阻抑催化光度法测定茶叶中的微量氟化物

在氨基乙酸 HCl缓冲溶液中 ,Fe3+对H2 O2 氧化 2 ,4 二氨基苯酚 (DAP)褪色具有催化作用 ,游离F- 离子与Fe3+形成的稳定络离子 [FeF6]3- 可抑制褪色 ,抑制程度与F- 量线性相关。基于此建立了测定微量F- 的阻抑催化光度分析的新方法。结果表明 ,有色溶液的最大吸收波长为 5 0 0nm ,测定的线性范围为 0～ 9.0mg/L ;摩尔吸光系数为 2 .1× 1 0 5L/mol/cm ;RSD(n =6)为 5 0 %。已应用于茶叶中微量F- 的测定     

阻抑动力学法测定痕量镁

pH=11．92的Brilton－Robinson缓冲溶液中，Mn（Ⅱ）催化KIO4氧化酸性铬蓝K的反应可被痕量Mg2+有效的阻抑，据此建立了动力学法测定痕量镁的新方法，方法的线性范围是0.0-0.48mg/L，检出限为7．6×10－9g／mL，方法用于血清中痕量Mg2+及大豆中微量镁的测定获得满意结果。     

阻抑反应动力学光度法测定微量钙

提出了测定微量钙的阻抑反应动力学光度法。在0．012mol/L硫酸中,KBrO3氧化偶氮氯磷Ⅲ褪色,Ca^2 可阻抑该褪色反应的速度。最大吸收波长为550nm,Ca^2 浓度在0－1．4mg/L范围内与ΔSA呈线性关系,检出限0．0042mg/L。方法准确,灵敏,简便,用于直接测定水样中的微量钙,获得满意的结果。     

阻抑动力学分光光度及荧光光度法测定微量碘

在稀磷酸介质中,微量碘离子对亚硝酸根催化溴酸钾氧化吡罗红B褪色及荧光猝灭的反应有显著阻抑作用,以此为指示反应提出了测定微量碘离子的阻抑动力学光度和阻抑动力学荧光分析新方法。测定碘离子的线性范围分别为4-200μg/L和3-40μg/L,检出限分别为2.8μg/L和1.6μg/L。用于食品中微量碘的测定,结果满意。     

废水中痕量酚的流动注射停流-催化光度法测定

基于在硫酸介质中痕量酚对溴酸钾氧化罗丹明B反应的催化作用,建立了测定痕量酚的快速、简便的流动注射流－催化光度分析的新方法。该方法的线性范围为0．60－4．00mg/L,检出限为0．1mg/L,进样频率为34／h。11次重得测定的相对标准偏差小于2．0％。该法用于废水中酚的测定,并与4－氨基安替比林比色法对照,结果满意。     

表面活性剂增敏阻抑动力学光度法测定痕量草酸

在稀盐酸介质中，微量草酸对H2O2氧化靛红的褪色反应有显著的阻抑作用，非离子表面活性剂Triton X-100对此体系有强烈的增敏作用，据此建立了表面活性剂增敏阻抑动力学光度分析测定微量草酸的新方法。方法的线性范围是0．005-0．50mg/L，检出限为0．005mg/L。方法简便，快速，灵敏度高，用于菠菜和尿样中草酸含量的测定，结果满意。     

阻抑动力学光度法测定痕量间二硝基苯

在盐酸介质中，痕量间二硝基苯能灵敏地阻抑Fe^3 催化高碘酸钾氧化孔雀绿的反应。研究了该阻抑反应的最佳条件及动力学参数，建立了测定痕量间二硝基苯的新方法，间二硝基苯的线性范围为0.0-10.0μg/L，检出限为1.8μg/L。该法灵敏、简便，选择性好，用于环境水样中间二硝基苯的测定，结果准确。     

离子色谱法测定柠檬酸、柠檬酸钠中的F^—、CI^—、SO4^2—、C2O4^2—等

利用离子色谱仪,对柠檬酸、柠檬酸钠中的痕量F^-、CI^-、SO4^2－、C2O4^2-等进行测定,采用DIONEX ION PAC AS11－HC分离柱,以电导检测器检测,对淋洗分离条件进行了试验。选择NaOH作淋洗液,0．025－0．050mol/L NaOH做梯度淋洗,可使F^-、CI^-、SO4^2－、C2O4^2-等很好地分离,其中CI^-在0．01－200mg/L,F^-在0．05－200mg/L,SO4^2-在0.05-200mg/L,C2O4^2-在0.1-200mg/L范围内,浓度和响应值有良好的线性关系,检出限分别为F^-0.01mg/L、CI^-0.01mg/L、SO4^2-0.03mg/L、C2O4^2-0.03mg/L,回收率为90％－110％。该方法无需前处理,无基体干扰,可用于柠檬酸、柠檬酸钠中F^-、CI^-、SO4^2－、C2O4^2-的测定。     

测定驱油体系中碱度的流动注射分光光度法

采用流动注射分析技术，以酸碱指示剂－－间硝基酚溶液作载流，实现了三元复合驱油体系中碱的测定；该法可测定10－600mg/L NaOH(强碱），20－1400mg/L Na2CO3(弱碱）；方法的检出限为0．5mg/L NaOH,1mg/L,Na2CO3；对含量为200mg/L的样品测定6次的相对标准偏差为0.6%(NaOH),0.5%(Na2CO3);测定速率每小时达94个样；该法也适用于其它无机碱、有机碱的测定。     

流动注射分光光度法同时测定Fe(Ⅱ)和Fe(Ⅲ)

将流动注射技术引入邻菲罗啉分光光度法测定Fe2+分析体系,采用单阀双带镀镉锌片还原柱带隔离的阀体流路,建立了同时测定微量Fe2+和Fe3+的分析方法。Fe2+的测定范围为0~10 mg/L,检出限为1.2×10-6mg/L;Fe3+的测定范围为0~12 mg/L,检出限为1.8×10-6mg/L。方法用于水中Fe2+和Fe3+的同时测定。     

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

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.     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.