极谱催化波法测定磷酸氯喹

基于在3.2×10-2 mol/LNH3·H2O -NH4Cl(pH9.5) -1.4×10-2 mol/LK2S2O8 支持电解质中 ,磷酸氯喹于 -1.62V(vs.SCE)产生的极谱催化波 ,拟订了测定磷酸氯喹的新方法 ;其二阶导数峰峰电流与磷酸氯喹浓度在1.0×10 -9～1.0×10 -5mol/L范围内呈线性关系 (r=0.9988 ,n=9) ,检出限为4.0×10 -10mol/L;本方法灵敏、简便、快速 ,回收率在95 %～104 %之间 ;对片剂中磷酸氯喹的测定结果与标示值相符良好。     

血红蛋白模拟过氧化物酶催化反应体系的极谱分析

用极谱分析法研究了血红蛋白催化H2O2氧化邻苯二胺(OPD)的反应体系.血红蛋白具有类似过氧化物酶的功能,它能够催化OPD-H2O2的反应生成一种具有电化学活性的产物,该产物在滴汞电极上-0.64V(vs.SCE)产生一个峰形良好的极谱还原峰.优化了血红蛋白的催化反应条件和催化反应产物的极谱测定条件 在最佳条件下,该体系可用于血红蛋白含量的测定,线性范围为2.0×10-9～2.0×10-7mol/L,检测限为1.0×10-9mol/L;也可用于痕量H2O2的测定,线性范围为1.0×10-6～2.0×10-4mol/L,检测限为1.0×10-6mol/L.     

四磺基锰酞菁作为过氧化物模拟酶在过氧化氢化学发光测定中的应用

以四磺基锰酞菁 (MnTSPc)作为过氧化物模拟酶催化H2 O2 与鲁米诺的化学发光反应 ,建立了测定环境样品中H2 O2 的化学发光分析新方法。该法的线性范围为 4 .0× 10 - 8～ 2 .0× 10 - 5mol L ;检出限为 6 .8×10 - 9mol L ;对 1.0× 10 - 6 mol L的H2 O2 进行连续 10次平行测定 ,相对标准偏差为 2 .4 %。用本法对天然雨水进行了分析测定 ,结果良好。     

加替沙星的荧光光度法测定

提出了测定加替沙星的荧光光度法 ,并对影响加替沙星荧光性质的各种因素进行了研究 ;加替沙星浓度在3.0×10-7～1.0×10-5 mol/L范围内与荧光强度呈良好的线性关系,检出限为8.8×10-8 mol/L ,对5.0×10 -7mol/L的加替沙星平行测定13次的相对标准偏差为1.4 % ;将该法用于血清、尿样分析 ,回收率在98%～103% ,结果令人满意。     

化学发光法测定药物中的洛美沙星

利用洛美沙星对碱性luminol H2 O2 Cr3 + 化学发光体系有较强的抑制作用 ,建立了一种测定洛美沙星药物的新方法。线性范围为 5 .16× 10 -10 ～ 9.0 3× 10 -6mol/L ;平均回收率为 95 %～ 10 5 % ;检出限 (3δ)为 1.84× 10 -10 mol/L ;相对标准偏差为 0 .92 % (n =6 ,Cs =5 .16× 10 -10 mol/L)。用于胶囊、片剂和针剂中洛美沙星的测定 ,结果令人满意。     

血红蛋白作为催化剂高灵敏测定过氧化氢

用血红蛋白作为过氧化物酶的替代物,用于催化H2O2氧化对甲基酚的反应体系.研究发现,血红蛋白作为过氧化物酶的替代物,其催化活性比Hemin、β-CD-Hemin等过氧化物模拟酶要高.建立了高灵敏测定痕量H2O2的荧光分析法.该法的线性范围为3.19×10-8～3.19×10-6 mol/L,检出限为8.85×10-10 mol/L.用于雨水中H2O2的测定,结果满意.     

