• Korean Chemical Engineering Research
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• 제55권3호
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• pp.287-295
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• 2017

Using nanotechnology, magnetic nanoparticles of iron oxide were produced via co-precipitation method and followed modification with organic compounds. In the next step, functionalized monomer was provided via coupling ${\beta}$-cyclodextrine and allylamine onto modified magnetic nanoparticles. These nanoparticles were used to establish the adsorption rate of celecoxib. Magnetic nanoparticles are modified by (3-mercaptopropyl)trimethoxysilane. Nano-adsorbent was characterized by analytical and spectroscopic methods, such as Fourier transform infrared spectroscopy, elemental analysis, thermo-gravimetric analysis, and transmission electron microscopy (TEM). Laboratory parameters, such as the kinetics of adsorption isotherms, pH, reaction temperature and capacity were optimized. Finally, by using this nano-adsorbent in the optimized condition, extraction of celecoxib from biological samples as urine, drug matrix and blood plasma was carried out by high performance liquid chromatography with sensitivity and high accuracy.

• 공업화학
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• 제29권3호
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• pp.356-361
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• 2018

혈액과 같이 다성분으로 이루어진 복잡한 matrix로 구성된 시료에서 휘발성 유기화합물(VOC)이나 반휘발성 유기화합물(SVOC)의 분석은 분리공정을 거쳐 분석되는 것이 일반적이다. 흡착은 어떤 성분이 다른 상의 표면에 축적되는 물리적 현상이다. 전처리 과정에서 번거로움을 극복하기 위해 흡착이 적용되며 이를 위해 다공성 탄소인 carboxen (CAR)이 도포된 solid phase microextraction (SPME) 장치가 흔히 사용된다. 본 연구에서는 플라스틱 제조시 가소제 등으로 사용되는 4-octylphenol의 carboxen에 대한 흡착특성을 살펴보았다. 이를 위해 dichloromethane ($CH_2Cl_2$, DCM), ethylacetate ($CH_3COOC_2H_5$, EA) 및 diethylether ($C_2H_5OC_2H_5$, $Et_2O$)에 대한 추출효율과 bistrimethylsilyltrifluoroacetamide (BSTFA), methylchloroformate (MCF) 및 pentafluorobenzylbromide (PFBBr)에 대한 유도체화 반응의 특성을 조사하였다. 열역학적 특성 파악을 위한 추출용제로는 DCM이 양호한 효과를 보였으며 BSTFA를 이용한 silylation의 분석특성이 우수하여 이를 적용하였다. 열역학적 및 동력학적 흡착실험 결과 흡착과정은 흡열특성을 보였고 Langmuir식보다는 Freundlich 등온식에 더 근접하였으며 동력학적으로는 pseudo-$2^{nd}$ order kinetic model에 따르는 것을 보였다.

• Bulletin of the Korean Chemical Society
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• 제27권1호
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• pp.77-81
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• 2006

The commercially available Amberlite XAD-2 and XAD-4 resins were modified with macrocyclic protoporphyrin IX (PPIX) or tetrakis(p-carboxyphenyl) porphyrin (TCPP) to enhance the adsorption capacity for phenol and chlorophenols. The chemically modified polymeric adsorbents (XAD-2+PPIX, XAD-2+TCPP, XAD-4+PPIX, and XAD-4+TCPP) were applied to the solid phase extraction as an adsorbent material for the preconcentration of phenol and chlorophenols in environmental waters. Generally, the synthesized adsorbents showed higher recoveries than underivatized adsorbents, XAD-2 and XAD-4, without matrix interferences. Especially, XAD-4+PPIX showed more than 90% recoveries for all compounds used in this study including hydrophilic phenol. The major factor for the increase of the adsorption capacity was the increase of $\pi$-$\pi$ interaction between adsorbents and samples due to the introduction of the porphyrin molecule. However, the breakthrough volumes and recovery values of the XADs+TCPP columns were slightly decreased for the bulky chlorophenols such as TCP and PCP. Using molecular mechanics methods, the structures of TCPP and PPIX were compared with that of porphine, the parent molecule of porphyrin. Four bulky p-carboxyphenyl groups of TCPP were torsional each other, thus the molecular plane of TCPP were not on the same level. In conclusion, the decrease of breakthrough volumes and recovery values of XADs+TCPP columns for bulky phenols can be explained by the steric hindrance of the $\pi$-$\pi$ interaction between porphyrin plane and the phenols.

