金属材料分析方法的选择和施行第六讲金属材料中稀土元素的测定(续)

2.萃取分离-CPA-mA分光光度法测定稀土总量(摘自国家标准GB/T 223.49-1994)[适用范围]:碳钢、合金钢、高温合金及精密合金[测定范围]:w(∑RE)0.001%~0.20%[方法提要](1)试样溶解:按试样中总稀土的估计含量称取0.100 0~1.000 0 g试样,置于烧杯中,溶于适量的浓盐酸和浓硝酸的混合     

cotpp-pt/c作直接甲醇燃料电池阴极催化剂

四苯基钴卟啉;pt催化剂;直接甲醇燃料电池;氧还原     

双波长K系数—标准加入吸光光度法同时测定锰和锌

研究应用双波长K系数—标准加入吸光光度法同时测定锰和锌二组分混合物.试验确定了锰和锌测定中K_(Mn)与K_(Zn)的回归方程.对合成试样、人发试样测定,结果满意.     

铜中杂质成分标准物质的研制

介绍铜中9种杂质成分标准物质的研制方法。以1号纯铜为基体，配入硫、铁、铅、锌、镍、铋、锑、磷、砷及锡共10种杂质成分，采用雾化喷粉加工工艺，保证了样品的均匀性。对样品表面作了抗氧化保护处理。采取多家实验室协作定值的方式对除砷外的9种杂质成分进行定值。5年的跟踪检验结果表明，该标准物质稳定性良好。     

A New Reaction-controlled Phase-transfer Catalyst System

A new reaction-controlled phase-transfer catalyst system was designed and synthesized.In this system, heteropolytungstate [C7H7N(CH3)3]9PW9O34 was used for catalytic epoxidation of cyclohexene with H2O2 as the oxidant. The conversion of H2O2 was 100% and the yield of cyclohexene oxide was 87.1% based on cyclohexene. Infrared spectra showed that both fresh catalyst and the recovered catalyst do have completely same absorption peak, indicating the structure of catalyst is very stability and can be recycled.     

Surface functionalization of ordered mesoporous carbons--a comparative study

Hexagonally structured mesoporous carbons C15 and CMK-5 and cubically structured carbon C48 were synthesized using ordered silica SBA-15 and MCM-48 as templates and carbon precursors of different structures. The surfaces of these ordered carbons were chemically functionalized by employing an approach, in which the selected diazonium compounds were in situ generated and reacted with the carbon frameworks of the mesoporous carbons. The aromatic organic molecules containing chlorine, ester, and alkyl groups were covalently attached to the surface of these ordered mesoporous carbons. The presence of functional groups on the modified carbons was confirmed with Fourier transform infrared spectroscopy, thermogravimetric analysis, and nitrogen adsorption. The BET-specific surface area and the pore width of ordered carbons were significantly reduced, whereas the primary structure of these ordered carbons and their unit cells were intact. Basically, the density of grafted functional groups is related to the specific surface area of the sample, particularly the surface area of mesopores. The surface functionalization reaction takes place only on the external surface of carbon C15, while it occurs on both of the internal and external surface of CMK-5 carbon with the nanopipe structure. The presence of the micropores in CMK-5 carbon should be responsible for its lower grafting density because the small micropores are inaccessible in the reaction. It was also proposed that the preferred adsorption/reaction in C48 may be related to the observed unsymmetrical degradation of the XRD patterns for the functionalized C48 samples. The chemical modification process considerably reduced the primary mesopores in these ordered carbons by approximately 1-1.5 nm, affording carbons with micropores in the cases of C15 and C48, and mixed micropores and small mesopores in the case of CMK-5. A grafting density of approximately 0.9-1.5 micromol/m(2) was achieved under current research.     

水热微乳液法合成BaLiF3∶Er3+纳米微粒及表征

采用水/CTAB/正丁醇/正辛烷体系微乳液法及水热技术制备了BaLiF3∶Er3+纳米微粒.利用X射线衍射(XRD)、环境扫描电镜(ESEM)和红外荧光光谱等手段对所制备产物进行了表征.X射线衍射数据表明, 所制备微粒与JCPDS 标准卡片18-715吻合很好, 利用谢乐公式计算所制备产物平均粒径在98.45 nm左右, 与环境扫描电镜观察结果基本相同.BaLiF3∶Er3+纳米微粒的红外发射图谱由4个峰构成, 最强峰位于1540 nm处, 属于Er3+的f→f跃迁.     

Effects of Oxygen and Water Vapor on Volatile Organic Compounds Decomposition Using Gliding Arc Gas Discharge

The combined effects of oxygen and water vapor on three typical volatile organic compounds, i.e. tetrachloromethane, n-butane and toluene, decomposition efficiency under gliding arc gas discharge conditions are studied. The electron density and the density of the reactive radicals such as O and OH are modified by addition of oxygen and water vapor. Consequently, the decomposition process can be enhanced or suppressed, depending on the involved chemical structures and reaction channels. The addition of oxygen and water vapor suppresses the tetrachloromethane decomposition which indicates that this process is mainly controlled by the electron dissociation reactions. By contrast, the n-butane and toluene decompositions are enhanced, which shows that they can be mainly ascribed to the radical induced reactions. Especially, in a moist atmosphere the OH radicals are supposed to play the most important role in the n-butane decomposition process.     

Gear-like array of (H_2O)_(12) as building blocks in one-dimensional supramolecular assembly

The preparation and crystal structure of complex Co(Hsae)_2·2H_2O (1,H_2sae=N-salicylidene-2-iminoethanol) are reported.X- ray analysis revealed that every six Co(Hsae)_2 forms a cyclic chip and every 12 water forms a novel gear-like cluster.Acting as building blocks,the gear-like water cluster and complex chip are connected in A-B fashion and extend into one-dimensional supramolecular chain.Hydrogen bond is the primary bridging force in the formation of supramolecular framework.     

离子对色谱法测定万乳康注射液中淫羊藿苷和盐酸左旋咪唑含量

建立了反相离子对色谱法同时测定万乳康样品中淫羊藿苷和盐酸左旋咪唑的含量。本法使用Shim-pack VP-ODS色谱柱(250×4.6 mm,5μm),该流动相为65%甲醇(V/V),10.0 mmol/L的十二烷基磺酸钠,pH=3.0;等度洗脱样品中的淫羊藿苷和盐酸左旋咪唑。紫外检测波长270 nm。结果表明:淫羊藿苷测定的线性范围为2.73~54.58μg/mL,加标回收率为99.45%~100.69%,理论塔板数达6 641;盐酸左旋咪唑测定的线性范围为26.23~524.54μg/mL,加标回收率为99.58%~100.23%,理论塔板数5 564。该方法可用于淫羊藿提取物和万乳康样品中的淫羊藿苷和盐酸左旋咪唑的测定。