• 제목/요약/키워드: XAD-4

검색결과 122건 처리시간 0.02초

치자황색소로부터 변환된 색소의 특성 (Characteristics of the Conversion Pigment from Gardenia jasminoides Yellow Pigment)

  • 정형석;박근형
    • 한국식품과학회지
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    • 제30권2호
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    • pp.319-323
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    • 1998
  • 치자의 황색소를 L. plantalium, V. vulinficus, P. aeruginosa, S. mutans, B. subtilis, S. epidermidis, S. typhimurium, S. aureus 등 8종의 균주의 배지에 첨가하고 배양하면 청녹색계 색소로 변환된다. 미생물에 의해 변환된 색소의 분광학적 성질을 경시적으로 추적하면 색소의 변환형태는 3군으로 나뉘어지며, 색차계로 측정된 ${\Delta}E$ 값의 변환형태도 그러하였다. 청녹색계색소로의 변환속도는 균주에 따라 차이를 보였는데 8종의 미생물중 S. epidermidis는 가장 빨라 배양 16시간에 색소변환이 완성되었다. 치자황색소와 변환된색소는 $H_2O-MeOH$ 용매계에 의한 Amberlite XAD-4 column chromatography에 의해 완전히 분리되었으며, 광과 열에 대한 저장안정성은 치자황색소보다 변환된 색소가 보다 안정함을 나타냈다.

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Preconcentration of Iron(III), Lead(II), Cobalt(II) and Chromium(III) on Amberlite XAD-1180 Resin Loaded with 4-(2-Pyridylazo)-resorcinol (PAR) and Their Determination by FAAS

  • Tokalloglu, Serife;Kartal, Senol
    • Bulletin of the Korean Chemical Society
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    • 제27권9호
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    • pp.1293-1296
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    • 2006
  • In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

XAD-16-[4-(2-thiazolylazo)]orcinol 킬레이트 수지에 의한 금속이온의 분리 및 농축에 관한 연구 (Studies on the Separation and Preconcentration of Metal Ions by XAD-16-[4-(2-thiazolylazo)] orcinol Chelating Resin)

  • 이원;설경미;안혜숙;이창헌;임재희
    • 분석과학
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    • 제10권4호
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    • pp.282-290
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    • 1997
  • XAD-16-[4-(2-thiazolylao)]orcinol (TAO)형 킬레이트 수지에 대한 U(VI), Tb(IV), Zr(IV), Cu(II), Pb(II), Ni(II), Zd(II), Cd(II) 및 Mn(II) 이온의 흡착 및 탈착 특성을 용리법으로 조사하였다. 각 금속이온의 총괄용량과 pH 변화에 따르는 혼합 금속이온의 분리능 및 금속이온의 최적 흡착 조건을 조사하기 위하여 금속이온의 흡착에 미치는 흐름속도, 완충용액의 농도에 대한 영향을 검토하였다. 킬레이트 수지에 의한 금속이온의 총괄 흡착 용량은 각각 0.35nmol U(VI)/g resin, 0.49nmol Th(VI)/g resin, 0.41nmol Cu(II)/g resin 및 0.31nmol Zr(IV)/g resin이었다. 그리고 pH 5.0에서 돌파점 용량과 총괄 용량으로부터 얻은 금속이온의 용리순서는 Th(IV)>Cu(II)>U(VI)>Zr(IV)>Pb(II)>Ni(II)>Zn(II)>Mn(II)>Cd(II)이었다. 흐름속도 0.28mL/min 및 pH 2~5범위에서 혼합 금속이온을 분리한 결과 pH가 증가함에 따라 이들 이온의 군분리가 가능하였다. 한편, $HNO_3$, HCl, $HClO_4$, $H_2SO_4$$Na_2CO_3$ 등의 탈착제에 의한 탈착특성을 조사한 결과 2M $HNO_3$는 Zr(IV)을 제외한 대부분의 금속이온들은에 대하여 높은 탈착효율을 나타냈으며, 1M $H_2SO_4$ 용액을 사용하면 Zr(IV)의 탈착 및 회수가 가능하였다. 또한 킬레이트 수지를 이용하여 미량의 U(VI) 이온이 함유된 인공 해수 시료를 용리시키고 회수한 결과 94%이상의 높은 회수율을 나타내었다. 아울러 XAD-16-TAO 킬레이트 수지는 희토류 금속의 혼합시료를 2M $HNO_3$ 용액으로 용리시키면 U(VI)의 선택적인 분리, 농축 및 회수에 유용함을 알 수 있었다.

