Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002     

盐酸氨溴索在碳糊电极上阳极伏安法的研究

在０．５ ｍｏｌ／Ｌ Ｈ２ＳＯ４底液中，用碳糊电极阳极伏安法测定盐酸氨溴索，被测的阳极峰电位为１．１０Ｖ（ｖｓ．ＳＣＥ），另外，在０．４６Ｖ处还产生一对可逆的氧化还原峰。１．１０ Ｖ处的峰电流与盐酸氨溴索的浓度在３．９８×１０~（－７）～６．３４ × １０~（－５）ｍｏｌ／Ｌ范围内呈良好的线性关系，该方法的检出下限为３．０ × １０~（－８）ｍｏｌ／Ｌ。用标准加入法测得回收率范围为９２．８％～１０２％，ＲＳＤ为２．９％（ｎ＝１０）。对电极响应机理进行了初步探讨，氨溴索在１．１０ Ｖ处的氧化为不可逆过程，其氧化产物在０．４６０Ｖ处产生一对２电子２质子受扩散控制的可逆波，用该波也可进行定量测定并且干扰较少，但灵敏度略低。     

Simultaneous analysis of oxidized and reduced glutathione in cell extracts by capillary zone electrophoresis

Glutathione (GSH) and glutathione disulfide (GSSG) levels in cells constitute a thiol redox system. They can be used as an indicator of oxidative stress of the cell. In this study, a capillary zone electrophoresis (CZE) method is described that enables quantitation of GSH and GSSG from cellular extracts. The CZE buffer used was 20 mM ammonium acetate containing 5% (v/v) acetic acid at pH 3.1 in conjunction with a polybrene coated capillary operated in reverse polarity mode. Effects of different acids used to prepare cell samples were investigated on CZE performance. The acids include meta phosphoric acid (MPA), trichloroacetic acid (TCA), phosphoric acid (PA) and sulfosalicylic acid (SSA) and are used to stabilize GSH and GSSG before performing CZE analysis. The method features a limit of detection of 4 microM and a limit of quantitation of 12 microM for both GSSG and GSH and recoveries of 94% for GSH and 100% for GSSG. Quantitative analysis of GSSG and GSH in HaCaT cell extracts (5% SSA, w/v) was performed with this method and changes in the ratio of GSH to GSSG in N-ethylmaleimide treated cell sample was observed by comparing with control cell samples.     

六甲基环三硅氧烷非平衡聚合的研究

六甲基环三硅氧烷(D_3)在为催化剂,二甲亚砜为促进剂的情况下聚合,得到了分子量分布窄且没有大环体的聚二甲基硅氧烷。本文指出了反应溶液中溶解的氧会降低催化剂的活性。在除去了溶液中的氧以后,聚合反应速度大为加快,D_3转化率几乎达100％,而且得到的聚合物是活性高分子,可以继续进行聚合。同时还研究了在除氧以后D_3非平衡聚合反应的特点。     

Deposition of Oral Bacteria and Polystyrene Particles to Quartz and Dental Enamel in a Parallel Plate and Stagnation Point Flow Chamber

The aim of this paper is to determine to what extent (i) deposition of oral bacteria and polystyrene particles, (ii) onto quartz and dental enamel with and without a salivary conditioning film, (iii) in a parallel plate (PP) and stagnation point (SP) flow chamber and at common Peclet numbers are comparable. All three bacterial strains showed different adhesion behaviors, and even Streptococcus mitis BMS, possessing a similar cell surface hydrophobicity as polystyrene particles, did not mimic polystyrene particles in its adhesion behavior, possibly as a result of the more negative ζ potentials of the polystyrene particles. The stationary endpoint adhesion of all strains, including polystyrene particles, was lower in the presence of a salivary conditioning film, while also desorption probabilities under flow were higher in the presence of a conditioning film than in its absence. Deposition onto quartz and enamel surfaces was different, but without a consistent trend valid for all strains and polystyrene particles. It is concluded that differences in experimental results exist, and the process of bacterial deposition to enamel surfaces cannot be modeled by using polystyrene particles and quartz collector surfaces.     

