항공유에 fatty acid methyl esters (FAME)가 혼합될 경우 연료 공급시스템과 항공기 엔진에 치명적인 고장의 원인이 될 수 있기 때문에 항공유 품질규격에서 FAME 함량을 50 mg/kg 이하로 규정 하고 있다. 무수히 많은 탄화수소로 구성된 항공유 중의 FAME 성분을 선택적으로 분석하기 어렵기 때문에 본 연구에서는 MDGC-MS를 사용한 새로운 시험방법을 개발하였다. Deans switching 시스템이 설치된 MDGC-MS를 이용하면 코코넛 오일이나 팜유 유래의 저분자량 FAME 성분도 분석이 가능함을 확인하였다. 개발된 시험방법은 FAME 피크의 머무름 시간을 약간 뒤로 이동시키는 매질 효과(matrix effect)를 현행의 기준 시험방법(IP 585)보다 약 20배 이하로 감소시킬 수 있었다. MDGC-MS는 항공 유에 미량의 FAME가 오염되었는지 여부를 정성 및 정량적으로 확인할 수 있는 시험방법으로 적합하였다.
고급지방산 메틸 에스테르류의 소포제를 합성하고 FT-IR과 1H-NMR 분석을 통해 확인하였 다. FT-IR을 이용하여 합성된 물질의 특징인 -C=O기는 1740 cm-1 부근에서, 그리고 C-O기는 1175 cm-1 피크 값을 가지는 것을 확인하였다. 또한 1H-NMR 분석을 통해 에스테르의 -C=O의 Chemical shift가 2.29 ppm에서 나타나는 것을 확인하였다.
표면장력은 Surface Tensiometer CBVP-43을 이용하여 측정하였다. 표면장력은 17.7에서 21 dyne/cm 값을 가진다. SLS 수용액에서의 소포능은 Ross-Miles법을 통해 측정되었다. 4종류의 소포제 중 소포능 은 스테아르산메틸을 이용하여 제조한 소포제가 가장 뛰어난 것으로 측정됐다.
It is known that the content of saturated fatty acids methyl ester (SFAME) affect the pour point of biodiesel at low temperature. In this study, biodiesel (BD) was produced from beef tallow (TAL) by alkali catalyst. To reduce the saturation in BD, acetone fractionation was applied. Besides, TAL was also solvent-fractionated to reduce the saturated fatty acid (SFA) content for further producing BD. With acetone, TAL or TAL methyl ester (5:1 v/w) were fractionated at 10, 0, -10, and -15℃, respectively. At -10℃, 17.35% of SFA was observed in fractionated TAL (liquid part, -10TAL) when 5:1 solvent ratio was used for 24 hr. Under the same condition, fractionated BD (liquid part, -10BD) showed SFA (33.14%) with 78wt % yield. Also, fractionation of BD with different concentration of crystallizer 209 (0.1, 0.5, and 1%) along with different time (2, 6, 12, and 24 hr.) was observed. The best condition for reducing the SFA was 0.5% of crystallizer 209 addition for 12 hr of fractionation time at -10℃, in which 30.14% of SFA content was observed in BD (liquid part). Among different crystallizer, ps 66 showed the least content of SFA content (23.28%) in BD after fractionation (-10℃ and 24 hr) with 0.5wt% addition.
The effects of procedures for preparation of fatty acid methyl esters for gas chromatography were investigated. A quantitative comparison of four procedures for the preparation of the fatty acid methyl esters from Korean sesame seed lipids which can be representative of fatty acid ranges of Korean vegetable oils has been made. The procedures employed were BF3-methanol, HCI-methanol, sodium methoxide-methanol, and tetramethylammonium hydroxide-methanol. Twelve fatty acids ranged from 14:0 to 24:0 were identified in the lipids from Korean white and black sesame seeds. All four procedures gave similar results for the fatty acids, 16:0, 18:0, 18:1, 18:2, and 18:3 present in the range of 1~44% but only in the HCI-methanol procedure, the fatty acids, 16:1, 20:0, 22:0, 24:0 present in the range of 0.02~1% showed the lowest values. When using tetramethylammonium hydroxide-methanol procedure for determination of total fatty acid composition from white and black sesame seed lipids, unsaponifiable matters including sesamol, sesamolin and sesamin present in the seed lipids are not removed from the resulting reaction mixture. Thus the transesterification mixture is used without further treatment for injection into the gas chromatography. However, the gas chromatographic analysis of the transesterification mixture showed that the unsaponifiable matters had no effect on the fatty acid composition of the seed lipids. From the results, it appears that the BF3-methanol, sodium methoxide-methanol and tetramethylammonium hydroxide-methanol procedures can be used to prepare fatty acid methyl esters from Korean vegetable oils. Among the methods, the tetramethylammonium hydroxide-methanol procedure, which give total fatty acid composition, glyceride fatty acid composition and composition of free fatty acids present, appears to be a simple, convenient and quantitative procedure and applicable to samples containing broad ranges of fatty acids.