A Study on the Color Reaction of Nickel with a New Chromogenic Reagent 1- (5-Nitro-2-Pyridylazo) - 2.7 - Dihydroxy - naphthalene and its Application

There has been study on heterocyclicazo reagent for the determination of microamount of nickel,but no study on the color reactron of nickel with a new chromogenic reagent 1- (5 -nitro - 2 - pyridylazo) - 2.7 - dihydroxy - naphthalene (5- NO₂ - PADN). So, here is a systematic study on condition under which the color reaction takes place. It proved that within PH 5.5~6.5,the maximnm absotption of the reagent lies at 460nm, that of the 2:1 turquoise chelate by 5 - NO₂ - PADN with nickel (Ⅱ) together is 650nm, and the apparent absorptivity is 1.02×10⁵ L · mol^-1 · cm^-1. The proposed method can be applied in the standard steel and the determination of microamounts of nickel in ore with satisfactory results.     

新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸分光光度法测定微量钴

近年来,杂环偶氮苯甲酸类显色剂取得了较快的发展。由于氨基取代结构对试剂性能有较大的影响^[1],因此本文合成了新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸,(TAEB)并研究了它与钴的显色反应。     

溶液中钪与草酸离子的配位作用

提钪工艺中常使草酸钪溶于过量草酸铵溶液中。但文献中有关钪与草酸离子配位作用的报导甚少。等用分光光度法测定了ScC₂O₄⁺配离子的稳定常数,而J·Stary则用分配法测定了SC(C₂O₄)₃^3-配离子的稳定常数,这些工作都没有对溶液中可能生成各级配离子进行研究。     

Determination of Trace Silver( Ⅰ ) in Basic Aqueous Solution by Electrochemiluminescence of a New Reagent 6-(2-Hydroxy-4-Diethylaminophenylazo)-2,3-Dihydro-1,4-Phthalazine-1,4-Dione

The electrochemiluminescence (ECL) of a new reagent 6- (2-hydroxy- 4 diethy laminophenylazo)-2,3-dihydro-1 ,4-phthalazine-1,4-dione (HDEA) in a basic aqueous so lution was studied by using the apparatus designed by ourselves. Trace amounts of silver ( Ⅰ ) shows a significant effect on the efficiency of light emission of HDEA during a positive trigonometrical wave pulse was exerted on the solution. The linear relationship between the light intensity and the concentration of silver( Ⅰ ) occurs in the range of 5. 0×10-8 to 3. 0×10-8 mol/L Ag(Ⅰ ) in a medium of KOH-KCl-HDEA (pH= 12. 8). The detection limit of the method is 2. 0×10-8 mol/LAg( Ⅰ ), and the r. s. d. for 1.0×10-7 mo)/L Ag ( Ⅰ ) is 5%. Of 21 metal ions concerned, only nickel( Ⅱ ), cerium( Ⅳ ) and cobalt( Ⅱ ) interfere the silver detection seriously; Ⅰ and Br also have some interference.     

柱前衍生非水毛细管电泳分离钴、镍和铜

提出柱前衍生非水毛细管电泳分离金属离子的方法.应用新合成的2-(6-甲基-2-苯并噻唑偶氮)-5-二乙胺基酚作为柱前衍生试剂,乙醇和N,N-二甲基甲酰胺为非水溶剂,在6min内实现了钴、镍和铜的分离,灵敏度高,检测限分别为9.18×10^-8mol/L、2.79×10^-7mol/L和4.47×10^-7mol/L.考察了柱前衍生条件、非水溶剂配比以及分离参数对分离的影响.     

非水溶性meso-四-(4-乙酰氧基苯)卟啉的合成及其与铅显色反应的研究

目前在用水溶性卟啉衍生物作显色剂方面已有文献总结^[1]。但对非水溶性卟啉则研究得较少。就测定痕量铅而言,皆用水溶性卟啉衍生物,而用非水溶性卟啉测定铅,则尚未见报导^[2-6]。     

钴与铬天青S、吡啶及其衍生物阳离子表面活性剂体系显色反应的研究

钴与铬天青S、溴化羟十二烷基三甲铵在吡啶的水溶液中可发生灵敏的显色反应,但吡啶作用的机理未论及,且吡啶气味恶臭,不便于应用.为了探讨吡啶在钴多元络合物形成中的增稳作用以及寻找其它含氮中性配位体代替吡啶,对Co(Ⅱ)与CAS,吡啶(Py)及其衍生物(α-氨基吡啶α-AP、5-氯-α-氨基吡啶5-Cl-α-AP),阳离子表面活性剂(CSF)体系进行了系统的研究.     

