中国化学快报

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STUDY OF THEREE ELEMENT TRIPLE EXCIPLEX FORMATION

Li Min ZHANG, Yui Ping ZHANG

中国化学快报. 1990, 1(02): 97-100.

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Three element triple exciplex formation has been observed first in the system of terephthalic dimethylester,1,4-dicyanzene and naphthalene by comparing its fluorescence spectra with those of the system of terephthalic dimethylester and naphthalene,and the system of 1,4-dicyanobsnzene and naphthalene at the same experimental conditions.

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THEORETICAL STUDIES ON THE REACTION MECHANISM OF AMMONIA WITH FORMALDEHY DE

Yun Zhu HAN, Qiu Chang ZHAO, Cheng Da ZHAO

中国化学快报. 1990, 1(02): 101-104.

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The reaction mechanism of ammonia with formaldehyde was investigated by using the intrinsic reaction coordinate (IRC) method on the ab initio RHF/STO-3G basis set. our results indicate that the reaction proceeds in two stages:the first step yields the molecular complex and the second one is the rearrangement from molecular complex to the reaction proauct.

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SIMULTANEOUS DETERMINATION OF MULTICOMPONENT IN MIXED ACIDS BY MATHEMATICAL METHOD

Yong Nian NI

中国化学快报. 1990, 1(02): 105-108.

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A new method for the determination of components in mixed acids has been developed.The mathematical model is obtained from samples of known composition and is then used to predict the concentrations of components in unknown sample.The practical utility of this method is demonstrated for simultaneous determination of two systems of ternary mixed acids and the results are satisfactory.

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LOCATION OF DOUBLE BOND POSITION OF INSECT SEX PHEROMONE BY GC/MS ANALYSIS WITH CHEMICAL IONIZATION

Fan Lei KONG

中国化学快报. 1990, 1(02): 109-112.

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Ozonolysis products of four lepidopteral pheromone were identified by methane CI-MS.The spectra obtained were notably simpler than those of EI-MS,the peak of molecular ion was normally close to the base peak,and the characteristic fragment ions were high in m/z,thereby the interpretation was facilitated.

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CARBON WIRE AMPEROMETRIC FLOW THROUGH DETECTOR

Jian Nan YANG, Qun FANG, Shao Hui ZHANG

中国化学快报. 1990, 1(02): 113-116.

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A carbon wire amperometric flow through detector is described which is easily constructed at low cost for application to flow injection analysis,continuous stream analysis and liquid chromatography.The theoretical limiting current of the detector is 2.14×10⁶nCD^2/3u_f^1/3 with 36% actual current efficiency.By use of flow injection analysis,thedetecting limits for Ag(I) and Cr(VI) had achieved 1 ppb and 0.4 ppb respectively with 1.2% (n=20) relative standard deviation after preliminary experiments.

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THE SYNTHESIS AND CHARACTERISTICS OF THE COORDINATION COMPOUNDS OF 2-MERCAPTOPYRIDINE-1-OXIDE WITH THE FIPST TRANSITION SERIES METALS

Bao Lin SONG, Zai Sheng LU, De Zhong NIU, Yang CAO, Cheng ZENG

中国化学快报. 1990, 1(02): 117-118.

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The stability of the coordination compounds of the first transition series metal ions(Mn(Ⅱ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ) and Zn(Ⅱ)) with 2-mercaptopyridine-1-oxide is reported.A coordination compound CoL₂ is synthesized and characterized for the first time.

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COMPLEXES OF RARE EARTH NITRATE WITH SCHIFF BASE DERIVED FROM VANILLIN AND P-TOLUIDINE

Guo Fa LIU, Bin LI, Chong Wu NA, Kun Yuan MAO

中国化学快报. 1990, 1(02): 119-120.

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In this paper,complexes of rare earth nitrate with Schiff base derived from vanillin (3-methoxy-4-hydroxy-benzaldehyde) and p-toluidine [LnL₂(NO₃)₂]NO₃ (Ln=La-Eu except Pm,L=Schiff base ligand) have been prepared and characterized.