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환경 오염물질의 정량법 개발과 거동에 관한 연구(III) : 미량 페놀류의 HPLC 정량을 위한 온 라인 농축 (A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants(III) : On-Line System for Preconcentration and Separation of Trace Phenols by HPLC)

  • 이대운;김진영;박영훈;문명희
    • 분석과학
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    • 제7권1호
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    • pp.33-39
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    • 1994
  • 환경오염수에 미량 존재하는 페놀류를 정량하기 위한 분석법의 개발을 위하여 8가지 페놀류를 대상 시료로, 고체상 추출법을 이용한 전처리 방법을 연구하였다. XAD-4와 Dowex $1{\times}8$ 수지를 연결하여 HPLC로 분석하는 온 라인 시스템을 만들어 농축과 분리의 선택성을 높이며 자동화에 중점을 두었다. 시료를 XAD-4 컬럼에 용리시켜 페놀류를 분자흡착으로 농축시킨 후 염기성 아세토니트릴을 용리시켜 탈착시키고 계속해서 Dowex $1{\times}8$ 컬럼에 음이온교환으로 페놀류만을 선택적으로 재흡착시킨다. Dowex $1{\times}8$ 컬럼에 재흡착된 페놀류를 물로 세척한 후 HCl을 포함하는 메탄올 용액으로 재탈착시킨다. 전처리 단계는 switching 밸브에 의해 온 라인으로 연결하였고 탈착된 페놀류를 HPLC에 직접 주입하여 신속하고 신뢰성 있는 정량이 가능하였다. 각 페놀류는 90% 이상의 회수율을 나타내었다. 본 분석법의 활용성을 평가하기 위해 환경오염수에서 페놀류와 공존 가능한 유기 화합물들을 첨가시켜 조제한 실험실적 오염수를 만들어 방해 효과를 조사한 결과, 페놀류만을 선택적으로 농축-분석할 수 있었다.

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Determination of Trace Metals in Waters by FAAS after Enrichment as Metal-HMDTC Complexes Using Solid Phase Extraction

  • Tokalioglu, Serife;Kartal, Senol;Elci, Latif
    • Bulletin of the Korean Chemical Society
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    • 제23권5호
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    • pp.693-698
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    • 2002
  • A method has been described for the determination of Cu(Ⅱ), Pb(Ⅱ), Ni(Ⅱ), Cd(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ) by flame atomic absorption spectrometry (FAAS) after preconcentration on Amberlite XAD-16 resin, using hexamethyleneammonium-hexamethylenedithiocarbamate (HMA-HMDTC) as a chelating agent, and NH3/NH4Cl buffer solution (pH 9). Influences of various analytical parameters such as pH, concentration of nitric acid, amount of analytes, diverse ions and sample volume were investigated. The relative standard deviation (RSD) and the detection limit (LOD) were found in the range of 0.8-2.9% and 0.006-0.277 ㎍/mL,respectively. Recoveries obtained by the column method were quantitative ( >95%) at optimum conditions.The method was applied to the determination of some metal ions in seawater and wastewater samples. A high preconcentration factor (about 150 for seawater and 75 for wastewater samples) and simplicity are the main advantages of this suggested method.

Preparative HPLC를 이용한 KRF-001의 대량분리정제 (Large Scale Purification of KRF-001 on the Preparative HPLC)

  • 이항우;김무경정태숙복성해
    • KSBB Journal
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    • 제9권4호
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    • pp.385-394
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    • 1994
  • 항진균물질 KRF -001의 분리정제 공정에 있어서 XAD-7 크로마토그래피, 산침전법, microfiltration 을 사용하여 crude KRF-001을 분리정재하였을 때, microfiltration 방법 이 기존의 다른 두 방법보다도 회수율이 2-3배 뒤어난 것으로 판명되었으며, 실리 카겔 크로마토그래피, $C_{18}$ 크로마토그래피법을 이용 하여 분리정제방법을 간소화할 수 있였다 또한 Bonda PAK $C_{18}$ column과 Delta PAK $C_{18}$ col­ umn을 prep HPLC에 사용한 결과, 순도 90% KRF-OOI의 대량분리 정제가 가능하여 산엽화시 이를 이용할 수 있는 기초를 확립하였다.

