Finnigan Mat 4515色/质联用仪真空系统的维护与维修

叙述大型精密仪器Finnigan Mat4515色/质联用仪的真空系统的维护与维修,利用报废的旧仪器零部件,在技术上稍加改动,便可修复即将报废的色/质联用仪,使其继续发挥作用,为科研工作赢得了时间.投资少,见效快,事半功倍,具有一定的经济和社会效益,是维修旧的大型仪器的有效途径.     

理学D/MAX—1400全自动X射线衍射仪真空及其控制电路故障部位判定和排除

在简要介绍真空控制流程图的基础上,选择了TMP轴承受损、TMP叶轮打烂、电路参数改变TMP加速过快OLL报警烧保险、转靶磁密封不良VAC1报警、供电缺相过流保护和真空控制放大器自激离子规衰老等6个有代表性的、已排除的故障实例进行深入分析研究,提出了排除故障的思路和方法。     

Trace 1300气相色谱仪故障排查与期间核查

使用赛默飞Trace 1300气相色谱仪进行环境样品分析过程中,出现了FID信号变弱、点火困难的现象,严重影响检测数据的准确性,干扰正常分析工作。从样品性质、仪器方法的设置、气路系统以及检测系统进行故障排查,确定故障原因为FID喷嘴堵塞,点火线圈锈蚀严重。对维修好后的气相色谱仪进行期间核查,核查结果:基线噪声为0.066 pA,基线漂移(30 min)为0.321 pA,FID检测限为0.094 1 ng/s,定性重复性为0.062%,定量重复性为1.41%,均满足技术指标要求。     

H-800型电镜真空系统故障部位判定和维修

本文将“故障要因图”法应用于电镜真空系统的维修中,作出了H-800型透射电镜真空系统的故障要因图,并依据这一要因图对H-800型电镜真空系统的实际故障进行分析,比较准确地判定了故障部位,指出利用故障要因图分析和查找电镜真空系统故障的部位和原因能取得好的效果。     

JASCO-1500凝胶色谱仪的维护与故障排除

介绍了JASCO-1500型凝胶色谱仪的原理、应用及维护,对使用过程中的常见故障进行了分析与排除.     

色质联用仪真空系统维护经验点滴

叙述了大型精密色质联用仪高真空系统在日常工作中的维护和维修以及出现的部分故障与排除方法.     

VITALAB21型半自动生化分析仪常见故障及故障排除方法

介绍VITALAB21型半自动生化分析仪常见故障、故障原因及故障排除方法。     

液相色谱的故障排除——自动进样器的维护

介绍了自动进样器的工作原理,讨论了使用中经常遇到的问题及其解决的办法。     

霍尼韦尔2140型硅酸根离子分析仪的常见故障及故障排除方法

介绍了美国霍尼韦尔2140型在线硅酸根离子分析仪的特点、日常维护的注意事项、常见故障及故障排除方法.     

超高真空条件下表面辅助反应

在金属单晶表面上直接合成制备各种共价键连接聚合结构,由于其独特的路线及在电子学、光电子学等方面的潜在应用价值而得到了广泛的关注。与传统的有机合成反应不同,表面辅助反应能够在一定程度上控制产物的结构,知悉具体的反应过程,更重要的是还能制备一些采用传统方法所不能得到的新型材料。前驱体分子的种类、衬底的选择以及反应条件等因素都与反应的发生紧密相关。在表面上制备出的有序共价组装结构除了比传统的自组装单层膜(SAMs)结构具有更高的机械强度及热力学稳定性外,分子间连接的共价键还能作为电子传输的通道,使其应用范围得到很大地扩展。本文对近年来报道的超高真空环境下的一些表面辅助反应进行了介绍,分析了各个反应发生的机理,并将其与溶液中发生的反应相对比,讨论了衬底表面在反应过程中所起到的重要作用。     

Enlarged Area A-type Zeolite Membranes Prepared by Vacuum Seeding Method

High quality A-type zeolite membranes, with enlarged area over 70 cm^2, were successfully synthesized on a tubular ~-A1203 support by applying the vacuum seeding method.     

Tunable Surface Area,Porosity, and Function in Conjugated Microporous Polymers

Simple inorganic salts are used to tune N‐containing conjugated microporous polymers (CMPs) synthesized by Buchwald–Hartwig (BH) cross‐coupling reactions. Poly(triphenylamine), PTPA, initially shows a broad distribution of micropores, mesopores, and macropores. However, the addition of inorganic salts affects all porous network properties significantly: the pore size distribution is narrowed to the microporous range only, mimicking COFs and MOFs; the BET surface area is radically improved from 58 m² g^?1 to 1152 m² g^?1; and variations of the anion and cation sizes are used to fine‐tune the surface area of PTPA, with the surface area showing a gradual decrease with an increase in the ionic radius of salts. The effect of the salt on the physical properties of the polymer is attributed to adjusting and optimizing the Hansen solubility parameters (HSPs) of solvents for the growing polymer, and named the Beijing–Xi'an Jiaotong (BXJ) method.     

Tunable Surface Area,Porosity, and Function in Conjugated Microporous Polymers

Simple inorganic salts are used to tune N‐containing conjugated microporous polymers (CMPs) synthesized by Buchwald–Hartwig (BH) cross‐coupling reactions. Poly(triphenylamine), PTPA, initially shows a broad distribution of micropores, mesopores, and macropores. However, the addition of inorganic salts affects all porous network properties significantly: the pore size distribution is narrowed to the microporous range only, mimicking COFs and MOFs; the BET surface area is radically improved from 58 m² g^?1 to 1152 m² g^?1; and variations of the anion and cation sizes are used to fine‐tune the surface area of PTPA, with the surface area showing a gradual decrease with an increase in the ionic radius of salts. The effect of the salt on the physical properties of the polymer is attributed to adjusting and optimizing the Hansen solubility parameters (HSPs) of solvents for the growing polymer, and named the Beijing–Xi'an Jiaotong (BXJ) method.     