完全未知混合体系中纯组份的红外光谱解析

提出一种新的目标转化因子分析，其初始向量的构造基于实际最大差异光谱，无需分离即可从红外混合体系中解析出纯组份光谱。该算法简单易懂，不必迭代，运算量小，应用于模拟及实际体系，结果令人满意。     

精神分裂症患者头发5种元素含量变化及临床意义

采用原子吸收光谱法测定了９６例精神分裂症患者和１０１名正常对照组的头发Ｚｎ、Ｃｕ、Ｆｅ、Ｃａ、Ｍｇ元素含量。结果发现，精神分裂症患者头发ｎ和Ｍｇ元素含量明显低于对照组，而Ｃｕ、Ｆｅ和Ｃａ元素含量明显高于对照组。提示精神分裂症的发病，可能与Ｚｎ和Ｍｇ元素含量降低，Ｃｕ、Ｆｅ和Ｃａ元素含量升高有关。     

轻希土硫氰酸盐与2, 3, 11, 12, -四苯基-1, 4, 7, 10, 13, 16-六氧-2, 11-十八环二烯配合物的合成及XPS研究

合成了六种轻希土硫氰酸盐与标题不饱和冠醚的新固体配合物,进行了元素分析,摩尔电导率、DTA、UV、IR和XPS等表征.对Ln(NCS)₃·L和Ln(NCS)₃的XPS研究中,得到它们组成原子芯能级电子(Ln3d_5/2,Ols,Nls,S2p)的结合能信息;观察到除Y3d_5/2外Ln3d_5/2(Ln=La、Ce、Pr、Nd、和Sm)的伴峰结构,Ln3d_5/2结合能与原子序数呈线性关系,并推断类似化合物Pm³d_5/2结合能在1035eV附近.     

Zur Elektronenstruktur metallorganischer Komplexe der f‐Elemente. 64 Äußert sich die zwitterionische Natur des Triphenylphosphanoxid‐Liganden auch in seinen spektrochemischen Eigenschaften?

Electronic Structures of Organometallic Compounds of f Elements. 64 Does the Zwitterionic Nature of the Triphenylphosphine Oxide Ligand Manifest itself in its Spectrochemical Properties? The triphenylphosphine oxide mono adducts of the moiety tris(η⁵‐cyclopentadienyl)lanthanide(III) (Ln(Cp)₃; Ln = Pr ( 1 ), La ( 2 )) were synthesized and structurally characterized. The Ln–O distances of these compounds are noticeably shorter than those of the corresponding THF adducts. A crystal field (CF) analysis of the optical spectra of 1 leads to a low absolute value of the quadratic CF parameter which is comparable with those of [Pr(Cp)₃(L)]^? adducts with anionic bases but not with [Pr(Cp)₃(MeTHF)]. Reasons for the latter finding are presented.     

Preparation of polymide-imides by direct polycondensation with triphenyl phosphite. V. Aliphatic-aromatic polyamide-imides based on N,N′-bis(ω-carboxyalkyl) benzophenone-3,3′,4,4′-tetracarboxylic diimides

Five diimide-dicarboxylic acids were prepared from benzophenone-3,3′,4,4′-tetracarboxylic dianhydride and glycine, β-analine, 4-aminobutyric acid, 6-aminocaproic acid, and 11-aminoundecanoic acid. New aromatic-aliphatic polyamide-imides were prepared by the direct polycondensation of these diacids with aromatic diamines using triphenyl phosphite in N-methyl-2-pyrrolidone (NMP)–Pyridine solution in the presence of calcium chloride. The resulting polymers were characterized by inherent viscosity, infrared spectra, elemental analyses, solubility, differential scanning calorimetry (DSC), thermogravimetry, and wideangle x-ray diffraction measurements.