一种采用非水滴定法测定长春胺酸含量的方法

一种应用于化学分析领域中采用非水滴定法测定长春胺酸含量的方法,以无水甲酸、冰乙酸和乙酐组成的混合溶剂,定量溶解长春胺酸,用高氯酸溶液为滴定剂,采用电位滴定法或者指示剂滴定法进行滴定;所述的电位滴定法是指用电位指示剂确定终点并计算长春胺酸含量;所述的指示剂滴定法是指用结晶紫为指示剂确定终点并计算长春胺酸含量;所述混合溶剂的体积由配制混合溶剂各组分的体积直接相加而得;所述的定量溶解长春胺酸的方法为以无水甲酸先溶解长春胺酸,再加入冰乙酸和乙酐;所述高氯酸溶液的溶剂为无水冰乙酸。该发明样品用量小、仪器设备简单、操作简便、省时节料、原料易得、成本低、易于掌握、精密度高、含量准确、重复性好。     

可见光协同钴铈铁氧体高效活化过一硫酸盐降解噻虫胺

本实验采用溶胶-凝胶燃烧的方法,将Co掺入到CeFeO3（CFO）钙钛矿晶格中制备了具有晶格缺陷的CeFe0.8Co0.2O3（CFCO）纳米颗粒催化剂。通过扫描电镜（SEM）、透射电镜（TEM）、X射线衍射（XRD）、Ｘ射线光电子能谱（XPS）等表征技术对CFCO催化剂进行表征分析,结果表明在CFCO上形成了表面氧空位（VO）。同时,还研究了过硫酸氢钾（PMS）用量、不同pH值对CFCO降解噻虫胺（CTD）的影响。结果表明,在CFCO投加量为0.6 g?L-1,PMS用量为0.8 mmol?L-1,pH为7时,20 mg?L-1的噻虫胺在30分钟内完全降解。并且经过4次循环使用后,噻虫胺降解率仍能达到91.2%。CFCO对于PMS的高效活化能力,主要归功于晶格缺陷所产生的电位差促使自由电子顺着氧空位快速定向传导到PMS上。为了模拟在天然水体环境中CFCO光催化活化PMS去除CTD,进行阴离子和有机酸的对比实验,分析了不同环境因素对CFCO降解噻虫胺的影响;此外,本文通过自由基淬灭实验与电子自旋共振（ESR）检测确定了CFCO光催化活化PMS降解噻虫胺实验中起主要作用的活性物种为单线态氧（1O2）与羟基自由基（?OH）,并分析推测了自由基的产生机理。最后采用高效液相色谱-质谱联用仪（LC-MS）检测分析了CTD降解过程中可能产生的代谢产物,并基于代谢产物的产生顺序归纳出了三条可能的降解路径。     

化学振荡

为了说明化学振荡的概念,首先介绍两个有趣的演示实验。 (1)在1000毫升烧杯内先倒入600毫升蒸馏水,再依次溶解16克丙二酸(0.25M),6克溴酸钾(0.06M),指示剂2—4毫升(邻菲罗啉Ferroin 0.05克,硫酸亚铁0.07克溶于10毫升     

可降解光交联聚酸酐与聚酰胺-甲基丙烯酰胺凝胶的合成及药物控释

合成聚酰胺-胺型树状分子（PAMAM）并进行端基甲基丙烯酰基修饰,将最外层接枝光化学活性双键,修饰产物与甲基丙烯酸酐化癸二酸(MSA)用DMSO溶解并在光引发剂存在下,经过紫外光照射得到具有一定生物相容性的凝胶。运用1H NMR和FT-IR对聚酰胺-甲基丙烯酰胺的结构进行表征。凝胶的降解实验表明,聚酸酐含量为50-60wt%的凝胶以表面溶蚀的方式降解,随着甲基丙烯酸酐化癸二酸（MSA）在凝胶中含量不同,降解时间在45~60天之间,pH在6.5-8.06范围内改变。包埋氧氟沙星凝胶的降解实验表明,可以通过改变聚酸酐的含量控制降解时间和药物释放量。     