• 대한화학회지
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• 제58권3호
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• pp.283-288
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• 2014

A column solid phase extraction procedure based on modified polyurethane foam (PUF) by a newly synthesized Schiff base ionophore, named 2,2'-{iminobis[propane-3,1-diylnitrilo(1E)prop-1-yl-1-ylidene]}diphenol, was developed for preconcentration step of trace amounts determination of copper ions in water samples by atomic absorption flame spectroscopy. The influence of parameters on the adsorption process such as sample pH, amount of modified PUF packed in the column, type and volume of stripping reagent and its flow rate were investigated and optimized. Under optimum experimental conditions, the calibration graph was linear in a relatively wide range ($0.005-210{\mu}g/ml$) with a limit of detection $0.002{\mu}g/ml$ of copper. The proposed method allows achieving to a concentration factor of >133. The capacity of a column (1.6 cm i.d.) packed by 6 g of PUF modified by 12 mg of the Schiff base was found to be $247.7({\pm}2.1){\mu}g$ of copper. It was found that the adsorption process was highly selective towards copper ions with respect to some associated metal ions. The presented procedure was successfully applied for determination of copper in some water samples.

• 대한화학회지
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• 제14권1호
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• pp.97-107
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• 1970

액체 구조의 천이상태 이론을 써서 고체 표면에 기체가 흡착된 계에 대한 상태합을 유도하였다. 이 상태합을 써서 아르곤, 질소, 벤젠 등이 여러 가지 흡착제에 흡착되었을 때의 흡착등온 곡선을 계산하였으며, 이 계산 값들은 측정치와의 좋은 일치를 보여 준다. 그리고 벤젠이 흑연 표면에 흡착되었을 때의 표면압, 물엔트로피, 물에너지, 몰흡착열 들을 계산하였다. 몰엔트로피는 표면이 단분자층으로 완전히 덮였을 때 최소값을 갖는다. 아울러 흡착에 관여된 여러 가지 물리적인 성질들의 계산 방법을 설명하였다.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1557-1561
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• 2006

The use of chemically modified silica-salen$(NEt_2)_2$ was studied for the separation and concentration of the metal ions from an aqueous solution by a solid phase extraction. After the salen(NEt2)2 was synthesized, it was chemically bonded to silica gel by a diazonium coupling reaction. The adsorption capacities and binding constants were obtained with respect to Cu(II), Mn(II), Pb(II) and Zn(II) by a graphical method. Some experimental conditions were optimized for the determination of the trace elements. After the silica-salen(NEt2)2 was pulverized in a sample solution of which the pH was adjusted, the solution was stirred to pre-concentrate the metal ions. The metal ions adsorbed were desorbed with nitric acid solution. And the concentrated analytes were determined by a flame AAS. The method proposed here was so rarely influenced by a sample matrix that the procedure was applied to 3 types of water samples. The reproducible results of less than 10% RSD were obtained at the concentration level of ca. 100 ng/mL and the recoveries of 95-109% were obtained in the spiked samples in which given amounts of analytes were added.

• Bulletin of the Korean Chemical Society
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• 제28권12호
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• pp.2389-2395
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• 2007

Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

• Bulletin of the Korean Chemical Society
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• 제30권11호
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• pp.2675-2679
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• 2009

This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

• 대한의용생체공학회:의공학회지
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• 제14권3호
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• pp.209-220
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• 1993

Microspheres are expected to be applied to biomedical areas such as solid-phase immunoassays, drug delivery systems, Immunomagnetic cell separation. To synthesize micro-spheres for biomedical application, "two stage shot growth method" was developed. The uniformity ratio or synthesized microspheres was always smatter than 1.05. And the surface charge density (or the number of ionizable functional groups) of the microspheres synthesized by "two stage shot growth method" was 6-13 times higher than thats of the ml crospheres synthesized by conventional seeded batch copolymerization. As a previous step for biomedical application, adsorption experiments of bovine albumin on microspheres were carried out under various conditions. The maximum adsorbed amount was obtained in the neighborhood of pH 4.5. Isoelectric point of bovine albumin Is pH 5.0, so experimental result shows that it shifted to acid area. The adsorption Isotherm was obtained, the plateau region was always reached at 2.Og/L (bulk concentration of bovine albumin ) . The effect of the kind and the amount of surface functional group was also examined.p was also examined.

• 상하수도학회지
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• 제19권6호
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• pp.713-719
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• 2005

SPME (Soild phase microextraction) has been used in the analysis of many volatile organic compounds, such as geosmin and 2-methylisoborneol (2-MIB), trihalomethanes (THMs) in drinking water. SPME fiber is characterized by high adsorption capacity (DVB/CAR/PDMS, DVB/PDMS etc.). Although the highly active adsorption capacities of the SPME fiber are often to the chemical functional group, surface properties play a significant role in determining the surface adsorption capacities. The objectives of this study were to evaluate effect of residual chlorine on analysis of geosmin and 2-MIB. Image taken by SEM before preloaded with chlorine, the surface and porous media was almost perfect spherical shape and no clogging of pores. However, after preloaded with chlorine the surface was aggregated and pore was blocked. The recovery rate of geosmin and 2-MIB coexisting with chlorine was reduced by 35 to 62%. The recovery rate with preloaded with chlorine was reduced by 25 to 43%. The lower concentration of geosmin and 2-MIB and the higher concentration of chlorine existed in water, the lower the recovery rate was.