共查询到20条相似文献,搜索用时 62 毫秒
1.
报道了新息夫碱试剂水杨醛缩-5-碘-5-氨基喹啉(SAIAQ)的合成。用元素分析、红外光谱法确定了其结构。测定了SAIAQ的酸度常数Ka1=2.40×10^-4,Ka2=2.98×10^-9。在pH3.50 ̄5.00范围内SAIAQ与Ga^3+形成稳定的荧光螯合物,且在λex/λem=428nm/540nm产生强烈荧光。其荧光强度与Ga^3+的浓度在1.5μg/L ̄260μg/L范围内呈线性关系, 相似文献
2.
氨基萘磺酸盐无保护流体室温磷光的取代基位置效应 总被引:1,自引:0,他引:1
以TINO3作重原子微扰剂,Na2SO3作化学除氧剂,在无需加入任何保护介质条件下,仅需仪器光源适当照射,1-氨基4-萘磺酸盐、1-氨基5-萘磺酸盐、2-氨基1-萘磺酸盐水溶液均能产生强而稳定的室温磷光信号(RTP)。3种氨基萘磺酸盐浓度分别在4.0×10^-8 ̄1.2×10^-5mol/L;1.2×10^-6 ̄1.6×10^-5mol/L;1.6×10^-7 ̄8.0×10^-6和8.0×10^- 相似文献
3.
水杨醛缩-5-碘-8-氨基喹啉的合成及荧光光度法测定煤渣中痕量镓的研究 总被引:2,自引:0,他引:2
报道了新息夫碱试剂水杨醛缩-5-碘-8-氨基喹啉(SAIAQ)的合成。用元素分析、红外光谱法确定了其结构。测定了SAIAQ的酸度常数Ka1=2.40×10-4,Ka2=2.98×10-9。在pH3.50~5.00范围内SAIAQ与Ga3+形成稳定的荧光螯合物,且在λex/λem=428nm/540nm产生强烈荧光。其荧光强度与Ga3+的浓度在1.5μg/L~260μg/L范围内呈线性关系,检出限1.5μg/L,考察了共存离子的影响,选择性高。已应用于煤渣中痕量镓的分析。 相似文献
4.
本文利用鲁米诺-KIO4-Fe(1,10—phen)32+配合物体系产生化学发光反应,建立了测定痕量铁的新的化学发光分析方法。该法以1,10-phen为配位体,铁的检出限为1.6×10-7g/L,工作曲线响应浓度范围在1×10-5-1×10-3g/L。在测定2×10-4g/L铁的相对标准偏差为3.5%。用于检测工业沉淀BaSO4中痕量铁获得满意结果。 相似文献
5.
含α-溴代萘(a-BrNp)的水溶液仅以Na2SO3作化学除氧剂,在仪器光源的照射下,即能很快触发α-BrNp强而稳定的室温光(RTP)信号。体系RTP性质和所需光诱导的时间对有机试剂的存在及其种类和用量极为敏感。0.5%(V/V)乙腈或丙酮的存在所需光照时间短,RTP强度高。α-BrNp浓度分别在 1.0 × 10-6~ 2. 4 × 10-5 mol/L和 4. 0 × 10-7~ 2. 0 × 10-5mol/L范围内与 RTP强度呈良好线性关系,检出限分别为 3,8 × 10-8 mol/L和 6.5 × 10-8 mol/L。 相似文献
6.
本文研究了应用Ga(没食子酸)-H2O2-OH^-化学发光体系,流动注射技术测定乙醛的条件,如反应介质及其pH值,Ga及H2O2溶液的浓度,温度,试液混合次序与化学发光强度的关系等,选择了流动注射系统的若干参数,所拟定的方法测定乙醛的浓度范围为每mL1.7×10^-3~4.4×10^-7g,相对标准偏差为1.8%(2×10^-5g/mL,乙醛溶液进行11次平行测定)检出限为每mL3.1×10^-8 相似文献
7.
5,10,15,20-四(3-溴-4-磺酸苯基)卟啉光度法测定痕量锌的研究 总被引:1,自引:0,他引:1
本文研究了新水溶性卟啉试剂5,10,15,20-四(3-溴-4-磺酸苯基)卟啉[T(3-BrP)PS4]与锌的显色反应。在pH4,锌与5,10,15,20-四(3-溴-4-磺酸苯基)卟啉形成稳定的1:1配合物,其最大吸收波长位于422.0nm,摩尔吸光系数为3.9×105L·mol(-1)·cm(-1)。锌量在0~2.5μg/25mL范围符合比尔定律。方法具有较高的灵敏度和较好的选择性,用于人发和大米中痕量锌的测定,结果与原子吸收法一致。 相似文献
8.
安力农的极谱测定及其电化学行为 总被引:4,自引:0,他引:4
在pH5.6,0.15mol/L磷酸盐缓冲溶液(PBS)中,得到了安力农的灵敏极谱吸附波,波的二阶导波高在2×10^-8~8×10^-6mol/L范围内与安力农的浓度成直线关系,检测下限为1×10^-8mol/L,测定出电极过程的电子传递系数a=0.43,表面电极反尖速率常数ks=3.3s^-1,安力农在汞电极上的吸附遵从Langmuir等温式,测得其吸附系数β=8.1×10^5。 相似文献
9.
10.
吲哚乙酸与磷钼黄反应及其极谱分析的研究 总被引:1,自引:0,他引:1
在NH3-NH4Cl缓冲溶液中(pH=9.5),吲哚乙酸与磷钼黄的还原产物在滴汞电极上于-1.10V(vs.SCE)处产生一灵敏的极谱波,该波波高与吲哚乙酸的浓度在1.0×10-7-5.0×10-6mol/L范围内成线性关系,检测下限为5.0×10-8mol/L。如在上述还原产物中加入偶氮胭脂红B、孔雀绿、甲基紫等染料及聚乙烯醇,可使极谱波的灵敏度提高,使吲哚乙酸的浓度在5.0×10-8-1.0×10-6mol/L范围内与波高成线性关系,检测下限降低至1.0×10-8mol/L。 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.
Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
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
13.
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
14.
Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
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
15.
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
16.
N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
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
17.
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
18.
19.
《Tetrahedron》2014,70(21):3377-3384
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. 相似文献
20.
袁都奇 《化学物理学报(中文版)》2001,14(3):381-384
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. 相似文献