分光光度法测定指示剂解离常数的实验教学改进与实践*

设计了一种不需测定指示剂浓度,只需测定指示剂吸光度即可计算获得指示剂解离常数的实验教学方法。实验通过调节溶液pH,使指示剂呈现不同颜色,通过分光光度法测定了溴百里酚蓝指示剂的解离平衡常数pKa=7.24,并与文献值pKa=7.30进行了对比,结果基本一致。通过该实验学生不仅能理解指示剂的化学解离平衡,还能更好地掌握紫外-可见分光光度计的工作原理及操作方法。本实验教学将化学分析原理与仪器分析测定进行了有机结合,提出了一种采用分光光度法实现高效、简单的测定指示剂解离常数的方法,不仅增强了学生的动手能力,而且培养了学生的创新能力,提高了学生的学习兴趣。     

硫酸亚铁铵和硫酸亚铁稳定性的对比研究

对硫酸亚铁铵晶体以及硫酸亚铁晶体在不同环境下的稳定性进行了实验对比研究,并根据实验结果进行了理论分析,明晰了不同环境下2者稳定性的差别,研究认为硫酸亚铁铵晶体内氢键比硫酸亚铁晶体内氢键多,众多的氢键可以提高亚铁离子“遮蔽效应”的稳定性是硫酸亚铁铵晶体较硫酸亚铁晶体稳定的根本原因。     

131I标记海藻酸钠包裹明胶微球的制备及性能评价

建立了明胶微球和海藻酸钠(SA)包裹微球的制备方法,并通过实验比较了明胶微球和包裹微球的各种特性,最后用氯胺T法将125I及131I分别标记在微球上.结果表明,包裹微球对碘有更高的负载量和稳定性;在相同条件下,包裹微球的降解时间比明胶微球的降解时间长;将标记后的明胶微球通过直接注射介入到新西兰大白兔的肝脏,采用发射单光...     

高中化学教材中硫酸亚铁溶解度引用数据的纠正

硫酸亚铁在水中的溶解度在高中化学教材《实验化学》人教版和苏教版的引用数据悬殊很大。通过实验测定七水硫酸亚铁在水中的溶解度以便证明教材中引用的溶解度数据是否正确。结果表明,2套教材中硫酸亚铁的表达形式和溶解度数据之间都不吻合,需要对教材中硫酸亚铁溶解度引用数据进行纠正。     

脂肪胺及其盐的水溶液的表面张力和脂肪胺用作滴定指示剂

1.用氣泡最大压力法测定了三乙胺、正戊胺、正己胺、正庚胺、正辛胺、異戊胺、二異戊胺和三異戊胺,以及胺及其盐的不同浓度的水溶液在20°时的表面张力。對於胺溶液在极稀浓度时的不正常表面张力变化情形予以解释。 2.觀测了三異戊胺盐酸盐和正已胺硫酸盐水溶液在不同浓度時和不同测定时间的表面张力,并作了可能的解释。 3.根據表面张力-浓度曲线,计算出三乙胺、正戊胺、正己胺、正辛胺、異戊胺及二異戊胺在溶液饱和吸附时每一分子所佔的平均面積。结果说明了各胺在饱和吸附时,分子在表面作垂直的定向排列,而在氮原子上有分枝的胺,则可能有枝鏈互相交叉的排列情形。 4.本文说明脂肪胺可以作酸鹼滴定指示剂,而以二異戊胺最为合適。此类指示剂还用到金属盐溶液的滴定。     

用植物色素作酸碱指示剂的实验

为了找寻易得的植物色素作酸碱指示剂,并测知这样获得的代用指示剂的变色范围,我们做了以下实验。将新鲜植物的花瓣、叶片或果皮洗净、沥干、捣碎,加适量(按制备浓溶液的要求)的市售白酒浸泡1—2小时,挤出液汁,如浑浊可离心分离,去除沉渣,所得溶液即为以该植物色素制成的指示剂(这种浸出液可保存较长时间)。     

