Photometric determination of small amounts of magnesium in rocks

The method of Mann and Yoe has been adapted to the determination of small amounts of magnesium in a “rapid method” scheme of rock analysis. The effect of calcium is found to be different from that described by the original authors. Tricthanolamine is introduced as a masking agent for aluminum. Anomalous instability of the color system requires a revised photometric technique,     

Design and synthesis of a DNA-crosslinking azinomycin analogue

The azinomycins are potent antitumour antibiotics that are able to crosslink DNA, but are relatively unstable and unlikely to progress as therapeutic candidates. A prototype analogue 4 with more clinical potential has been designed and synthesised and incorporates the epoxide function of the azinomycins and a nitrogen mustard. Two further analogues 5 and 6 that can alkylate DNA but cannot crosslink the duplex have also been synthesised. Compound 4 crosslinks DNA efficiently at nM concentrations. Compounds 4-6 were submitted to the NCI 60 cell line screen and have similar antitumour activity, although 4 is slightly less active than the non-crosslinking compounds. These observations will be important in the design of further azinomycin analogues with antitumour activity.     

新型正极材料三硫代环磷氮烯无机聚合物的合成

采用缩合聚合方法合成了新型三硫代环磷氮烯无机聚合物[(NPS₃)₃]_n，利用红外光谱测试与元素含量分析技术证明了[(NPS₃)₃]_n的分子结构与组成，并对聚合物材料的粒度、比表面积及微观形貌进行了考察。TG/DTA 实验证明材料在200 ℃ 以下具有良好的热稳定性。循环伏安测试表明[(NPS₃)₃]_n正极材料在锂电池体系具有2.15 V的电化学还原电位和2.45 V的电化学氧化电位，经充放电循环实验观察，材料的首次放电容量达到749.0 mAh·g^-1，与理论容量(759.0 mAh·g^-1)十分接近；经过50次充放电循环后，放电容量保持在674.8 mAh·g^-1，具有很高的使用容量和优秀的循环性能。     

Syntheses and oxygenation of iron(II) “strapped” porphyrin complexes

A general route to ‘strapped’ porphyrins which are bridged between diagonally opposite meso-positions is described. Studies on the oxygenation and carbonylation of their iron(II) complexes have shown that they are inferior to ‘capped’ porphyrins as models for the oxygen-carrying haemoproteins. The results reported herein suggest that strapping structures which do not enforce well-defined and rigid cavities for oxygen binding afford little protection against irreversible oxidation of (dioxygen) (porphyrin) iron(II) complexes.     

Qualification of automated low-field NMR relaxometry for quality control of polymers in a production setting

Implementation of a low-field time-domain nuclear magnetic resonance (NMR) scanner as a diagnostic tool in the production of new polymer components is described in the context of qualification of a new QA/QC device. A study to determine the optimal experimental parameters was performed and a robotic autosampler was built to enable scanning of multiple pads. Relationships between T₂ values and physical properties of DC745 slabs were investigated, and the appropriate sampling parameters for the production setting were determined. Two versions of a robotic autosampler were built and, for the component described here, a fourth radial axis was required in addition to traditional X, Y, and Z movement to eliminate the large variability in T₂ due to inconsistent sample coverage caused by the complex rib geometry of the component. Data show that with appropriate choice of experimental conditions of the NMR detector and the detection geometry of the robotic autosampler, sufficient resolution of variations in cross-link density on the millimeter scale could be determined. All data to date demonstrate that low-field NMR devices are a feasible tool for use in production settings for non-destructive quality control of polymer components.     

Local Structure of Glassy Lithium Phosphorus Oxynitride Thin Films: A Combined Experimental and Ab Initio Approach

Lithium phosphorus oxynitride (LiPON) is an amorphous solid-state lithium ion conductor displaying exemplary cyclability against lithium metal anodes. There is no definitive explanation for this stability due to the limited understanding of the structure of LiPON. Herein, we provide a structural model of RF-sputtered LiPON. Information about the short-range structure results from 1D and 2D solid-state NMR experiments. These results are compared with first principles chemical shielding calculations of Li-P-O/N crystals and ab initio molecular dynamics-generated amorphous LiPON models to unequivocally identify the glassy structure as primarily isolated phosphate monomers with N incorporated in both apical and as bridging sites in phosphate dimers. Structural results suggest LiPON′s stability is a result of its glassy character. Free-standing LiPON films are produced that exhibit a high degree of flexibility, highlighting the unique mechanical properties of glassy materials.