不同环境条件对土壤-巴戟天系统重金属分布的影响

采用AA-6800型石墨炉原子吸收光谱仪研究了土壤-巴戟天系统中铅的分布情况,包括不同地段、不同土壤类型、不同土壤pH值对土壤-巴戟天入药部位根和果实中铅的含量影响。实验结果表明,环境条件变化对土壤-巴戟天系统铅含量有一定的影响,其中土壤的pH值对土壤中的有效铅浓度及巴戟天的铅含量影响较大。     

气相色谱-质谱法测定土壤中2,4,6-三溴苯酚的含量

<正>2,4,6-三溴苯酚(TBP)是一种重要的精细化工中间体,广泛用于合成无毒溴系阻燃剂、医药、农药和防霉防腐剂等[1]。含2,4,6-三溴苯酚的产品在生产和使用过程中通过物理或化学等方式进入环境水体和土壤中[2-3],因具有持久性、生物累积性和生物毒性等,可能对生态环境和人体健康构成严重威胁[4]。2,4,6-三溴苯酚可经呼吸道、皮肤和胃肠道进入人体内,引起肺部明显病变,损害呼吸系统,引发全身震颤,有时抽搐,甚至死亡。目前,2,4,6-三溴苯酚的研究主要集中在其上述应用领域或水体中[5-13],对于土壤的测定报道较     

4-氨基-3-氟苯酚的合成工艺研究

4-氨基-3-氟苯酚(CAS No·399-95-1)是农药杀虫剂氟虫脲(flufenoxuron)的重要中间体,也是医药,化工制备的重要中间体,其制备方法报道较少,美国学者Benner[1],Brown等[2],Derrenbacker等[3],以及日本学者田中等[4],厦本等[5]分别用铂碳催化,进行还原重排反应制得4-氨基-3-氟苯酚     

模板法合成有孔的锂离子电池正极材料LiFePO_4/C

<正>橄榄石型LiFePO4因其具有170mAh·g-1的理论容量,3.4V的放电平台,良好的循环性能和热稳定性能,无毒和价格低廉等优点,自1997年被Goodenough等[1]首次报道以来受到人们广泛关注[2-3],并被认为在动力电池应用上极有潜力[4]。但此材料的电导率低及扩散性能差[1],限制其大规模应用。针对上述缺点研究人员对LiFePO4的改性研究主要包括:包覆碳[5-7]和金属粉末[8]、掺杂金属离     

毛细管电泳-间接紫外检测法分离和测定食品中的有机酸

有机酸毛细管电泳（CE）分析是90年代初首先被报道的[1],近年来有了较大的发展[2]．采用CE法可进行不同基质样品如食品、饮料、尿液等样品中多种有机酸的同时分析[1,3,4]．该法采用CE的阴离子分离模式,在电解质溶液中加入电渗流改性剂,使电渗流方向逆向,从而与阴离子的电泳方向一致,以缩短分析时间．常见有机酸在200um以上大多无紫外吸收,一般采用间接紫外检测方法[1,3],也可采用低波长紫外检测[4]．低分子量阴离子的CE研究报道不多[5,6],有机酸的CE分离系统研究尚未见报道．本文系统地研究了毛细管电泳-间接紫外检测法分析…     

2-羟基脱氧雌酚酮的合成

2-羟基雌甾化合物是人体内对生理机能有重要意义的雌激素代谢产物,其在生物体内的含量极少,需用化学方法合成来满足研究、应用的需要。迄今为止,已报道了较多合成2-羟基和4-羟基雌甾化合物的方法[1-3],但选择性和产率并不十分理想。我们在文献报道的合成路线[1]的基础上,合成了     

示差脉冲溶出伏安法测定食盐中痕量铅

铅是一种具有蓄积性、多亲和性的毒物,对人体各组织都有毒性作用,主要损害神经系统、造血系统、消化系统和肾脏,还损害人体的免疫系统,使机体抵抗力下降,因此在环境监测及食品分析中,铅的准确测定受到人们的普遍关注。人类每天要摄入一定量的食盐,如果食盐中的铅含量大于等于 1.0 mg·kg-1,就会对人体产生危害。因此,选择一种简便、灵敏、快速、准确的测铅方法,就显得非常重要。测定铅的方法报道较多的是原子吸收光谱法[1,2],电化学分析法也有报道[3,4],本文研究了用示差脉冲溶出伏安法测定铅[5~9],本法的仪器设备简单、灵敏度高、准确…     

