凹面光栅整体组合狭缝五通道原子吸收式血液五元素分析仪的研制

自行研制了一种凹面光栅整体组合狭缝五通道原子吸收式血液五元素分析仪,用于人全血中5种元素Ca,Cu,Mg,Fe和Zn的测定.采用1支五元素空心阴极灯作为光源,以单反射方式聚焦在火焰中心,以凹面光栅为色散元件.设计了五元素锐线通过的整体组合狭缝.采用顺序注射变速恒流在线稀释的溶液注入方式.为消除干扰谱线对钙的原子吸收的影...     

SYNTHESIS AND CHARACTERIZATION OF A SOLUBLE LADDERLIKE POLYSILSESQUIOXANE CONTAINING REACTIVE ESTER GROUPS*

A novel soluble ladderlike polysilsesquioxane containing reactive ester groups (Ester-T) was synthesized for thefirst time by stepwise coupling polymerization including preammonolysis, controlled hydrolysis and polycondensation. Themonomer, 3-trichlorosilylpropoxy 4-acetoxybenzoate (M), was synthesized by hydrosilylation of allyloxy 4-acetoxybenzoatewith trichlorosilane in the presence of dicyclopentadienylplatinum (II) chloride (Cp_2PtCl_2) catalyst. Combination of FTIR,~1H-NMr, ~(13)C-NMR, ~(29)Si-NMR, XRD, DSC, TGA and VPO methods was used to demonstrate that the polymer obtained hasan ordered ladderlike structure. The synthesized Ester-T may have promising applications as a precursor of advanced functional polymers.     

SYNTHESIS AND MESOMORPHIC PROPERTIES OF FISHBONE-LIKE LIQUID CRYSTALLINE POLYSILSESQUIOXANES——Ⅰ. FISHBONE-LIKE, β-DIKETONE-BASED LIQUID CRYSTALLINE POLYSILSESQUIOXANES AND THEIR COPPER COMPLEXES*

Two kinds of fishbone-like, β-diketone-based liquid crystalline polysilsesquioxanes(FBDKLCP'S), homopolymeric (H-FBDKLCP) and copolymeric (C-FBDKaLCP) have been first synthesized via the hydrosilylation reaction of a vinyl-terminated β-diketone with the homopolymeric ladderlike polyhydrosilsesquioxane (LPHSQ) and random copolymethylhydrosilsesquioxane (LRPMHSQ) respectively. These new kinds of FBDKLCP with M of 10~4 is thermotroic liquid crystalline polymer and its clearing temperatures T_i's and mesophase range △T's are much higher than those of the corresponding comb-like β-diketone liquid crystalline polysiloxane (DKLCP) by about 200℃. Similar results have been observed with the comparison of the two different structure Cu-coordinating compounds The significant increases in T_((?))'s and △T's of the FBDKLCP and Cu-FBDKLCP are mainly attributed to the great rigidity of the ladderlike polysilsesquioxane backbone.     

超分子构筑调控合成结构规整的梯形聚合物及其应用研究

综述了"超分子构筑调控的逐步偶联/聚合法",该方法将高分子化学与超分子化学相结合,利用多种类型的超分子弱键协同作用首先构筑预期的梯形超分子结构,再经聚合得到共价键梯形高分子.利用该方法合成了一系列结构规整的氧桥基和有机桥基梯形聚硅氧烷以及碳基梯形聚酯,并利用侧基间π-π叠加作用实现了对聚合物立体构型控制.扼要介绍了梯形聚合物在先进材料方面的应用,例如梯形聚硅氧烷液晶光致取向膜;由梯形聚硅氧烷合成的管状聚硅氧烷在高室温储存期微电子环氧塑封料方面的应用;以及基于梯形聚硅氧烷的拟筛板聚合物在二阶非线性光学材料方面的应用等.     