New layered materials: syntheses, structures, and optical properties of K(2)TiCu(2)S(4), Rb(2)TiCu(2)S(4), Rb(2)TiaAg(2)S(4), Cs(2)TiAg(2)sS(4), and Cs(2)TiCu(2)Se(4)

The new compounds K(2)TiCu(2)S(4), Rb(2)TiCu(2)S(4), Rb(2)TiAg(2)S(4), Cs(2)TiAg(2)S(4), and Cs(2)TiCu(2)Se(4) have been synthesized by the reactions of A(2)Q(3) (A = K, Rb, Cs; Q = S, Se) with Ti, M (M = Cu or Ag), and Q at 823 K. The compounds Rb(2)TiCu(2)S(4), Cs(2)TiAg(2)S(4), and Cs(2)TiCu(2)Se(4) are isostructural. They crystallize with two formula units in space group P4(2)/mcm of the tetragonal system in cells of dimensions a = 5.6046(4) A, c = 13.154(1) A for Rb(2)TiCu(2)S(4), a =6.024(1) A, c = 13.566(4) A for Cs(2)TiAg(2)S(4), and a =5.852(2) A, c =14.234(5) A for Cs(2)TiCu(2)Se(4) at 153 K. Their structure is closely related to that of Cs(2)ZrAg(2)Te(4) and comprises [TiM(2)Q(4)(2)(-)] layers, which are separated by alkali metal atoms. The [TiM(2)Q(4)(2)(-)] layer is anti-fluorite-like with both Ti and M atoms tetrahedrally coordinated to Q atoms. Tetrahedral coordination of Ti(4+) is rare in the solid state. On the basis of unit cell and space group determinations, the compounds K(2)TiCu(2)S(4) and Rb(2)TiAg(2)S(4) are isostructural with the above compounds. The band gaps of K(2)TiCu(2)S(4), Rb(2)TiCu(2)S(4), Rb(2)TiAg(2)S(4), and Cs(2)TiAg(2)S(4) are 2.04, 2.19, 2.33, and 2.44 eV, respectively, as derived from optical measurements. From band-structure calculations, the optical absorption for an A(2)TiM(2)Q(4) compound is assigned to a transition from an M d and Q p valence band (HOMO) to a Ti 3d conduction band.     

SYNTHESES AND CRYSTAL STRUCTURES OF (Et_4N)_2(Fe_2Se_2(SPh)_4) AND (Et_4N)_2(Fe_4Se_4Cl_4)

<正> Since the discovery of iron-sulfur proteins , a number of analogous compounds of the active sites of iron-sulfur proteins has been synthesized and characterized . Due to the similarity between sulfur and selenium, some selenoproteins with similar active site as iron-sulfur proteins were found . We have synthesized a series of iron-selenium compounds in correlative study with the iron-sulfur compounds. In this paper, we will discuss the syntheses and crystal stuctures of the title compounds. The spectroscopic properties of these compounds have been under investigation.     

Synthesis and Characterization of Gd2[Pt2(SO4)4(HSO4)2](HSO4)2

Red single crystals of Gd₂[Pt₂(SO₄)₄(HSO₄)₂](HSO₄)₂ (triclinic, , Z = 1, a = 844.02(9), b = 908.50(9), c = 939.49(8) pm, α = 107.73(1)°, β = 112.10(1)°, γ = 103.53(1)°) were obtained by the reaction of [Gd(NO₃)(H₂O)₇][PtCl₆]·4H₂O with sulfuric acid at 320 °C in a sealed glass ampoule. In the crystal structure, Pt₂ dumbbells are coordinated by four chelating sulfate groups and two monodentate hydrogensulfate ions. Two further HSO₄^? ions are not bonded to the Pt₂ dumbbell. The Gd³⁺ ions are eightfold coordinated by oxygen atoms. The IR data of Gd₂[Pt₂(SO₄)₄(HSO₄)₂](HSO₄)₂ are typical for these type of compounds. The thermal decomposition of the compound leads to elemental platinum and Gd₂O₃.     