A Capacity Supercapacitor Electrode Material of Ni-MOF with High Surface Area and Porosity

Materials with high surface area, tailored pore size and good electrical conductivity are needed for improved supercapacitors(SCs). Metal-organic frameworks(MOFs) have high surface areas and tailored pore sizes. Here, the MOF(1) of [Ni3(μ3 OH)(pba)3(bpdc)1.5]·11.5 DMA· 0.5 CH3 OH·7 H_2O is good enough to result in electrode materials with nearly ideal supercapacitive behavior at the rate up to 50 mV?s-1 in a KOH electrolyte. The super capacitive performance of MOF(1) was measured using cyclic voltammogram, galvanostatic discharge and electrochemical impedance spectroscopy measurements. This MOF(1) as electrode exhibits the highest super capacitive properties with 417 F?g-1, the maximum storage energy and power density are 9.27 and 2.38 kW?kg-1. The long term stability of MOF(1) as SCs is checked that the capacitance is decreased by 17% after 1000 cycles.     

Heat Treatment Condition Influence on Novokuibyshevsk Vacuum Residue Component Composition

The article presents the information about thermal degradation of Novokuibyshevsk vacuum residue and change of products composition during this process. The optimal conditions for the thermal destruction of vacuum residue components were established. The regularities of material balance composition change, S_general were determined depending on cracking conditions. The basic directions of resin-asphaltene component transformations were identified, changes in their structural-group parameters in the process of initiated cracking were analyzed. Conducting of Novokuibyshevsk vacuum residue thermolysis leads to deep resins-asphaltenes average molecules structure characteristic changes. Developed alkyl and naphthenic moieties, which are presented in initial molecule, undergo degradation, amount of structural blocks in resins and asphaltenes molecules reduces, their average size decreases. Also the reduction in total content of the rings (saturated and aromatic) was established in average structural unit, at the same time decrease of rings substitution and length of the aliphatic fragments can be observed. In general the process of vacuum residue thermal cracking causes partial degradation of saturated (aliphatic and naphthenic) fragments and, partially, aromatic rings, which contain heteroatomic elements.     

共轴双脉冲激光诱导击穿光谱和最小二乘支持向量机法定量分析植物油中铬

利用共轴双脉冲激光诱导击穿光谱( DP-LIBS)技术对植物油(大豆油、花生油和玉米油)中的重金属铬( Cr)含量进行定量分析。采用Ava-Spec双通道高精度光谱仪采集样品的LIBS光谱,然后通过其LIBS谱线图确定了CN分子谱线(421.49 nm)、Ca原子谱线(422.64 nm)及Cr的3条原子谱线(425.39、427.43和428.87 nm),根据上述谱线建立了Cr元素的单变量定标模型和最小二乘支持向量机(LS-SVM)校正模型,并用验证样品对它们进行检验。研究结果表明,对于单变量定标法,大豆油、花生油及玉米油验证样品的平均预测相对误差(PRE)分别为12.57%,12.11%和13.72%;对于三变量LS-SVM法,其定标样品真实值与预测值之间的拟合度 R2分别为0.9785,0.9792和0.9654,验证样品的平均 PRE 分别为8.92%,8.33%和10.98%;对于五变量LS-SVM法(增加两基体元素谱线变量),其定标样品真实值与预测值之间的拟合度R2分别为0.9895,0.9901和0.9855,验证样品的平均PRE分别为7.46%,8.96%和8.95%。由此可知,LS-SVM校正模型性能优于单变量定标法,且五变量LS-SVM校正模型性能优于三变量LS-SVM校正模型;采用LS-SVM法及引入合适的基体元素谱线( CN、Ca)能有效减小定量分析误差,提高LIBS技术对植物油中Cr含量预测的精度。     

真空冷冻干燥制备高比表面积纳米氧化铝

采用真空冷冻干燥技术结合反相微乳液法, 于环己烷/聚乙二醇辛基苯基醚(曲拉通X-100)-十六烷基三甲基溴化铵(CTAB)/正丁醇/水溶液体系中, 合成了纳米Al2O3粉体. 采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)及比表面积与孔隙度分析仪对产物的形貌、结构、比表面积、孔容与孔径进行了表征. 经过煅烧, 该纳米Al2O3比表面积约550.0 m2·g-1(随反应参数不同而变化), 属γ-Al2O3晶型, 粒径均匀, 颗粒直径小于10.0 nm. 考察了不同的干燥方式(电热鼓风干燥、普通真空干燥、真空冷冻干燥)以及真空冷冻干燥过程中主要参数对产物比表面积、孔容、平均孔径等物理性质的影响. 结果表明, 采用真空冷冻干燥法制备的纳米Al2O3的比表面积和孔容远高于采用另外两种干燥方式制备的纳米Al2O3. 采用真空冷冻干燥法制备纳米Al2O3时, 降温速率、预冻时间、冻干时间等参数对最终制备的产物比表面积与孔结构有显著影响.     

离子色谱仪维护及常见故障排除

简述了离子色谱仪的原理,详细介绍了离子色谱仪各个部件的日常维护。分析了在离子色谱仪日常使用中容易出现的故障,并提出了解决办法,有助于离子色谱仪器的有效工作并延长仪器使用寿命。