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1.
陈建荣  吴香梅 《分析化学》1994,22(9):928-930
本研究了1-(5-溴-2-吡啶偶氮)-2-萘酚-6-磺酸(5-Br-PAN-S)与铁(Ⅱ)的显色反应,试验表明,在pH3-10范围内铁(Ⅱ)与5-Br-PAN-S型成稳定的络合物,络合物在550nm和750nm有二个吸收峰,其表现摩尔吸光系数分别为2.31×10^4和1.77×10^4L.mol^-^1.cm^-^1。络合物组成比为铁(Ⅱ):5-Br-PAN-S=1:2,络合物稳定常数为1.82  相似文献   

2.
张光  张林林 《分析化学》1994,22(11):1155-1157
本研究了2-(6-硝基-2-苯并噻唑偶氮)-5-二甲氨基苯甲酸(6-NO2-BTAMB)与铜的显色反应。结果表明,在pH2.0 ̄4.5的乙醇水溶液中6-NO2-BTAMB与铜形成一种稳定的蓝绿色络合物,其最大吸收波长位于650nm处,表观摩尔吸收系数为7.75×10^4L·mol^-1·cm^-1,络合物的组成为6-NO2-BTAMB∶Cu=1∶1,铜浓度在0 ̄10μg/10ml范围内服从比尔定  相似文献   

3.
徐斌  邹欣平 《分析化学》1995,23(5):579-581
本研究了试剂安替比林基重氮氨基-24-二硝基苯(APDNBT)与汞的显色反应,在Tween-80存在下和pH=10.2~12.3的缓冲溶液中,APDNBT与汞生成黄色络合物,其络合比为Hg∶APDNBT=1∶2,建立了以445nm为参比波长,538nm为测量波长的双波长分光光度法,其表观摩尔吸光系数为2.1×10^5L·mol^-1·cm^-1,线性范围是0  相似文献   

4.
本文研究了在pH11.0的硼砂-NaOH缓冲介质中,以Hg(Ⅱ)作催化剂,在乳化剂(OP)和溴化十六烷基三甲基铵(CTMAB)协同作用下,meso-四(对磺基苯)卟啉(TPPS4)测定钇(Ⅲ)的显色反应,其摩尔吸光系数ε417为5.46×10^6L·mol^-1·cm^-1,钇浓度在0 ̄0.030μg/10mL内符合比耳定律,在室温下显色迅速,100倍重稀土不干扰,测定合成稀土混合样品中钇(Ⅲ)含  相似文献   

5.
朱有瑜  刘金华 《分析化学》1994,22(2):133-137
合成了新试剂2-[2-(6-甲基-苯并噻唑)偶氮]-5-二氨基苯磺酸,并研究了其与钯(Ⅱ)的显色反应。实验表明,该试剂与钯(Ⅱ)反在生成1:1蓝色水溶性络合物,在阴离面活性剂十二烷基硫酸钠(SDS)存在下可稳定24h,其最大吸收波长为615nm,表观摩尔吸光系数为7.94×10^4.mol^-^1.cm^-^1。钯量在0-0.8μg/ml范围内符合比尔定律。本法是目前测定钯(Ⅱ)的高灵敏度显色反应  相似文献   

6.
含有吸附络合物溶液的倒数示波计时电位法的应用   总被引:3,自引:0,他引:3  
Pb(Ⅱ)在0.2%乙二胺-5×10^-3mol·L^-1HOx-0.3mol·L^-1KOH溶液中,有良好的全数示波图,其峰电位Ep=-1.05(vs.SCE),峰高与Pb^2+溶度在4.0×10^-7~2.0×10^-5mol·L^-1内成正比,检测下限可达2.0×10^-7mol·L^-1。本实验采用倒数示波计时电位法对铝合金“A”中铅进行了测定,并直接通过示波图,对络合物的吸附属于性进行了  相似文献   

7.
马东兰  张雷 《分析化学》1994,22(6):619-622
本研究了新合成的显色剂N-烯丙基N'-(氨基对苯磺酸钠)硫脲与铜(Ⅱ)发生显色反应的条件实验,结果发现,在pH3.6-5.4的HAc-NaAc体系中,铜和显色剂形成1:3的蓝色水溶性络合物,最大吸收波长为303nm,摩尔吸光系数为1.34×10^5L·mol^-1·cm^-1Cu(Ⅱ)在5-40μg/25ml遵从比尔定律,相关系数r=0.9996,将此方法应用于铝矿样,头发和麦麸中微量铜的测定,  相似文献   

8.
研究了新试剂1-(2-苯并噻唑)-3-(4-偶氮苯基)-三氮烯(BTPAPT)与汞的显色反应,在Tween-80存在下,pH为11.20时,Hg(Ⅱ)与试剂生成红色的1:1配合物,最大吸收峰位于510nm,表现摩尔吸光系数为1.10×10^5L.mol^-1.cm^-1线性范围0-14μg/25mL,建立了可用于饮用水,生活用水和工业废水汞含量测定的方法。  相似文献   

9.
魏永巨  李克安 《分析化学》1994,22(2):183-185
本用双系列线性回归法研究了Pb(Ⅱ),Zn(Ⅱ)与5-Br-PADAP的络合反应,发现在pH5-6.5,30%乙醇溶液中,Pb(Ⅱ)与5-Br-PADAP形成1:1络合物,Zn(Ⅱ)主要形成1:2络合物。两种络合物的稳定常数(1gβ)分别为11.17,22.31,最大吸收波长分别为575,550nm,摩尔吸光系数分别为6.01×10^4,1.34×10^5L.mol^-^1.cm^-^1。  相似文献   

10.
本文研究了新试剂2-(2-(6-甲基苯并噻唑)偶氮)-5-二乙氨基苯甲酸(6-Me-BTAEB)与Fe(Ⅱ)的显色反应,结果表明,在十二烷基硫酸钠存在下新试剂与Fe(Ⅱ)在弱酸性介质中形成稳定的蓝紫色络合物,其组成为Fe(Ⅱ):6-Me-BTAEB=1:2,最大吸收波长为635nm,表观摩尔吸光系数为1.10×10^5L.mol^-1.cm^-1,Fe(Ⅱ)浓度在每25mL0~10μg范围的内服从  相似文献   

11.
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%.  相似文献   

12.
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.  相似文献   

13.
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.  相似文献   

14.
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.  相似文献   

15.
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.  相似文献   

16.
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.  相似文献   

17.
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.  相似文献   

18.
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.  相似文献   

19.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
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.  相似文献   

20.
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.  相似文献   

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