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1.
用 Amberlyst A-26大孔阴离子交换树脂分离金(Ⅲ)、铂(Ⅳ)和钯(Ⅱ).在 HAc-NaAc缓冲液中,用易溶于水的显色剂N-烯丙基-N′-(对氨基苯磺酸钠)硫脲(ASATu)和N-间甲苯基-N′-(对氨基苯磺酸钠)硫脲(MMPT)测定.前者测定金(Ⅲ),后者同时测定铂(Ⅳ)和钯(Ⅱ).该法用于催化剂和阳极泥...  相似文献   

2.
N-烯丙基-N′-(对苯磺酸钠)硫脲与铋的显色反应及其应用   总被引:5,自引:0,他引:5  
N-烯丙基-N′-(对苯磺酸钠)硫脲(NaNTu)是一种新的硫脲类衍生物[1],它合成简便,原料易得,性质稳定,无毒,易溶于水;在一定条件下,能与少数金属离子生成非常稳定的配合物,某些配合物还具有特征的颜色,因此具有很好的分析特性.  相似文献   

3.
介绍了N-辛基-N′-(氨基对苯磺酸钠)硫脲(OPT) 的合成方法。通过红外、紫外和元素分析等方法测试,确定了其组成和结构。并研究了该试剂与钯(Ⅱ)的显色反应,从而建立了光度法测定微量钯的新方法。在 pH4.0~5.5 的 HAc-NaAc 缓冲体系中,Pd  相似文献   

4.
N-烃基-N'-(氨基本对苯磺酸钠)硫脲作为一种稳定的光度试剂,已用于铜、钯、铂、银等元素的分析[1-5].N-甲基-N'-(氨基对苯磺酸钠)硫脲(MPT)[6]用于测定微量铂(Ⅳ),结果表明,在pH5.2~6.4的HAc-NaAc缓冲溶液中,Pt(Ⅳ)与MPT形成一种稳定的1∶3的绿色水溶性配合物,其λmax为682.0nm,表观摩尔吸光系数ε682.0=5.46×104L·mol-1·cm-1,铂(Ⅳ)含量在0~3.7mg·L-1范围内符合比尔定律,相关系数r=0.9988,方法简便、快速、选择性好,测定范围宽,用于矿石及催化剂中铂的分析,结果满意.  相似文献   

5.
新试剂HABST分光光度法测定铜   总被引:4,自引:1,他引:3  
硫脲类试剂因含有S ,N配位原子而可与无机离子形成配合物 ,近年来已被用于定性分析和定量测定。对氨基苯磺酸钠类硫脲因其良好的水溶性而避免了以往测铜试剂需有机相中进行的繁琐处理。N 庚基 N′ (对氨基苯磺酸钠 )硫脲(HABST) [1 ] 是继N 烯丙基 N′ (对氨基苯磺酸钠 )硫脲 (ASATU) [2 ] 后又合成的一种水溶性光度试剂 ,通过初步研究 ,发现它与Ag+、Cu2 +有特征性反应。在此基础上 ,对其与铜的显色反应作进一步研究 ,探讨了HABST分光光度法测定铜的最佳条件 ,在pH4.5~ 6.0的HAc NaAc缓冲溶液中 ,C…  相似文献   

6.
介绍了一种用新合成的显色剂N-烯丙基-N′-(氨基对苯磺酸钠)硫脲(ASAT)光度法测定微量金(Ⅲ)的方法。在pH35~55的HAc-NaAc缓冲体系中,该试剂和金(Ⅲ)形成一种稳定的水溶性配合物,其组成为n(Au3+)∶n(ASAT)=1∶2,配合物的最大吸收峰位于2986nm处,表观摩尔吸光系数为114×105L·mol-1·cm-1。Au3+量在72~568μg/L服从比尔定律,相关系数r=09993。将该法应用于金矿石中微量金的测定,获得满意的结果。  相似文献   

7.
介绍了新试剂N-对甲苯基-N’-(氨基对苯磺酸钠)硫脲(PMPT)和N-辛基-N‘-(氨基对苯磺酸钠)硫脲(OPT)的合成。经过红外、紫外、核磁和元素分析等方法测试,确定了其组成和结构。并分别研究了新试剂与Cu(Ⅱ)的显色反应,建立了测定微量铜的新方法,方法具有灵敏度高,操作简便,显色速度快等特点。试验了四十余种常见离子对显色反应的干扰情况,表明方法具有较好的选择性。并将方法不经分离直接用于合金标  相似文献   

