The thermal decomposition of NaHCO3 powders and single crystals

The thermal decomposition of four commercial powders and of differently stored single crystals of sodium hydrogen carbonate is studied by power compensation DSC and by optical and FT-IR microscopy. Independently of manufacturer, specified purity and price, the thermal curves of all the commercial powders show a more or less pronounced low temperature peak preceding the one due to the main decomposition. Such small peak is not observed when samples of laboratory recrystallized material are used. However the thermal behaviour of the latter preparation differs remarkably depending on storage conditions: the material kept in closed glass containers decomposes at temperatures higher than those of the material stored in a dessiccator in the presence of concentrated H₂SO₄. The observation by optical microscopy of the behaviour of the surfaces of single crystals coming from different storage conditions when the temperature is raised in a Kofler heater helps the interpretation of the data collected. The mechanism of the decomposition is discussed and the relevant kinetic parameters reported.     

Synthesis of carbamoylformhydroxymoyl chlorides and study of their reactivities

Carbamoylformhydroxymoyl chlorides were synthesized by the reactions of carbamoylformamide oximes with sodium nitrite in the presence of hydrochloric acid, and their reactivities were examined.     

Growth Mechanism of Large Monodispersed Silica Particles Prepared from Tetraethoxysilane in the Presence of Sodium Dodecyl Sulfate

Monodispersed silica particles up to ca. 1.2 μm in diameter were prepared by hydrolysis of tetraethoxysilane in the presence of sodium dodecyl sulfate (SDS). The particle size was increased with an increase of SDS added. The geometrical standard deviation of the particles was decreased with an increase of SDS. In the earlier reaction stage, double spherical particles by the coalescence of the particles were frequently observed when large amounts of SDS were added. Particle size was gradually increased after the coalescence occurred and spherical particles were finally obtained. The results of Nielsen’s chronomal analysis suggest that the polynuclear layer growth took place after the coalescence of the particles in the presence of larger amount of SDS.     

氯化钠在球形纳米氧化铈形成过程中的作用

以水合碳酸铈为原料, 以氯化钠作为助磨剂和阻聚剂, 采用机械活化法制备了球形纳米氧化铈, 用XRD法研究了水合碳酸铈与氯化钠质量比、球磨时间、煅烧温度对CeO2粉体晶粒度的影响, 用TEM对最终产物粒子进行形貌观察. 结果表明: 在碳酸铈的球磨过程及其随后的煅烧过程中, 氯化钠的存在起到了很好的助磨和阻聚作用, 所得CeO2为类球形粒子, 分散性较好, 晶粒度约为30～50 nm.     

Cleavage of the Fe-Fe Bond of(Me_2SiSiMe_2)[η~5-C_5H_4Fe(CO)_2]_2 with Na/Hg and Molecular Structure of the Ring-Opened Complex

The reaction of the title cyclic complex(1) with sodium amal-gam in THF resulted in the expected cleavage of the Fe--Febond to afford bis-sodium salt (Me_2SiSiMe_2) [η~5-C_5H_4Fe(CO)_2Na]_2 (4). The latter was not isolated and was used di-rectly to react with MeI, PhCH_2Cl, CH_3C(O)Cl, PhC(O)Cl,Cy_3SnCl (Cy=cyclohexyl) or Ph_3SnCl to afford correspondingring-opened derivatives (Me_2SiSiMe_2) [η~5-C_5H_4Fe(CO)_2R]_2[5, R=Me; 6, R=PhCH_2; 7, R=CH_3C(O); 8, R=PhC     

Densities and Apparent Molar Volumes of Aqueous NaNO3 Solutions at Temperatures from 292 to 573 K and at Pressures Up to 30 MPa

Densities of four aqueous NaNO₃ solutions (0.100, 0.303, 0.580, 0.892 mol-kg^–1 H₂O) have been measured in the liquid phase with a constant-volume piezometer immersed in a precision liquid thermostat. Measurements were made at ten isotherms between 292 and 573 K. The range of pressure was 0.1–30 MPa. The total uncertainty of density, pressure, temperature, and concentration measurements were estimated to be less than 0.06%, 0.05%, 10 mK, and 0.014%, respectively. Values of saturated densities were determined by extrapolating experimental P- data to the vapor pressure at fixed temperature and composition. Apparent molar volumes were derived using measured values of density for the solutions and for pure water. The apparent molar volumes were extrapolated to zero concentration to yield partial molar volumes at infinite dilution. The temperature, pressure, and concentration dependence of partial and apparent molar volumes were studied. The measured values of density and apparent and partial molar volume were compared with data reported in the literature.     