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대기 중 다환방향족 탄화수소의 측정을 위한 시료포집방법의 비교평가 (Evaluation of Sampling Methodology for the Measurement of Polycyclic Aromatic Hydrocarbons in the Atmosphere)

  • 백성옥;최진수
    • 한국대기환경학회지
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    • 제14권1호
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    • pp.43-62
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    • 1998
  • This study was carried out to investigate the influence of different sampling methods on the measured concentrations of polycyclic aromatic hydrocarbons (PAH) both in the vapor and particulate phases, and to evaluate the effects of ambient temperature and sampling duration on the losses of PAH associated with particle samples due to volatilization. The experimental protocol of this study is consisted of two parts. The first part is related to the comparison of PAH concentrations measured by 4 different sampling systems, each of which involves different sampling principles for comparison purposes, including a medium-volume sampler with XAD-2 adsorbent, a high-volume sampler with polyurethane foam (PUF), two identical low-volume samplers: one with XAD-2 and the other with PUF, respectively. The second part of this study is to quantitatively estimate the losses of particulate PAH samples by volatilization during sampling, using two identical low-volume samplers: one was used for changing the filters every 3 hrs, 6 hrs, 12 hrs, and 24 hrs sampling, while the other was maintained for continuous 48 hours sampling without changing the filter. The concentrations of volatile PAH including 2-3 rings appeared to be significantly affected by the type of adsorbent. Measured levels of these lower-molecular weight PAH by XAD-2 adsorbent were much higher than those by PUF for both high-volume and low-volume sampling. PUF was found to give rise to unknown components that interfered with the PAH analysis, even after extensive clean-up. In addition, the retention efficiency of PUF for lower molecular weight PAH was subject to a large variation, being significantly influenced by sampling conditions such as ambient temperature. However, the effect of sampling methods with different adsorbents on the measured levels of semi-volatile compounds including 4 rings PAH such as fluoranthene, pyrene, BaA and chrysene, was not so much significant as more volatile PAH compounds. It was also clear from this study that volatilization losses of the semi-volatile PAH collected on the filters were inevitably occurred during prolonged sampling, and hence the results obtained from conventional sampling methods may not be expected to yield an accurate distribution of PAH between the vapor and particulate phases.

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탈착용매에 따른 PAHs 흡착매체의 탈착효율 평가 연구 (A Study on Desorption Efficiency of PAHs according to Desorption Solvents by HPLC with Sonication Extraction)

  • 홍좌령;이지은;정명구;최광민
    • 한국산업보건학회지
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    • 제26권3호
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    • pp.307-316
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    • 2016
  • Objectives: In general, NIOSH method 5506 is most widely used for the occupational exposure measurement of PAHs, but 2-4 ring PAHs have poor desorption efficiency, especially for a filter. The purpose of this study was to determine a method to increase the desorption efficiency of 16-PAHs using an ultrasonic extraction procedure. Methods: Test samples prepared spiked XAD-2 tubes and PTFE filters in the range of $0.01-1.0{\mu}g/mL$ for desorption efficiency study. Four different extraction solvents, acetonitrile, acetone, tetrahydrofuran and dichloromethane, were tested in order to select the most suitable solvent for the extraction of the 16 PAHs. The addition of dimethyl sulfoxide and sonication time were considered in order to determine the method with the highest extraction efficiency. All samples were made in three sets and analysis was replicated seven times by HPLC. Results: Acetonitrile and acetone were the optimized as an extraction solvent and desorption efficiency of 2-ring PAHs such as naphthalene, acenaphthylene were increased 3~19% with dimethyl sulfoxide for XAD-2. Acetone was the best extraction solvent for PTFE filter and the desorption efficiency was increased 3~13% for 2- to 4-ring PAHs. The optimum sonication time was 60 minutes and desorption efficiency increased with extraction time. Conclusions: As a result, the best extraction solvent was acetone with dimethyl sulfoxide for ultrasonic extraction procedure and the desorption efficiency of this method was better than NIOSH 5506's. This study could be applied as a method for occupational exposure measurement of PAHs.

The adsorption-desorption behavior of strontium ions with an impregnated resin containing di (2-ethylhexyl) phosphoric acid in aqueous solutions

  • Kalal, Hossein Sid;Khanchi, Ali Reza;Nejatlabbaf, Mojtaba;Almasian, Mohammad Reza;Saberyan, Kamal;Taghiof, Mohammad
    • Advances in environmental research
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    • 제6권4호
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    • pp.301-315
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    • 2017
  • An Amberlite XAD-4 resin impregnated with di(2-ethylhexyl)phosphoric acid was prepared and its adsorption-desorption behaviors with Sr(II) ions under various conditions was examined. The resin was characterized by fourier transform infrared and thermal analysis techniques. The effects contact time, temperature, pH, interfering ions and eluants were studied. Results showed that adsorption of Sr (II) well fitted with pseudo-second-order kinetic model. The equilibrium adsorption data of Sr (II) on the impregnated resin were analyzed by Jossens, Weber-van Vliet, Redlich-Peterson and Fritz-Schlunder models to find out desirable equilibrium condition. Among them, the Fritz-Schlunder model best fitted to the experimental data. The maximum sorption capacity of impregnated resin amounted to 0.45 mg/ g at pH 8.0 and $20^{\circ}C$.