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《分析测试技术与仪器》2009,15(1):62-63
一种蜂蜜中氯霉素残留量的液相色谱-串联质谱测定方法;一种油品中饱和烃、芳烃、胶质、沥青质含量测定方法;一种同时检测血或尿中多种酚酸类化合物的测定方法;一种鲎试剂质量的监测方法;对样品中元素进行定量或者半定量性测定的流动分析系统 相似文献
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将沙特轻质原油的减压渣油在395℃临氮条件下进行热反应,利用在线取样装置得到不同热反应时间的样品,借助小角X射线散射(SAXS)技术,测定了各液相残渣油中沥青质聚集体尺寸。结果表明,热反应生焦诱导期的初期沥青质聚集体的尺寸逐渐减小,为29~21 nm;在生焦诱导期后期,其尺寸急剧增大,在热反应进行到150 min时达到43 nm;达到生焦诱导期后,沥青质聚集体尺寸变化较小,在46~42 nm变化。在渣油热反应过程中沥青质聚集体的尺寸受沥青质热裂解、沥青质解缔和缔合等过程的共同影响,与沥青质含量无明显关系。 相似文献
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对比了大港常压渣油临氮和临氢热反应过程中的胶体稳定性变化。结果表明,随着反应时间的延长,在热反应生焦诱导期内,渣油样品的胶体稳定性迅速下降;开始生焦后,胶体稳定性缓慢下降。从组分组成和组分性质角度,对大港常压渣油样品在热反应过程中胶体稳定性变化原因进行了分析。结果表明,随着反应时间的延长,沥青质含量先上升、后下降,在生焦诱导期结束时达到最大值,与体系胶体稳定性的变化特征相一致。随着热反应的进行,饱和分和轻芳烃组分的含量在上升,重芳烃、轻胶质、中胶质、重胶质含量下降,临氮热反应过程中轻胶质、中胶质、重胶质含量的下降更为显著。对渣油样品各组分的数均相对分子质量和平均偶极矩进行了研究。结果表明,随着热反应的进行,轻、中、重胶质组分的数均相对分子质量和平均偶极矩呈下降趋势,而沥青质的数均相对分子质量和偶极矩先增大后减小,从而使沥青质和胶质的分子性质差别先增加后减小,与体系胶体稳定性的变化趋势一致;同时沥青质的偶极矩变化表明,强极性的沥青质优先聚集生焦、临氢热反应过程中,氢与催化剂的作用有助于抑制沥青质分子量增大和极性增强,从而有助于抑制生焦。 相似文献
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液化气中元素硫的高效液相色谱法分析 总被引:6,自引:0,他引:6
应用溶剂萃取、冷却气化方法对液化气样品进行前处理。对前处理制备的样品使用高效液相色谱法进行测定,以甲醇/水=95/5(V/V)为流动相,紫外检测(254nm),在C18柱上成功地分离并测定了元素硫的含量。方法检测限为0.1ng/g,有良好的准确度与精密度,能充分满足各种液化气中元素硫的测定需要。 相似文献
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以塔河常渣脱沥青油掺兑不同含量的沥青质为原料,于高压釜反应器内进行加氢转化反应实验,考察沥青质含量对渣油加氢转化残渣油收率和性质的影响。研究结果表明,随原料中沥青质含量的增加,加氢残渣油的收率逐渐降低,加氢残渣油中的沥青质和焦炭产量之和与原料中沥青质含量的比值逐渐减小,在实验选定的条件下,高沥青质含量时沥青质更倾向于发生氢解反应生成小分子组分。与原料相比,反应后所得>350 ℃残渣油的平均相对分子质量、H/C摩尔比减小,密度增大,硫含量降低,氮含量增加,饱和分和沥青质含量增加,芳香分及胶质含量降低。随渣油中沥青质含量的增加,硫、氮脱除率先增加后降低。 相似文献
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渣油重组分沥青质结构分析及其对临氢热反应过程生焦的影响 《燃料化学学报》2016,44(3):357-365
以塔河常压渣油(THAR)为原料,正己烷为溶剂分离获得重组分C6-沥青质及其脱沥青油,并将所得沥青质回调至脱沥青油中配制成不同沥青质含量的渣油,以此为原料进行了高压釜临氢热反应实验。首先利用元素分析、1H-NM R及13CNM R、GPC分子量测定、FT-IR、XRD及SEM对沥青质的分子结构参数、官能团、晶体结构及表面形貌进行了分析研究。结果表明,该沥青质芳环侧链中长链部分较少且支链化程度较高,并以甲基、乙基、丙基结构为主,其芳香度fA高达0.57,芳环缩合程度及芳香片层结构较大,且芳香环系同时存在迫位缩合和渺位缩合的结构,已经形成连接致密的高芳香度结构。鉴于沥青质结构的复杂性,考察了其含量对临氢热反应过程的影响,结果表明,随着沥青质含量的增加,渣油的转化率逐渐增加,当沥青质含量超过5.12%时,其转化率的增加以快速生成焦炭为代价。另外,渣油中长链脂碳含量f3C与轻质油收率存在一定规律性,即随着f3C增加,轻质油收率先增加后趋于平缓,而残炭值、芳香度fA与焦炭收率表现出良好的线性关系。 相似文献
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Near infrared emission spectroscopy (NIRES) allows the determination of the induction time (IT) of edible oils in accelerated oxidation experiments by monitoring the emissivity of a band at 2900 nm, which corresponds to the formation of hydroperoxides. In this work, a new near infrared emission photometer dedicated to the determination of oxidative stability is described. The photometer presents several advantages compared to the previously reported NIRES instrument, such as lower cost and extreme simplicity of design and maintenance. The results obtained in the evaluation of the proposed instrument were compared with the official Rancimat method and instrument. The significant advantages include: faster analysis, lower sample consumption and operational simplicity. It is demonstrated that the procedure for determination of oxidative stability of oils can be significantly simplified and performed by measuring the sample emission at only one spectral region centered at 2900 nm. Also, the proposed instrument and method present precision equivalent to the Rancimat method (coefficient of variation = 5.0%). A significant correlation between the methods has been found (R2 = 0.81). 相似文献
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Mohammad Tavakkoli Vahid Taghikhani Mahmoud Reza Pishvaie Mohsen Masihi Sai R. Panuganti 《Journal of Dispersion Science and Technology》2014,35(8):1155-1162