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SYNTHESIS AND STRUCTURE OF A TRITHIOCARBONATO Mo(Et₄N)₂[(S₂)MO₂O₂(μ-S)₂(CS₃)]

Qiu Tian LIU, Liang Ren HUANG

中国化学快报. 1990, 1(02): 121-122.

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A new trithiocarbonato Mo complex (Et₄N)₂ [(S₂)MO₂O₂(μ-S)₂(CS₃)] was obtained from a system containing MoO₄^2-,S_x^2-,and CS₂ and characterized by IR and X-ray structural analysis.The complex crystallizes in the monoclinic space group P2₁/c with a=9.539(3)Å,b=20.745(2)Å,c=15.452(2)Å,β=94.58(2)°,and Z=4.The structure was solved by direct and difference Fourier synthesis methods.Least squares refinement using 2910 reflections with I>3σ(I) converged to R=0.054.The CS₃^2- ligand in the complex chelates to Mo atom and values of the C-S bond distances in the CS₃^2- ligend indicate a substantial contribution of three resonance forms.

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SYNTHESIS,CRYSTAL STRUCTURE AND PROPERTIES OF TETRAETHYLAMMONIUM BIS [BIS(2-OXYPHENYL) DISULFIDE-O,O',S] MANGANESE

Xue Tai CHEN, Han Qin LIU, Ling Hong WENG, Liang Ren HUANG, Da Xu WU, Xin Jian LEI, Bei Sheng KANG, Jia Xi LU

中国化学快报. 1990, 1(02): 123-124.

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The synthesis,crystal structure and properties of the first Mn(Ⅲ)-disulfide complex (Et₄N) [Mn(mp-mp)₂] were reported with the Mn(Ⅲ) ion in a S₂O₄ octahedron distorted due to Jahn-Teller effect.Spectroscopic data revealed its paramagnetic properties.

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STUDIES ON THE SYNTHESIS OF (±)-CEMBRENE-A

Ying LI, Jian Min MAO, Yu Lin LI, Xiao Tian LIANG

中国化学快报. 1990, 1(02): 125-126.

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A precursor 2 of cembrene-A (a termite trail pheromone) was prepared from geraniol through 7 steps.

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REPLACED SITE OF Eu²⁺ ION IN THE COMPLEX FLUORIDES WITH THE PEROVSKITE CRYSTAL STRUCTURE

Chun Shan SHI, Ze Ren YE, Jin Yu YAO, Jia Yao SUN

中国化学快报. 1990, 1(02): 127-130.

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The replaced site of Eu²⁺ ion is dependent on the electronegativity difference of the cations in complex fluorides.In the mixed fluoride KMgF₃:Eu²⁺,Eu²⁺ ion occupies K⁺ site,its emission spectrum is a sharp line and its valence-state is stable.

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HIGHLY SENSITIVE SPECTROPHOTOMETRY OF NIOBIUM

Zong Ming LUO

中国化学快报. 1990, 1(02): 131-132.

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In pH 2.0-3.0 medium,niobium(v) forms molybdoniobic acid with sodium molybdate.A spectrophotometric method has been developed for the determination of niobium based on the formation of ion-associate compound of molybdoniobate with butyl Rhodamine B in aqueous solution in the presence of polyvinyl alcohol and 0.4-0.7 mol/L H₂SO₄.The molar absorptivity is 7.5×10⁵ L.mol^-1.cm^-1 for niobium at 585 nm.

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A FACILE METHOL FOR THE DEBROMINATION OF α-BROMOCARBONYL COMPOUNDS WITH DIBUTYL TELLURIDE

Qi ZHONG, Feng MA, Chang Qing LIU, Jian Guo SHAO

中国化学快报. 1990, 1(02): 133-134.

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α-bromocarbonyl compounds can be debrominated with dibutyl telluride in the presence of triethylamine in high yields.