食用合成色素柠檬黄高灵敏度荧光光度法测定钯(Ⅱ)的研究

首次报道了食用合成色素柠檬黄(TTZ)荧光光度法测定钯(Ⅱ)的新方法。沸水浴中加热20～60min,在pH2.6～4.0的HCl-NaAc缓冲溶液中,钯(Ⅱ)与TTZ形成组成比为Pd(Ⅱ):TTZ=1:2的络合物(λ_ex=528nm,λ_em=558nm)。K_稳^f=9.71×10<¹¹·ε_ex=1.45×10⁴L/mol·cm,φ=0.011。钯含量在0～12μg/25mL范围内与荧光强度成正比,检出下限为4×10^-3μg/mL。本法可不经分离直接测定某些贵金属矿样中的微量钯,结果满意。     

PMBP与中性磷萃取剂对铽(Ⅲ)的协同萃取

本文研究了1-苯基-3-甲基-4-苯甲酰基吡唑啉酮-5(PMBP)与丁基膦酸二丁酯(DBBP)或磷酸三丁酯(TBP)的氯苯溶液在硝酸介质中对铽(Ⅲ)的协同萃取。测得了萃合物的组成及其萃取平衡常数,讨论了萃合物的可能结构式及协同萃取机理。     

以锌试剂显色法测定蛋白质的研究

有关蛋白质染色测定的分光光度研究已有不少报道,其中有些已用于蛋白质的分析测定［１～４］．锌试剂常用于金属离子的分光光度法测定,但作为生物大分子分析试剂的研究,目前还未见报道．实验表明,在ｐＨ４左右的缓冲溶液中,锌试剂与ＢＳＡ反应生成有色复合物,吸收光...     

瓜环与喹啉衍生物包结配合行为研究

利用¹H NMR以及荧光技术研究了六、七、八元瓜环与2-苯基喹啉、N-正丙基溴化异喹啉、3-氨基喹啉及7,8-苯并喹啉的相互作用.两种方法的考察结果均表明,2-苯基喹啉能与这3种瓜环发生相互作用,其中六、七元瓜环与2-苯基喹啉形成1∶1的稳定包结配合物,包结常数分别为1.6×10⁴和3.2×10³L/mol.八元瓜环能与2-苯基喹啉形成1∶2包结物.¹H NMR结果还表明,3种瓜环均能与N-正丙基溴化异喹啉相互作用,其化学计量比均为1∶2;七元瓜环与7,8-苯并喹啉相互作用,化学计量比约为1∶1.荧光法也表明八元瓜环能与N-正丙基溴化异喹啉、3-氨基喹啉及7,8-苯并喹啉发生相互作用,并且荧光强度随瓜环浓度增加而下降,其化学计量比为1∶2.同时,讨论了上述主客体包结配合物的作用模式.     

对甲基二溴偶氮胂的合成及其与稀土显色反应的研究

本文报道了对甲基二溴偶氮胂的合成,该显色剂在酸性介质中与稀土元素产生高灵敏度显色反应,大多数常见元素不干扰,所拟分析方法已成功地应用于小麦和铝合金中稀土总量的测定     

Spectrophotometric determination of manganese with 1-(2-pyridylazo)-2-naphthol and a non-ionic surfactant

A spectrophotometric method for the determination of trace amounts of manganese with 1-(2-pyridylazo)-2-naphthol (PAN) is described. The method is based on the measurement of absorbance of the manganese—PAN chelate solubilized with a non-ionic surfactant, Triton X-100. No extraction procedure is required in the method proposed. High concentrations of calcium, aluminium and magnesium do not interfere. The presence of up to 10 ppm of lead can be tolerated. Iron, cadmium, zinc, cobalt and nickel can be effectively masked with potassium cyanide. Beer's law is obeyed up to 2 ppm of manganese. The molar absorptivity of the manganese—PAN chelate found was 4.4 × 10⁴ l. mole ⁻¹. cm⁻¹ at 562 nm. The overall stability constant of Mn(PAN)₂ in 0.4% Triton X-100 medium is 10^16.8.     

