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1.
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   

2.
合成了新试剂N-对甲苯基-N′-(氨基对苯磺酸钠)硫脲(PMPT)。经红外、紫外、核磁共振和元素分析等方法测试,确定了其组成和结构,并研究了新试剂与钯(Ⅱ)的显色反应,建立了光度法测定微量钯(Ⅱ)的新方法。在pH3.6~5.8的HAc-NaAc缓冲体系中,该试剂和钯(Ⅱ)形成一种稳定的组成比(摩尔比)为1∶2的水溶性配合物,其最大吸收峰位于318.6nm处,表观摩尔吸光系数为2.66×105L·mol-1·cm-1。钯(Ⅱ)在8.0~424μg/L服从比尔定律,相关系数r=0.9997。将该法应用于阳极泥和矿石样品中微量钯的测定,获得满意的结果。  相似文献   

3.
N-辛基-N'-(氨基对苯磺酸钠)硫脲是新合成的一种显色剂,该试剂极易溶于水而形成无色溶液。在pH3.6~5.2的HAc-NaAc缓冲体系中,试剂与铜(Ⅱ)形成一种稳定的蓝色水溶性配合物,其组成比为:Cu(Ⅱ):OPT=1:3。配合物的最大吸收波长位于301.4nm,表观摩尔吸光系数ε_(301.4)=1.82×10 ̄5L·mol ̄(-1)·cm ̄(-1)。Cu(Ⅱ)在0~10μg/25mL服从比尔定律,相关系数r=0.9996,方法的检出限为3.85×10 ̄(-9)g/mL。本法灵敏度高,选择性好、操作简单,可直接在水相中测定。将本法用于合金钢和生物制品中微量铜的测定,均获得满意结果。  相似文献   

4.
本文报道了新试剂N-烯丙基-N′-(氨基对苯磺醚钠)硫脲(ASATu)的合成并确定了结构。该试剂与45种元素在不同介质中反应,仅有Cu ̄(2+)、Ag ̄+、Bi ̄(3+)、Hg ̄(2+)和Fe ̄(3+)等离子产生特征性反应。实验证明,它可作为Cu ̄(2+)、Ag ̄+等新的鉴定试剂;在酸性和近中性介质中测定了该试剂与稀土元素等四十多种金属元素反应的摩尔吸光系数。  相似文献   

5.
N-辛基-N’-(氨基对苯磺酸钠)硫脲是新合成的一种显色剂。该试剂极易溶于水而形成无色溶液,在pH3.6~5.2的HAc-NaAc缓冲体系中,试剂与铜(Ⅱ)形成一种稳定的蓝色水溶性配合物,其组成比为:Cu(Ⅱ):OPT=1:3。配合物的最大吸收波长们于301.4nm,表观摩尔吸光系数ε301.4=1.82×10^5L.mol^-1.cm^-1。Cu(Ⅱ)在0~10μg/25mL服从比尔定律,相关系  相似文献   

6.
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。N-甲基-N′-(氨基对苯磺酸钠)硫脲(MPT)用于测定微量铂(Ⅳ),  相似文献   

7.
本文合成新试剂N-间甲苯基-N′-(氨基对苯磺酸钠)硫脲(MMPT),经红外、紫外、核磁、元素分析等测试,确定其结构。研究测定了试剂与40多种离子的反应及其配合物的表观摩尔吸光系数,它可作为Cu2+(m=0.015μg,c=0.5μg/mL)、Ag+(m=0.1μg,c=3.3μg/mL)的新鉴定试剂和光度法测定Pd2+(ε309.7=6.32×104L·mol-1·cm-1)、Pt(Ⅳ)(ε754.4=8.58×104L·mol-1·cm-1)等的显色剂,方法灵敏度高、选择性好,用于阳极泥、人发、矿石及催化剂中上述元素的鉴定或测定,均获满意结果。  相似文献   

8.
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   

9.
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   

10.
研究了N-庚基-N’-(对氨基苯磺酸钠)硫脲与钯的反应条件。结果表明:在pH4.8-5.8的HAc-NaAc介质中,并有溴化十六烷基三甲胺存在下,试剂HPT与钯形成稳定的黄色配合物,其最大吸收波长为295.2nm,表观摩尔吸光系数为2.98×10^5L.mol^-1.cm^-1。  相似文献   