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A UNIFIED RETENTION MODEL OF SOLUTE IN LIQUID CHROMATOGRAPHY

Xin Du GENG, Liu Jiao BIAN

中国化学快报. 1990, 1(02): 135-138.

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Based on six thermodynamic equilibria,a unified retention model of solute in liquid chromatography(LC) is first proposed.The unified model was tested and proved to be valid for a LC system with mobile phase consisting of a complete range of multiple,ternary or binary components and each kind of LC except size exclusion chromatography.In addition,so long as making some assumptions and mathematical conversions,the expressions of various popular models in LC can be derived by using the unified model.

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STUDY AND APPLICATION OF A NOVEL CHEMILUMINESCENCE REACTION

Xiao Hu LU, Ming Gang LU

中国化学快报. 1990, 1(02): 139-142.

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The present paper reports a novel chemiluminescence,i.e,isopropyl alcohol-C10^--H₂O₂ system.The chemiluminescence intensity is proportionalto the concentration of C10^- within certain range.Based on this fact,a new chemiluminescence method for the determination of micro amount of C10^- has been developed.The detection limit is 2.6 x 10^-8g/ml C10^- and the dynamic linear range is 2.6 x 10^-8g/ml to 2.3 x 10^-5g/ml C10^-.The method has good selectivlty and reproducibility.

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GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS OF ANABOLIC STEROIDS IN HUMAN URINE

Ji ZHANG, Chun Sheng LIU, Yi Zhong ZHANG, Chang Jiu ZHANG, Li YE, Tong Hui ZHOU

中国化学快报. 1990, 1(02): 143-146.

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A new GC/MS method for detection and identification of 19 anabolic steroids in human urine is presented.The procedure involves adsorption and isolation on a macroporous XAD-2 resin,enzymatic hydrolysis,alkaline extraction,derivatization,GC separation and MS detection.Gas chromatographic-mass spectrometric data illustrate artifacts arising from enzymatic hydrolysis of steroid glucuronides and the structural characterization of their metabolites.Using this method,metabolic studies of these steroids in human urine were made after their ingestion by normal and healthy male volunteers.This method was proven to be suitable for large-scale routine analysis of anabolic steroids and was used successfully in passing the doping control test held by the Medical Commission of the International Olympic Committee.

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ELECTROLYTIC REMOVAL OF COPPER FROM GUANYL-O-ALKYL-ISOUREA COPPER COMPLEX

Kai Chi PANG, Chi Rui CHEN, Xiao Min WANG

中国化学快报. 1990, 1(02): 147-148.

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A facile method for removing copper from guanyl-0-alkylisourea copper complex was found by using electrolysis.The complex was electrolyzed at a copper cathode in dilute hydrochloric or nitric acid to give guanyl-O-alkylisourea salt in high yield and current efficiency.

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DO FLAT MOLECULES WITHOUT A SIDE-CHAIN READILY FORM AGGREGATES ? A FLUORESCENCE STUDY OF PYRENE EXCIMER AND EXCIPLEX FORMATION IN ETOH-H₂O AND MEOH-H₂O SOLVENT SYSTEMS

Ji Liang SHI, Yuan Chao ZHANG, Li Jun XIA, Xi Kui JIANG

中国化学快报. 1990, 1(02): 149-152.

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The speculation that a flat molecule without a side-chain might not readily undergo the hydrophobicity-driven process of aggregation has been shown to be a plausible proposition by the fact that pyrene molecules do not form excimers even in a supersaturated solution with relatively high solvent aggregating power (SAgP).

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ORGANOPHOSPHINE INITIATED REACTION OF PERFLUOROALKYL IODIDES WITH ALKENES

Wei Yuan HUANG, Han Zhong ZHNG

中国化学快报. 1990, 1(02): 153-154.

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perfluoroalkyl iodides reacted with alkenes in acetonitrile solu-tion containing catalytic amount of organophosphine under mild condition to give the corresponding adducts in moderate to good yields.Reaction was shown to involve a free radical mechanism.

