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1.
利用二次通用旋转组合设计的方法,建立了吸光度与显色剂、增敏剂用量以及pH值之间的数学模型,进而得到使吸光度最大的显色剂用量、增敏剂用量及pH值。在此优化的基础上,用目标转换因子分析分光光度法对银、铜、铁、镍的合成样品的合谱进行了解析处理,得到较为满意的结果。  相似文献   

2.
利用二次通用旋转组合设计的方法 ,建立了吸光度与显色剂、增敏剂用量以及p H值之间的数学模型 ,进而得到使吸光度最大的显色剂用量、增敏剂用量及 p H值。在此优化的基础上 ,用目标转换因子分析分光光度法对银、铜、铁、镍的合成样品的合谱进行了解析处理 ,得到较为满意的结果。  相似文献   

3.
利用二次通用旋转组合设计法建立了吸光度与显色剂,增敏剂用量及pH 值之间的数学模型,进而得出使吸光度最大的显色剂用量,增敏剂用量及PH值,在优化的基础上,用B-P人工地Pb,Cd,Hg,Ni同时测定的数据进行解析,并与经典最小二乘法进行了对比,结果较准确。  相似文献   

4.
卟啉胶束增敏导数分光光度法测定微量锰   总被引:1,自引:0,他引:1  
卟啉的分子截面积大,与一些金属离子配合都具有很高的摩尔吸光值,已被称之为“超高灵敏度的显色剂”。文献研究了在阳离子表面活性剂存在下,锰与阴离子卟啉的增敏反应,本文在阴离子表面活性剂存在下,采用导数光度法,探讨的锰与阳离子卟啉的增敏作用。试验表明,试液中无论是单体还是胶束对锰与阳离子卟啉生成的Mn-T(4-TAP)P二元配合物均有增敏作用,最大吸收波长紫移。  相似文献   

5.
利用洗洁精为增敏、增溶剂试,以金试剂为显色剂,拟定了吸光光度法测定了人发中微量铜的方法,方法简便快速,准确度高,人发中常见离子不干扰铜的测定。  相似文献   

6.
漂蓝6B(ECAB)是一种有实用价值的显色剂。十二烷基硫酸钠(SDS)对吡啶偶氮衍生物与某些金属离子体系有强烈的增敏作用,但阴离子表面活性剂对三苯甲烷酸性染料与金属离子的络合物体系的增敏作用尚未见报导。本文研究了SDS对三苯甲烷类酸性染料之一——ECAB与铍络合物体系的增溶增敏作用。结果表明,在SDS存在下,在pH6.3左右,Be(Ⅱ)-ECAB体系的最大吸收波长为616nm,试剂空白在此波长下吸光度很低,表观摩尔吸光系数为1.11×10~5,比相应的二元络合物灵敏度提高4倍多,亦比采用阳离子表面活性剂作增敏剂时灵敏度高。该体系具有显色速度快,络合物稳定性好,不沾污吸收池和容量瓶,实验操作简便等优点。加入掩蔽剂后,已被用于直接测定矿石中微量铍及铜铍合金试样中含铍量,获得了满意的结果。  相似文献   

7.
丁亚平  吴庆生 《分析化学》1998,26(3):294-297
用meso-四-(对-三甲铵苯基)卟啉作显色剂,以四阶导数光谱技术进行测定,提出了测量痕量铜的新方法。在pH4.4的HAc-NaAc介质中,在盐酸羟胺催化和乙醇增稳增敏作用下,于沸水浴中加热1min,显色反应即呆完成。其四阶导数光谱表观摩尔吸光系数ε'达1.00×10^7L·mol^-1·cm^-1,最低检出限为0.062μg/L,分别是常规光度法的21.2和12.3倍。同时,绝大多数离子不干扰测  相似文献   

8.
TMK是推荐为测定金的显色剂,具有较高的灵敏度,但选择性尚不能令人满意。本实验用TMK为测金的显色剂,非离子表面活性剂Triton X-100为增溶、增敏剂,在水溶液中研究用导数分光光度法消除其它贵金属宽带背景吸收的干扰条件。所制定的方法,不需分离可直接测定电解铜阳极泥及合金中的微量金。选择性很好,而且精密度和准确度均得到满意的结果。  相似文献   

9.
本文报道以偶氮氯膦Ⅲ为显色剂,利用流动注射pH梯度技术测定多个不同pH下的吸光度,借助卡尔曼滤波算法进行数据处理,对不同比例的钡锶(Ba:Sr=1:8~8:1)标准混合样品进行了测定,取得了满意的结果。  相似文献   