新型化合物[Ni(en)3]2[Ni(en)2(H2O)2][As6V15O42]·4H2O晶体的水热合成与表征

金属氧酸盐因其在医药临床、工业催化、功能材料等方面的广泛应用而引起人们的关注[1～6], 其中, 有关钒化学的研究一直很活跃, 钒具有与钼、钨明显不同的结构特性, 钒可以采取VO4, VO5和VO6方式配位, 同时, 钒的价态可以是+3, +4和+5价. 由于钒可采取多种配位方式及多种价态, 与钼酸盐和钨酸盐相比, 钒酸盐更具有结构柔顺性, 同时易形成低价或混合价态物种.在以往的文献中, 有关P-V-O体系多金属氧酸盐的水热合成的研究已有大量的报道[7], 在常规溶液合成中, 人们已对As-V-O体系进行了相对深入的研究, 而有关水热合成的研究报道却很少, 已见报道的砷钒化合物有K6*6H2O[8,9], 4-[10], 6-[11](X=SO2-3, SO2-4, H2O). 为了探究水热条件下As-V-O体系的反应特性, 我们开展了这方面的研究工作, 并取得了突破性进展. 本文采用中温水热技术合成了含有机基团的砷矾超分子化合物2**4H2O, 探讨这类化合物的非线性光学性质、催化性质及其它功能特性将是一个非常有意义的研究领域.     

成都市土壤-植物系统铅污染状况初步研究

为研究成都市土壤-植物系统铅污染状况，分析了成都市五种蔬菜及其根系土的铅含量。结果表明，土壤铅含量变化范围61．0～115．0mg/kg，均值为77．3mg/kg，所有样品含量均超过成都市土壤环境背景值，以城东和城南污染最为严重；蔬菜中铅含量以莴笋叶最高，萝卜最低，叶菜类高于瓜果类；蔬菜污染严重区与土壤污染区差别明显，说明土壤铅和植物铅污染源不同。     

脱铝超稳Y沸石的SiO2/Al2O3比与催化性能的研究

脱铝超稳Y沸石(简称DUSY)是八面沸石经脱铝改性后的固体酸催化材料,在石油化学工业和精细化学品合成中应用较广.我们曾报道了DUSY催化系列酯化反应,莰烯与乙酸的加成酯化反应[1],乙酸与β-苯乙醇的酯化反应[2],乙酸与烯丙醇的酯化反应[3],效果很好.克服了过去采用浓H2SO4作催化剂所带来的污染严重,设备腐蚀的问题,是具有应用前景的一类固体酸催化材料.谭志新等人曾报道α-蒎烯在固体超强酸上的异构化反应[4],王亚明等人报道了HMC-60催化α-蒎烯的异构化反应[5].与之相比较,用DUSY催化,其反应条件更温和.本文将DUSY的表面酸性与α-蒎烯异构反应相关联,探讨了硅铝比与催化性能的关系.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

关于"对‘燃料电池物理及化学性能的有限时间热力学分析方法'的讨论”答复

把有限时间热力学理论用于化学过程的研究,将会得到一系列新的结论,开展这方面的研究是很有意义的.文献[1]以燃料电池为例,在同时考虑化学反应及传热不可逆性的情况下,研究了燃料电池的性能界限,文献[2]指出了文献[1]计算化学反应及传热不可逆性而引起系统与有关环境的总熵产生率的错误以及由此而导致的结论所存在的问题,并进行了富有启发性的分析与讨论.但文献[2]对于系统与有关环境的总熵产生率的计算也是不正确的,由此得到的其它结论自然不能成立.本文将就此情况下系统与有关环境的总熵产生率的计算再次进行讨论,并给出电池功率和效率的有限时间热力学性能界限.