• 제목/요약/키워드: Phase extraction method

검색결과 759건 처리시간 0.028초

Extraction Methods of Organic Components from Rubber Composites and Analysis of the Extract Using Gas Chromatography/Mass Spectrometry

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • 제54권3호
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    • pp.188-200
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    • 2019
  • Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.

1,4-Dioxane의 분석방법 연구 (A Study on the Research of Analytical Method for 1,4-Dioxane in Water)

  • 박선구;김태호;임연택;명노일
    • 한국물환경학회지
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    • 제21권6호
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    • pp.549-563
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    • 2005
  • The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

감마선분광분석기와 액체섬광계수기를 이용한 226Ra 분석법 비교 연구 (Evaluation of 226Ra analysis methods using a gamma-ray spectrometer and a liquid scintillation counter)

  • 주병규;김문수;김현구;김동수;조성진;양재하;박선화;김형섭;권오상;김태승
    • 분석과학
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    • 제28권3호
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    • pp.228-235
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    • 2015
  • 본 연구는 지하수 중 라듐(226Ra) 분석을 위해 고상추출디스크(solid phase extraction disk)를 이용한 감마선분광분석법(이하 고상추출디스크법)을 제안하고 액체섬광계수기를 이용한 액체섬광계수(liquid scintillation counter, LSC)법 및 마리넬리비커(Marinelli beaker)를 이용한 감마선분광분석기(gamma ray spectrometer)법(이하 마리넬리비커법)과의 회수율 비교를 통해 적용성을 검토하였다. 226Ra을 회수한 고상추출디스크는 딸핵종의 방출을 방지하기 위해 폴리에틸렌 필름으로 밀봉 후 감마선분광분석기로 분석하였다. 24일 경과 후, 226Ra과 딸핵종인 214Bi과 214Pb이 방사평형 된 것으로 확인되었다. 라듐 표준물질을 이용하여 고상추출디스크법으로 분석한 딸핵종 214Bi와 214Pb의 회수율은 각각 80% (295.21 Kev)와 104% (351.92 Kev)로 액체섬광계수법보다 높게 나타났다. 바탕시료(blank) 측정시 감마선분광분석기 챔버내 질소를 주입했을 경우는 주입하지 않았을 경우보다 간섭치가 약 10% 이하로 낮아지는 것을 확인하였으며, 5 L 시료를 8만초 동안 측정한 검출한계는 0.17~0.40 pCi/L로 분석되어 미국 EPA 기준치인 1pCi/L를 만족하였다. 고상추출디스크법과 액체섬광계수법을 이용한 7개 지하수 시료 분석 결과, 두 방법의 상관계수(correlation coefficient)는 0.987로 나타나 추가적인 분석을 통해 통계적 유의성을 확보한다면 고상추출디스크법의 적용가능성이 높을 것으로 판단된다. 결과적으로, 고상추출디스크법을 이용한 지하수 중 226Ra 농도 분석은 전처리 과정이 비교적 단순하여 분석시간이 절약되고 높은 회수율과 낮은 검출한계치 등의 장점을 가지고 있는 것으로 분석되었다. 또한 고상추출디스크법은 액체섬광계수법과 마리넬리비커법에 비해 많은 양의 시료를 전처리하기 쉽기 때문에 저준위 시료 분석에 유용할 것으로 판단된다.

가열 조리된 돼지고기의 Heterocyclic Amines 분석을 위한 Solid-phase 추출 방법의 비교 (Comparison of Different Solid-Phase Extraction Methods for the Analysis of Heterocyclic Amines from Pan-Fried Pork Meat)