10.
CTMAB—TritonX—100存在下BPR光度法测定铝   总被引:1,自引:0,他引:1  
痕量铝的分析测定主要用光度法 ,而此法稳定性差 ,检测浓度范围窄 ,发色反应受温度、pH值、介质等条件影响较大 ,铝的光度测定是一大难题之一[1] 。目前 ,在铝的光度测定中引入新显色剂及加入表面活性剂形成多元络合物已日渐增多 ,许多资料表明混合表面活性剂能起到增溶、增稳等作用[2 ] 。关于Al BPR CTMAB用于水和工业废水、土壤、炉渣中铝的测定已见报道[3] 。本文在Al BPR CTMAB体系中引入TritonX 10 0 ,试验表明 ,加入TritonX 10 0能使显色剂、CTMAB用量范围增大 ,pH值范围也比单用CTM…  相似文献   

11.
The representative of P,P,P-trichloroylides-5-methyl-2-phenyl-4-(trichlorophosphoranylidene)-2,4-dihydro-3H-pyrazol-3-one-was synthesized. Its constitution was confirmed by 1H, 13C, and 31P NMR spectroscopy and by X-ray analysis. Some chemical properties were studied and compared with ones of P,P,P-trimethylylide-5-methyl-2-phenyl-4-(trimethylphosphoranylidene)-2,4-dihydro-3H-pyrazol-3-one. DFT calculations of the model molecules were carried out.  相似文献   

12.
Microwave spectra have been recorded for 1-phenyl-2-propanol, methamphetamine, and 1-phenyl-2-propanone from 11 to 24 GHz using a Fourier-transform microwave spectrometer. Only one spectrum from a single conformational isomer was observed for each species. The rotational transitions in the spectrum of 1-phenyl-2-propanone were split into separate transitions arising from the A- and E-torsional levels of the methyl rotor. The fit of the E-state transitions to a "high-barrier" internal rotation Hamiltonian determines V3 = 238(1) cm-1 and rotor-axis angles of thetaa = 87.7(5) degrees, thetab = 50.0(5) degrees, and thetac = 40.0(5) degrees. Ab initio optimizations (MP2/6-31G**) and single-point calculations (MP2/6-311++G**) were used to model the structures of 1-phenyl-2-propanol, methamphetamine, and 1-phenyl-2-propanone. The lowest energy conformations of these species were found to be stabilized by weak OH-pi, NH-pi, and CH-pi hydrogen-bonding interactions. Moments of inertia, derived from the model structures, were used to assign the spectra to the lowest energy conformation of each species. A series of MP2/6-31G* partial optimizations along the internal rotation pathway were used to estimate the barrier to methyl rotation to be 355 cm-1 for 1-phenyl-2-propanone.  相似文献   

13.
The reaction of the 1,2,3,5-dithiadiazolyls (4-R-C(6)H(4)CN(2)S(2))(2) (R = Me, 2a; Cl, 2b; OMe, 2c; and CF3, 2d) and (3-NC-5-tBu-C(6)H(3)CN(2)S(2))(2) (2e) with [CpCr(CO)(3)](2) (Cp = eta(5)-C(5)H(5)) (1) at ambient temperature respectively yielded the complexes CpCr(CO)(2)(eta(2)-S(2)N(2)CC(6)H(4)R) (R = 4-Me, 3a; 4-Cl, 3b; 4-OMe, 3c; and 4-CF(3), 3d) and CpCr(CO)(2)(eta(2)-S(2)N(2)CC(6)H(3)-3-(CN)-5-(tBu)) (3e) in 35-72% yields. The complexes 3c and 3d were also synthesized via a salt metathesis method from the reaction of NaCpCr(CO)(3) (1B) and the 1,2,3,5-dithiadiazolium chlorides 4-R-C(60H(4)CN(2)S(2)Cl (R = OMe, 8c; CF(3), 8d) with much lower yields of 6 and 20%, respectively. The complexes were characterized spectroscopically and also by single-crystal X-ray diffraction analysis. Cyclic voltammetry experiments were conducted on 3a-e, EPR spectra were obtained of one-electron-reduced forms of 3a-e, and variable temperature 1H NMR studies were carried out on complex 3d. Hybrid DFT calculations were performed on the model system [CpCr(CO)(2)S(2)N(2)CH] and comparisons are made with the reported CpCr(CO)(2)(pi-allyl) complexes.  相似文献   

14.
A simple and efficient one-pot three-component azide-alkyne cycloaddition of 5-chloro-1-phenyl-pyrazole-4-carbaldehyde with 2-(prop-2-yn-1-ylthio)-5-(substituted phenoxy)methyl-1,3,4-oxadiazole and sodium azide is reported. The newly synthesized compounds were characterized by spectral and analytical data. They were screened for in vitro anti-inflammatory activity by bovine serum albumin denaturation assay. All the tested compounds showed moderate anti-inflammatory activity, whereas three compounds ( 4d , 4i , and 4k ) showed excellent activity comparable with that of the standard drug diclofenac sodium. The quantitative structure-activity relationship (QSAR) study was carried out for anti-inflammatory activities of the synthesized compounds and developed a QSAR model. Inspired by their in vitro anti-inflammatory activities, they were docked to the active site of COX-2 to know the anti-inflammatory potency in silico.  相似文献   

