 120, and 150 days, respectively, and the degradation pattern of acrinathrin was identical in both soils. Acrinathrin in soil turned out to be degraded to 3-phenoxybenzaldehyde cyanohydrin by hydrolytic cleavage of the ester linkage adjacent to the $^{14}C$ with a cyano group, the removal of hydrogen cyanide therefrom led to the formation of 3-phenoxybenzaldehyde as one of the major products, and the subsequent oxidation of the aldehyde to 3-phenoxybenzoic acid, followed by decarboxylation would lead to the evolution of $^{14}CO_2$.

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Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Improvement of an Analytical Method for Fluoroimide Residue in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Fluoroimide의 잔류농약 분석법 개선)

  • Kim, Nam Young;Park, Eun-Ji;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.220-227
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    • 2021
  • Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO4 and NaCl were used with acetonitrile. C18 (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

Depolymerization of Kraft Lignin at Water-Phenol Mixture Solvent in Near Critical Region (물-페놀 혼합 용매의 근임계 하에서의 크래프트 리그닌의 저분자화)

  • Eom, Hee-Jun;Hong, Yoon-Ki;Chung, Sang-Ho;Park, Young-Moo;Lee, Kwan-Young
    • Journal of Energy Engineering
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    • v.20 no.1
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    • pp.36-43
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    • 2011
  • Plant biomass has been proposed as an alternative source of petroleum-based chemical compounds. Especially, aromatic chemical compounds can be obtained from lignin by depolymerization processes because the lignin consist of complex aromatic materials. In this study, kraft lignin, the largest emitted substance among several kinds of lignin in Korea, was used as a starting material and was characterized by solid-state $^{13}C$-Muclear Magnetic Resonance($^{13}C$-NMR), Fourier Transform Infrared Spectroscopy(FT-IR), Elemental Analysis(EA). The depolymerization of kraft lignin was studied at water-phenol mixture solvent in near critical region and the experiments were conducted using a batch type reactor. The effects of water-to-phenol ratio and reaction temperature($300-400^{\circ}C$) were investigated to determine the optimum operating conditions. Additionally, the effects of formic acid as a hydrogen-donor solvent instead of $H_2$ gas were examined. The chemical species and quantities in the liquid products were analyzed using gas chromatography-mass spectroscopy(GC-MS), and solid residues(char) were analyzed using FT-IR. GC-MS analysis confirmed that the aromatic chemicals such as anisole, o-cresol(2-methylphenol), p-cresol(4-methylphenol), 2-ethylphenol, 4-ethylphenol, dibenzofuran, 3-methyl cabazole and xanthene were produced when phenol was added in the water as a co-solvent.

Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

생강엑기스의 제조에 관한 연구

  • 신애자
    • Food Industry
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    • s.94
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    • pp.37-40
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    • 1988
  • 1) 본 연구에서 시료로 선정한 충남 서산산 건강(dry ginger)은 수분이 $9.4\%$, 회분이 $8.7\%$ 그리고 alcohol에 의한 추출량이 약 $9\%$이다. 이는 선진국에 채택사용하고 있는 건강의 규격기준에 의하면 양호하다. 2) Non- flavor물질의 추출을 최소화하고 특히 증류과정에서 유효성분 손실을 최소화 할 수 있고, 엑기스내의 용매 잔류량이 인체에 유해하지 않고 추출효율을 높일 수 있는 용매는 ethyl alcohol이다. 3) 널리 사용하고 있는 관류추출(percolation)의 성능을 분석하고 이의 개선방안을제시하였다. - 추출효율을 높이기 위하여 건강(dry ginger)의 입자를 작게하면 압력강하가 증대되어순환되는 용액의 유속을 제어하기가 힘들다. - 입자가 작을 시에는 유체의 흐름이chan-nelling현상을 나타낸다. - 위와 같은 조건에서는 물질 전달속도가 느리므로 추출효율을 증대시킬 수가 없다. - 따라서 percolation추출에 사용되는 건강의 입자크기는 30mesh크기 이상이어야 운전조작이 용이하나 추출효율이 낮으므로, 추출시간 6시간에 회수된 생강엑기스양은 약 $2.5\%$이다. 4) percolation추출의 단점을 보완하기 위하여 기계적교반 추출을 선택하여 다음과 같은 개선점을 찾았다. - 교반형 추출에서는 고 - 액분리시 cake 저항에서 문제가 야기되지 않는 범위까지 건강의 입자를 작게할 수 있으므로 추출효율을 크게 향상시킬 수 있었다. 즉, 작게 분쇄된 건강(30mesh통과$90\%$)을 대상으로 추출시간 3시간에 $7\%$의 회수율로 증대시켰다. 최적 운전조건은 다음과 같다. 건강시료:1kg 시료크기:-30mesh$90\%$ 용매:ethyl alcohol 3$\iota$ 교반속도:900r.p.m 추출온도:상온($15\~25^{\circ}C$) 추출시간:3시간 일차 추출조건과 동일하게 하여 얻어진 엑기스의 수율이 $2\~2.5\%$이므로 총엑기스의 수율은 건강(dry ginger)무게기준으로 $8.5\~9.5\%$이었다. 5) 교반추출의 효율이 개선되었다 하더라도 추출물의 분리가 용이하여야만 공정의 이용이 가능하다. 그러므로 교반추출후 고 - 액분리를 위하여 정압여과 장치를 이용하여 여과시 cake의 평균 비저항을 얻었으며, 이의 값은 $4.31\times10^8cm\;/\;gr$으로서 여과에는 어려움이 없다는 것을 의미한다. 따라서 추출속도와 효율이 상대적으로 우수한 교반형 추출기의 가능성을 예시할 수 있음을 알 수 있었다. 6) 추출물을 농축과정에서 휘발성 oil의 손실을 최대로 줄이기 위해서는 단순증류를 하지 말고 분별증류를 수행하여야 하며, gingerol과 같은 중요성분의 열분해 반응을 억제하기 위해서는 열전달 효율을 증대시켜 증류조작을 원활히 수행하여야 하므로, still내의 농축물을 계속 교반시켜야 하며 감압상태에서 증류온도는 $40\~50^{\circ}C$로 유지시키는 것이 가장 바람직하다. 7) Ethyl alcohol로 추출된 엑기스내의 수분이나 회분함량은 외국산 제품에 비하여 약간 낮고, 반면에 조지방 및 조단백 성분의 함량은 약간 높게 나타나고 있어 대체적으로 본 연구에서 얻어진 엑기스내의 비풍미성분(non- fla-vour component) 함량은 외국산에 비하여 많은 차이가 없다. 8) 수입 외국산에 비하여 국산엑기스(본 연구에서 ethyl alcohol로 추출)내의 무기성분등의 함량은 비교적 낮은 편이다. 9) 건강에서부터 oleoresin을 얻어 paradol을 제거시킨 후 순수한 gingerol을 분리하여 IR과 NMR로 확인한 결과, 국산건강의 엑기스에는 주로 6-gingerol이고 약간의 10-gingerol이 함유된 것으로 나타났다. 10) 순수하게 분리된 gingerol을 열분석(TGA와 DTG)한 결과 약 $75^{\circ}C$에서 gingerol의 열분해 반응이 일어남을 알수 있었다. 11) 건강 분말시료와 엑기스내의 미생물 검사 결과 건강분말에서는 세균수가 많이 존재하는 것으로 나타났으나, 이는 ethyl alcohol로 추출하는 공정 중 대부분의 균들이 사멸된 것으로 나타났다. 12) 관능적 측면에선, 본 연구에서 제조한 엑기스와 수입엑기스를 비교한 결과 생강 특유의 맛은 비슷했으나, 수입엑기스에서는 쓴맛과 톱밥냄새를 느낀다는 결과를 나타내었으며 전체적인 종합적 풍미는 국산 건강엑기스가 좋은 것으로 나타났다.

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Selective Recovery of Platinum Group Metals by Solvent Extraction and Electrolysis in Non-aqueous Solution Based on Ionic Liquids (이온성액체 기반 비수계 용액에서 용매추출과 전해에 의한 백금족 금속의 분리회수)

  • Park, Gwang-won;Park, Jesik;Lee, Churl Kyoung
    • Resources Recycling
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    • v.28 no.2
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    • pp.46-53
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    • 2019
  • In this study, the extraction and reduction behavior of platinum group metals in a non-aqueous solvent based on ionic liquids was investigated in order to confirm a new extraction technology of platinum group metals. Platinum was selectively extracted using an ionic liquid $[C_4mim]PF_6$ from a mixed solution of $PdCl_2$, $PtCl_4$ and $RhCl_3$ dissolved with concentration ratio of 10:1:0.5 M. After stripping of the metals by 1 M $HNO_3$ solution, the platinum was preferentially reduced by aqueous electrolysis on gold electrode at -0.8 V (vs. Pt-QRE). The residual palladium and rhodium were transferred to ionic liquid of $[C_4mim]Cl$. The metallic palladium and rhodium could be sequentially reduced on gold and STS304 as working electrodes by non-aqueous electrolysis, respectively.

Recovery of Nickel from Waste Iron-Nickel Alloy Etchant and Fabrication of Nickel Powder (에칭 폐액으로부터 용매추출과 가수분해를 이용한 니켈분말제조에 관한 연구)

  • Lee, Seokhwan;Chae, Byungman;Lee, Sangwoo;Lee, Seunghwan
    • Clean Technology
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    • v.25 no.1
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    • pp.14-18
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    • 2019
  • In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).