8.
张雷  黄运瑞 《分析化学》1999,27(12):1449-1453
详细介绍了新试剂N-对甲苯基-N’-(氨基对苯磺酸钠)硫脲(PMPT)的合成。经过红外光谱、紫外光谱、核磁共振和元素分析等方法测试,确定了试剂的组成和结构。研究了试剂与铂(Ⅳ)的显色反应,建立了光度法测定微量铂(Ⅳ)的方法。在pH3.6~5.2的HAc-NaAc缓冲体系中,该试剂和铂(Ⅳ)-形成一种稳定的组成比为1:3的绿色水溶性络合物,其最大吸收峰位于756nm处,表观摩尔光系数为ε756=1.  相似文献   

9.
将邻苯甲酰磺酰亚胺、1,3,4-噁二唑2个杂环同时引入到酰基硫脲中,合成了12种新的N-′(5-芳基-1,3,4-噁二唑-2-基)-N-(邻苯磺酰甲酰亚胺乙酰基)硫脲化合物,化合物的结构均经元素分析、1H NMR和IR等测试技术得以确证。抑菌法生物活性测试结果表明,大部分化合物对黄瓜灰霉病菌、油菜菌核病菌抑制效果很好,特别是化合物5b和5l对5种病菌抑制率均在87%以上,有的病菌抑制率达到100%。  相似文献   

10.
功能化离子液体中两步高效合成N-取代硫脲   总被引:1,自引:0,他引:1  
赵华绒  王海燕  陆丰平 《化学学报》2011,69(19):2293-2298
两步高效合成N-取代硫脲:(1)在[emim]SCN中以酰与伯胺为起始原料先合成得到N-烃基-N'-酰基硫脲,反应速度快,产率高,功能化离子液体既作为第一步反应原料,又作为反应介质;(2)N-烃基-N′-酰基硫脲在NaOH/H2O/EtOH体系中以近100%的转化率水解得目标产物.提供了一种高效合成N-取代硫脲的绿色、...  相似文献   

11.
Two new hydrazinium lanthanide(III) oxalates, (N2H5)[Nd(C2O4)2(H2O)]·4H2O (1) and (N2H5)[Gd(C2O4)2(H2O)]·4.5H2O (2) have been prepared and their crystal structures determined by single-crystal X-ray diffraction. The crystal structures were solved by the direct methods and Fourier difference techniques, and refined by a least-squares method on the basis of F2 for all unique reflections. Crystallographic data: 1, triclinic, space group , , b=9.762(4), , α=62.378(5), β=76.681(5), γ=73.858(5), Z=2, R1=0.0335 for 172 parameters with 3430 reflections with I?2σ(I); 2, triclinic, space group , , b=9.51(3), , α=62.11(4), β=76.15(5), γ=73.73(5), Z=2, R1=0.0325 for 172 parameters with 1742 reflections with I?2σ(I). The two isotypic structures are built from a three-dimensional (3D) arrangement of lanthanide and oxalate ions. The lanthanide atom is coordinated by eight oxygen atoms from four tetradentate oxalate ions and one aqua oxygen. Alternating lanthanide and oxalate ions form six-membered rings that delimit tunnels running down three directions and occupied by hydrazinium and water molecules. Starting from these lanthanide(III) compounds two isotypic mixed Ln(III)/U(IV) oxalates, (N2H5)0.75[Nd0.75U0.25(C2O4)2(H2O)]·4.5H2O (3) and (N2H5)0.75[Gd0.75U0.25(C2O4)2(H2O)]·4H2O (4), are obtained by partial substitution of Ln(III) by U(IV) in the nine-coordinated site, the charge excess being compensated by removal of monovalent ions from the tunnels. Finally, using Na+ gel, two mixed Ln(III)/U(IV) sodium oxalates, Na0.5[Nd0.5U0.5(C2O4)2(H2O)]·3H2O (5) and Na0.65[Gd0.65U0.35(C2O4)2(H2O)]·4.5H2O (6) have been obtained without any change in the 3D framework.  相似文献   

