硅钼杂多阴离子薄膜修饰电极线性扫描伏安法测定黑液中要溶性硅

本报导了以玻碳电极为基体的１∶１２硅钼杂多阴离子薄膜化学修，铈电极的制备及其电化学特性。并应用于导数伏安法测定。在４．０×１０＾－３ｍｏｌ／Ｌ９ＮＨ４）６Ｍｏ７Ｏ２４－６６．８×１０＾－２ｍｏｌ／ＬＮａ３Ｃｉｔ－０．４８ｍｏｌ／Ｌ ＮＨＯ３体系中，硅浓度在８．３×１０＾－７～１．７×１０＾－３ｍｏｌ／Ｌ。对可溶性硅（以ＳｉＯ２计）为２４５．０５ｍｇ／Ｌ的黑液，稀释１０倍后，取２．００ｍＬ平行测定     

烟酰胺极谱行为的研究

用单扫示波极谱法，烟酰胺在ＫＨ２ＰＯ４－Ｎａ３２Ｂ４Ｏｒ－ＮａＯＨ，底液中呈出现良好的二阶导数峰，Ｅｐ＝－１．８０±０．０１Ｖ，在５×１０＾－７－２×１０＾－５ｍｏｌ／Ｌ范围内，峰高与浓度成线性关系，检测限为２．２×１０＾－７ｍｏｌ／Ｌ。此法用于ＮＡ片剂含量的测定，其结果良好。     

葡萄糖脱氢酶微型生物传感器的研制及应用

以甲苯胺兰（ＴＢ）修饰碳糊微电极为基体，将葡萄糖脱氢酶（ＧＤＨ）用丝素蛋白膜固定于修饰微电极表面制成了生物传感器，在ｐＨ７．０的ＮａＯＨ－ＮａＨ２ＰＯ４缓冲溶液中，烟酰胺腺嘌呤二核苷酸（ＮＡＤ）的浓度为１．０４×１０＾－３ｍｏｌ／Ｌ的条件下，其响应电流与葡萄糖浓度在１．０×１０＾－４～３．２×１０＾－３ｍｏｌ／Ｌ范围内有良好线性关系，响应时间为２０ｓ；检测限为４．０×１０＾－５ｍｏｌ／Ｌ。该传感器     

一种基于形成杂多核络合物的荧光增敏效应的研究：Ⅲ.锰（Ⅱ）,钴（…

本研究了Ｍｎ＾２＋和Ｃｏ＾２＋对７－（８－羟基－３，６－二磺基萘偶氮）－８－羟基喹啉－５－磺酸－硼砂反应体系的混合荧光增敏作用。实验条件下，荧光增敏强度满足线性加和关系的范围是：Ｍｎ＾２＋浓度０￣２．９×１０＾－７ｍｏｌ／Ｌ；Ｃｏ＾２＋浓度０￣８．８～１０＾－７ｍｏｌ／Ｌ；总浓度不超过１．０×１０＾－６ｍｏｌ／Ｌ。检出限量为Ｍｎ＾２＋４．５×１０＾－９ｍｏｌ／Ｌ和Ｃｏ＾２＋１．４×１０＾－８ｍｏ     

大量锆存在下铪镧钼杂多酸—耐尔蓝体系测定给

本文研究了耐尔蓝（ＮＢ）－给镧钼杂多酸（ＨｆＬａＭｏ－聚乙烯醇（ＰＶＡ）体系测定铪的超高灵敏光度法。在ＰＶＡ存在下，铪，镧和钼酸铵形成杂多酸，继而与耐尔蓝形成离子缔合物。其适宜条件为〔ＨＣｌｏ４〕＝１．２ｍｏｌ／Ｌ，〔Ｌａ×３＋〕＝２．９×１０＾－７ｍｏｌ／Ｌ，〔ＭｏＯ４×２－〕＝１．１×１０＾－３ｍｏｌ／Ｌ，〔ＮＢ〕＝２．７×１０＾－６ｍｏｌ／Ｌ，ＰＶＡ０．０８％。离子缔合物的最大吸收波长在５９     

氨基萘磺酸盐无保护流体室温磷光的取代基位置效应

以ＴＩＮＯ３作重原子微扰剂,Ｎａ２ＳＯ３作化学除氧剂,在无需加入任何保护介质条件下,仅需仪器光源适当照射,１－氨基４－萘磺酸盐、１－氨基５－萘磺酸盐、２－氨基１－萘磺酸盐水溶液均能产生强而稳定的室温磷光信号（ＲＴＰ）。３种氨基萘磺酸盐浓度分别在４．０×１０＾－８￣１．２×１０＾－５ｍｏｌ／Ｌ;１．２×１０＾－６￣１．６×１０＾－５ｍｏｌ／Ｌ;１．６×１０＾－７￣８．０×１０＾－６和８．０×１０＾－     

异硫氰酸异鲁米诺的电致化学发光性质及其机理

研究了异硫氰酸异鲁米诺的电致化学发光性质及其反应机理。在ＫＯＨ－ＫＣｌ－Ｈ２Ｏ２介质中，施加三角波脉冲电压使异硫氰酸异鲁米诺产生较强的电致化学发光，其浓度在２．５×１０＾－１１－１．０×１０＾－７ｍｏｌ／Ｌ范围与发光强度成线性关系，检测限为６．２×１０＾－１２ｍｏｌ／Ｌ。     

鸟嘌呤—铜配合物在汞电极表面上的电吸附性的研究

在０．０２ｍｏｌ／Ｌ ＮａＨＣＯ３－０．０５ｍｏｌ／Ｌａ２ＳＯ４介质中、用极谱法和伏安法研究表明,铜－乌嘌呤配合物在汞电极表面上的吸附服从Ｌａｎｇｍｕｉｒ吸附,测得其饱和吸附量Γｍ＝１．１×１０＾－１０ｍｏｌ／ｃｍ＾２,吸附系数β＝４．７×１０＾４,吸咐自由能△Ｇ°＝－３６．６ｋＪ／ｍｏｌ。在８×１０＾－６ｍｏｌ／Ｌ Ｃｕ＾２＋离子存在下,可用示差脉冲阴极吸附溶出法测定８×１０＾－１０～１×１０＾     

聚乙二醇辛基苯基醚—铁（Ⅱ）—过氧化氢化学发光体系研究及应用

本报道了聚乙二醇辛基苯基醚（ＯＰ）－Ｆｅ（Ⅱ）－Ｈ２Ｏ２化学发光体系，建立了高等反悔一测定微量铁的化学发光新方法，检出限为７．６×１０＾－８ｍｏｌ／Ｌ，线性响应的浓度范围为１．０×１０＾－７－１．０×１０＾－３ｍｏｌ／Ｌ，该法所受金属离子孤干扰小，用于实际水样及铜精矿样品的全铁的测定，结果令满意。     

头孢噻肟钠的降解及其产物伏安行为的研究

头孢噻肟钠在ＮａＯＨ溶液中降解后，于０．１ｍｏｌ／ＬＮａＯＨ中得一灵敏的吸附伏安原峰，Ｅｐ＝－０．７８Ｖ（νｓＡｇ／ＡｇＣｌ），ｉｐ与头孢噻肟钠浓度在１．０×１０＾－＾９－１．０×１０＾－＾８，１．０×１０＾－＾８－１．０×１０＾－＾７，１．０×１０＾－＾７－１．０×１０＾－＾６ｍｏｌ／Ｌ范围内呈线性关系，检出限为５．０×１０＾－＾１＾０ｍｏｌ／Ｌ。用多种电化学手段研究其降解产物的伏安行为，测定了     

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.     

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.     

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.