直读光谱仪分析不锈钢中氮

直读光谱分析不锈钢中氮含量 ,确定了氮的光谱分析线、最佳分析条件 ,分析样品的制备要求 ,共存元素的影响和氮校准曲线的拟合情况。本法具有良好的准确度和精密度 ,氮元素的分析检出限为6 .3μg/ g,检测范围为 0 .0 0 1%— 0 .4 2 %。     

串联毛细管柱对甲基叔丁基醚产品及其杂质的色谱分析

采用非极性的OV-1柱及极性的FFAP柱串联而成的毛细管柱分析甲基叔丁基醚(MTBE)产品的全组成,该法能完全分离MTBE及其杂质组分,相对标准偏差小于3．5％。具有分离效果好、结果准确、操作简单等优点。     

内置胶囊混凝土的裂缝自愈合行为分析和试验

研究了一种具有裂缝自愈合行为的内置胶囊混凝土．首先,建立了描述修复胶囊在混凝土中的分布和取向函数;然后,根据混凝土的破坏机理,确定了修复胶囊的破坏应力;第三,通过实验分析了修复胶囊的几何参数和体积率对混凝土性能的影响,得到了几何参数和体积率的最佳取值范围;第四,利用ANSYS对修复胶囊进行了有限元分析,确定了其合理的壁厚,为修复胶囊材料的选择提供了一种研究方法;最后,进行了内置胶囊混凝土试验,取得了一定的自愈合效果。     

ARL-4460金属分析仪测定低合金钢中微量五害元素

应用瑞士 ARL- 446 0金属分析仪 (真空光电直读光谱仪 ) ,测定了石油管材 (低合金钢 )中的微量五害元素 (Pb、Sn、As、Sb、Bi)含量 ,优化了分析条件 ,讨论了分析结果和影响因素 ,确定了方法的检出限。本方法具有操作简便、准确度较高、成本低等优点 ,用于炉前快速分析与管材检验 ,取得了满意的效果。     

Photo‐polymerized lauryl methacrylate monolithic columns for CEC using lauroyl peroxide as initiator

Lauryl methacrylate (LMA)‐ester based monolithic columns photo‐polymerized using lauroyl peroxide (LPO) as initiator were prepared, and their morphological and CEC properties were studied. The composition of the polymerization mixture (i.e. ratios of monomers/porogenic solvents, 1,4‐butanediol/1‐propanol and LMA/crosslinker) was optimized. The morphological and chromatographic properties of LMA columns were evaluated by means of SEM pictures and van Deemter plots of PAHs, respectively. The polymerization mixture selected as optimal provided a fast separation of a mixture of PAHs with excellent efficiencies (minimum plate heights of 8.9–11.1 μm). Satisfactory column‐to‐column (RSD<4.5%) and batch‐to‐batch reproducibilities (RSD<6.3%) were achieved. The LMA columns photo‐polymerized with LPO were compared with those prepared with AIBN. Using PAHs, alkylbenzenes and basic compounds for testing, the columns obtained with LPO gave the best compromise between efficiency, resolution and analysis time.     

Optimization of two-dimensional gradient liquid chromatography separations

An almost orthogonal comprehensive two-dimensional liquid chromatography was developed for the separation of phenolic and flavone natural antioxidants by using combinations of a polyethylene glycol silica micro-column in the first dimension and a porous-shell fused-core C18 column in the second dimension, both in the reversed-phase mode. System orthogonality was improved using parallel gradients of acetonitrile in buffered mobile phase. A new approach was proposed to optimize matching segmented gradient profiles in the two dimensions. An algorithm was developed for automatic corrections of the shifts in retention in the second dimension induced by the parallel two-dimensional gradient operation technique. Using the porous-shell C18 column in the second dimension at elevated temperature (60 degrees C) and high pressure (480 bar) with optimized segmented profiles of the parallel gradients in the two dimensions, the overall separation time for comprehensive LC x LC was reduced to 30 min.     

