GaPO4 high temperature crystal microbalance demonstration up to 720°C

Quartz-homeotypic gallium (ortho-) phosphate, GaPO₄, is of special interest for resonator applications asking for temperature compensated cuts with higher electro-mechanical coupling than quartz and operational temperatures up to 970°C. The crystal microbalance technique, well known for quartz (QCM) which can be used only at moderate temperatures, can now be extended to much higher temperatures using GaPO₄ crystals, benefiting from all three advantages mentioned above. Two different experiments were done to demonstrate the advantages of a crystal microbalance based on GaPO₄. First, the GaPO₄ resonator was used for film thickness determination and compared with a commercial QCM. This experiment demonstrated that the measuring range can be extended by using GaPO₄ resonators instead of quartz. The second experiment demonstrates the possibility for thermogravimetric analysis up to 720°C by using a new concept for resonator mounting.This revised version was published online in November 2005 with corrections to the Cover Date.     

TiSiW_(12)O_(40)/TiO_2催化合成磷酸三甲苯酯的研究

应用TiSiW_(12)O_(40)/TiO_2催化剂合成磷酸三甲苯酯研究结果表明，该催化 剂具有较高的催化活性。考察了催化剂用量、反应温度和反应时间对酯产率的影响 。在典型反应条件（催化剂用量为原料总量的1.0%，反应温度为100-120 ℃，反应 时间为8h）下所得磷酸三甲苯酯的产率为85.5%。该催化剂易于回收且可重复使用 ，具有良好的活性稳定性。     

Precise Conductance Measurements on Dilute Aqueous Solutions of Sodium and Potassium Hydrogenphosphate and Dihydrogenphosphate

Precise conductance measurements are reported on dilute aqueous solutions of the sodium and potassium salts of orthophosphoric acid at 25 ^∘C. Conductance measurements on solutions of electrolytes such as these phosphate salts that exist in solution as complicated mixtures of ions have previously proved difficult to interpret. To overcome this, a mathematical method has been developed to calculate the concentrations of all the species in the aqueous system M₃PO₄/M₂HPO₄/M₂HPO₄/H₃PO₄ (M = Na or K) over a continuous range of stoichiometries. The Lee–Wheaton conductance equation has been used to interpret the conductance of these multicomponent solutions in terms of the limiting ionic conductances and concentrations of all the ions in the solution. The limiting molar conductances of the ions H₂PO₄ ⁻ and HPO₄ ²⁻ and the ion-pair formation constants of these ions with sodium and potassium ions were determine This work has enabled the accurate determination of solution parameters for the important hydrogenphosphate ions in water and provides an excellent example of the use of an advanced conductance theory in the analysis of the conductance of multicomponent electrolyte systems.     

磷肥和硒施用对稻米硒、钙、锌等营养累积的影响

研究了施用不同水平磷肥和硒对稻米中硒、钙、锌、镁、硫等人体必需营养吸收累积的影响。结果表明，适量施磷，降低米中硒含量；大量施磷，又促进硒在米中累积。施磷肥一般不利于钙和锌在稻米中累积，适量施磷增加稻米中镁、硫含量，而过量施用磷肥显著降低钙、锌、镁、硫等矿质营养的含量，影响稻米营养品质。适量施硒，一般提高稻米的矿质营养含量；过量施硒，特别在高磷水平下则降低矿质营养含量。     

四苯基卟啉在改性磷酸锆层间的插入及荧光增强

近年来,出于节约一次性能源的考虑,人们已经加大对太阳能等天然资源的利用,致力于模拟天然光合作用的研究[1￣3],而光合作用中的捕光复合物又称为光子天线。光子天线中往往存在一种或几种猝灭剂,猝灭剂吸收光子后产生激发态的能量可以在不同分子或者同一分子的不同生色团之间转移,转移出能量的一方为能量给体,另一方为能量受体。     