重铬酸钾在25°的溶解度与轻水重水混合物组成的关系

我們在25±0.03°測定了重鉻酸鉀於輕水-重水混合物中的溶解度,由此得到下列經驗式: S_n=0.5024-0.1467n+0.0174n～2 S_x=0.1478-0.0540x+0.0049x～2 式中S_n表示每55.51克分子含n克分子分數D_2O的輕水-重水混合物中所溶K_2Cr_2O_7的克分子數;S_x表示每克含x重量分數D_2O的輕水-重水混合物中所溶K_2Cr_2O_7的克數。實驗誤差約±0.25％。由式得出:S_n～(D_2O)=0.3731;S_x～(D_2O)=0.0987。重鉻酸鉀在25°的溶解度舆重水濃度間所呈現的這種非直線性關係,表明了第二個D原子代入水分子中時所產生的效應只有第一個D原子代入作用的76％。 從這兩個經驗式可以計算出重鉻酸鉀在25°時在HDO中的溶解度:S_n～(HDO) =0.4291;S_x～(HDO) =0.1208。     

SYNTHESIS AND-CHARACTERIZATION OF THE SOLUBLE, HIGH MOLECULAR WEIGHT AND LADDERLIKE POLYHYDROSILSESQUIOXANE AND ITS COPOLYMERS

The high molecular ladderlike polyhydrosilsesquioxane (LPHSQ) and its copolymer, ladderlike random copolymethylhydrosilsesquioxane (LR-PMHSQ) and ladderlike block copolymethylsilsesqui-oxane(LB-PMHSQ) have been synthesized by a preaminolysis reaction of the corresponding trichlorosilane with 1 ,4-phenylene diamine(PDA) then by hydrolysis and polycondensation reactions The thermographs of these polymers measured by DSC method indicate that these macromolecular backbones are very rigid as seen from the DSC curves which are almost horizontal from room temperature until 350 ~C without noticeable glass transition. The content of Si—H group in the polymers can be regulated by changing the composition of the two copolymerized monomers. So the ladderlike polymers including its copolymers can be the useful precursors for the functional polymers, especially such as fishbone-like liquid crystalline polymers.     

五苯基环戊二烯基氯化镥的合成

本文介绍高空间位阻的五苯基环戊二烯基氯化镥(包括单取代和双取代)的合成及鉴定。这二化合物要比文献上迄今所报道的其它稀土有机化合物有更高的空气稳定性。     

SYNTHESES OF THE SOLUBLE,HIGH MOLECULAR WEIGHT AND LADDERLIKE POLYPH ENYLSILSESQUIOXAN E AND COPOLYMETHYLPHENYLSILSESQUIOXANES BY PREAMMINOLYSIS METHOD

Soluble, high molecular weight (MW) and ladderlike polyphenylsilsesquioxane (LPPSQ) and its copolymers, ladderlike random and block copolymethyiphenylsilsesquioxanes(LR-PMPSQ and LB-PMPSQ)have been prepared by preamminolysis, hydrolysis and polycondensation reactions. The preparation method can be carried out easily at the temperature below 95℃with high yield of 95 %, instead of the conventional way by using high-boiling solvent and any reaction activator or by precipitation with methanol. Three kinds of ladderlike polymers have been characterized. The MW's of the polymers reached to 10~6 without noticeable gelling. The scheme for synthetic route has been proposed.     

高规整梯形聚乙烯基倍半硅氧烷的合成

采用具有"同步增长,同步断撑和原位缩合"特性的超分子构筑调控逐步偶联和聚合方法,合成了高规整的反应性梯形聚乙烯基倍半硅氧烷Vi-LPSQ.该反应性乙烯基可进一步功能化,是制备功能高分子材料的重要前驱体.29Si-NMR是表征梯形聚合物规整性最有效的方法,Vi-LPSQ的重复结构单元共振吸收峰的化学位移δ=-21.6,且峰宽Δca.1,说明其规整性很高.它的XRD谱图上存在两个明显的衍射峰,分别对应于梯形的宽度(d1=0.74 nm)和厚度(d2=0.40 nm),这证实了Vi-LPSQ以典型的梯形结构存在.另外,Vi-LPSQ的玻璃化转变温度Tg高达191.3℃,表明Vi-LPSQ分子具有很高的刚性和规整性.