6-疏基嘌呤,硫唑嘌呤,8-氮杂鸟嘌呤的滤纸基质室温燐光法研究

建立了 6 巯基嘌呤、硫唑嘌呤和 8 氮杂鸟嘌呤 3种抗癌嘌呤化合物的滤纸基质室温光分析新方法。详细探讨了影响其室温光发射的各种因素。该方法的线性范围、检出限、精密度分别为 6 巯基嘌呤2 0～ 4 .0× 10 2 μmol/L ,1.3μmol/L ,4 .1% ;硫唑嘌呤 2 .0～ 6 .0× 10 2 μmol/L、1.2 μmol/L、3.8% ;8 氮杂鸟嘌呤1.1～ 2 .2× 10 2 μmol/L、7.4× 10 -2 μmol/L、1.3%。用该方法进行尿液中嘌呤化合物的回收测定 ,回收率为 96 .2 %～ 10 1.7% ;进行 6 MP在药片中的回收测定 ,回收率为 96 .2 %～ 10 2 .1%。     

辣根过氧化物酶催化过氧化氢氧化隐性亮绿显色反应的研究

以隐性亮绿 (RBG)为氢供体底物 ,研究了辣根过氧化物酶 -H2 O2 -RBG显色反应体系的酶催化特性。在 p H 5.0～ 6.0的条件下反应形成的酶催化产物亮绿 (BG)于 63 0 .6nm处有最大吸收 ,该显色反应测定 H2 O2 的表观摩尔吸光系数为 5.64×1 0 4 L·mol- 1·cm- 1,线性范围为 3 .55× 1 0 - 8～ 6.0× 1 0 - 6 mol/ L,检出限为 3 .55×1 0 - 8mol/ L。方法用于雨水中痕量 H2 O2 的测定 ,结果满意     

极谱法测定维生素B12中的痕量钴

在pH 10,0.04 mol/L的NH3*H2O-NH4Cl缓冲溶液中,钴-百里香酚酞在NaNO2存在下,于-1.25 V(vs.SCE)产生一尖锐、灵敏的二次导数极谱波,峰电流与钴(Ⅱ)浓度在5.0×10-8～5.0×10-6 mol/L范围内呈线性关系,检出限为2.0×10-8 mol/L.研究了该波的性质,证明该波为吸附波.方法用于维生素B12中痕量钴的测定,结果满意.     

酶催化动力学光度法测定H2O2

H2O2能够氧化偶氮染料刚果红使之褪色,而模拟酶—血红蛋白对其具有催化作用。据此建立了一种以刚果红为指示剂的H2O2-刚果红-血红蛋白酶催化反应体系测定痕量H2O2的新方法。确定了反应的最佳条件,体系的酸度为pH10.7的NH3-NH4Cl缓冲溶液,最大吸收波长为497 nm。该法的线性范围为8.0×10^-8-8.0×10^-5mol/L,检出限为1.97×10^-9mol/L,表观摩尔吸光系数为4.6×10^4L.mol-1.cm^-1。该方法可用于雨水及消毒水中H2O2的测定。     

Sc2MgGa2 and Y2MgGa2

Scandium magnesium gallide, Sc₂MgGa₂, and yttrium magnesium gallide, Y₂MgGa₂, were synthesized from the corresponding elements by heating under an argon atmosphere in an induction furnace. These intermetallic compounds crystallize in the tetragonal Mo₂FeB₂‐type structure. All three crystallographically unique atoms occupy special positions and the site symmetries of (Sc/Y, Ga) and Mg are m2m and 4/m, respectively. The coordinations around Sc/Y, Mg and Ga are pentagonal (Sc/Y), tetragonal (Mg) and triangular (Ga) prisms, with four (Mg) or three (Ga) additional capping atoms leading to the coordination numbers [10], [8+4] and [6+3], respectively. The crystal structure of Sc₂MgGa₂ was determined from single‐crystal diffraction intensities and the isostructural Y₂MgGa₂ was identified from powder diffraction data.     

