• 제목/요약/키워드: spectrofluorimetry

검색결과 23건 처리시간 0.025초

차량용 폐윤활유에 함유된 다환 방향족 탄화수소 (PAHs)의 분석 (Determination of polycyclic aromatic hydrocarbons (PAHs) in used lubricating car oils)

  • 유광식;정지영;정선이;우상범
    • 분석과학
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    • 제16권5호
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    • pp.339-348
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    • 2003
  • 본 연구에서는 동시 형광분광법과 GC/FID법을 이용하여 폐윤활유 시료 중의 PAHs를 acetonitrile 용매로 추출하여 정량분석 하였다. 동시 형광분광법을 이용하여 7종의 PAHs, 즉 acenaphthene (Ace), anthracene (Anth), benzo(a)pyrene (BaP), chrysene (Chry), phenanthrene (Phen), fluoranthrene (Fl) 및 perlyrene (Per)을 분석하였다. 이들 성분의 검정선은 모두 0.4~166 ppb(상관계수; 0.9985~0.9999)의 범위에서 직선을 보였다. 다른 8종의 PAHs를 GC법으로 분석하기 위한 검량선은 10.0 ppm 표준용액을 사용하였고, split ratio를 10에서부터 100까지 변화시킬 때에 발생되는 peak 면적을 이용하여 작성하였다. 검출감도는 동시 형광분광법이 GC법보다 적어도 100배 이상 우수하였다. 폐윤활유 시료 중의 총 PAHs 함량은 LNG(버스)와 LPG(택시)의 폐윤활유에서 각각 5.5 ng/g과 10.5 ng/g의 수준으로 검출되었으며, 가솔린을 사용하는 일반승용차, 경유를 사용하는 승합차 및 트레일러의 폐윤활에서 각각 92.2 ng/g, 92.6 ng/g 및 130.3 ng/g 등이 측정되어 경유를 사용하는 대형트레일러에서 가장 많은 양이 발생됨을 알 수 있었다.

보조 형광증가제를 이용한 L-Dopa의 형광분광법적 정량 (Determination of L-Dopa by Spectrofluorimetry Using Co-fluorescence Enhancer)

  • 이상학;안정미
    • 대한화학회지
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    • 제44권6호
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    • pp.541-546
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    • 2000
  • 리간드 증감 유발 형광법을 이용하여 Tb(III)-L-dopa (L-3,4-dihydroxyphenyl alanine) 착이온의 방출세기를 측정함으로써 수용액 중의 L-dopa를 정량하는 방법에 대하여 연구하였다. 들뜸파장, pH, 보조 형광증가제의 선택, Tb(III) 이온의 농도, 보조 형광증가제로 사용된 Lu(III) 이온의 농도 및 방출파장의 방출세기에 대한 영향을 조사하였다. 보조 형광증가제로서 Lu(III) 이온을 첨가하였을때 Tb(III) 이온의 방출세기가 현저히 증가함을 관찰하였고, L-dopa의 검출한계를 낮출 수 있었다. 보조 형광증가제를 첨가하지 않았을 경우에 L-dopa 검정곡선의 직선감응범위는 들뜸파장, pH 및 Tb(Ⅲ) 이온의 농도가 각각 300 nm, 8.0 및 $1.0{\times}10^{-4}$ M였을때, $5.0{\times}10^{-7}$ M~$1.0{\times}10^{-4}$ M였다. 이 조건에서의 검출한계는 $4.0{\times}10^{-8}$ M였다. 보조 형광증가제를 첨가하였을 경우에는 들뜸파장, pH, Tb(III) 이온의 농도, 보조 형광증가제로 사용된 Lu(III) 이온의 농도 및 방출파장이 각각 300 nm, 8.5, $1.0{\times}10^{-5}$ M, $1.0{\times}10^{-5}$ M 및 545 nm였을 때, 직선감응범위가 1.0×$10^{-8}$ M~2.0{\times}10^{-4}$ M였고, 이 때의 검출한계는 $1.0{\times}10^{-9}$ M였다.

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Optimal Optical Filters of Fluorescence Excitation and Emission for Poultry Fecal Detection

  • Kim, Tae-Min;Lee, Hoon-Soo;Kim, Moon-S.;Lee, Wang-Hee;Cho, Byoung-Kwan
    • Journal of Biosystems Engineering
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    • 제37권4호
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    • pp.265-270
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    • 2012
  • Purpose: An analytic method to design excitation and emission filters of a multispectral fluorescence imaging system is proposed and was demonstrated in an application to poultry fecal inspection Methods: A mathematical model of a multispectral imaging system is proposed and its system parameters, such as excitation and emission filters, were optimally determined by linear discriminant analysis (LDA). An alternating scheme was proposed for numerical implementation. Fluorescence characteristics of organic materials and feces of poultry carcasses are analyzed by LDA to design the optimal excitation and emission filters for poultry fecal inspection. Results: The most appropriate excitation filter was UV-A (about 360 nm) and blue light source (about 460 nm) and band-pass filter was 660-670 nm. The classification accuracy and false positive are 98.4% and 2.5%, respectively. Conclusions: The proposed method is applicable to other agricultural products which are distinguishable by their spectral properties.