11.
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   

12.
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   

13.
The reaction of 1,2- and 1,3-benzenedithiol C6H4(SH)2 with chloro(phosphine)gold(I) complexes R3PAuCl (R = Et, Ph) in the presence of triethylamine in tetrahydrofuran gives stable gold(I) complexes 1,2-C6H4(SAuPR3)2 [R = Et ( 1 ) and Ph ( 2 )] or 1,3-C6H4(SAuPPh3)2 ( 3 ), respectively, in high yield. The compounds have been characterized by analytical and NMR spectroscopic data. From the reaction of 1,2-C6H(SH)2 with Et3P? AuCl a by-product [(Et3P)2Au]+ [Au(1,2? C6H4S2)2]? ( 4 ) has also been isolated in low yield. The crystal structures of compounds 2 and 4 have been determined by single crystal X-ray diffraction. The gold(I) atoms in complex 2 are two-coordinate with bond angles S? Au? P of 175.2(1) and 159.5(1)°, Au? S bond distances of 2.304(1) and 2.321(1) å, and a short Au…?Au contact of 3.145(1) Å. The gold(I) atom in the cation of complex 4 is also linearly two-coordinate with a P? Au? P angle of 170.1(1) Å and Au? P distances of 2.296(3) and 2.298(3) Å. The geometry of the anion in 4 shows a square-planar coordination of gold(III) by two chelating 1,2-benzenedithiolate ligands with Au? S distances between 2.299(3) and 2.312(3) Å (for two crystallographically independent, centrosymmetrical anions in the unit cell).  相似文献   

14.
New complexes of the formulae K3[RhL 3]·2 H2O, [PdL]·H2O and [M(LH2)Cl2] [whereM = Pd, Pt andLH2 = bis(o-aminobenzenesulfonyl)ethylenediamine] have been prepared and characterized by conductivity measurements, thermogravimetric analysis, X-ray powder patterns and IR, Ligand Field and1H-NMR spectroscopy.
Rhodium(III), Palladium(II)- und Platin(II)-Komplexe mit Bis(o-aminobenzolosulfonyl)ethylendiamin (Kurze Mitteilung)
Zusammenfassung Neue Komplexe der allgemeinen Formeln K3[RhL 3]·2H2O, [PdL]·H2O und [M(LH2)Cl2] mitM = Pd, Pt undLH2 = Bis(o-aminobenzolosulfonyl)ethylendiamin wurden dargestellt und mit Konduktionsmessungen, thermogravimetrischen Analysen, Röntgenstrukturanalysen, IR, Ligandfeld- und1H-NMR-Spektroskopie charakterisiert.
  相似文献   

15.
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   

16.
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   

17.
Some novel (diorgano)chloro(4-chlorobutoxy)silanes were obtained by the reaction of dichlorodiorganosilanes with tetra hydrofuran in the presence of chloroplatinic acid.Translated fromIzvestiva Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 943–945, April, 1996.  相似文献   

18.
X-Ray study of the (3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine oxide showed that the phosphorylmethyl group is bonded to the nitrogen atom of the cycle. Reaction of the tris(chloromethyl)phosphine sulfide with sodium diallylisocyanurate gave (3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine sulfide, and treatment of the tris(3,5-diallylisocyanuratomethyl)phosphine oxide with phosphorus pentasulfide gave a tris(3,5-diallylisocyanuratomethyl)bis(chloromethyl)phosphine sulfide.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1446–1448, August, 1993.  相似文献   

19.
贺殿  杨竹青  侯猛 《结构化学》2014,33(9):1388-1394
The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benzamide(C22H17ClN2O5, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N-(m-tolyl)benzamide with 2-(2-nitrophenyl)acetyl chloride. The structure of the product was confirmed by 1H NMR, 13 C NMR, IR, HRMS(ESI) and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269(10), b = 6.7251(6), c = 23.9313(16) , β = 99.931(6)o, V = 2065.1(3) 3, Z = 4, Dc = 1.366 g/cm3, F(000) = 880, μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections(I 2σ(I)). X-ray analysis indicates that the chloro-phenyl ring(C(10)~C(15)) and the methyl-substituted benzene ring(C(16)~C(21)) are not coplanar with the nitro-substituted benzene ring(C(1)~C(6)), with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C(2)–H(2)···O(2) and C(7)–H(7B)···O(5) are observed.  相似文献   

20.
本文合成了一组新的不对称的双核配合物,[Cu_2(C_2O_4)_2terp]和〔Cu Zn(C_2O_4)_2terp〕(图1),terp表示联三吡啶。配合物〔Cu_2(C_2O_4)2terp〕的变温磁化率已测,其数值已用最小二乘法与Bleaney-Bowers方程拟合,求得交换积分J=-47.20cm~(-1)。文中还用Kahn理论解释了这种较弱的反铁磁自旋交换作用。  相似文献   

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