15.
The cyano-substituted metallocenes [M(C5H4CN)2] (M=Fe, 1; Co, 2; Ni 3) and [M(C5Me5)(C5H4CN)] (M=Fe, 4; Co, 5; Ni, 6) were synthesized in yields up to 58 % by treating K(C5H4CN) or Tl(C5H4CN) with suitable transition-metal precursors. Cyclic voltammetry indicated that the oxidation and reduction potentials of all the cyanometallocenes were shifted to positive values by up to 0.8 V. Single-crystal X-ray structure analysis showed that 1 had eclipsed ligands, formed planes in the lattice, and--unlike usual metallocenes--lined up in stacks perpendicular to these planes. Powder X-ray studies established that 1 and 2 are isotypic. The 1H and 13C NMR spectra were recorded for all the new compounds. Signal shifts of up to delta=1500 ppm were recorded for the paramagnetic molecules 2 and 3 and were, at a given temperature, strikingly different for solution and solid-state spectra. These results pointed to antiferromagnetic interactions as a consequence of molecular ordering in the lattice, as confirmed by magnetic measurements. The temperature-dependent susceptibilities were reproduced by Heisenberg spin-chain models (H=-J sum n- 1 i=1 SiSi+1), thus yielding J=-28.3 and -10.3 cm(-1) for 2 and 3, respectively, whereas J=-11.8 cm(-1) was obtained for 3 from the Ising spin-chain model. In accordance with molecular orbital (MO) considerations, much spin density was found to be delocalized not only on the cyclopentadienyl ligand but also the cyano substituents. The magnetic interaction was interpreted as a Heitler-London spin exchange and was analyzed based on how the interaction depends on the singly occupied MOs and the shift of parallel metallocenes relative to each other.  相似文献   

16.
The reaction of N-cyano-N′-(6-amino-2-pyridyl)acetamidine ( 5a ) and homophthalic anhydride followed by ring closure of the 2-[2-(carboxymethyl)phenyl]-5-methyl-1,3,4,6,9b-pentaazaphenalene intermediate ( 4a ) gave 5-methyl-13-oxo-13H-4,6,7,13a,13c-pentaazabenzo[hi]chrysene ( 8a ). An analogous series starting with 3-N-(6-amino-2-pyridyl)amino-2-cyano-2-butenenitrile ( 5b ) in place of 5a gave in two steps 5-methyl-13-oxo-13-H-4,7,13a,13c-tetraazabenzo[hi]chrysene-6-carbonitrile ( 8b ). Elemental analysis, ir and pmr spectra of 8a , 8b and several new model compounds aided in confirming the structures of 8a and 8b. The synthesis of one of these model compounds for 5b and phenylacetic anhydride led surprisingly to 2-methyl-9-phenyl-7H-3,7,-10,10b-tetraazacyclohepta[de]naphthalene ( 10 ) in addition to the expected 2-benzyl-4-cyano-5-methyl-1,3,-6,9b-tetraazaphenalene ( 7b ).  相似文献   

17.
Representative members of a new family of covalently bonded charge-transfer molecular hybrids, of general formula [(eta5-C5H5)Fe(mu,eta6:eta1-p-RC6H4NN)Mo(eta2-S2CNEt2)3] +PF6- (R: H, 5+PF6-; Me, 6+PF6-; MeO, 7+PF6-) and [(eta5-C5Me5)Fe(mu,eta6:eta1-C6H5NN)Mo(eta2-S2CNEt2)3]+PF6-, 8+PF6-, have been synthesized by reaction of the corresponding mixed-sandwich organometallic hydrazines [(eta5-C5H5)Fe(eta6-p-RC6H4NHNH2)]+PF6- (R: H, 1+PF6-; Me, 2+PF6-; MeO, 3+PF6-) and [(eta5-C5Me5)Fe(eta6-C6H5NHNH2)]+PF6-, 4+PF6-, with cis-dioxomolybdenum(VI) bis(diethyldithiocarbamato) complex, [MoO2(S2CNEt2)2], in the presence of sodium diethyldithiocarbamato trihydrate, NaSC(=S)NEt2.3H2O, in refluxing methanol. These iron-molybdenum complexes consist of organometallic and inorganic fragments linked each other through a pi-conjugated aryldiazenido bridge coordinated in eta6 and eta1 modes, respectively. These complexes were fully characterized by FT-IR, UV-visible, and 1H NMR spectroscopies and, in the case of complex 7+PF6-, by single-crystal X-ray diffraction analysis. Likewise, the electrochemical and solvatochromic properties were studied by cyclic voltammetry and UV-visible spectroscopy, respectively. The electronic spectra of these hybrids show an absorption band in the 462-489 and 447-470 nm regions in CH2Cl2 and DMSO, respectively, indicating the existence of a charge-transfer transition from the inorganic donor to the organometallic acceptor fragments through the aryldiazenido spacer. A rationalization of the properties of 5+PF6--8+PF6- is provided through DFT calculations on a simplified model of 7+PF6-. Besides the heterodinuclear complexes 5+PF6--8+PF6-, the mononuclear molybdenum diazenido derivatives, [(eta1-p-RC6H4NN)Mo(eta2-S2CNEt2)3] (R: H, 9; Me, 10; MeO, 11), resulting from the decoordination of the [(eta5-C5H5)Fe]+ moiety of complexes 5+PF6--7+PF6-, were also isolated. For comparative studies, the crystalline and molecular structure of complex 10.Et2O was also determined by X-ray diffraction analysis and its electronic structure computed.  相似文献   