  • 이재환;백유미;이광근;신한승
    • 한국축산식품학회지
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    • 제28권5호
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    • pp.637-644
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    • 2008
  • 식품 중 HCAs을 검출하기 위한 최적 전처리 방법을 확립하기 위해 가열 조리된 돼지고기 패티를 이용하여 서로 다른 4가지 SPE(solid-phase extraction)방법을 비교하였다. 4가지 전처리 방법을 통해 얻은 15가지 HCAs 회수율은 3.0%(방법 A, Tri-P-1)-74.7%(방법A, Tri-P-2)이었다. 그 중 $MeA{\alpha}C$가 평균적으로 73.4%로 가장 높은 회수율을 보였으며 Tri-MeIQx가 15.2%의 가장 낮은 회수율을 보였다. 4가지 전처리 방법 중 방법A와 방법D가 가장 높은 회수율과 검출빈도를 보였으며 방법B와 방법C는 Harman(14.8%)을 제외하고는 전혀 검출되지 않았고 회수율을 구할 수 없었다 발암 가능 물질인 IQ, $A{\alpha}C$, $MeA{\alpha}C$, Glu-P-1, Glu-P-2, MeIQ, MeIQx, PhIP 등을 검출하는 방법에는 방법A(48.7-74.6%)가 4가지 방법 중 가장 유리하다. HCAs는 극성에 따라 polar amines과 less-polar amines으로 구분할 수 있는데 방법A는 less-polar amines검출에 유리하고 방법D는 polar amines검출에 유리하다. 방법A와 방법D의 chromatogram을 비교한 결과 방법A와 방법D 모두 15가지 HCAs가 깨끗하게 분리되었지만 Tri-MeIQx 등을 검출하는데 방법A가 더욱 유리하다. SPE 전처리 방법 및 LC/MS 분석방법에 대한 유효성을 확인하기 위해 LOD(0.2-2.1 ng/mL)와 LOQ(0.8-9.7 ng/mL), 표준 편차(0.2-8.6)를 구하였다.

Ionic liquid coated magnetic core/shell CoFe2O4@SiO2 nanoparticles for the separation/analysis of trace gold in water sample

  • Zeng, Yanxia;Zhu, Xiashi;Xie, Jiliang;Chen, Li
    • Advances in nano research
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    • 제10권3호
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    • pp.295-312
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    • 2021
  • A new ionic liquid functionalized magnetic silica nanoparticle was synthesized and characterized and tested as an adsorbent. The adsorbent was used for magnetic solid phase extraction on ICP-MS method. Simultaneous determination of precious metal Au has been addressed. The method is simple and fast and has been applied to standard water and surface water analysis. A new method for separation/analysis of trace precious metal Au by Magnetron Solid Phase Extraction (MSPE) combined with ICP-MS. The element to be tested is rapidly adsorbed on CoFe2O4@SiO2@[BMIM]PF6 composite nano-adsorbent and eluted with thiourea. The method has a preconcentration factor of 9.5-fold. This method has been successfully applied to the determination of gold in actual water samples. Hydrophobic Ionic Liquids (ILs) 1-butyl-3-methylimidazole hexafluorophosphate ([BMIM]PF6) coated CoFe2O4@SiO2 nanoparticles with core-shell structure to prepare magnetic solid phase extraction agent (CoFe2O4@SiO2@ILs) and establish a new method of MSPE coupled with inductively coupled plasma mass spectrometry for separation/analysis of trace gold. The results showed that trace gold was adsorbed rapidly by CoFe2O4@SiO2@[BMIM]PF6 and eluanted by thiourea. Under the optimal conditions, preconcentration factor of the proposed method was 9.5-fold. The linear range, detection limit, correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.01~1000.00 ng·mL-1, 0.001 ng·mL-1, 0.9990 and 3.4% (n = 11, c = 4.5 ng·mL-1). The CoFe2O4@SiO2 nanoparticles could be used repeatedly for 8 times. This proposed method has been successfully applied to the determination of trace gold in water samples.

Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • 제25권4호
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    • pp.545-548
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    • 2004
  • A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with $C_{18}$ membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with $C_{18}$ membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was $1.32{\times}10^5L\;mol^{-1}cm^{- 1}$ at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 ${\mu}$g/mL. This method was applied to the determination of nickel in water and biological samples with good results.