형광시약 Safranine-O를 이용한 유리 시안화 이온의 분광형광법 정량 (Spectrofluorimetric determination of free cyanide ion with fluorescent safranine-O)

  • 최희선
    • 분석과학
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    • 제25권3호
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    • pp.159-163
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    • 2012
  • A spectrofluorimetric method has been developed for the determination of free $CN^-$ in real samples with fluorescent safranine-O. When safranine-O interacts electrostatistically with $CN^-$, the fluorescent intensity of safranine-O is decreased. Several experimental conditions such as pH of the sample solution and the amount of safranine-O were optimized. $Ag^+$ interfered higher than any other ions. Interference of $Ag^+$ could be disregarded because $Ag^+$ was scarcely contained or mostly complexed with $CN^-$ in selected real samples. With this proposed method, the linear range of $CN^-$ was from 5.0 to 110 ng/mL and the detection limit of $CN^-$ was 2.9 ng/mL. For validating this technique, real samples (Cu, Ag, Au electroplating wastewater, and untreated wastewater in university and in sewage treatment plant) were used. Recovery yields of 91.5%~106.0% were obtained. Based on experimental results, it is proposed that this technique can be applied to the practical determination of free $CN^-$.

Cu(II)-tiron 킬레이트를 이용한 EDTA 분광형광법 정량 (Spectrofluorimetric determination of EDTA with Cu(II)-tiron chelate)

  • 최희선
    • 분석과학
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    • 제24권3호
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    • pp.231-235
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    • 2011
  • A spectrofluorimetric method for the determination of EDTA in real samples such as mayonnaise, powder detergent and cleansing cream with tiron (4,5-dihydroxy-1,3-benzenedisulfonic acid) as a fluorimetric reporter was developed. When tiron is chelated with Cu(II), the fluorescent intensity is decreased by a quenching effect. However, when Cu(II)-tiron chelate reacts with EDTA, fluorescent intensity is increased as tiron is released. Several experimental conditions such as pH of the sample solution, the amount of Cu(II), the amount of tiron, heating temperature and heating time were optimized. Fe(III) interfered more seriously than any other ions, interference of Fe(III) could be disregarded, because Fe(III) was scarcely contained in selected real samples. The linear range of EDTA was from $8.0{\times}106{-8}\;M$ to $2.0{\times}10^{-6}\;M$. With this proposed method, the detection limit of Fe(III) was $5.2{\times}10^{-8}\;M$. Recovery yields of 92.7~99.3% were obtained. Based on experimental results, it is proposed that this technique can be applied to the practical determination of EDTA.

Application of Organized Media for Rapid Spectrofluorimetric Determination of Trace Amounts of Cr(VI) in the Presence of Cr(III)

  • Madrakian, Tayyebeh;Afkhami, Abbas;Mohammadnejad, Masoumeh
    • Bulletin of the Korean Chemical Society
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    • 제30권6호
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    • pp.1252-1256
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    • 2009
  • A simple, selective and sensitive fluorescence quenching method was developed to the determination Cr(VI). The method is based on the oxidation of $I^-\;to\;{{I_3}^-}$ by Cr(VI) in sulfuric acid solution followed by immediate formation of ion association compound between I3 − and rhodamine 6G in Tween-80 micellar media at room temperature. The influence of several surfactants on rhodamine 6G fluorescence signal was studied; particular attention was paid in the aggregation behavior of rhodamine 6G–Tween-80 system. The experimental parameters (e.g., type of surfactant, reagent concentration) were studied and the optimal conditions were established. The linear calibration graph was obtained in the range 2.0 - 100.0 ng m$L^{-1}$ Cr(VI). The detection limit of the method was 0.37 ng m$L^{-1}$. The relative standard deviation (R.S.D.) is less than 5% (n = 5). The efficiency of the method for the determination of Cr(VI) in the presence of Cr(III) in the sample was investigated. The method was applied successfully to the determination of Cr(VI) and total Cr in water, and liver tissue samples.

