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61.
This research presents the results of an experimental study on the determination of pyrolysis behaviour and kinetics of six
crude oils by differential scanning calorimetry (DSC) and thermogravimetry (TG/DTG). Crude oil pyrolysis indicated two main
temperature ranges where loss of mass was observed. The first region between ambient to 400°C was distillation. The second
region between 400 and 600°C was visbreaking and thermal cracking. Arrhenius-type kinetic model is used to determine the kinetic
parameters of crude oils studied. It was observed that as crude oils gets heavier (°API decreases) cracking activation energy
increases. Activation energy of cracking also show a general trend with asphaltene content.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
62.
In this work, an analytical procedure was developed to monitor the ethanolysis of degummed soybean oil (DSO) using Fourier-transformed mid-infrared spectroscopy (FTIR) and methods of multivariate analysis such as principal component analysis (PCA) and partial least squares regression (PLS). The triglycerides (reagents) and ethyl esters (products) involved in ethanolysis were shown to have similar FTIR spectra. However, when the FTIR spectra derived from seven standard mixtures of triolein and ethyl oleate were treated by PCA at the region that represents the CO stretching vibration of ester groups (1700-1800 cm−1), only two principal components (PC) were shown to capture 99.95% of the total spectral variance (92.37% for the former and 7.58% for the latter PC). This observation supported the development of a multivariate calibration model that was based on the PLS regression of the FTIR data. The prevision capability of this model was measured against 40 reaction aliquots whose ester content was previously determined by size exclusion chromatography. Only small discrepancies were observed when the two experimental data sets were treated by linear regression (R2=0.9837) and these deviations were attributed to the occurrence of non-modeled transient species in the reaction mixture (reaction intermediates), particularly at short reaction times. Therefore, the FTIR/PLS model was shown to be a fast and accurate method to predict reaction yields and to follow the in situ kinetics of soybean oil ethanolysis. 相似文献
63.
阳离子交换柱分离-导数光度法测定原油中钒 总被引:1,自引:0,他引:1
以 5Br PADAP为显色剂 ,用阳离子交换柱分离干扰离子 ,在波长 6 30nm采用一阶导数光度法测定原油中钒 ,方法灵敏度高 ,摩尔吸光系数为 3.0× 10 5L·mol- 1·cm- 1,较其它光度法测定钒的摩尔吸光系数提高 1~ 2个数量级。对实际样品进行分析并做加标回收试验 ,钒的回收率在97.5 %~ 10 4 .0 %。与ICP AES方法进行对照试验 ,结果相吻合。 相似文献
64.
Fernández-Varela R Suárez-Rodríguez D Gómez-Carracedo MP Andrade JM Fernández E Muniategui S Prada D 《Talanta》2005,68(1):116-125
The combination of attenuated total reflectance-fourier transform mid-infrared spectrometry (ATR-FTMIR) and multivariate pattern recognition is presented as a fast and convenient methodology to ascertain the source product an oil slick comes from and to evaluate the extent of its weathering. Different types of hydrocarbons (including crude oils, several heavy distillates and the Prestige's heavy fuel oil) were spilled on metallic containers designed ad hoc and their fate monitored by ATR-FTMIR. Not only environmental conditions were considered for weathering but artificial IR- and UV-irradiation. Pattern-recognition studies revealed that the different hydrocarbons clustered at different locations on the score plots and that the samples corresponding to each oil became ordered according to the extent of their weathering. Among them, fuel oil samples coming from the recent disaster of the Prestige tanker off the Galician shoreline showed a distinctive behaviour. Comparison of natural-, IR- and UV-weathering of a crude oil showed that IR solar radiation can be important in oil-weathering, in addition to broadly-reported UV degradation. 相似文献
65.
66.
人造芥子油中异硫氰酸烯丙酯与硫氰酸烯丙酯的气相色谱分析 总被引:4,自引:0,他引:4
采用2m×3mm玻璃柱,涂布0.5%EGA的80~100目GaschromQ为固定相,以异辛醇为内标物,分析芥子油中异硫氰酸烯丙酯与硫氰酸烯丙酯异构体。该方法既可用于人造芥子油的含量分析,也可用于市售芥子油的质量鉴定。 相似文献
67.
