电感耦合等离子体原子发射光谱法测定辛酸铑催化剂中铂钯铅铁铜铝镍

准确测定辛酸铑催化剂中杂质元素含量,是判定产品是否合格的重要指标之一。以往常采用直流电弧发射光谱法(摄谱法)进行检测,但测定周期长,且重复性较差。用电感耦合等离子体原子发射光谱法(ICP-AES)测定辛酸铑催化剂中微量杂质元素时,辛酸铑催化剂样品中含有的大量有机组分和铑基体会对测定有严重干扰。实验采用反复滴加硝酸消解样品中有机组分,再用王水溶解盐类,选用合适背景点扣除的方式消除铑基体的干扰,建立了使用ICP-AES测定辛酸铑催化剂中0.001%~0.1%(质量分数)Pt、Pd、Pb、Fe、Cu、Al、Ni等7种微量杂质元素的方法。各元素在0.10~10.00μg/mL范围内与其发射强度呈线性关系,相关系数均大于0.9999;方法检出限(μg/mL)为0.075(Pt)、0.0033(Pd)、0.015(Pb)、0.0036(Fe)、0.010(Cu)、0.001(Al)、0.012(Ni)。实验方法用于测定辛酸铑催化剂样品中Pt、Pd、Pb、Fe、Cu、Al、Ni,结果的相对标准偏差为(RSD,n=7)为1.4%~9.6%。按照实验方法测定辛酸铑催化剂中Pt、Pd、Pb、Fe、Cu、Al、Ni,并与直流电弧发射光谱法的测定结果进行比对,结果相一致。     

高分辨连续光源原子吸收光谱法测定铀铌铅多金属矿中痕量银

铀铌铅多金属矿组成成分复杂,准确有效的测定其中的痕量银,有利于银的回收利用。采用HCl-HNO₃-HF-HClO₄处理铀铌铅多金属矿样品,以HCl(1+4)-2g/L酒石酸为测定介质,以λ_Ag=328.068nm为分析谱线,建立了高分辨连续光源原子吸收光谱法(HR-CS-AAS)测定铀铌铅多金属矿样品中痕量银的新方法。对仪器参数进行了优化,确定采用迭代基线校正(IBC)背景校正方式,CCD检测器有效像素点选择5个;由银的平均吸收光谱图和吸光度-波长-时间三维吸收光谱图可知,银的CCD检测器分辨率为0.0020nm/pixel,λ_Ag=328.068nm在327.86~328.27nm范围内没有受到溶液中其他共存元素的谱线干扰。在优化的实验条件下,银的吸光度与其质量浓度在0.40~1.60μg/mL范围内运用二次方程最小二乘法拟合校准曲线,相关系数为0.9999,特征浓度为0.0148μg/mL,方法检出限为0.0013μg/mL。将HR-CS-AAS测定样品中银的参数与空心阴极灯原子吸收光谱法(HCL-AAS)相比,其检出限更低,特征浓度更低,标准溶液系列的吸光度更高。按照实验方法对铀铌铅多金属矿样品中的银进行测定,结果与电感耦合等离子体质谱法基本一致,相对标准偏差(RSD,n=9)为0.63%~3.3%。按实验方法在铀铌铅多金属矿样品中加入银标准溶液进行加标回收试验,回收率为97%~104%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。     

Insight into selective oxidation of dual-phase steel after annealing in pure H2 atmosphere at different heating rates and temperatures

In this paper, the oxidation behaviors of DP980 advanced high strength steel (AHSS) are studied during annealing in a hydrogen atmosphere with different temperatures and heating rates. It is revealed that with the increase in holding time, the different heating rates affecting the surface oxide precipitation on the strip surface will be weakened. Mass transfer of Mn in heating, soaking, and cooling stages has been considered to illustrate the effect of heating rate on the oxide morphology of steel. And then, the Wagner model and aluminothermic reaction kinetics were performed to discuss the transition from external to internal and maximum reduction diameter of MnO oxidation.     

恒湿文物展柜用吸附式空气取水方法

博物馆恒湿文物展柜的湿度控制至关重要，为实现展柜的自动恒湿功能，本文基于吸附式空气取水原理，提出了一种将环境水汽自动补充至恒湿文物展柜系统水箱的方法，并搭建了相应的小型空气取水装置，证明了该方法的可行性；同时，构建了传热传质耦合的空气取水装置数学模型，在获取环境温湿度对装置取水量的影响规律后，分析加热功率和吸附床结构对装置单位能耗取水量的影响；此外，为便于装置的后期推广应用，提出了两个基于吸附床高度和直径的量纲为1参数。结果表明：进口空气的温度对取水量影响较小，但进口空气的湿度对取水量影响较明显，取水量随着湿度增加而增加；加热功率存在最优值，单位能耗取水量随着加热功率先增大后减小；在当前几何参数组合下，两个量纲为1参数η=2、β=4时，装置的单位能耗取水量最高。     

