본 연구에서는 지방 알코올을 이용하여 탄소 길이에 따른 술폰산계 음이온 계면활성제를 합성하였으며, 합성한 계면활성제들의 구조를 FT-IR과 1H NMR 분석을 통하여 확인하였다. 음이온 계면활성제의 임계미셀농도(critical micelle concentration: cmc)는 10-5∼10-3mol/L이며, 임계미셀농도에서의 표면장력 값은 26∼32 mN/m이었다. 합성한 술폰산계 계면활성제의 분자당 최소 영역값은 1.68∼1.30nm2이다. 음이온 계면활성제의 분자당 최소 영역이 감소하였다. 합성한 계면활성제의 물성은 임계미셀농도, 기포력, 유화력, 접촉각을 측정하였다.

Detergency and surface active properties of mixed anionic surfactants with amphoteric and nonionic were investigated. Sodium dodecyl sulfate (SDS) and ammonium dodecyl sulfate (ADS) as anionic surfactants and cocamidopropyl betaine (CAPB) as an amphoteric surfactant were used. Nonionic surfactants, which are butyl glucoside (BG), octyl glucoside (OG), decyl glucoside (DG), lauryl dimethylamine oxide (AO) and saponin were also used. To study the synergy effects of mixed SDS/ADS anionic surfactant systems, amphoteric and nonionic surfactants were added into the mixed anionic surfactants. Investigated properties of surfactant mixtures were critical micelle concentration (CMC), surface tension (γ), wettability. In addition, based on these properties, detergency of each sample was examined. Surfactant mixtures are anionics (SDS/ADS), anionic/amphoteric/nonionic (SDS/ADS/CAPB/ saponin), and anionic/nonionic (SDS/ADS/BG/saponin, SDS/ADS/OG/saponin, SDS/ADS/ DG/saponin, and SDS/ADS/AO/saponin). With the addition of amphoteric and nonionic to mixed anionic surfactants, CMC and γ were decreased. Addition of CAPB, which is amphoteric, showed the best property at CMC and γ. Furthermore, as the chain length of hydrocarbon in alkyl glucosides was increased, the CMC and γ were enhanced. However, the wettability did not exactly match up with CMC and γ. The surfactant mixture, which contained DG, showed the best performance at wetting time. Detergency was measured at various temperatures (15 oC, 30 oC, 50 oC). The cleaning performance was enhanced by increasing washing temperature. Moreover, detergency was influenced by not only CMC and γ but also wettability. Although CMC and γ were not minimum at surfactant mixture that included DG, the best cleaning performance showed in that sample.

In this study, we developed and validated microanalysis methods for the determination of linear alkylbenzenesulfonate (LAS), sodium lauryl sulfate (SLS), and alpha olefin sulfonate (AOS). The conditions for the analysis of the surfactants using HPLC with FLD, RID, and ELSD detectors were investigated. The methods were validated by determining the linearity, limits of detection (LODs), limits of quantification (LOQs), recovery, precision, and accuracy. LAS analysis by FLD revealed calibration curves that were linear in the range of 10-200 mg/L for an LAS mixture. The calibration curves for C10-C13 had correlation coefficients of 0.995, 0.997, 0.996, and 0.997, respectively. SLS analysis using RID generated a linear calibration curve in the range of 10-300 mg/L. The calibration curve for SLS C12 had a correlation coefficient of 0.9994. AOS analysis using ELSD resulted in a correlation coefficient of 0.9940. For LAS, the LODs and LOQs were 0.09-0.56 and 0.30-1.87 mg/L, respectively. For SLS C12, the LOD and LOQ were 0.07 and 2.33 mg/L, respectively. For AOS C14, the LOD and LOQ were 16.55 and 21.83 mg/L, respectively. The recoveries were 97.17-98.84% for LAS C10-C14, 97.94% for SLS C12, and 96.11% for AOS C14. The established methods provide acceptable precision and accuracy. Our methods could be useful for the detection of anionic surfactants in dishwashing detergents.