The role of radicals in enzymatic processes

Research on the mechanism of action of coenzyme B12, adenosylcobalamin, as a graduate student introduced the author to the field of organic free radicals in enzymology. Twenty years later, related work on S-adenosylmethionine (SAM) as a "poor man's coenzyme B12" was initiated in a detailed analysis of the mechanism of action of lysine 2,3-aminomutase (LAM). The interconversion of L-lysine and L-beta-lysine is catalyzed by LAM, which requires SAM, pyridoxal-5'-phosphate (PLP), and a [4Fe-4S] cluster as coenzymes. The mechanism of this reaction has been delineated as a radical isomerization, in which radical formation is initiated by the [4Fe-4S]-dependent cleavage of the SAM into methionine and the 5'-deoxyadenosyl radical. The mechanism of this process is discussed, together with the role of this radical in hydrogen abstraction from lysine to initiate the substrate radical isomerization. The chemistry underlying the functions of SAM, PLP, and [4Fe-4S] in the action of LAM is novel in all respects, except for the formation of a lysine-PLP aldimine at the active site. Of the four free radicals in the mechanism, three have been characterized by EPR spectroscopy. In the suicide inactivation of adenosylcobalamin-dependent dioldehydrase (DDH) by glycolaldehyde, the formation of cob(II)alamin and 5'-deoxyadenosine is accompanied by the conversion of glycolaldehyde to cis-ethanesemidione radical at the active site. The cis-ethanesemidione radical has been characterized by EPR spectroscopy. Its exceptional stability at the active site is the basis for the inactivation of DDH by glycolaldehyde.     

Synthesis and Structure of the New Ammonium Indium Phosphate (NH4)In(OH)PO4

A new ammonium indium phosphate (NH₄)In(OH)PO₄ was prepared by hydrothermal reaction in the In₂O₃-NH₄H₂PO₄-NH₃/OH system (T=200°C, autogenous pressure, 7 days). The formula (NH₄)In(OH)PO₄ was determined on the basis of chemical and thermal analysis (TG/DSC), X-ray powder diffraction and IR-spectroscopy. (NH₄)In(OH)PO₄ crystallizes in the tetragonal system with space group P4₃2₁2 (No. 96); a=9.4232(1) Å, c=11.1766(1) Å, V=992.45(2) ų; Z=8. The crystal structure was refined by the Rietveld method (R_w=6.35%, R_p=5.10%). The second-harmonic generation study confirmed that structure of (NH₄)In(OH)PO₄ does not have a center of symmetry. The cis-InO₄(OH)₂ octahedra form helical chains, parallel to the c-axis. The In-O-In bonds are nearly equidistant. The chains are interconnected by phosphate tetrahedra and create tunnels containing the NH₄⁺ ions along the c-axis. (NH₄)In(OH)PO₄ is isostructural with RbIn(OH)PO₄.     

两性离子流动相测定杂多酸中的磷酸根、氯离子和硫酸根

采用离子色谱法测定杂多酸中痕量阴离子。由于常规的淋洗液(如Na2CO3,NaOH)呈碱性,使杂多酸迅速分解生成磷酸根,致使测定结果偏高。实验通过在常规淋洗液中加入适量两性离子后,调节淋洗液的pH为中性,从而能准确测定杂多酸中磷酸根氯离子和硫酸根的含量值。经过比较分别用去离子水和流动相稀释的样品中磷酸根的测定结果,确定淋洗液的最佳条件为2.5mmol/LNa2CO3-9.0mmol/LCHES,在该条件下测定,快速、准确、灵敏,且有较好的灵敏度和重现性。     

磷酸酯甜菜碱两性表面活性剂的合成与性能

磷酸酯甜菜碱从皮肤溶出的氨基酸量少,脱脂低,毒性和刺激性低,易降解,是一类性能优良两性表面活性剂[1,2]。它的合成大多以长链卤烷或胺为原料,成本较高。本文以高级脂肪醇、氯乙醇以及二甲胺为原料、P2O5为磷酸化剂,合成了C12H25OCH2CH(OOCCH3)CH2N+(CH3)2CH2CH2OP(O)(O )(OH)磷酸酯甜菜碱。测定了表面张力、泡沫性能、钙皂分散力及增溶能力。1　合成十二烷基缩水甘油醚(Ⅰ)[2]　在500ml三颈烧瓶中加入月桂醇0 2mol,正已烷200ml和四丁基溴化铵0 01mol;在室温和强烈搅拌下加入50%的NaOH水溶液48g,滴加环氧氯丙烷0 4mol后升…     

冰点下降法测定正十六烷中TBP的活度系数

磷酸三正丁酯(TBP)是核燃料及多种稀有金属水冶过程中使用的重要萃取剂,Healy 等人用蒸气压法、Alcock 用溶解度法先后测定过它在一些溶剂中的活度系数,不同作者的数据分歧很大,测定的浓度范围一般也较小.高宏成等人用磷-32标记TBP 分配法在较大浓度范围内测定过TBP 在氯仿、四氯化碳、苯、正已烷等8～9种溶剂中的活度系数,