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TRIFLUOROMETHANESULFONIC ACID AS A USEFUL REAGENT FOR CLEAVAGEOF PEPTIDYL RESIN

De Xin Wang, Gui Shen Lu

中国化学快报. 1990, 1(02): 155-156.

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The efficiency of TFMSA as a cleaving reagent for peptidyl resin(I-VⅢ) was evaluated by quantitative ninhydrin test of peptide substitution degree (SD) on resin.Under different conditions,such as variation of C-terminal residue,resin linkage,the temperature and reaction time etc.,TFMSA can be used very conveniently instead of HF in many cases.

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HIGH-PERFORMANCE GAS DIFFUSION POROUS STARVED OF ELECTROLYTE SOLUTION

Jin Kua YOU, Zu Geng LIN, Zhao Wu TIAN

中国化学快报. 1990, 1(02): 157-160.

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The performance of gas diffusion porous electrode starved of electrolyte solution can be significantly increased by decreasing the thickness of uneven liquid film covering the catalyst agglomerates.

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STUDIES ON MECHANIS OF PHOTOSENSITIZED ISOMERIZATION OF NORBORNADIENE DERIVATIVES

Yang Fu MING, Qian Hong WU, Yi CAO

中国化学快报. 1990, 1(02): 161-164.

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Using acridine dyes as sensitizers,the photoisomerization of three norbornadiene derivatives was investigated.The valence isomerization of nor-bornadiene derivatives (Ⅰ_a,Ⅰ_b,Ⅰ_c) gave their corresponding isomers of quadri-cyclane (Ⅱ_a,Ⅱ_b,Ⅱ_c) operating with relatively high efficiency in an electron transfer mode.Their quantum yields of isomerization were determined and the reaction mechanism was discussed.

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PERFLUOROALKANESULFONYL IODIDE GENERATED FROM THE REACTION OF PERFLUOROALKANESULFINATE SALT WITH IC1

Wei Yuan HUANG, Yuan XIE

中国化学快报. 1990, 1(02): 165-166.

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The reaction between perfluoroalkanesulfinate salts (1) [R_fSO₂MR_f=a,Cl(CF₂)₄;b,Cl(CF₂)₆;c,Cl(CF₂)₈;d,n-C₆F₁₃;e,n-C₈F₁₇;M-Na;K;Hg(I)] and iodine monochloride in dichloromethane at low temperature(e.g.-30- -50℃) resulted in the formation of the corresponding perfluoroalkane-sulfonyl iodides (2),which were identified by their ¹⁹F NMR spectra.The perfluoroalkanesulfonyl iodides generated in situ reacted smoothly with olefins to forum 1:1 adducts with good yields.Thus,these reactions provide another method for the synthesis of the very unstable perfluoroalkanesulfonyl iodide.

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SYNTHESIS AND TAUTOMERISM OF KETENE N,O-ACETALS WITH BENZOXAZOLINE RING

Zhi Tang HUANG, Ping Cheng ZHANG

中国化学快报. 1990, 1(02): 167-170.

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Benzoxazoline ring substituted ketene N,O-acetals 3 were synthesized by the reaction of ketene S,S-acetals 2 with 2-aminophenol.The tautomeric equilibrium of some 3 was also observed.

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ADDITION OF SODIUM BISULFITE TO BILIVERDIN

Jin Shi MA, Fang YAN, Chang Qi WANG, Jin Hua CHEN

中国化学快报. 1990, 1(02): 171-172.

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Sodium bisulfite could add to the central methine bridge of biliver-din in methanol,and give sodium bilirubin-10-sulfonate,however no bilirubin was formed.

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THE STRUCTURE OF ARMILLARIZIN,A NEW PROTOILLUDANE SESQUITERPENOID AROMATIC ESTER FROM ARMILLARIA MELLEA (VAHL.EX FR) QUEL.