본 연구에서는 계면활성제 분석법의 개발을 위하여 High performance liquid chromatography-evaporative light scattering detection(HPLC-ELSD) 기기를 이용하여 음이온 및 비이온 계면활성제 중 다소비 계면활성제인 Alkyl polyglucoside(APG)와 Alpha olefin sulfonate(AOS)를 분석하였다. 실험 결과 APG와 AOS 모두 직선성의 상관관계 계수(R2)가 0.99 이상으로 직선성이 양호하였으며, 검출한계는 APG가 2.29 mg/L, AOS가 16.55 mg/L로 나타났고, 정량한계는 APG가 7.63 mg/L, AOS가 55.16 mg/L로 나타났다. 또한, 회수율 검증을 실시한 결과 APG는 99.29%, AOS는 96.11%로 나타나 회수율 100±10% 이내의 검증기준을 모두 만족하였다. 정밀성 및 정확성을 판단한 결과 APG의 정밀성은 상대표준편차 0.30%, 정확성은 0.26-0.52%로 분석되었으며, AOS의 정밀성은 상대표준편차 0.10%, 정확성은 0.01-0.52%로 분석되어 모두 상대표준편차 1.0% 이하의 검증기준에 적합하였다. 확립된 분석법을 주방세제에 적용하여 분석한 결과 샘플 3종 모두에서 APG와 AOS가 각각 검출되었으며, 표준사용량을 기준으로 APG, AOS의 평균 함유량은 각각의 LD50에 크게 미치지 못하는 것으로 나타났다. 따라서 본 연구를 통하여 확립된 음이온 및 비이온 계면활성제의 분석법은 모든 성분에 대해 감응함으로 한가지 검출기를 이용하여 여러성분을 동시에 측정할 수 있어 식기 등의 잔류물질 혹은 식품 중 혼입되어 있는 다양한 계면활성제 함유량 분석에 적용하여 계면활성제의 관리를 위한 기초자료로 활용될 것으로 본다.

Silicone dioxide absorbed polyoxyethylene alkylether sulfate (EU-S133D) surfactant was prepared. Core-shell polymers of inorganic/organic pair, which have both core and shell component, were synthesized by sequential emulsion polymerization using Acrylate as a shell monomer and potassium persulfate (KPS) as an initiator. We found that when Acrylate core prepared by adding 2.0 wt% EU-S133D, silicone dioxide/Acrylate core-shell polymerization was carried out on the surface of silicone dioxide particle without forming the new silicone dioxide particle during acrylate shell polymerization in the inorganic/organic core-shell polymer preparation. The structure of core-shell polymer were investigated by measuring to the thermal decomposition of polymer composite using thermogravimetric analyzer and morphology of latex by scanning electron microscope(SEM).

The inorganic-organic composite particles with core-shell structure were polymerized by using styrene and potassium persulfate (KPS) as a shell monomer and an initiator, respectively. We studied the effect of surfactants on the core-shell structure of silicone dioxide/styrene composite particles polymerized in the presence of sodium dodecyl sulfate(SDS), polyoxyethylene alkylether sulfate (EU-S133D), and at none surfactant condition. We found that SiO2 core / polystyrene(PS) shell structure was formed when polymerization of styrene was conducted on the surface of SiO2 particles, and the concentration SDS and EU-Sl33D was 8.34×10-2mole/L. The core-shell structure was confirmed by measuring the thermal decomposition of the polymer composite using thermogravimetric analyzer (TGA), and the morphology of the composite particles was characterized by transmission electron microscope (TEM).

The core-shell composite particles of inorganic/organic were polymerized by using styrene(St) as a shell monomer and potassium persulfate (KPS) as an initiator. We studied the effect of core-shell structure of silicone dioxide/styrene in the presence of an anionic surfactant sodium lauryl sulfate (SLS) and polyoxyethylene alky lether sulfate (EU-S133D). We found that when SiO2 core/PSt shell polymerization was prepared on the surface SiO2 particle, to minimize the coagulation during the shell polymerization, the optimum conditions were at concentration of 2.56×10-2mole/L SLS. The structure of core-shell polymer was confirmed by measuring the thermal decomposition of polymer composite using thermogravimetric analyzer and morphology of core-shell polymer particles by transmission electron microscope (TEM).

The core-shell latex particles were prepared by sequential emulsion polymerization using alkyl methacrylate as a shell monomer and potassium persulfate (KPS) as an initiator. We study the effects of core-shell structure of calcium carbonate/alkyl methacrlyate in the presence of an anionic surfactant sodium lauryl sulfate (SLS) and polyoxyethylene alkyl ether sulfate (EU-S133D)). The structure of core-shell polymer were investigated by measuring to the thermal decomposition of polymer composite using thermogravimetric analyzer and morphology of latex by transmission electron microscope (TEM).

