• Bulletin of the Korean Chemical Society
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• 제26권6호
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• pp.943-946
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• 2005

An effective spectrophotometric determination of palladium with 4-(2-pyridylazo)-resorcinol (PAR) using molten naphthalene as a diluent has been studied. A red complex of palladium with PAR is formed at 90 ${^{\circ}C}$. In the range of pH 9.0-11.0, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in $CHCl_3$ to be determined spectrophotometrically at 520 nm against the reagent blank. Beer’s law is obeyed over the concentration range of 0.1-2 ${\mu}g{\cdot}mL^{-1}$. The molar absorptivity and Sandell’s sensitivity are 8.0 ${\times}\;10^5\;L{\cdot}mol^{-1}{\cdot}cm^{-}1\;and\;0.49\;{\mu}g{\cdot}cm^{-2}$ respectively. From the results of tolerance limits, it was found that there was no interferences were observed for most of the ions examined and those somewhat high interferences by Co(II), Fe(II) and Bi(III) could be effectively masked by EDTA.

• 멤브레인
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• 제8권3호
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• pp.138-147
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• 1998

접촉분해 경유에 함유된 유용 방향족 성분(나프탈렌류 성분:탄소수 10-12)의 분리법으로서 추출법과 액막법을 분리성능 면에서 비교했다. 추출법의 용매로서는 dimethylsulfoxide수용액을, 액막법의 막상으로서는 dimethylsulfoxide와 saponin의 혼합수용액을 각각 사용했다. 추출법에서 얻어진 노르말-노난을 기준 성분으로한 나프탈렌류 성분의 선택도는 온도가 낮아짐에 따라 급격히 증가했으나, 액막법에서 얻어진 선택도는 온도에 무관한 경향을 나타내어, 실온에서의 추출법에 의한 나프탈렌류 성분의 선택도는 액막법에서 얻어진 선택도는 온도에 무관한 경향을 나타내어, 실온에서의 추출법에 의한 나프탈렌류 성분의 선택도는 액막법에 비해 컸다. 또, 회분 교반조를 사용하여 두 분리법으로 부터 나프탈렌류 성분의 물질이동속도를 측정한 결과, 추출법의 연속상측 물질이동계수는 액막법의 막상측 투과계수에 비해 약 280배 컸다.

• 한국식품과학회지
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• 제22권5호
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• pp.543-548
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• 1990

살구의 휘발성 향기성분 조성에 대한 분리 방법의 영향을 조사코저 살구 과육(pH 3.1)을 simultaneous distillation-extraction(SDE)법, headspace trapping법 또는 이를 pH 7.0으로 중화시킨 후 SDE법에 의해 얻어진 정유성분의 조성을 분석 비교하였다. GC-MS 및 GC에 의한 표준품과 머무름 시간의 비교에 의해 확인된 80종의 성분들 중 pH3.1에서 SDE법에 의해 얻어진 정유성분중에는 다른 두 가지 방법에 의해 얻어진 정유성분에서는 검출되지 않거나 또는 미량으로 검출된 n-hexanal, trans-2-hexenal, cis-3-hexen-1-ol, linalool oxide, linalool, ${\alpha}-terpineol$, nerol, geraniol, benzyl alcohol, ${\beta}-phenylethyl alcohol$ 및 naphthalene 유도체들이 많이 검출되었으며 이러한 결과는 살구에서 비휘발성인 glycoside 형태로 존재하는 위와 같은 성분들이 산성조건하에서 수증기 증류시 glycoside 결합이 가수분해되어 휘발성 성분으로 유리되는데 기인하는 것으로 판단되었다.

• 한국대기환경학회지
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• 제30권4호
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• pp.362-377
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• 2014

Polycyclic aromatic hydrocarbons (PAHs) have been of particular concern since they are present both in the vapor and particulate phases in ambient air. In this study, a simple method was applied to determine the vapor phase PAHs, and the performance of the new method was evaluated with a conventional method. The simple method was based on adsorption sampling and thermal desorption with GC/MS analysis, which is generally applied to the determination of volatile organic compounds (VOCs) in the air. A combination of Carbotrap (300 mg) and Carbotrap-C (100 mg) sorbents was used as the adsorbent. Target compounds included two rings PAHs such as naphthalene, acenaphthylene, and acenaphthene. Among them, naphthalene was listed as one of the main HAPs together with a number of VOCs in petroleum refining industries in the USA. For comparison purposes, a method based on adsorption sampling and solvent extraction with GC/MS analysis was adopted, which is in principle same as the NIOSH 5515 method. The performance of the adsorption sampling and thermal desorption method was evaluated with respect to repeatabilities, detection limits, linearities, and storage stabilities for target compounds. The analytical repeatabilities of standard samples are all within 20%. Lower detection limits was estimated to be less than 0.1 ppbv. In the results from comparison studies between two methods for real air samples. Although the correlation coefficients were more than 0.9, a systematic difference between the two groups was revealed by the paired t-test (${\alpha}$=0.05). Concentrations of two-rings PAHs determined by adsorption and thermal desorption method consistently higher than those by solvent extraction method. The difference was caused by not only the poor sampling efficiencies of XAD-2 for target PAHs and but also sample losses during the solvent extraction and concentration procedure. This implies that the levels of lower molecular PAHs tend to be underestimated when determined by a conventional PAH method utilizing XAD-2 (and/or PUF) sampling and solvent extraction method. The adsorption sampling and thermal desorption with GC analysis is very simple, rapid, and reliable for lower-molecular weight PAHs. In addition, the method can be used for the measurement of VOCs in the air simultaneously. Therefore, we recommend that the determination of naphthalene, the most volatile PAH, will be better when it is measured by a VOC method instead of a conventional PAH method from a viewpoint of accuracy.

