甲酸钠热分解行为的实验研究

用差热—热重方法对甲酸钠的热分解过程进行了实验研究,采用滴定分析技术分析了甲酸钠在不同条件下热分解产物的组成。研究发现：在甲酸钠脱氢制草酸钠的工艺中,加热速率和反应温度是影响草酸钠收率的重要因素。纯甲酸钠在253℃熔融,在330℃左右缓慢分解为碳酸钠、氢气、一氧化碳和少量草酸钠;高于400℃发生激烈的放热反应,甲酸钠脱氢转化为草酸钠;高于440℃,草酸钠分解生成碳酸钠。因此,为了高收率的获得目的产物草酸钠,需要快速升温,生成草酸钠的最佳温度为400～420℃,过度加热将导致草酸钠深度分解。     

Syntheses,structure and photoluminescent properties of lanthanide oxalatosulfocarboxylate coordination polymers

Hydrothermal reactions of oxalic acid(H2ox) and 2-sulfobenzoic acid(H2L) with lanthanide oxide or hydroxide yielded five lanthanide oxalatosulfocarboxylates.They have a general formula [Ln2L2(ox)(H2O)6]n[Ln = La(1),Nd(2),Eu(3),Gd(4),Tb(5)].Their structures were characterized by single crystal X-ray diffraction,powder X-ray diffraction(PXRD),infrared(IR) spectroscopy,elemental analysis(EA),and thermogravimetric analysis(TGA).1-5 are isostructural coordination polymers and feature one-dimensional(1D) chains,which are extended into 3D supramolecular frameworks through inter-chain hydrogen bonds between coordinated H2O donors and oxygen acceptors from carboxylate,sulfonate and oxalate groups.In addition,the solid-state photoluminescence properties of the Nd(2),Eu(3) and Tb(5) derivatives have been measured at room temperature.The Eu and Tb-containing coordination polymers(CPs) exhibit intense red and green luminescence emissions,respectively,with lifetimes in the order of millisecond.     

用离子色谱法测定人尿中的草酸

本文叙述了一种使用离子色谱技术测定人尿中的草酸的新方法。该方法只需要简单的样品制备:尿样用盐酸酸化,用去离子水按需要稀释,最后通过0.2μm孔径的微孔滤膜过滤就能直接注入离子色谱仪分析。本方法每分析一个尿样仅需10min,在稀释后的尿样中草酸的低检测限为0.1ppm(1.1μmol/l),用标准加入法获得的草酸平均回收率为100.28%。我们使用本方法测定了300多个尿样中的草酸,其线性范围为1～1000ppm,相对标准偏差为4%。本方法可以用于人尿中草酸的直接测定。     

二元羧酸对草酸钙结晶的调控作用

采用双扩散法系统研究了凝胶体系中二元羧酸对尿结石主要成分草酸钙结晶的影响,这些羧酸分别为含有0、1、2个羟基的丁二酸、羟基丁二酸、酒石酸,含有1个氨基的L-天冬氨酸,以及含有双键的顺丁烯二酸、反丁烯二酸．对于丁二酸、羟基丁二酸和酒石酸的研究表明,随着羧酸中羟基数目的增加,抑制一水草酸钙(COM)聚集和诱导二水草酸钙(COD)生成的能力逐渐增强;随着羧酸浓度的增大,抑制COM聚集和诱导COD生成的能力也增强;随着结晶时间的增加,COM晶体钝化程度加深．对L-天冬氨酸、顺丁烯二酸和反丁烯二酸的研究表明,三者影响不明显．     

Description of mechanism function about dehydration of cobalt oxalate dihydrate by multiple rates isotemperature method

0　IntroductionThetechnologyofthermalanalysishasbeenwidelyusedinthestudyofthermalbehaviorandthermalcharacterofsolidstatereaction ,theprimaryintentionofthermalanalysiskineticsistoestablishseparatevaluesofapparentactivationenergyE ,themostprobablemechanism g(α)andthepre exponentialfactorA ,meanwhilethedeterminationofg(α)hasgraduallybeenthefocusofthisfield .Inthisfield ,therearemostlygeneralkineticsmethodsused presently ,suchasCoats Redfern’s[1 ] integralmethod ,Achar’s[2 \〗differentialmet…     

配位聚合物[Nd2(C2O4)3·4H2O]n的水热合成和晶体结构

NdCl3·6H2O与4-羧基尿嘧啶于170℃水热反应96h，得到配位聚合物[Nd2（C2O4）3·4H2O]n，用X-射线单晶衍射分析确定了其晶体结构．配合物属于正交晶系，P2（1）2（1）2（1）空间群．晶胞参数：a=0．85927（9）nm,b=0．94648（11）nm，c=1．68373（19）nm，M=624．60，V=1．3693（3）nm^3，Z=4，Dcale=3．030Mg／m^3，F（000）=1168,乙二酸根以双齿桥联／双齿桥联和双齿桥联，三齿桥联两种配位方式与Nd（Ⅲ）离子键合，形成网状结构。     

钛酸钡纳米粉体的制备及表征

利用草酸盐共沉淀法合成BaTiO3纳米粉体,通过XRD分析、DTA-TG分析、IR分析及TEM形貌分析等分析手段,对制得的粉体进行了表征和测试,结果表明合成的BaTiO3粉体为单纯的立方相,粒径均匀,颗粒大小在30 nm左右,无严重的团聚现象.     

微波辐射氯化铁催化合成草酸二乙酯的研究

以氯化铁为催化剂,以草酸和乙醇为原料在微波辐射下直接酯化合成草酸二乙酯的方法.通过实验得出最佳反应条件为:醇酸摩尔比为4,催化剂用量为总投料量的6%,微波辐射功率为400W,辐射时间12min.在此条件下取得了较好的收率.     

A simple diagnostic method for the differentiation of Tamm-Horsfall glycoproteins from healthy probands and those from recurrent calcium oxalate renal stone formers

Tamm-Horsfall glycoproteins (THPs)^* from healthy probands, and those from a majority of recurrent calcium oxalate renal stone formers, reveal different properties when analyzed using isoelectric focusing. The pl-values of THPs from healthy probands are approximately 3.5 while THPs from recurrent renal stone formers have pl-values between 4.5 and 6. The two groups of THPs exhibit completely different protein patterns in IEF. This proves the structural difference of these THPs. The differences in IEF analysis allow the differentiation between THPs from healthy probands and those from recurrent calcium oxalate stone formers. These differences could possibly by used as a simple diagnostic method for the recognition of recurrent calcium oxalate renal stone formers.