12.
A new ammonium uranium (IV) oxalate (NH4)2U2(C2O4)5·0.7H2O (1) and three mixed uranium (IV)-lanthanide (III) oxalates, (N2H5)2.6U1.4M0.6(C2O4)5·xH2O (M=Nd (2) and M=Sm (3)), Na2.56U1.44Nd0.56(C2O4)5·7.6H2O (4) and Na3UCe(C2O4)5·10.4H2O (5), have been prepared. The crystal structures of compounds 1, 4 and 5 have been determined by single-crystal X-ray diffraction. The crystal structures were solved by the direct methods and Fourier difference techniques, and refined by a least square method on the basis of F2 for all unique reflections. Compounds 2 and 3 are isotypic with 1. Crystallographic data: 1, hexagonal, space group P63/mmc, a=19.177(3), c=12.728(4) Å, Z=6, R1=0.0575 for 52 parameters with 1360 reflections with I?2σ(I); 2, hexagonal, space group P63/mmc, a=19.243(4), c=12.760(5) Å, Z=6; 3, hexagonal, space group P63/mmc, a=19.211(3), c=12.274(4) Å, Z=6; 4, orthorhombic, space group Pbcn, a=18.79(3), b=11.46(1), c=12.77(2) Å, Z=4, R1=0.0511 for 183 parameters with 3026 reflections with I?2σ(I); 5, monoclinic, space group C2/c, a=18.878(6), b=11.684(4), c=12.932(4) Å, β=95.97(1)°, Z=4, R1=0.0416 for 213 parameters with 4060 reflections with I?2σ(I). The honeycomb-like structure of the five compounds is built from the same three-dimensional arrangement of metallic and oxalate ions. Similar hexagonal rings of alternating metallic and oxalate ions form layers parallel to the (001) plane that are pillared by another oxalate ion. Indeed, some torsions or rotations of the bridging oxalate ligands led to modifications of the network symmetry. The monovalent cations and the water molecules occupy the hexagonal tunnels running down the [001] direction. Starting from the uranium (IV) compound A2U2(C2O4)5·0.7H2O with A=NH4+ (1), the mixed U(IV)/Ln(III) oxalates are obtained by partial substitution of U(IV) by Ln(III) in a ten-coordinated site, the charge deficit being compensated by intercalation of supplementary monovalent ions within the tunnels. The distortion of the arrangement in the [001] direction for the Na-containing compounds allows the accommodation of a greater number of water molecules that insure an octahedral coordination of the Na atoms.  相似文献   

13.
手性二噁唑啉吡啶铁和镍配合物的制备与表征   总被引:1,自引:0,他引:1  
Tridentate bis(oxazolinylpyridine)(1) reacted with nickel chloride or ferrous chloride in anhydrous ethanol to form bis(oxazolinylpyridine) Nickel(Ⅱ) and Iron(Ⅱ) complexes. The stable solid complexes were characterized with IR, UV, MS, XPS and elemental analysis. No stable complexes were formed with bidentate bis(oxazoline)(2) ins- tead of bis(oxazolinylpyridine).  相似文献   

14.
通过原子转移自由基聚合(ATRP)合成了一种带有活性—NH2基团的温度敏感性亲水型共聚物P(NiPAAm-co-DMAA), 并将其作为引发剂, 合成了P(NiPAAm-co-DMAA)-co-P(L-Ala), 其分子量分布(PDI)在1.3左右. 聚合物通过自组装形成纳米胶束. 透射电镜(TEM)结果表明, 胶束大小200~300 nm, 具有明显的核壳结构. 共聚物的最低临界溶解温度(LCST)为45.5 ℃. 温度低于LCST时, 聚合物溶解形成胶束; 高于LCST时, 胶束解离, 聚合物不溶. 聚合物对温度的响应是快速而可逆的.  相似文献   