18.
In this study, a series of coumarin derivatives were designed and synthesized, their structures were characterized using nuclear magnetic resonance (NMR) and high-resolution mass spectrometry (HRMS) testing methods. In the pharmacological experiment, two behavior-monitoring methods, the forced swim test (FST) and the tail suspension test (TST), were used to determine the antidepressant activity of coumarin derivatives. Compounds that showed potential activity were analyzed for their effects on 5-hydroxytryptamine (5-HT) levels in the brains of mice. Molecular docking experiments to simulate the possible interaction of these compounds with the 5-HT1A receptor was also be predicted. The results of the pharmacological experiments showed that most coumarin derivatives exhibited significant antidepressant activity. Among these compounds, 7-(2-(4-(4-fluorobenzyl)piperazin-1-yl)-2-oxoethoxy)-2H-chromen-2-one (6i) showed the highest antidepressant activity. The results of the measurement of 5-HT levels in the brains of mice indicate that the antidepressant activity of coumarin derivatives may be mediated by elevated 5-HT levels. The results of molecular docking demonstrated that compound 6i had a significant interaction with amino acids around the active site of the 5-HT1A receptor in the homology model. The physicochemical and pharmacokinetic properties of the target compounds were also predicted using Discovery Studio (DS) 2020 and Chemdraw 14.0.  相似文献   

19.
A series of 5-substitued-3-(5-(4-(furan-2-yl)-6-methyl-2-oxo/thioxo-1,2,3,4-tetrahydropyrimidin-5-yl)-1,3,4-thiadiazol-2- ylimino)indolin-2-one derivatives were synthesized,characterized and were screened for anti-bacterial,anti-fungal and antitubercular activity.  相似文献   

20.
The study of the H+ concentration at the micellar interface is a convenient system for modeling the distribution of H+ at interfaces. We have synthesized salicylic acid derivatives to analyze the proton dissociation of both the carboxylic and phenol groups of the probes, determining spectrophotometrically the apparent pK(a)'s (pK(ap)) in sodium dodecyl sulfate, SDS, micelles with and without added salt. The synthesized probes were 2-hydroxy-5-(2-trimethylammoniumacetyl)benzoate; 2-hydroxy-5-(2-dimethylhexadecylammoniumacetyl)benzoate; 2-hydroxy-5-(2-dimethylhexadecylammoniumhexanoyl)benzoate; 2-hydroxy-5-(2-dimethylhexadecylammoniumundecanoyl)benzoate; 2-hydroxy-5-acetylbenzoic acid; and 2-hydroxy-5-dodecanoylbenzoic acid. Upon incorporation into SDS micelles the pK(ap)'s of both carboxylic and phenol groups increased by ca. 3 pH units and NaCl addition caused a decrease in the probe-incorporated pK(ap). The experimental results were fitted with a cell model Poisson-Boltzmann (P-B) equation taking in consideration the effect of salt on the aggregation number of SDS and using the distance of the dissociating group as a parameter. The conformations of the probes were analyzed theoretically using two dielectric constants, e.g., 2 and 78. Both the P-B analysis and conformation calculations can be interpreted by assuming that the acid groups dissociate very close to, or at, the interface. Our results are consistent with the assumption that the intrinsic pK(a)'s of both carboxylic and phenol groups of the salicylic acid probes used here can be taken as those in water. Using this assumption the micellar and salt effects on the pK(ap)'s of the (trialkylammonium)benzoate probes were described accurately using a cell model P-B analysis.  相似文献   

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