The presence of asphaltene means additional difficulties related to transport and processing due to the increased crude oil viscosity caused by the asphaltene. For a better knowledge of the flow properties of asphaltene containing crude oils, it is necessary to understand how asphaltene affects the rheological properties. The aim of this article is to provide information on such rheological properties of oil–asphaltene slurry systems. The results of rheological experiments show that the non-Newtonian flow curves can be approximated by the Bingham plastic model to determine the apparent viscosity and the yield stress as a function of asphaltene concentration and temperature. An explanation is also provided for the observed behavior. 相似文献
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Near-infrared (NIR) spectroscopy in the range 1100-2250 nm together with a latent-variable regression technique is used to analyze the content of asphaltene and resins in solution. It is shown that this technique is capable of determining the amount of these components individually. w/o emulsions were prepared from the separated components of asphaltenes and resins from crude oils. The stability was directly determined with the critical voltage in a dielectric instrumentation. The emulsion stability decreased linearly with an increase in the resin/asphaltene ratio. A final linear model correlating the critical voltage and the analytical concentrations (from the NIR spectra) could be established for this model system. Copyright 2000 Academic Press. 相似文献
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Determination of trace elements in olive oil by ICP-AES and ETA-AAS: A pilot study on the geographical characterization 总被引:5,自引:0,他引:5
The determination of trace elements in edible oils is important because of both the metabolic role of metals and possibilities for adulteration detection and oil characterization.The most commonly used techniques for the determination of metals in oil samples are inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectrometry (AAS). For this study, a microwave assisted decomposition of the olive oil in closed vessels using a mixture of nitric acid and hydrogen peroxide was applied as sample preparation.The low achievable LODs enable the determination by ICP-AES of even very low concentrations of most elements of interest. The proposed ICP-AES method permits the determination of Ca, Fe, Mg, Na, and Zn in olive oils. Elements present in small amounts (Al, Co, Cu, K, Mn, Ni) were measured by ETA-AAS in the same sample digest. The concentrations of Al, Co, Cu, K, Mn, and Ni were in the range from 0.15 to 1.5 μg/g and differ according to the geographical origin of the oils. For the amounts of Fe, Mg, Na, and Zn in the samples, no significant differences according to the geographical origin of the oils could be observed, the mean concentrations being 15.31, 3.26, 33.10, and 3.39 μg/g, respectively. The Ca content varies in the range of 1.3 to 9.0 μg/g.The dependency of the trace elemental content of olive oils on their geographical origin can be used for their local characterization. 相似文献
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Vahid Chalangaran Hamed Firoozinia Riyaz Kharrat Navid Chalangaran 《Journal of Dispersion Science and Technology》2014,35(3):313-321
