Molecular Weight Measurement of UG8 Asphaltene Using APCI Mass Spectroscopy

Abstract

Asphaltene molecular weight has been a controversial issue in the past several decades and continues on nowadays. From industrial application point of view, asphaltene molecular weight is important for setting up a heavy oil refining strategy so that the process is efficient and economically viable. If the measured average molecular weight of asphaltene is high and is the true molecular weight, then substantial amount of energy will be needed, in order to break the molecule into light products during refining process. This is likely not an economical option. On the other, if the measured high molecular weight is due to self-association and the true molecular weight is low (e.g., less than 1500 Da), it will be energetically attractive to refiners to develop heavy oil cracking technology. Vapor pressure osmometry (VPO) has been routinely used for measuring molecular weight. However, it measures the apparent molecular weight and is likely not the true molecular weight. In order to unambiguously measure the molecular weight, it is necessary to develop a convincing technology and a reliable experimental procedure that allows one to measure the molecular weight accurately and consistently. We chose the Atmospheric Pressure Chemical Ionization (APCI) technique and Atmospheric Pressure Photo Ionization (APPI) to measure UG8 asphaltene. Both APCI and APPI have mild ionization processes and have been applied to many unstable drug compounds such as proteins and peptides with reliable outcomes. In addition, we measured the sample on two APPI instruments to compare the results. We also demonstrated how one can choose wrong set of operating parameters and lead to erroneous results. The relevant parameters for APCI and APPI are temperature, voltage, and sample concentration. We chose 0.01 mg/mL as the concentration, much below any known critical aggregation concentration. As for temperature and ionization voltage, we varied systematically varied (T = 300–600°C; V = 30–150 V) in order to demonstrate the consistency of the methods and how one can easily make mistake. Through these measurements, an average molecular weight of 400 to 900 Da was obtained for UG8 asphaltene.     

Observation and formation mechanism of individual graphene foils inside multi-walled carbon nanotubes

The formation of individual graphene foils (GF) has been evidenced in the present study inside multi-walled carbon nanotubes. The graphene foils are attached on one side to a catalyst nanoparticle and on the other side to the internal walls of the nanotube. Moreover, results suggest that a necking process occurs in which internal carbon walls are deformed until formation of the graphene foil. A possible mechanism for the GF formation is then proposed.     

Grain boundary microstructure and fatigue crack growth in Allvac 718Plus superalloy

The correlation between grain boundary microstructure and fatigue crack growth with hold-times was investigated for two conditions of the superalloy Allvac 718Plus; a Standard condition with the recommended distribution of grain boundary phases and a Clean condition with virtually no grain boundary phases. Fatigue testing was performed at 704 °C using 10 Hz cyclic load with intermittent hold-times of 100 s at maximum tensile load. Microstructural characterization and fractography were conducted using scanning- and transmission electron microscopy techniques. Auger electron- and X-ray photoelectron spectroscopy techniques were used for oxide analyses on fracture surfaces. It was found that in the Standard condition crack growth is mostly transgranular for 10 Hz loading and intergranular for hold-times, while for the Clean condition crack growth is intergranular in both load modes. The lower hold-time crack growth rates in the Standard condition are attributed to grain boundary δ-phase precipitates. No effect of δ-phase was observed for 10 Hz cyclic loading crack growth rates. Two different types of oxides and oxide colours were found on the fracture surfaces in the Standard condition and could be correlated to the different loading modes. For cyclic loading a bright thin Cr-enriched oxide was dominate and for hold-times a dark and slightly thicker Nb-enriched oxide was dominant These oxide types could be related to the oxidation of δ-phase and the matrix respectively. The influence of δ-phase precipitates on crack propagation is discussed.     

Synergistic effect of composite template and La-doping on microdynamic behavior of photogenerated carriers in mesoporous nano-TiO2