藏红T萃取分光光度法测定岩石矿物中的微量汞

藏红T[SafraninT(C. I. BasicRed 2)]属于醌亚胺类对氮蒽碱性染料,虽已用于萃取光度法和萃取萤光光度法,但尚未见用于汞的测定.作者在研究和应用碘绿^[1]、乙基紫^[2]、酚藏花红^[3]和碱性品红^[4]等碱性染料作为汞的新显色剂基础上,应用藏红T作显色剂,建立了萃取分光光度法测定微量汞的新方法,并将此法用于岩矿中微量汞的测定.     

新型铈组稀土显色剂对乙酰基偶氮胂两类显色反应的研究

本文探讨了两类显色反应的特点和转化关系,并测定了两种络合物的组成。     

The Determination of Trace Amounts of Cadmium in Rice Samples by Dual-wave Length Spectrophotometry——cd(Ⅱ)-Cadion 2B-Tween 40 System

The optimal conditions of the Cd(Ⅱ)-Cadion 2B-Tween 40 system have been studied.In the alkaline medium of NaOH,a red Cd(Ⅱ)-Cadion 2B-Tween 40 complex forms with e510nm=9.80×104 The Ka ofCadion 2B and Surface tension in the system was estimated.It was proved that K was increased and the reagent species with absorption maximum at 605nm formed.Using the dual-wave length method at 510?605nm the apparent molar absorptivity for cadmium measured was 2.60×10 The molar ratio of cadmium to Cadion 2B is estimated to be 1:3 as estimated by the molar ratio method and continuous variation method.The Beer's law is obeyed in 0~6μg Cd/25ml.Using the proposed method with TEA,IDA and CIT masking mixture,the Cd content in rice samples was determined with satisfactory results.     

Cobalt and nickel complexes bearing 2,6-bis (imino) phenoxy ligands: syntheses, structures and oligomerization studies

A series of new cobalt and nickel complexes LMX₂ (M=Co, X=Cl; M=Ni, X=Br) bearing 2, 6-bis(imino)phenoxy ligands were synthesized. The solid-state structures of 1 and 4 have been determined by single-crystal X-ray diffraction study. Treatment of the complexes LMX₂ with methylaluminoxane (MAO) leads to active catalysts for oligomerization of ethylene with catalytic activities in the range of 1.2×10⁵–2.1×10⁵ g mol⁻¹ h⁻¹ atm⁻¹ for Ni complexes, and 10³ g mol⁻¹ h⁻¹ atm⁻¹ for Co complexes. The oligomers were olefins from C₄ to C₁₆.     

新显色剂偶氮胂DBF分光光度法测定稀土元素研究

变色酸双偶氮胂类化合物是光度法测定稀土元素的重要显色剂,如偶氮胂Ⅲ、三溴偶氮胂等。为研究各种取代基对这类显色剂与稀土配合物的影响,将对甲基二溴偶氮胂中的甲基换为甲酰基,合成得偶氮胂DBF,化学命名为2-(2-胂酸基苯偶氮)-7-(2,6二溴-4-甲酰基苯偶氮)-1,8-二羟基萘-3,6-二磺酸。     

铌-4,5-二溴苯基萤光酮-表面活性剂显色体系的研究——高灵敏分光光度法测定合金钢中的微量铌

铌的高灵敏度、高选择性的光度法似尚少见。最近有人^[1]合成过4,5-二溴苯基萤光酮(下称Br-PF),但至今未见该试剂用于铌的胶束增溶光度法的测定。为此本文较系统地研究了在CTAB及乳化剂OP存在下Nb(V)与Br-PF的显色条件,结果表明本法具有很高的灵敏度(ε=2.1×10⁵)和较高的选择性(存在掩蔽剂),可不经任何分离直接在水相中测定合金钢中的微量铌。     

稀土-氨基J酸偶氮氯膦-氯代十四烷基吡啶-乙醇多元络合物的研究及分析应用

本文研究了氨基-J酸偶氮氯膦在阳离子表面活性剂存在下与稀土元素形成多元络合物的显色反应,并进行了实样分析。