The usefulness of the asphaltene deposition envelope (ADE) is that no asphaltene flocculation occurs at conditions outside the envelope. Since artificial neural network (ANN) is best at identifying patterns or trends in data, it is well suited for prediction or forecasting needs. ANN is also capable of addressing case specific problems that may be encountered in the field such as deposition of asphaltene. In this article, the high pressure, high temperature setup used to perform pressure depletion experiments at three different temperatures on one the Iranian live oils and the ADE generated using ANN. 相似文献
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Yun Li Yongqiang Xiong Qianyong Liang Chenchen Fang Chunjiang Wang 《Journal of chromatography. A》2010,1217(22):3561-3566
In this study, headspace single-drop microextraction (HS-SDME) coupled with gas chromatography-flame ionization detection (GC-FID), was employed to determine short-chain fatty acids (SCFAs) in ruthenium tetroxide (RuO4) oxidation products of asphaltenes. Several significant parameters, such as drop solvent type, drop volume, sample solution ionic strength, agitation speed, extraction time, and ratio of headspace volume to sample volume were optimized. Under optimum extraction conditions (i.e., a 3-μL drop of 1-butanol, 20 min exposure to the headspace of a 6 mL aqueous sample placed in a 10 mL vial, stirring at 1000 rpm at room temperature, and 30% (w/v) NaCl content), the reproducibility and accuracy of the method have been tested and found to be satisfactory. The analysis of a real asphaltene sample using this method proved that HS-SDME can be a promising tool for the determination of volatile SCFAs in complex matrices. 相似文献
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离子液体对稠油的改质降黏作用影响因素研究 总被引:1,自引:0,他引:1
合成了烷基咪唑型离子液体\[BMIM\]\[AlCl4\],研究了稠油含硫量、含水量、过渡金属盐、温度等对离子液体进行稠油改质降黏作用的影响。实验结果表明,稠油含一定硫量是进行稠油改质降黏的必要条件。用\[BMIM\]\[AlCl4\]离子液体对稠油进行有效的改质降黏时,稠油含水量应小于10%。环烷酸镍(NiNaph)与离子液体复配使用对稠油改质降黏具有增效作用。用质量分数为5%的\[BMIM\]\[AlCl4\]离子液体在一定条件下处理新疆稠油,可使稠油降黏率达到60%,沥青质降低78%。用\[BMIM\]\[AlCl4\] 离子液体对新疆稠油进行改质降黏的最佳温度为65℃~85℃。 相似文献
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The 2,3,5-triphenyltetrazolium chloride (TTC) method for the determination of reducing carbonyl groups in cellulose in water
suspensions has been thoroughly evaluated. By reduction of TTC in alkaline medium, triphenylformazane (formazane) is produced.
It is thermally unstable and an unavoidable loss results in a relatively high detection limit for the determination of reducing
carbonyl groups in most celluloses with a low content of such groups. Besides, oxidized cellulose is unstable in the alkaline
media in which the reaction is performed. The determined content of reducing groups has also been shown to be affected by
the amount of sample, indicating that absorption of triphenylformazane takes place. A new method for determination of reducing
carbonyl groups in cellulose in homogeneous medium has been developed. Cellulose is dissolved in the solvent system LiCl/N,N-dimethylacetamide and reacts with TTC in the presence of tert-butylamine at 75 °C for 10 min and formazane is subsequently determined spectrophotometrically at 524 nm. None of the systematic errors inherent
in the “aqueous” suspension method can be defined. The new procedure is also more reproducible and has a lower detection limit
of 7 nmol reducing groups in a given mass of sample. The two procedures have been tested on five differently oxidised cellulose
samples and the difference in the determinations are discussed.
Received: 4 March 1996/Revised: 21 May 1996/Accepted: 25 May 1996 相似文献
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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