Oligomer type anionic surfactants(RmM-Na or RmD-Na were synthesized from C8~C16 long chain alkylvinylether and maleic anhydride (or maleic diethylether). And also their fluorescent anionic surfactants (RmF- Na) were obtained from alkali neutralization which opens the lactone ring of the condensing materials produced by maleic anhydride alkylvinylether copolymer and 3-aminophenol. The measurement results for the surface active properties of water soluble oligomer type anionic surfactants with fluorescent structure (RmF-Na) exhibited a remarkable surface tension lowing property, foam breaking property, and a ernulsing power.

Density, viscosity, conductance, dye solubility and carbon-13 nmr studies were performed in aqueous solution of three disodium 4-n-alkyl-3-sulfonatosuccinate anionic surfactant at 20℃. The cmc values were 0.14 mol/l for the disodium-4-n-octyl-3-sulfonatosuccinate(R8)S), 0.041mol/l for the disodium-4-n-decyl-3-sulfonatosuccinate(R10S), and 0.018mol/l for the disodium-n-dodecyl-3-sulfonatosuccinate 〈R12S). The aggregation numbers determined viscometrically and conductimetrically were 28 for R8S, 48 for R10S, and 67 for R12S. The volume changes upon micellization were 8.9cm3/mol for R8S, 9.5cm3/mol for R10S, and 10.1cm3/mol for R12S. Binding constants for the dye pada to the micelles and the fractions of unbound counter-ion were also obtained. The two polar heads with their carbon linkage were likely in an aqueous environment in the R8S micelles with the micelles themselves being spherical.

The sodium α-sulfo fatty acid vinyl ester oligomers, which are oligomer type surfactants were prepared by polymerization with fatty acid vinyl acetate. The α-sulfonation of fatty acid vinyl ester oligomers were carried by direct addition of sulfur trioxide. The dispersing performance of oligomer type anionic surfactants and sodium dodecyl sulfate(SDS) in the aqueous suspension of iron oxide and titanium dioxide particles was evaluated by particle size distribution and zeta-potential measurement. As results, the particles of iron oxide and titanium dioxide were flocculated by addition of small amount of oligomer type anionic surfactants and sodium dodecyl sulfate(SDS), then the flocks redispersed by more addition of oligomer type anionic surfactants and SDS. The flocculation, redispersion process was observed in lower concentration range of oligomer type anionic surfactants than SDS. Especially, the dispersing action of sodium α-sulfo palmitic acid vinyl ester oligomer was better than sodium α-sulfo lauric acid vinyl ester oligomer.

A series of long chain N-acyl amino acid type anionic surfactants were prepared by treating fatty acid chlorides with three kinds of amino acids, that is, sodium N-acyl-sarcosinates, sodium N-acyl-N-methyl-β-alaninates and sodium N-acyl-N-methyl-taurates in an alkaline solution. All prepared biodegradable surfactants were purified by thin layer chromatography and column chromatography, and identified their structures by spectral analysis.

Fluorescent anionic oligo surfactants were synthesized by the condensing products of long chain alkylvinylether-maleic anhydride cooligomers and resorcinol including dye structures. Their various surface activities and dispersing action were studied on the aqueous solution. These oligo surfactants exhibited a remarkable surface tension lowering property, lower foaming and a large dispersing action for the particles of α-copper phthalocyanine blue. Further it was ascertained that the binding of oligo surfactant onto the pigment surface caused the deviation towards lower wavelengths at the maximum fluorescent intensity as compared with aqueous oligo surfactant solutions, These surface active properties of the oligo surfactants may be attributed to rigid and hydrophobic structure of dye groups, besides surface-active groups of alkylether groups and carboxylic group of the anionic oligo surfactants.

The adsorption of the anionic surfactants, sodium lauryl sulfate (SLS) and sodium dodecylbenzene sulfonate (SDBS) anion surfactants from aqueous solutions with nonionic resins, Amberlite XAD-2, XAD-4 and XAD-7 at temperatures in 15∼45℃ range was studied. Several adsorption isotherm models were used to fit the experimental data. The best results were obtained with the Redlich-Peterson equation and the Freundlich model provided remarkably good fits. For a particular resin at a particular temperature, SDBS was more extensively adsorbed than SLS. The highest adsorption were obtained with XAD-4 resin and the specific surface area of the resins plays a major role in adsorption of the surfactants. Estimations of the isosteric heat of adsorption were indicative of an exothermic process, and their magnitudes manifested a physisorption process.