Determination of Heparin Using Norfloxacin-cerium Complex as a Fluorescence Probe by Spectrofluorimetry

  • Patil, Shailaja R.;Mote, Umesh S.;Patil, Shivajirao R.;Kolekar, Govind B.
    • Bulletin of the Korean Chemical Society
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    • 제30권12호
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    • pp.3034-3038
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    • 2009
  • A simple, rapid, practical and sensitive spectofluorimetric method was developed for the determination of trace amount of heparin (Hep). Under the Optimum conditions, we studied the interaction between NFLX-Ce$^{3+}$-Hep complex by using absorption and fluorescence spectra. It was observed that Hep remarkably enhance the fluorescence intensity of the NFLX-Ce$^{3+}$ complex at ${\lambda}$= 356 nm in the buffer solution of pH = 7.60 and the enhancement effect is shown to relate with the concentration of Hep. The linear range and detection limit for the determination of Hep was obtained. By the Rosenthal graphic method, the association constant (K) and binding numbers (N) of Hep with probe were investigated. This method is relatively free of interference from coexisting substances and successfully applied for the determination of heparin in heparin sodium injection samples. A suitable mechanism of fluorescence enhancement between NFLX-Ce$^{3+}$ and the NFLX-Ce$^{3+}$-Hep systems were proposed and discussed.

The Use of Crude Extract of Kohlrabi (Brassica oleracea gongylodes) as a Source of Peroxidase in the Spectrofluorimetric Determination of Thiamine

  • Amjadi, Mohammad;Manzoori, Jamshid L.;Orooji, Maghsood
    • Bulletin of the Korean Chemical Society
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    • 제28권2호
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    • pp.246-250
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    • 2007
  • The crude extract of kohlrabi (Brassica oleracea gongylodes) was prepared as a rich source of peroxidase and its enzymatic and specific activities in the presence of cross-linked polyvinylpyrrolidone as a stabilizer were determined. This extract was used to catalyze the oxidation of thiamine in the presence of hydrogen peroxide to thiochrome at pH 8.0. Thiochrome shows strong fluorescence at 436 nm with excitation at 370 nm. Based on the obtained results, a sensitive and simple spectrofluorimetric method was developed for the determination of thiamine. In the optimum conditions, the calibration graph was linear from 2 × 10-7 to 1 × 10-4 mol L-1, with a detection limit of 6.2 × 10-8 mol L-1. The relative standard deviation (RSD) was 1.2% for 5 × 10-6 mol L-1 thiamine. The method was successfully applied to the determination of thiamine in vitamin B1 and vitamin B complex tablets and vitamin B complex syrup.

Quinalizarin-β-cyclodextrin 내포 착물을 이용한 수용액 시료의 흔적량 Co(II)의 분광형광법 정량 (Spectrofluorimetric determination of trace Co(II) in aqueous samples with quinalizarin-β-cyclodextrin inclusion complex)

  • 백현정;최희선
    • 분석과학
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    • 제28권4호
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    • pp.255-259
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    • 2015
  • A technique on the determination of Co(II) in aqueous samples with quinalizarin-β-cyclodextrin inclusion complex was developed. The conditions such as pH of the sample solution, the concentration of quinalizarin and the concentration of β-CD were optimized to 11.3(±0.2), 1.2×10−6 M and 8.0×10−6 M, respectively. Under these optimum conditions, the calibration curve of Co(II) was obtained over concentration range of 5.0×10−9 ~ 1.2×10−7 M. The detection limit was 4.2×10−9 M (0.25 ng/mL). For validating this proposed technique, aqueous samples(stream water, reservoir water and tap water) were used. Recovery yields of 95~105% were obtained. The relative standard deviation(%) in aqueous samples were less than 7.0%. Based on experimental results, it is proposed that this technique can be applied to the practical determination of Co(II).

Europium(III)와 EDTA의 3차 복합체 형성에 의한 Levodopa의 분광분석적 정량 (Spectrofluorimetric Determination of Levodopa through Ternary Complex Formation with Europium(III) and Ethylenediaminetetraacetic Acid)

  • ;;김소연;조해진;이상학;김영호;김성홍
    • 응용화학
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    • 제15권1호
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    • pp.25-28
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    • 2011
  • A highly sensitive spectrofluorimetric method was developed for the determination of levodopa based on the formation of a ternary complex with Eu3+ in the presence of ethylenediaminetetraacetic acid. It was found that this complex manifests intense fluorescence at 591 and 613 nm with excitation at 372 nm and maximum intensity was obtained at 613 nm. Under the optimum conditions, the enhanced fluorescence intensity was proportional to the concentration of levodopa over the range of 3×10-9-2.5×10-7 mol L-1 with limit of detection (LOD) of 4.37×10-10 mol L-1. The method offers higher sensitivity and selectivity which could be effectively applied for the determination of levodopa in pharmaceutical and biological samples.