Jun Shan YANG, Ya Lun SU, Yu Lan WANG, Xiao Zhang FENG, De Quan YU, Xiao Tian LIANG

中国化学快报. 1990, 1(02): 173-174.

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A new protoilludane sesquiterpenoid aromatic ester,named armillarizin (1) has been isolated from the artificially cultured mycelium of Armillaria me-llea(Vahl.ex Fr)Quel.(Tricholomataceae).Its structure was deduced on the ba-sis of spectral analyses.The relative configuration was established from thenuclear Overhauser effects and from the values of ¹H-¹H coupling constants.

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SIMULTANEOUS DETERMINATION OF EPHEDRINE AND ITS ANALOGUES IN URINE BY CAPILLARY GAS CHROMATOGRAPHY

Lin LI, Jian Fang CUI, Kai Rong CUI, Yi ZHOU, Mu Zou WANG, Tong Hui ZHOU

中国化学快报. 1990, 1(02): 175-178.

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A method is developed for the simultaneous determination of ephedrine,pseudoephedrine,norephedrine,norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylamine is used as the internal standard.Calibration graphs are linear down to 1.30ug/ml urine.

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A SIMPLE,MANUAL SOLID-PHASE SYNTHESIS OF OLIGORIBONUCLEOTIDE

Chun Guang WANG, Sidney M. HECHT

中国化学快报. 1990, 1(02): 179-182.

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A simple,manual solid-phase synthesis of RNA fragments using 2'-(p-methoxyben-zyl) nucleosides and phosphoramidite chemistry is described.

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THEORETICAL STUDY ON THE CONFIGURATION OF [PdCl₂(C₂H₄OH)]^-

Yan Bo DING, Xiao Yuan FU

中国化学快报. 1990, 1(02): 183-184.

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The configuration of [PdCl₂(C₂H₄OH)]^- has been studied by pseudopotential ab initio method.A cis isomer was found to be the reaction intermediate in the Wacker process.

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STUDY ON BINUCLEAR COPPER(I) COMPLEXES Ⅲ.SYNTHESIS,CHARACTERIZATION AND ELECTROCHEMISTRY OF DICHLORO-TRIS (4-VINYLPYRIDINE)-DICOPPER(I) COMPLEX

Zhen Feng XI, Rui Na YANG, Dou Man JIN

中国化学快报. 1990, 1(02): 185-186.

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Recent years,many novel complexes have been prepared by using hetero-bidentate ligands.However,complexes with such ligands as 4-vinylpyridine which has two different coordinating sites have not been reported,and only a few complexes of Cu(I) have been published^1-3.The title complex Cu₂(C₅H₄N·CH=CH₂)₃Cl was prepared and characterized by elemental analyses,ICP,IR,and electronic spectra.Its conductivity,oxidation potential and reduction potential were measured.

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DETERMINATION OF VOLATILE PHENOLS IN CHINESE LIQUORS BY GC-MS

Chun Sheng LIU, Jia Rui GUAN, Mao Sun LU, Chang Tai YAN

中国化学快报. 1990, 1(02): 187-190.

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A new method for determining volatile phenols in Chinese liquors is proposed.Phenols are sorbed on a macroporous anion-exchange resin after the liquors were brought to a pH value of 12.5,then eluted with HCl-acetone,extracted with methylene dichloride and concentrated to a suitable concentration for derivatization with pentafluorobenzyl bromide (PFB).The PFB derivatives of phenols were successfully separated by gas chromatography on a 30 m SE-54 elastic glass capillary column and detected with Ni-63 electron capture detec-tor.The characteristics of this method are:high sensitivity,low interference and 95% average recovery of phenols.The method was used successfully in the determination of vola-tile phenols in eight kinds of Chinese liquors.

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1990年, 第1卷, 第02期　刊出日期：1990-08-20

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1990年, 第1卷, 第02期 刊出日期：1990-08-20

1990年, 第1卷, 第02期　刊出日期：1990-08-20