Study on the Solid Phase Extraction of Hg(II)-SBDTR Chelate with C18 Disks and Its Application to the Determination of Mercury in Tobacco and Tobacco Additive

  • Yang, Guan-Gyu;Xia, Zhen-Yuang;Wu, Yu-Ping;Sun, Han-Dong;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • 제25권4호
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    • pp.549-552
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination of mercury based on the rapid reaction of mercury(II) with p-sulfobenzylidenethiorhodanine (SBDTR) and the solid phase extraction of the colored chelate with $C_{18}$ disks. In the presence of pH 3.5 sodium acetate-acetic acid buffer solution and Emulsifier-OP medium, SBDTR reacts with mercury(II) to form a red chelate of a molar ratio 1 : 2 (mercury to SBDTR). This chelate was prconcentrated by solid phase extraction with $C_{18}$ disks. An enrichment factor of 50 was achieved. The molar absorptivity of the chelate is $1.28{\times}10^5 L{\cdot}mol^{-1}{\cdot}cm^{-1}$ at 545 nm in measured solution. Beer's law is obeyed in the range of 0.01-3 ${\mu}$g/mL. The relative standard deviation for eleven replicates sample of 0.01 ${\mu}$g/mL is 1.65%. This method was applied to the determination of mercury in tobacco and tobacco additive with good results.

Study on Solid Phase Extraction and Spectrophotometric Determination of Vanadium with 2-(2-Quinolylazo)-5-Diethylaminophenol

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • 제25권2호
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    • pp.263-266
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination ${\mu}$g/L level of vanadium ion based on the rapid reaction of vanadium(V) with 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) and the solid phase extraction of the colored chelate with $C_{18}$ cartridge. The QADEAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH = 3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1 : 2 (V(V) to QADEAP). This chelate was enriched by solid phase extraction with $C_{18}$cartridge and the enrichment factor of 50 was obtained by elution of the chelates from the cartridge with ethanol. The molar absorptivity of the chelate is $1.28 {\times}10^5L\;mol^{-1}cm^{-1}$ at 590 nm in the measured solution. Beer's law is obeyed in the range of 0.01-0.6 ${\mu}$g/mL. The detection limit is 0.04 ${\mu}$g/L in the original samples. This method was applied to the determination of vanadium(V) in water and biological samples with good results.

The High-throughput Solid-Phase Extraction in the Field of Synthetic Biology: Applications for the Food Industry and Food Managements

  • Hyeri SEONG;Min-Kyu KWAK
    • 식품보건융합연구
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    • 제10권3호
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    • pp.19-22
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    • 2024
  • The field of synthetic biology has emerged in response to the ongoing progress in the life sciences. Advances have been made in medicine, farming, eating, making materials, and more. Synthetic biology is the exploration of using living organisms to create new organisms. By manipulating specific genes to express targeted proteins, proteins can be created that are both productive and cost-effective. Solid-phase extraction (SPE) and liquid-liquid extraction (LLE) are employed for protein separation during the production process involving microorganisms. This study centers on Scanning Probe Microscopy (SPM) to showcase its utility in the food industry and food management. SPE is predominantly utilized as a pretreatment method to eliminate impurities from samples. In comparison to LLE, this method presents benefits such as decreased time and labor requirements, streamlined solvent extraction, automation capabilities, and compatibility with various other analytical instruments. Anion exchange chromatography (AEC) utilizes a similar methodology. Pharmaceutical companies utilize these technologies to improve the purity of biopharmaceuticals, thereby guaranteeing their quality. Used in the food and beverage industry to test chemical properties of raw materials and finished products. This exemplifies the potential of these technologies to enhance industrial development and broaden the scope of applications in synthetic biology.

Spectrometric Determination of Rhodamine B in Chili Powder After Molecularly Imprinted Solid Phase Extraction

  • Liu, Xiuying;Zhang, Xuan;Zhou, Qian;Bai, Bing;Ji, Shujuan
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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    • pp.3381-3386
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    • 2013
  • This paper reports a method using molecularly imprinted polymers that are grafted onto the surface of carboxyl-modified multi-walled carbon nanotubes as the solid-phase extraction adsorbents to detect Rhodamine B in chili powder samples. The polymers were characterized by FTIR and TGA. Various parameters which probably influence efficiency of extraction were optimized. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions. And the proposed method was applied to analysis of Rhodamine B in chili powder samples. The limits of detection and quantification were 2.57 and 8.56 ${\mu}g/g$, respectively. The recoveries for analytes were higher than 95% and relative standard deviation values were found to be in the range of 0.83-4.15%. This method was successfully applied for the determination of Rhodamine B.