N. A. Talzhanov D. T. Sadyrbekov F. M. Smagulova R. M. Mukanov V. A. Raldugin M. M. Shakirov A. V. Tkachev G. A. Atazhanova B. I. Tuleuov S. M. Adekenov 《Chemistry of Natural Compounds》2005,41(2):178-181
Chemical components from the aerial part of the Kazakhstan population of Artemisia pontica, from which the rarely encountered flavonoids 7-O-methyl- and 4′,7-di-O-methyl-esters of apigenin were isolated for the first time, were identified. The complete chemical composition of the essential oil was established using GC-MS.__________Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 143–145, March–April, 2005. 相似文献
68.
Isotope dilution determination of polycyclic aromatic hydrocarbons in olive pomace oil by gas chromatography-mass spectrometry 总被引:2,自引:0,他引:2
Diletti G Scortichini G Scarpone R Gatti G Torreti L Migliorati G 《Journal of chromatography. A》2005,1062(2):247-254
A gas chromatographic (GC) method with mass spectrometry detection (MS) for the determination of eight polycyclic aromatic hydrocarbons (PAHs) in olive pomace oil has been developed. The oil was diluted with n-pentane and extracted by liquid-liquid partition with dimethyl sulphoxide (DMSO). After water addition and back-extraction with cyclohexane, a thin-layer chromatography on silica gel was performed as a further purification step. The PAHs spot was scraped off from the plate and the final extract was concentrated and analysed by GC-MS in full scan mode. The eight PAHs under investigation were determined in the presence of the corresponding labelled compounds added as internal standards to the sample at the beginning of the analytical process. The identified PAHs were then quantified by the isotope dilution methodology assuring the compensation of the concentration of each analyte for any variation in the sample preparation. The method precision was satisfactory with relative standard deviation (R.S.D.) values in the range 3.6-12.7% for all PAHs. The average recovery rates ranged from 69.0 to 97.5%. Accuracy was also calculated for benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-cd]pyrene and benzo[ghi]perylene by analysing a certified reference material (CRM 458, coconut oil) with adequate results. All response curves exhibited a linear fit from 0.1 to 10 microg ml(-1) and the determination coefficients R2 were better than 0.9942. The limits of detection (0.1-0.4 microg kg(-1)) were acceptable when compared with the maximum permitted limit of 2 microg kg(-1) for each of the eight considered PAHs and 5 microg kg(-1) for the sum of the eight PAHs established by the Italian legislation. Measurement uncertainty was finally calculated identifying and quantifying the uncertainty components of the analytical process. The relative expanded uncertainties (Uc), expressed as percent values were in the range 8.5-11.4% thus appropriate for residues quantification in the range of concentrations considered in the present study. 相似文献
69.
J. López-Cervantes D.I. Sánchez-Machado J. Simal-Lozano P. Paseiro-Losada 《Chromatographia》2003,58(5-6):321-326
Summary A high-performance liquid-chromatographic method with UV detection (HPLC–UV) has been developed for quantification of ethylene terephthalate oligomers in olive oil, from which they were extracted with acetonitrile. Oligomers, from monomers (M1) to pentamers (M5), were jointly and/or individually identified by liquid chromatography with mass spectrometry (electron-impact mass spectrometry (EIMS) low- and high-resolution) and were quantified by HPLC–UV using an acetonitrile solution of the major oligomer (the trimer M3) as standard. For M3 recovery was 98.9%, the detection limit was 60 g L–2, and method precision was 2.03% (RSD). Migration of oligomers M1–M5 into 50 mL olive oil sealed in each of two brands of 10 cm × 10 cm poly(ethylene terephthalate) roasting bag was evaluated under two sets of conditions that approached but remained below the limit at which the bag material became physically deformed – heating for 7 min at 850 W in a microwave oven, or for 60 min at 200 °C in a conventional oven. Total migration was approximately 2.7 mg dm–2 under the former conditions and 3.5–4.1 mg dm–2 under the latter.Presented at the International Symposium on Separation and Characteristics of Natural and Synthetic Macromolecules, Amsterdam, The Netherlands, February 5–7, 2003 相似文献
70.
人参挥发油的提取和分析 总被引:7,自引:0,他引:7
应用GC-MS-DS联机分析人参挥发油是当前较好的方法,但人参挥发油的提取方法和GC-MS条件的选择明显影响人参挥发油这一复杂天然混合物的分离和鉴定。本工作严格控制提取条件,提高了挥发油收率,达0.95%;选择最佳GC-MS条件,鉴定出76种化合物,该法稳定重现性好。 相似文献