8-羟基喹哪啶固相萃取光度法测定水样中的铁

研究了8-羟基喹哪啶与铁的显色反应，在pH为8．0的氯化氨-氨水缓冲介质中，在十六烷基三甲基溴化铵(CTMAB)存在下，8-羟基喹哪啶与铁反应生成3：1稳定的蓝紫色络合物，该络合物可被Waters Sep-Park-C18固相萃取小柱萃取，用乙醇洗脱后用光度法测定，络合物λmax=600nm。在此波长下其它金属离子的络合物无光吸收，对铁选择性很好，铁含量在0-5mg/L内符合比尔定律，方法用于水样中痕量铁的测定，结果令人满意。     

Voltammetric Behavior of Water‐Soluble Endohedral Metallofullerene Derivatives

Voltammetric behavior of water‐soluble endohedral metallofullerene derivatives Gd@C₈₂(OH)₅(NHCH₂COOH)₉ (GN) and Gd@C₈₂(OH)₆(NHCH₂CH₂SO₃H)₈ (GS) was characterized in 0.1 M KCl solution by CV and DPV. They showed similar redox behavior, that is, a reversible electroreduction process on HMDE was found; in the mean time, an irreversible oxidation process and an irreversible reduction process on GC electrodes were also observed. The results reveal that these two water‐soluble endohedral metallofullerene derivatives have good electron donating ability and poor electron accepting ability due to hydroxy groups, aminoacetic acid and aminoethyl sulfonic acid connected to the C₈₂ cage in comparison with Gd@C₈₂.     

弯距翠雀花中二萜生物碱的结构鉴定

从弯距翠雀花(Delphinium campylocentrum Maxim.)全草中分离得到7种二萜生物碱, 其中弯翠生(1)和弯翠亭(2)为两个新的C₁₉-二萜生物碱, 其余5个为已知的二萜生物碱. 化合物1和2的结构通过现代波谱技术, 包括二维核磁共振谱和高分辨质谱, 予以了确证.     

富勒烯C60的柱色谱分离法研究

本文提出了由Ｃ（６０）、Ｃ（７０）及少量高级富勒烯混合物（来自电弧汽化石墨所形成的碳灰）中分离出纯度为９９．９％Ｃ（６０）的两种改进的、简便价廉的柱色谱分离法．第一种方法用中性氧化铝作固定机以石油醚与甲苯（Ｖ／Ｖ＝９２．５／７．５）混合液作流动相；另一种方法以活性炭与硅胶作固定相，以甲苯作流动相，柱顶氮压约为０．０１ａｔｍ．本文尚将这两种方法与文献报道的两种相近的方法分别进行了比较．     

新显色剂6,8-二磺酸萘偶氮氯磺酚与铌(Ⅴ)显色反应的研究及应用

本文研究了新显色剂6,8-二磺酸萘偶氮氯磺酚与Nb(Ⅴ)的显色反应和测定条件。在酸度为0.6～3mol/L盐酸时。络合物的组成比为Nb(Ⅴ):R=1:3,摩尔吸光系数为4.42×10~4L·mol·L~(-1)·cm~(-1)。可不经分离直接测定钢铁试样中的铌。     

Synthesis and chelation properties of new polymeric ligand derived from 8-hydroxy-5-azoquinoline hydroxy benzene

8-Hydroxy-5-azoquinoline phenyl methacrylate-formaldehyde (8H5AQPMA-F) macromonomer was prepared from methacryloyl chloride with condensation products of 8-hydroxy-5-azoquinoline phenol-formaldehyde, and polymerized in DMF at 70 °C using benzoyl peroxide as free radical initiator. Poly(8H5AQPMA-F) was characterized by infrared and nuclear magnetic resonance spectroscopic techniques. Polychelates were obtained when the DMF solution of the resin containing few drops of ammonia was treated with the aqueous solution of Cu(II)/Ni(II). Elemental analysis of the polychelates indicates that the metal to ligand ratio was about 1:2. The IR spectra of polychelates suggest that the metals were coordinated through the oxygen of the phenolic-OH group and nitrogen of the quinoline ligand. The DRS and magnetic moment data indicate a square planar for Cu(II) complex whereas octahedral for Ni(II) complex. The TGA data revealed the thermal stability of the resin and the polychelates. X-ray diffraction study revealed the incorporation of the metal ions significantly enhanced the degree of crystallinity. The sorption properties of the chelate-forming resin towards various divalent metal ions [Cu(II) and Ni(II)] were studied as a function of pH and electrolyte.     

Preparation, Characterization and Catalytic Properties of S2O8^2-／ZrO2 Supported by Tungsten Carbide

A WC-supported S2O8^2-/ZrO2(PSZ) catalyst was prepared and characterized by means of XRD, BET, FTIR and XPS. The isomerization of n-pentane over the catalyst was investigated as well. The results show that the skeletal isomerization and the crack of n-pentane proceed simultaneously on WC-supported S2O8^2-/ZrO2 catalyst. The addition of tungsten carbide showed a significant enhancement in the activity and stability of the catalyst for n-pentane isomerization. The catalyst showed evidently a better activity than S2O8^2-/ZrO2 supported by Pt and WO3. The results can be interpreted by the existence of the tungsten oxycarbide compound(WCxOy) with carbidic, oxide and acidic sites.     

A convergent synthesis of octadeca-2E, 13Z-dienyl acetate, a pheromone component ofSynanthedon tipuliformis C.

A convergent synthesis of octadeca-2E, 13Z-dienyl acetate, a pheromone component ofSynanthedon tipuliformis C., has been developed. The synthesis is based on cross-coupling of 8-iodooct-2E-en-I-ol THP ether with dec-5Z-enyl bromide catalyzed by CuBr. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1529–1531, August, 1997.     

Titanocen-cyandithioformiat-Komplexe

The reaction of titanocene dichloride,Cp ₂TiCl₂ (Cp=⁵-C₅H₅), with one or two equivalents of sodium cyanodithioformate affords the new mono- or bis(dithiocarboxylato) derivativesCp ₂TiCl(S₂CCN) (1) andCp ₂Ti(S₂CCN)₂ (2). Elimination of sulfur converts2 into the metallacyclicCp ₂TiS₂C₂(CN)₂ (3), which does not react with the diene isoprene, but can be reconverted into the appropriate titanocene dihalides by chlorine or bromine.

     

Reactions of 2H-3,4-dihydro-1,4-benzoxazin-6(8aH)-ones with 2,4,6-trimethylbenzonitrile oxide,III

Summary Regio-, stereo- and siteselectivity of the cycloadditions of trimethylbenzonitrile oxide with 2H-3,4-Dihydro-1,4-benzoxazin-6(8aH)-ones have been investigated. The structures of the obtained products were elucidated by means of homonuclear NOE difference spectroscopy and HMQC and HMBC spectra. The structure of 6-Benzyl-9a-methoxy-3-mesityl-9b-methyl-7,8,9a,9b-tetrahydro-3aH-1,2-oxazolo-[4,5-h]1,4-benzoxazin-4(6H)-on5 was elucidated from a single crystal X-ray structure analysis at ambient temperature: C₂₇H₃₀N₂O₄, M=446.55g/mol, monoclinic, P2₁/c,a=10.372 (34) Å,b=11.908 (21) Å,c=20.040 (34) Å, =97.16 (17)°,V=2455.8 (1.9)ų,Z=4,d _c=1.208g/cm³, =0.08mm^–1,R=0.0546.Dedicated to Prof. Ott with best wishes for his 70^th birthday