Thermal decomposition of (NH4)2MoS4 and (NH4)2WS4heat of formation of (NH4)2MoS4

The reactions (NH₄)₂MeS₄ = 2 NH₃ + H₂S + MeS₃ (Me = Mo, W) were investigated by measuring the decomposition vapour pressures. Thermochemical data were obtained from these measurements: ΔH = 52 kcal/mole and ΔS = 105 cal/deg.mole for the decomposition of the tetrathiomolybdate. Similarly, ΔH = 69 kcal/mole and ΔS = 106 cal/deg.mole were obtained for the decomposition of the tetrathiotungstate. The normal heat of formation of (NH₄)₂MoS₄ was found to be ΔH = ?140 kcal/mole. The kinetics of thermal decomposition of the above reactions were also measured.     

Kinetic and thermodynamic study of the Na4(UO2)2(OH)4(C2O4)2 complex

The synthesis, the characterization, and the thermal decomposition of the dioxouranium(VI) ternary complex of formula Na₄(UO₂)₂(OH)₄(C₂O₄)₂, has been studied. The identification of the compound was performed by chemical analysis and by infrared spectrometry. Thermal decomposition of the compound occurs in several steps due to the decomposition of the salt to Na₂O and UO₃ oxides. The stoichiometry of the steps, hypothesized by means of the thermodynamic and kinetic parameters, is confirmed by the evolved gas analysis studied by FTIR spectrometer coupled to TG/DSC apparatus. Model‐fitting and model‐free kinetic methods have been used in kinetic analysis. The latter allows determining kinetic scheme. © 2003 Wiley Periodicals, Inc. Int J Chem Kinet 35: 661–669, 2003     

Synthese und Struktur neuer Natriumhydrogensulfate Na(H3O)(HSO4)2; Na2(HSO4)2(H2SO4) und Na(HSO4)(H2SO4)2

Synthesis and Structure of New Sodium Hydrogen Sulfates Na(H₃O)(HSO₄)₂, Na₂(HSO₄)₂(H₂SO₄), and Na(HSO₄)(H₂SO₄)₂ Three acidic sodium sulfates have been synthesized from the system sodium sulfate/sulfuric acid and have been crystallographically characterized. Na(H₃O)(HSO₄)₂ ( A ) crystallizes in the space group P2₁/c with the unit cell parameters a = 6.974(2), b = 13.086(2), c = 8.080(3) Å, α = 105.90(4)°, V = 709.1 Å3, Z = 4. Na₂(HSO₄)₂(H₂SO₄) ( B ) is orthorhombic (space group Pna2₁) with the unit cell parameters a = 9.970(2), b = 6.951(1), c = 13.949(3) Å, V = 966.7 ų and Z = 4. Na(HSO₄)(H₂SO₄)₂ ( C ) crystallizes in the triclinic space group P1 with the unit cell parameters a = 5.084(1), b = 8.746(1), c = 11.765(3) Å, α = 68.86(2)°, β = 88.44(2)°, γ = 88.97(2)°, V = 487.8 Å3 and Z = 2. All three compounds contain SO₄ tetrahedra as HSO₄^? anions and additionally in B and C in form of H₂SO₄ molecules. The ratio H:SO₄ determines the connectivity degree in the hydrogen bond system. In A , there are zigzag chains and dimers additionally connected via oxonium ions. Complex chains consisting of cyclic trimers (two HSO₄^? and one H₂SO₄) are present in B . In structure C , several parallel chains are connected to columns due to the greater content of H₂SO₄. Sodium cations show a distorted octahedral coordination by oxygen in all three structures, the NaO₆ octahedra being “isolated” (connected via SO₄ tetrahedra only) in A . Pairs of octahedra with common edge form Na₂O₁₀ dimeric units in C . Such double octahedra are connected via common corners forming zigzag chains in B .