气相色谱法分离和测定对甲硫基苯酚

采用气相色谱法分离和测定对甲硫苯酚。在Ф６ ×１ ．５ ×１ ５００ ｍ ｍ 玻璃柱内填充５ ％ Ｏ Ｖ１０１／ Ｃｈｒｏｍ ｏｓｏｒｂ Ｗ Ａ Ｗ Ｄ Ｍ Ｃ Ｓ 的色谱柱上,对甲硫基苯酚与内标物磷酸三丁酯及杂质之间具有较好的分离效果;而且以磷酸三丁酯为内标物时其重量校正因子相当稳定,即 ｆｗ ． Ａ ＝ ０ ．９４８ ±０ ．００５ ４（ｎ ＝ ９ ,α＝ ０ ．０５） 。该方法操作简便、快速、准确。对同一试样的８ 次平行独立测定其标准偏差为０ ．２５ ,变异系数为０ ．００７ ２ 。并且,该方法的３ 次加入法回收率达９８ ．１８ ％ ～９９ ．２２ ％ 。     

若干1,1,2,2-四乙酰基乙烷阴离子(TAE2-)桥联的联吡啶双核铜配合物的合成,结构和磁性

合成了２ 个以１ ,１ ,２ ,２四乙酰基乙烷阴离子（ Ｔ Ａ Ｅ２ － ） 为桥联的双核铜配合物［（ｂｉｐｙ Ｃｕ）（ｂｉｐｙ Ｃｕ Ｈ２ Ｏ） Ｔ Ａ Ｅ］（ Ｃｌ Ｏ４）２ ·２ Ｈ２ Ｏ（ Ⅰ） 和（ｂｉｐｙ Ｃｕ）２ Ｔ Ａ Ｅ（ Ｐ Ｆ６）２ ·３ Ｈ２ Ｏ（ Ⅱ） 及１ 个多核铜配合物［ Ｃｕ Ｔ Ａ Ｅ·２ Ｈ２ Ｏ］ｎ（ Ⅲ） ,并进行了表征。对配合物（ Ⅰ） 进行了 Ｘ射线晶体结构分析,该配合物属于单斜晶系,空间群为 Ｐ２１／ ｎ ,晶胞参数为ａ ＝ ７ ．９２３（１） ．４６５（５） 〓, ｂ ＝ １６ ．０６８（３） 〓, ｃ ＝ ３０ ．１８２（７） 〓, β＝ ９３ ．１８（２）°,晶胞体积 Ｖ＝ ３８３６ ．５（１２） 〓３ , Ｚ＝ ４ , 最终偏离因子 Ｒ１ ＝ ０ ．１１３５ ,ｗ Ｒ２ ＝ ０ ．３１２１ 。磁性质研究表明在这两个双核铜配合物中两个金属铜之间存在弱的反铁磁性相互作用。     

气相色谱法测定化妆品中的 VE 含量

介绍了一种用气相色谱法准确快速测定品中ＶＥ２含量的新方法。该法以ＶＣ作保护剂,用环已烷提取样品,ＳＥＰ－ＰＡＫ ＡＬＵＭ－Ａ小柱净化。以氯氰菊酯内标物,在１？５％ＯＶ＝－１７色谱柱上进行分离,测定化妆口中ＶＥ含量。内标物与样品的分离度为１．５５。平均回收纺为９４．３％～９８．８％,相对标准偏差为１．７％～３．５％（ｎ＝５）。     

反相高效液相色谱法测定食品中水溶性维生素的含量

采用反相色谱法同时测定食品中水溶性维生素（Ｖｉｔａｍｉｎ）Ｃ、Ｂ５、Ｂ６、Ｂ１、Ｂ２和Ｂ１２的含量，ＰＣ８１０／Ｓ２５０４（４．０ｍｍ×２５０ｍｍ，１０μｍ）柱，０．１ｍｏｌ／Ｌ甲酸铵甲酸溶液（ｐＨ＝４．５，含０．４％二乙胺）＋甲醇（７５＋２５）为流动相，流速１ｍＬ／ｍｉｎ，ＵＶ２５４ｎｍ，１２ｍｉｎ内实现了良好分离，乙酰苯胺为内标物。苹果及强化奶粉中维生素平均回收率分别为９２．５０％～１０５．６０％和９５．００％～１０２．８０％，该法操作简便、迅速、可靠、测试费用低。     

(Ce_(0.67)Tb_(0.33))MgAl_(11)O_(19)和BaMgAl_(10)O_(17)∶Eu~(2 )荧光体的微波辐射合成及其发光性能

用微波辐射法合成了（Ｃｅ０．６７Ｔｂ０．３３）ＭｇＡｌ１１Ｏ１９（ＰＧ）和ＢａＭｇＡｌ１０Ｏ１７（ＰＢ）两种荧光体，经Ｘ射线粉末衍射分析，其ｄ值和Ｉ／Ｉ０值与ＪＣＰＤＦ３６７３和２６１６３基本一致。计算得到ＰＧ的晶胞参数ａ＝０５５８２ｎｍ，ｃ＝２１８８４ｎｍ；Ｐ－Ｂ的晶胞参数α＝０５６１６ｎｍ，ｃ＝２２６１４ｎｍ。测定了两种荧光体的激发光谱和发射光谱。Ｐ－Ｇ的色坐标ｘ＝０３１６，ｙ＝０５６５；Ｐ－Ｂ的色坐标ｘ＝０１５６，ｙ＝０１０６。与市售同类荧光粉相比，Ｐ－Ｇ的相对发光强度为８８％，Ｐ－Ｂ的相对发光强度为８０％。     