• Bulletin of the Korean Chemical Society
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• 제25권10호
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• pp.1465-1470
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• 2004

A short and efficient synthesis, solvent extraction and potentiometric measurements of new thiazole-containing naphtho-crown ethers are reported. The naphthalene moiety enhances the ammonium ion selectivity over potassium ion. The selectivity of ${NH_4}^+/K^+$ follows the trend $3\;{\approx}\;2\;>\;1$, indicating that the differences in conformational changes of 2 and 3 in forming ammonium complexes affect little on the resulting ammonium/potassium extraction selectivity ratio. The ammonium ion-selective electrodes were prepared with noctylphenyl ether plasticized poly(vinyl chloride) membranes containing 1-4 the effect of one naphthalene unit introduced on either right (2) or left (3) side of thiazolo-crown ether on their potentiometric properties (e.g., ammonium ion selectivity over other cations, response slopes, and detection limits) were not apparent. However, the ammonium ion selectivity of 1, 2 and 3 over other alkali metal and alkaline earth metal cations is 10-100 times higher than that of nonactin.

• 한국지하수토양환경학회지:지하수토양환경
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• 제18권4호
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• pp.1-7
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• 2013

Subcritical water which acts as organic solvent with increasing temperature and pressure because dielectric constant and viscosity decrease can be used to remediate PAHs-contaminated soil. Factors influencing on extraction were studied with varying the water temperature $200{\sim}275^{\circ}C$, extraction time 0~90 min, flow rate 10~100 mL/min and pressure 3.9~10MPa. 300 g of soil sample which was contaminated with PAHs(naphthalene, phenanthrene, fluoranthene and pyrene; 423, 420, 539 and 428 mg/kg of initial concentration) was packed into the cell and placed to reactor and then the subcritical water was pumped through the cell for PAHs extraction. Naphthalene was removed almost 100% at relatively low temperature ($200^{\circ}C$). The removal rate of phenanthrene, fluoranthene, and pyrene increased by 8, 26, and 23% when the temperature increased from 200 to $275^{\circ}C$; and it was gradually increased as extraction time increased from 0 to 90 min. Decreasing removal rate when water flow rate increased from 10 to 30 mL/min, but there was no significant change after 30 mL/min. This is supposed due to channeling phenomenon. The pressure was not an effective factor for extraction of PAHs in this study. Based on the results, the importance of effective factor was in following sequence: temperature >> time > flow rate.

• Korean Chemical Engineering Research
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• 제46권3호
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• pp.555-560
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• 2008

저등급 석탄으로부터 무회분 초청정 석탄 제조를 위하여 온도 $200-430^{\circ}C$, 0.1MPa에서 추출실험을 수행하였다. 세 가지의 서로 다른 등급의 석탄시료를 사용하였으며 추출용매는 극성용매 N-methyl-2-pyrrolidinone(NMP)와 비극성 용매 1-methyl naphthalene(1-MN), Light Cycle Oil(LCO)를 사용하였다. 실험결과 NMP에 의한 추출율이 1-MN이나 LCO에 의한 추출율 보다 높게 나타났다. 그러나 회분농도는 1-MN에 의한 추출탄이 가장 낮았다. 세가지 추출 운전모드, 즉 무교반운전모드, 교반운전모드, 그리고 초음파를 이용한 운전모드를 각각 수행하였다. 추출온도 $350^{\circ}C$에서 NMP를 사용한 추출실험에서, 교반운전모드에서의 추출율 및 추출탄의 회분농도는 각각 70.09wt%(daf), 1.03wt%(db) 이었으며, 초음파를 이용한 운전모드에서의 추출율 및 추출탄의 회분농도는 각각 80.70wt%(daf), 0.76wt%(db) 이었다. 1-MN를 사용한 추출에서도 NMP의 경우와 같이 초음파 추출이 가장 우수한 추출특성을 나타냈다. 초음파를 이용한 추출방법은 교반추출과 비교하여 추출율을 15-20%, 회분 저감은 최대 26% 까지 향상시킬 수 있었다.

• 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.

• Preventive Nutrition and Food Science
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• 제13권1호
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• pp.18-22
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• 2008

Volatile components in field bean (Dolichos lablab) were collected by simultaneous steam distillation and solvent extraction and analyzed by gas chromatography-mass spectrometry. One hundred and five components were identified including alcohols (32), ketones (18), aldehydes (9), acid (1), alkanes (5), aromatics compounds (4), esters (2), furans (2), naphthalene (1), pyrazines (4), pyridine (3), sulfur-containing compounds (4) and terpenes (7) and miscellaneous compounds (13). Relatively high concentration of n-hexanal found in the field bean might be undesirable to some consumers.

• 공업화학
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• 제22권5호
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• pp.495-500
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• 2011

나프타 분해 공정에서 필수적으로 발생되는 분해연료유(PFO, pyrolyzed fuel oil)에서 나프탈렌을 재결정해내고 남는 PFO 잔유물을 이용하여 $300{\sim}800^{\circ}C$에서 질소 조건에서 탄소구조체를 합성하여 보았다. PFO를 헥산이나 메탄올로 처리 후 얻은 탄소물질 프리커서를 열처리하면 $350^{\circ}C$에서는 수 십 ${\mu}m$ 크기의 flake 상의 탄소체가 만들어졌으나, $400^{\circ}C$ 이상에서는 수 ${\mu}m$로 크기가 줄며 공 모양의 탄소구조체로 변형되었다. BET와 XRD 스펙트럼에 따르면 공모양으로 합성된 메조상 탄소체는 큐빅상으로 미세 기공인 mesopore가 아직 잘 발달되지 많은 부정형 탄소임을 알려주고있다.