Adsorption Study of Methane on Activated Meso-carbon Microbeads by Density Functional Theory

A combined method of density functional theory (DFT) and statistics integral equation (SIE) for the determination of the pore size distribution (PSD) is developed based on the experimental adsorption data of nitrogen on activated mesocarbon microbead (AMCMB) at 77K. The pores of AMCMB are described as slit-shaped with PSD.Based on the PSD, methane adsorption and phase behavior are studied by the DFT method. Both nitrogen and methane molecules are modeled as Lennard-Jones spherical molecules, and the well-known Steele‘s 10-4-3 potential is used to represent the interaction between the fluid molecule and the solid wall. In order to test the combined method and the PSD model, the Intelligent Gravimetric Analyzer (IGA-003) was used to measure the adsorption of methane on the AMCMB. The DFT results are in good agreement with the experimental data. Based on these facts,we predict the adsorption amount of methane, which can reach 32.3ω at 299K and 4 MPa. The results indicate that the AMCMBs are a good candidate for adsorptive storage of methane and natural gas. In addition, the capillary condensation and hysteresis phenomenon of methane are also observed at 74.05K.     

半开口立方烷型簇合物[WOS3Cu3I(4-bpy)3]·0.25EtOH的合成及晶体结构(4-bpy=4-叔丁基吡啶)

Reaction of (NH₄)₂[WOS₃] with CuI and 4-tert-butylpyridine (4-bpy) in EtOH afforded a tetranuclear neutral cluster [WOS₃Cu₃I(4-bpy)₃]·0.25EtOH. This compound was characterized by elementary analysis, IR, ¹H NMR, TGA, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group P2/c with a=2.220 9(2) nm, b=1.364 66(11) nm, c=2.490 6(2) nm, β=104.953(2)°, V=7.292 9(12) nm³, Z=4. The title compound may be viewed as having a half-open cubane-like structure in which three [Cu(4-bpy)]⁺ units are linked by a triply-bridging [WOS₃]^2- unit and a doubly-bridging iodine atom. CCDC: 266412.     

Li＋在基于N,N-二甲基甲酰胺混合溶剂中的溶剂化

利用红外和拉曼光谱技术研究了Li^＋在不同浓度、不同溶剂组成的LiBF₄/N,N-二甲基甲酰胺-乙腈、LiBF₄/N,N-二甲基甲酰胺-四氢呋喃电解质溶液中的优先溶剂化现象. 红外和拉曼光谱的分析表明, Li^＋主要与DMF分子相互作用, 导致该分子的C＝O伸缩振动谱带、N—C＝O形变谱带、CH₃摇摆谱带等发生了分裂. Li^＋与其它溶剂分子的相互作用较弱, 谱带的分裂现象并不明显. Li^＋溶剂化数的计算显示, Li^＋第一溶剂化层内DMF分子的数目一般大于2, 这说明 Li^＋在混合溶剂体系内优先与DMF分子相互作用. 量子化学计算支持了这一结论.     

TRANSESTERIFICATION IN POLYPHENYLSILSISQUIOXANE(PPSQ)/POLY ETHYLENE TEREPHTHALATE (PET) BLENDS

The chemical structure of copolymer formed in the transesterification of PPSQ/PET blendsduring melt-processing is deduced from the ~1H-NMR spectra. The transesterification extent ofthis blend is interpreted by the changes of crystalline melting peak in DSC thermograms of the in-soluble products containing unreacted PET and some block PPSQ segments. Effects of composi-tion of blend ladderlike regularity of PPSQ on the reaction extent have also been discussed.Inclusion of some block PPSQ segments in PET has no influence on the crystalline morphology ofPET.     

固相微萃取-气相色谱法测定食品添加剂中有害有机挥发杂质

建立了固相微萃取（SPME）-气相色谱法（GC）测定食品添加剂中有害有机挥发杂质：二氯甲烷、三氯甲烷、苯、三氯乙烯和1、4-二n恶烷的方法。以聚二甲基硅氧烷（PDMS）涂层的萃取纤维萃取糖精钠、柠檬酸、苯甲酸钠溶液中的待测组分。以HP-5毛细管柱为分离柱，火焰离子化检测器（FID）定量测定。优化了固相微萃取条件：萃取纤维、萃取方式、萃取温度、平衡时间、pH及电解质浓度等。在优化的试验条件下，进行了方法的检出限、精密度、回收率试验。5种组分的回收率在97．3％～103．9％之间。     

南海软珊瑚Sarcophyton molle化学成分的研究(一)

从中国南海软珊瑚（Sarcophytonmolle）中分离到三个含氮化合物，其结构经紫外光谱（UV）、红外光谱（IR）、质谱（MS）和核磁共振（1HNMR、13CNMR）分析分别确定为神经酰胺Sinumeramide（Ⅰ），胸腺嘧啶（Ⅱ）和脱氧尿核嘧啶苷（Ⅲ）．本文是首次报导该种属软珊瑚的化学成分。     

低吸光度差示分光光度法测定油品中的铁

将一新的低吸光度差示分光光度法用于油品中铁的测定并与普通分光光度法测定结果的精密度和准确度进行了比较。结果表明，对于低吸光度样品的测定，该法较普通分光光度法准确。同时，该法克服了以前低吸光度差示分光光度法中差示吸光度与样品含量不成线性关系的不足。     

2—（对—十二烷氧基苯基）吡嗪—5—羧酸的合成及其成膜性

在含有吡嗪环的对位双环羧酸化合物中,2-(对-十二烷氧基苯基)吡嗪-5-羧酸具有良好的成膜性。由于引入了推-拉电子的基因,因而分子长轴方向偶极矩较大,分子较舒展、刚直、形成的LB膜取向性较高。这类化合物可能在LB膜等有机功能材料上得到应用。本文报导化合物的合成及其成膜性的初步结果。     

鲍鱼多糖Hal-A的甲醇解研究

从鲍鱼中分离出一种鲍鱼多糖Hal-A，并用改进甲醇解方法研究了Hal-A的组成 ，该多糖甲醇解产物经三甲硅醚衍生后，进行GC/MS，结果表明鲍鱼多糖Hal-A主要 由葡萄糖、半乳糖、甘露糖和少量木糖、岩灌糖和半乳糖醛酸组成。     

用铬黑T作为共振光散射探针测定蛋白质

研究了金属指示剂铬黑T（EBT）作为共振光散射探针测定蛋白质的分析方法。实验表明，在pH=4.10的Britton-Robinson缓冲溶液条件下，铬黑T只有极弱的光散射，它与蛋白质结合后有强烈的共振光散射作用。在λ=375nm处，光散射强度最大，光散射强度与蛋白质的浓度成正比。据此建立了一种测定蛋白质的新方法。该方法简便、快速、灵敏度高，对HSA的检出限达到39μg/L;线性范围为0－15mg/L，用于人体血清样品的分析并用考马斯亮蓝法比较，取得了令人满意的结果。同时亦研究了牛血清白蛋白（BSA）、λ球蛋白、鸡蛋白蛋白、溶菌酶与染料EBT之间的作用。比较了2种不同类型的荧光仪器绘制的共振光散射光谱，并探讨了共振光散射的机理。