The traditional view that the role of the composite template that is adopted in the preparation of nano-TiO₂ is only for forming a pore structure and increasing the material's specific surface area is challenged by this study. The complex impact of the composite template and La-doping on the microdynamic behavior of photo-generation free charge carriers (FCCs) in the mesoporous nano-TiO₂ is investigated using the transient photovoltaic (TPV) technique, supplemented by electric field-induced surface photovoltaic spectroscopy and a computer simulation method. The experimental results reveal that utilizing an appropriate composite template, such as polyethylene glycol and octadecylamine with a molar ratio of 1:1, may result in the rapid separation and prolonged diffusion distance of electron–hole pairs that were excited by a 355 nm and 50 μJ laser pulse. These may be responsible for the stronger and broader TPV response in the microsecond and millisecond regions of the La-doped nano-TiO₂ in TPV spectroscopy, as compared with that for materials that used other composite templates. This response is closely related to the reduced content of the surface state located at 367 nm. A suitable level of La-doping, however, was only responsible for the stronger and broader TPV response in the microsecond region of the spectrum of the nano-TiO₂. The computer simulation results confirm that the photo-generation FCCs microdynamic characteristics in the microsecond region may partially originate from the state density distribution of both the d-electron in the antibonding orbital and the p-electron in the bonding orbital moving up to higher levels, and from a broader band-gap after La-doping in the anatase lattice cell.     

The corrosion behaviour of WC-VC-Co hardmetals in acidic media

The effect of increasing vanadium carbide (VC) content on the corrosion behaviour of tungsten carbide - 10 wt% cobalt hardmetals was investigated in 1 M hydrochloric (HCl), and sulphuric (H₂SO₄) acids solutions. Increasing VC content makes the open circuit potential (OCP) in the test solutions more negative than the base alloy. Specimens exhibited pseudo passivation in all the test solutions. Increasing VC led to decreasing corrosion current density. However, the corrosion current densities during chronoamperometric tests were lower for 0 wt% VC. XRD and Raman spectroscopy showed that hydrated WO₃ formed in the surface films of all specimens in hydrochloric acid (HCl), while hydrated vanadyl sulphate also formed for higher VC content specimens in sulphuric acid (H₂SO₄).     

FTIR研究红外光曝露对于高血糖大鼠的影响

研究红外场曝露对于高血糖疾病模型大鼠的影响.主要利用红外场曝露高血糖大鼠30天,然后通过考查红外场曝露对于高血糖大鼠血液组织红外光谱特征的影响来研究红外线曝露对于大鼠血糖水平产生的影响,研究结果认为红外场曝露有助于高血糖大鼠血糖水平的恢复,并进一步通过红外光谱数据的二阶导数谱的分析探讨了红外场曝露对于大鼠血糖水平产生影响的机理.     

元素俘获测井在库车深层致密砂岩中的应用

库车前陆盆地深层砂岩气藏表现为低孔隙度特低渗透率特征,由于钻井取心少,评价复杂岩性储层存在困难。元素俘获测井(ECS)利用矿物成分获取地层岩性和骨架参数,能够指导评价复杂岩性地层。利用元素俘获测井获取的元素干重百分比,建立反演矿物模型求取矿物的含量。用ECS测井资料获得的矿物含量计算地层变骨架密度(地层骨架密度随深度变化而变化),再计算地层孔隙度,其孔隙度结果与岩心孔隙度基本吻合,验证了ECS测井技术求取地层孔隙度方法的可靠性。对库车前陆盆地深层7口井已知数据的验证,提高了地层孔隙度的解释精度。实践表明,ECS测井技术用于求取塔里木盆地库车深层致密砂岩地层中的储层参数,取得了很好的应用效果。     

Potential of fluorescence spectroscopy in detection of low-levels of gluten in flour: A preliminary study

Celiac disease is caused due to the ingestion of gluten containing food products. Eating gluten free diet is only way to avoid its occurrence. Gluten free products may get contaminated during the handling and processing operation which leads to the adverse impact on the gluten intolerant patients. Three different gluten free mixes were adulterated with two different types of wheat flours to get the gluten concentration in the range of 0–5 % by making 94 sample combinations. The obtained fluorescence spectra from these samples were transformed using multiplicative scatter correction (MSC) pre-processing to develop partial least square regression (PLSR) model for the prediction of low-levels of gluten. The obtained results showed a high value of 0.90 correlation coefficient (R²) with 0.46 % root mean square error of cross-validation (RMSECV). The calibration and prediction models also showed the same R² with root mean square error of calibration (RMSEC) and prediction (RMSEP) of 0.41 % and 0.46 % respectively. Hence fluorescence spectroscopy can be used to estimate the level of adulteration which is helpful for developing a sensor for determination of low-levels of gluten as a rapid and non-invasive method in food applications.     

Polyalkylthiophene thin films and their characterisation with transmission spectroscopy

Polyalkylthiophene thin films have been prepared to enable the characterisation of the films with transmission spectroscopy and profilometry for the first time. The optical properties of the films as a function of annealing temperature are discussed. The changes in absorption with time are related to thermochromism.