Flow-through pore characteristics of monolithic silicas and their impact on column performance in high-performance liquid chromatography

In order to elucidate the role of the flow-through characteristics with regard to the column performance in high-performance liquid chromatography (HPLC) native and n-octadecyl bonded monolithic silica rods and columns, respectively of 100 mm length and 4.6 mm ID with mesopores in the range between 10 and 25 nm and macropores in the range between 0.7 and 6.0 μm were examined by mercury intrusion/extrusion, scanning electron microscopy, image analysis and permeability. The obtained data of the flow-through pore sizes and porosity values as well as surface-to-volume ratio of the stationary phase skeleton enabled to predict their influence to the chromatographic separation efficiency. Our data demonstrate that mercury porosimetry is a reliable technique to obtain all the characteristic parameters of the flow-through pores of silica monoliths. An important result of our examination was that the surface-to-volume ratio of monolithic silica skeletons had more significant impact to the separation process, rather than the average flow-through pore sizes. We could also show the essential differences between the particulate and monolithic stationary phases based on theoretical computation. The results, obtained from other characterization methods also indicated the structural complexity of monolithic silica samples. Permeability of columns is a generally applicable parameter to characterize all chromatographic phases no matter the chemistry or format. The correlation coefficient obtained for mercury intrusion and permeability of water was 0.998, though our investigation revealed that the surface modification is more likely influencing the obtained results. Further, the assumption of the cylindrical morphology of flow-through pores is not relevant to the investigated monolithic silica columns. These results on the morphology of the flow-through pores and of the skeletons were confirmed by the image analysis as well. Our main finding is that the flow-through pore sizes are not relevant for the estimation of the chromatographic separation efficiency of monolithic silica columns.     

Density gradients in packed columns: I. Effects of density gradients on retention and separation speed

Density gradients in packed capillary columns operating under the extreme pressure drops typical for solvating gas chromatography were investigated by on-column spectroscopic measurements and compared to a theoretical model. Laser-induced fluorescence was used to follow the elution of various analytes, and Raman spectroscopy was used to measure the density of the mobile phase, each with respect to column position. Mobile phase linear velocity initially increases gradually, and then rises rapidly near the column outlet. High flow rates near the column outlet are offset by a loss of mobile phase solvating power which ultimately limits the speed of separation. These results represent an extreme case for illuminating factors affecting supercritical fluid separation techniques in general.     

后加混凝土-砌体组合结构简化计算模型研究

后加混凝土构件的加固方法是在原有砌体结构外部新增钢筋混凝土构件,形成一种新型的组合结构．本文提出了考虑连接节点的后加混凝土构件-砌体组合结构的简化理论计算模型,并推导了不同构件的等效计算公式．考虑均布分布荷载和倒三角分布荷载作用,对组合结构的变形、剪力分配进行计算分析．计算结果从定性方面验证了本文提出的简化计算模型的可行性和有效性．同时针对某实际工程进行理论计算,与三维空间模型在弹性阶段的计算结果进行对比,从定量方面验证了本文提出的简化计算模型的准确性．     

A simplified model for nonlinear dynamic analysis of steel column subjected to impact

This paper presents a new simplified model of the nonlinear dynamic behavior of a steel column subjected to impact loading. In this model, the impacted column, which undergoes large displacement, consists of two rigid bars connected by generalized elastic–plastic hinges where the deformation of the entire steel column as well as the connections is concentrated. The effect of the rest of the structure on the column is modeled by an elastic spring and a point masse both attached to the top end of the column which is also loaded by a compressive force. The plastification of the hinges follows the normality rule with a yield surface that accounts for the interaction between M and N. The latter is described by a super-elliptic yield surface that allows ones to consider a wide range of convex yield criterion by simply varying the roundness factor that affects the shape of the limit surface. By including these features, the model captures both geometry and material nonlinearities. Both the flow rule and the equations of motion are integrated using the midpoint scheme that conserves energy. The non-smooth nature of impact is considered by writing the equations of motion of colliding masses using differential measures. Contact conditions are written in terms of velocity and combined with Newton's law to provide the constitutive law describing interactions between masses during impact. Numerical applications show that the model is able to capture the behavior of a column subjected to impact.