Experimental and Numerical Studies on the Diffusion of CO2 from Oil to Water

Injecting CO2 into oil reservoirs can improve the oil recovery,meanwhile achieve CO2 storage.The diffusion of CO2 in oil-water systems has a substantial impact on this process.The interface significantly affects the mass transfer of CO2 between oil and water phase.In this paper,based on the determination of the CO2 diffusion coefficient in oil or water phases,the diffusion processes of CO2 from oil to water were experimentally investigated under different pressures.A numerical method was proposed to calculate the pressure drop and the diffusion coefficient in the process of CO2 diffusion from oil to water.The experimental results indicated that the CO2 diffusion coefficient in oil or water increased rapidly with pressure up to the critical pressure of CO2 and gradually slowed down thereafter.The CO2 diffusion from oil to water was much slower than that in oil or water.The diffusion coefficient of CO2 from oil to water was one magnitude lower than that in the single liquid phase of oil or water,and the effect of pressure was not significant.Based on the diffusion coefficient of CO2 in a single liquid phase and the proposed numerical method,the pressure drop and the numerical diffusion coefficient in the process of CO2 diffusion from oil to water were calculated.The relative errors between the experimental and numerical results were within 9%.Therefore,the numerical method proposed herein can be used to predict the diffusion process of CO2 from oil to water and the diffusion coefficient associated with this process.     

Mapping haze-komi on rice koji grains using β-glucuronidase expressing Aspergillus oryzae and mass spectrometry imaging

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PAN纤维共聚单体作用机理的光电离质谱研究

本工作以丙烯腈/衣康酸（IA）二元共聚原丝以及丙烯腈/IA/丙烯酸甲酯（MA）三元共聚原丝为研究对象，利用热重分析仪（TG）和热解-同步辐射真空紫外光电离质谱（Py-SVUV-PIMS）对其热稳定化过程进行研究。TG结果表明，氮气气氛下，二元共聚原丝（PAN/IA）和三元共聚原丝（PAN/IA/MA）分别呈现三阶段和两阶段的热分解过程，其中PAN/IA的第一和第二阶段均对应PAN线型分子链的断裂，但前者是由自由基环化反应放热引发的，后者则是由正常温度下的热分解所致，而单体MA的加入显著抑制了自由基环化反应，使得PAN原丝的热稳定化能够以单体IA诱导的离子型环化反应为主较平缓地进行，相应的热失重过程也由两阶段转变为了单阶段。Py-SVUV-MS的实验结果表明，两种共聚PAN原丝在程序升温过程中会生成包括含氮小分子、丙烯腈单体及低聚物、成环化合物在内的三类主要热解产物，对比各类产物的生成趋势和产量，推断单体MA通过降低PAN结构的规整度，使其无定形化，从而增加环化反应的引发点，促进PAN原丝向稳定的预氧丝转变，同时由典型热解产物——甲基丙烯腈的生成路径可知，MA本身并不参与PAN大分子的环化反应，属于中性共聚单体。空气气氛下，CO₂的产量差异也间接证明了MA单体能够有效提升PAN纤维的固碳能力，采用三元共聚方法制得的PAN纤维热稳定性能更佳。     

龙滩坝8#采场地压监测与结果分析

为掌握龙滩坝8#采场矿体在开采过程中地压的变化规律，在结合现场实际情况的同时，根据开挖揭露的地质条件，采用钻孔应力计、锚杆应力计、收敛计、多点位移计和声发射对采场矿柱、顶板及巷道变形情况进行监测，得到回采过程中矿柱、顶板、巷道的受力状况。掌握采场地压的变化规律，为矿体的开采设计提供参考。     

Soret and Dufour effects between two rectangular plane walls with heat source/sink

This study addresses the thermo‐diffusion and the diffusion‐thermo phenomena in a semi‐infinite absorbent channel whose walls are contracting/expanding, with heat source/sink effects. The governing partial differential equations with suitable boundary conditions are transformed to a system of dimensionless ordinary differential equations. An analytic solution of the problem has been found using a technique called homotopy analysis method (HAM). HAM gives consistently valid answers to the problem over an extensive variety of parameters and also provides better accuracy. To validate the analytical results, a comparison has been presented with a numerical solution calculated by using the parallel shooting method. The effects of dimensionless parameters, that is, deformation parameter, Reynolds number, Soret and Dufour numbers, and heat source/sink parameter on the expressions of velocity, temperature, and concentration profiles are analyzed graphically to understand the physics of the deformable channel. It has been noted that the velocity across the channel is higher for the expanding channel, as compared to that for the contracting channel. Also the Soret and Dufour number increases the temperature of the fluid, and decreases the concentration. The temperature profile has an increasing behavior in the case of heat source, and a decreasing behavior in the case of heat sink.     

固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量

目的建立固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量。方法样品用乙腈提取,经活性炭/氨基复合柱(Envi-Carb/NH_2)净化,经Rxi-5MS石英毛细管色谱柱分离,采用电子轰击源质谱检测,选择离子监测(selective ion monitoring,SIM)模式检测,外标法定量。结果扑草净在2~1000μg/L范围内具有良好的线性关系,相关系数r~2=0.9998。扑草净在5、10、20、50μg/kg 4种条件下,样品加标回收率在95.1%~107.9%,RSD在5.36%~7.77%(n=6),方法检出限为1μg/kg,定量限为4μg/kg。结论该方法操作简单,准确度与精密度较好,能快速简便地检测紫菜中扑草净的残留量。