HPLC法测定中成药制剂中10-羟基-2-癸烯酸的含量

采用ＳｐｈｅｒｉｓｏｒｂＣ１８柱,以甲醇∶水∶磷酸（４５∶６５∶０．５）为流动相,以ＵＶ２１０ｎｍ为检测波长,测定中成药制剂中１０－羟基－２－癸烯酸（１０－ＨＤＡ）的含量,１０－ＨＤＡ浓度在０．００６～０．０３０ｇ／Ｌ范围内线性关系良好（ｒ＝０．９９９９,ｎ＝５）,检测限为０．２ｍｇ／Ｌ（Ｓ／Ｎ＝３∶１）。方法具有定量准确、快速及主峰和杂质分离度高等特点。     

铕-对氨基苯甲酸-邻菲咯啉配合物[Eu(p-ABA)_3Phen·H_2O](C_2H_5OH)的晶体结构

［Ｅｕ（ｐＡＢＡ）３Ｐｈｅｎ·Ｈ２Ｏ］（Ｃ２Ｈ５ＯＨ）（ｐＡＢＡ＝对氨基苯甲酸根，Ｐｈｅｎ＝邻菲咯啉）配合物晶体属三斜晶系，Ｐ１空间群，ａ＝１２２６８（３）ｎｍ，ｂ＝１４００５（３）ｎｍ，ｃ＝１０４４０（３）ｎｍ；α＝１０２６９（２）°，β＝１０８９３（２）°，γ＝９２８５（２）°；Ｚ＝２，Ｔ＝２７３Ｋ。最终的Ｒ因子为００３９。配合物中心Ｅｕ３＋离子与周围ｐＡＢＡ的６个氧原子和Ｐｈｅｎ的一对氮原子以及一个水分子的氧原子配位，配位多面体属畸变的单帽四方反棱柱体，水分子的氧原子占据帽位。     

N-(2-对甲苯磺酰胺基乙基)氮杂12-冠-4合碘化氯仿的合成及晶体结构

Ｎ－（２－对甲苯磺酰胺基乙基）氮杂１２－冠－４（Ａ）与碘在氯仿溶液中反应，得到了电荷转移配合物Ａ·［ＩＨＣＣｌ３］晶体．Ｉ…Ｈ—Ｃ氢键的键长为０．３８９ｎｍ．晶体属单斜晶系，空间群Ｐ２１／ｎ，ａ＝０．７３６４（７）ｎｍ，ｂ＝１．６７３２（０）ｎｍ，ｃ＝２．１４１３（６）ｎｍ，β＝９９．０９（１）°，Ｚ＝４，Ｖ＝２．６０５５（５）ｎｍ３，Ｒ１＝０．０４７９，Ｒ２＝０．０４２４     

二氯[1,2-二(2-甲酰甘氨酸苯硫基)乙烷]合钯(Ⅱ)的合成和结构

本文首次报道标题化合物的合成和分子结构。该配合物属单斜晶系。空间群为Ｃ２／ｃ。ａ＝１．６３４（２）ｎｍ，ｂ＝０．８０７（１）ｎｍ，ｃ＝２．２２３（２）ｎｍ；β＝１２０．３８（５）。Ｒ＝０．０２５７，ｗＲ２＝０．０６７１。结构测定表明，Ｐｄ（Ⅱ）与硫和氯形成四方平面形配合物。硫原子采取不等性ｓｐ３杂化。在该配合物中未形成Ｐｄ（Ⅱ）－酰胺氮配键     

高效液相色谱手性流动相法拆分甲状腺素对映体

运用高效液相色谱手性流动相法（ＨＰＬＣ－ＣＭＰ）对影响甲状腺素对映体（Ｄ－,Ｌ－Ｔ４）分离方法的因素：三乙胺（ＴＥＡ）浓度,流动相ｐＨ值,铜离子（Ｃｕ２＋）浓度,Ｌ－脯氨酸（Ｌ－ｐｒｏ）浓度,柱温以及流动相的流速进行了系统的研究。同时,考察了色谱方法分离Ｔ４对映体的线性关系,精密度和准确度。线性响应范围为０．６～３．２　ｎｍｏｌ　（Ｄ－,Ｌ－Ｔ４）,线性相关系数为ｒＤ－Ｔ４＝０．９９８０,ｒＬ－Ｔ４＝０．９９９０,日内和日间的精密度分别为ＲＳＤ＜２．３％（ｎ＝６）,ＲＳＤ＜３．１５％（ｎ＝５）。结果表明本实验所得的色谱条件较文献报道的优越,分离条件简单,重现性好。ＨＰＬＣ－ＣＭＰ法测定甲状腺素对映体其意义在于该方法可为定量测定药品及人体血液中Ｄ－,Ｌ－Ｔ４两种异构体,为治疗药物监测（ＴＤＭ）和药物不良反应监测（ＡＤＲｓ）提供了依据。     

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.     

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.     

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.     

Formal [(2+2)+2] and [(2+2)+(2+2)] nonconjugated dienediyne cascade cycloadditions

[reaction: see text] Fluoranthene 2 and heptacycle 3 are easily accessible from the reaction of diyne 1 and norbornadiene (NBD) in the presence of the rhodium catalyst. The unusual [(2+2)+(2+2)] adduct 3 was confirmed by the X-ray crystal structure analysis.