Zur Kenntnis der Dialkalimetalldichalkogenide β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 und Rb2Te2

On Dialkali Metal Dichalcogenides β-Na₂S₂, K₂S₂, α-Rb₂S₂, β-Rb₂S₂, K₂Se₂, Rb₂Se₂, α-K₂Te₂, β-K₂Te₂ and Rb₂Te₂ The first presentation of pure samples of α- and β-Rb₂S₂, α- and β-K₂Te₂, and Rb₂Te₂ is described. Using single crystals of K₂S₂ and K₂Se₂, received by ammonothermal synthesis, the structure of the Na₂O₂ type and by using single crystals of β-Na₂S₂ and β-K₂Te₂ the Li₂O₂ type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na₂O₂ type to the Li₂O₂ type will be explained by means of the examples α-/β-Na₂S₂ and α-/β-K₂Te₂. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb₂S₂ is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.     

Crystal Structures of [Bu2Sn(O2PPh2)2], [Ph2Sn(O2PPh2)2], and [PhClSn(O2PPh2)OMe]2. Raman Spectra of [Ph2Sn(O2PPh2)2] and [PhClSn(O2PPh2)OMe]2

[(n‐Bu)₂Sn(O₂PPh₂)₂] ( 1 ), and [Ph₂Sn(O₂PPh₂)₂] ( 2 ) have been synthesized by the reactions of R₂SnCl₂ (R=n‐Bu, Ph) with HO₂PPh₂ in Methanol. From the reaction of Ph₂SnCl₂ with diphenylphosphinic acid a third product [PhClSn(O₂PPh₂)OMe]₂ ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P2₁/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)₂ linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.     

Electrochemical study of (NEt4)2Cl2FeS2MoS2 and (NEt4)2Cl2FeS2MoS2FeCl2

Summary The ability of [MoS₄]^2–, anions to be used as ligands for transition metal ions has been widely demonstrated, especially with Fe²⁺. The present study has been restricted to linear complexes such as (NEt₄)₂ [Cl₂FeS₂MoS₂] and (NEt₄)₂[Cl₂FeS₂MoS₂FeCl₂]. Their electrochemical properties are described: upon electrochemical reduction, these compounds yield MoS₂, as a black precipitate, and an iron complex in solution, assumed to be [SFeCl₂]^2–. The electrochemical reduction goes through two electron transfers, coupled with the breakdown of the molecular skeleton: a DISPl and an ECE mechanism. Depending on the solvent, the following equilibrium may be observed: [Cl₄Fe₂MoS₄]^2–[Cl₂FeMoS₄]^2–+FeCl₂. The equilibrium constant, K_D, was evaluated by differential pulse polarography. K_D is tightly related to the donor number of the solvent.     

Syntheses,Spectroscopic Studies,and Crystal Structures of Me2Sn(O2PPh2)2, Ph2Pb(O2PMe2)2, and Ph2Pb(O2PPh2)2

Me₂Sn(O₂PPh₂)₂ ( 1 ), Ph₂Pb(O₂PMe₂)₂ ( 2 ), and Ph₂Pb(O₂PPh₂)₂ ( 3 ) have been synthesized by the reactions of Me₂SnCl₂ or Ph₃PbCl with the corresponding diorganophosphinic acid in methanol. X‐ray diffraction studies show that the diorganophosphinate groups behave as double bridges between the metal atoms leading to polymeric ring‐chain structures with M₂O₄P₂ (M = Pb, Sn) eight‐membered rings. The organic groups bonded to the metal atoms are in trans‐position in the resulting octahedral arrangement around the metal atoms. The IR and the mass spectra were reported and discussed.     

Thermal decomposition of Me3SnO2PCl2, Me2Sn(O2PCl2)2 and Ph3SnO2PCl2

TG and DTA studies on Me₃SnO₂PCl₂, Me₂Sn(O₂PCl₂)₂ and Ph₃SnO₂PCl₂ were carried out under dynamic argon atmosphere. The results show that the decomposition proceeds in different stages leading to the formation of Sn₃(PO₄)₂ as a stable product. This compound was characterized by IR spectroscopy. Decomposition schemes involving reductive elimination reactions were proposed.     

The alkali hypophosphites KH2PO2, RbH2PO2 and CsH2PO2

The structures of the hypophosphites KH₂PO₂ (potassium hypophosphite), RbH₂PO₂ (rubidium hypophosphite) and CsH₂PO₂ (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.