15.
Abstract

The synthesis of (E)- and (Z)-1.2-bis(p-fluorophenylsulphenyl)stilbenes (2a and 2b) and 1,2-bis(p-fluorophenylsulphonyl)stilbenes (3a and 3b) was carried out and their configurations were consistent with their stereospecific synthesis. The isomeric 1,1-bis(p-fluorophenylsulphenyl)- and 1,1-bis(p-fluorophenylsulphonyl)-2,2-bis(phenyl)ethylenes (8 and 9) were also synthesised and configurations were established by degradative oxidation. Mass spectral rearrangements of all these compounds were examined. Mass spectra of 1,1-bis-sulphide and 1,1-bis-sulphone bears close relationship with those of (E)- and (Z)-isomeric counterparts. Smiles-type rearrangement observed in 1,2-bis-sulphides was absent in 1,2-bis-sulphones. McLafferty-type rearrangement involving hydrogen migration, from aryl group was noticed in both bis-sulphides and bis-sulphones. Vinyl migration to the sulphone oxygen predominates over aryl migration in three isomeric bis-sulphones.  相似文献   

16.
界面缩聚法合成双(烯基环戊二烯基)钛(锆)聚醚的研究   总被引:1,自引:0,他引:1  
本文通过界面缩聚法利用双(烯基环戊二烯基)钛(锆)二氯化物与二酚反应,制成了16个新的高分子化合物,对它们进行了IR、TGA和分子量的测定。文中还对反应条件与分子量的关系进行了讨论。  相似文献   

17.
Reaction of phosphorus trichloride with tert-butanol and fluoroalcohols gave bis(fluoroalkyl) phosphites (RFO)2P(O)H in 42-89% yield, where RF=HCF2CH2, H(CF2)2CH2, H(CF2)4CH2, CF3CH2, C2F5CH2, C3F7CH2, (CF3)2CH, (FCH2)2CH, CF3(CH3)2C, (CF3)2CH3C, CF3CH2CH2, C4F9CH2CH2 and C6F13CH2CH2. Treatment of these with chlorine in dichloromethane gave the bis(fluoroalkyl) phosphorochloridates (RFO)2P(O)Cl in 49-96% yield. The chloridate (CF3CH2O)2P(O)Cl was isolated in much lower yield from the interaction of thionyl chloride with bis(trifluoroethyl) phosphite. Heating the latter in dichloromethane with potassium fluoride and a catalytic amount of trifluoroacetic acid gave the corresponding fluoridate (CF3CH2O)2P(O)F in 84% yield. Treatment of bis(trifluoroethyl) phosphite with bromine or iodine gave the bromidate (CF3CH2O)2P(O)Br and iodidate (CF3CH2O)2P(O)I in 51 and 46% yield, respectively. The iodidate is the first dialkyl phosphoroiodidate to have been isolated and characterised properly—its discovery lags behind the first isolation of a dialkyl phosphorochloridate by over 130 years. The fluoroalkyl phosphoryl compounds are generally more stable than known unfluorinated counterparts.  相似文献   

18.
A simple and effective procedure for the enantioselective synthesis of (R)-and (S)-moprolol was described.The key step was the asymmetric synthesis of enantiopure (R)-and (S)-guaifenesin,which were synthesized from enantioenriched (R)-3-chloro-1,2-propanediol and (S)-epichlorohydrin via kinetics of hydrolysis resolution of racemic epichlorohydrin by chiral Salen-CoIIII complex.The e.e.values of both the optical compounds were above 98%,and the chemical structures of the target compounds were confirmed by 1H NMR,13C NMR,IR,and MS.  相似文献   

19.
基于铁和锰的双核配合物在生物氧化还原过程中的重要作用及在化学的氧化还原过程中可能做为催化剂的应用前景,本文合成了两个新的以氯醌酸二价阴离子为桥联配体的Fe(Ⅲ)双核和Mn(Ⅱ)双核配合物:[Fe_2(phen)_4(μ-CA)](ClO_4)_4·2H_2O(1)和[Mn_2(phen)_4(μ-CA)](ClO_4)_2·3H_2O(2)(phen=1,10菲咯啉;CA=氯醌酸二价阴离子)。经元素分析、IR、电子光谱及磁性等测定,对两配合物进行了表征。  相似文献   

20.
The phase relationship in the pseudobinary Co3V2O8-CoMoO4 system have been determined by differential thermal analysis (DTA) and X-ray diffraction (XRD). A new compound Co2.5 VMoO8, stable up to 1080±5°C has been found in the system. The results obtained are presented in the form of a phase diagram. This revised version was published online in July 2006 with corrections to the Cover Date.  相似文献   

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