Vapor pressure,speciation, and chemical activities in highly concentrated sodium borate solutions at 277 and 317°C

The system H₂O-B₂O₃-Na₂O has been studied experimentally at 277 and 317°C. The activities of water and boric acid have been determined at mole ratios Na/B from 0 to 1.5, and total dissolved solids 3 to 80 weight percent. The activity of boric acid has been fitted to within experimental error using a speciation model with eight complex species. This model is consistent with the model previously published by Mesmer et al. The electrolyte properties of the liquid are modeled using the Pitzer-Simonson model of very concentrated electrolyte solutions. The calculated values of water activity agree with experiment, and the activity of NaOH and pOH have also been calculated. The potassium borate system also was briefly studied at 317°C, and is adequately described by a model with five complex species. The potassium borate liquid is more alkaline at K/B= 1 than a sodium borate liquid at the same mole ratio, but pOH in the two systems is the same at lower mole ratios.     

水溶性含C_(60)聚电解质的制备及其与重氮树脂自组装膜AFMFFM的初步研究

通过BPO引发的溶液聚合 ,合成了水溶性的星状C6 0 苯乙烯 苯乙烯磺酸钠的三元共聚物 [Star shapedC6 0 poly(St SS) ],运用自组装技术 ,在水溶液中 ,含C6 0 的三元共聚物与重氮树脂 (Diazoresin)通过正负离子间的吸附力在云母基片上交替一层一层有序地组装成固体膜 .自组装膜经紫外光幅照反应 ,通过重氮基的分解 ,层间连接的离子键转变成共价键 ,从而增加薄膜的稳定性和堆砌密度 .用原子力显微镜 摩擦力显微镜(AFM FFM)考察了C6 0 在膜中的承载作用及比较不同链结构、不同链长、不同层数自组装膜的表面形貌和微摩擦性能 .初步的研究结果显示了聚合物薄膜的微摩擦性能与聚合物的化学结构、链长和膜的层数有密切关系     

钙羧酸钠褪色光度法测定微量碘的研究

提出了以钙羧酸钠褪色光度法测定微量碘的新方法。在盐酸介质中 ,表面活性剂十六烷基三甲基溴化铵 (CTMAB)存在下 ,碘酸根离子定量氧化钙羧酸钠褪色。最大吸收波长λmax=5 95nm ,表观摩尔吸光系数ε =3.1× 10 4 L·mol-1·cm-1。碘浓度在 0～ 5 0 μg 2 5ml范围内服从比耳定律。方法用于加碘食盐中碘的测定 ,结果满意     

Phase Diagram of the System NaF-KF-AlF3

The phase diagrams of the binary system KF-AlF₃ as well as the ternary system NaF-KF-AlF₃ in the range up to 50 mol% AlF₃, were measured using the thermal analysis method. In the system KF-AlF₃ the coordinates of the eutectic points are: E ₁: 8.0 mol% AlF₃, 821.2°C, and E ₂: 45.5 mol% AlF₃, 565.0°C. In the investigated concentration range of the ternary system 2 eutectic points have been found with the calculated coordinates: E ₁: 36.3 mol% NaF, 62.7 mol% KF, 1.0 mol% AlF₃; t=711.2°C; and E ₂: 51.9 mol% NaF, 27.4 mol% KF, 20.7 mol% AlF₃; t=734.5°C. Other eutectic points lie most probably beyond the investigated part of the system. This revised version was published online in July 2006 with corrections to the Cover Date.