Spectrophotometry Determination of Iron(II) Separated by Means of Adsorption of Its 3-(2-Pyridyl)-5, 6-Diphenyl-1, 2, 4-Triazine Complex with Tetraphenyl-Borate on Microcrystalline Naphthalene

A procedure is describe for the adsorption of ion-associated complex of iron(II) 3-(2-pyridyl)-5, 6-diphenyl-1, 2, 4-triazine (abbreviated as PDT) cation with tetra phenylborate (TPB) anion on macrocrystalline naphthalene. A water-insoluble ion-associated complex formed with PDT and TPB is quantitatively adsorbed on micro-crystalline naphthalene. The solid mixture containing the colored complex is dissolved in acetonitrile and the absorbance was measured at 553 nm. The other factors such as pH, amounts of reagents and naphthalene, shaking and standing times, diverse ions are studied. The method has been applied for the determination of iron in alloys and water samples.     

Atomic Absorption Spectrophotometric Determination of Copper (I) after Adsorption of its 4′-(p-Methoxyphenyl)-2, 2′:6′, 2″-Terpyridine Tetraphenylborate Ion-Associated Complex on Microcrystalline Naphthalene

A new atomic absorption spectrophotometric method has been developed for the trace determination of copper after adsorption of its 4′-(p-methoxyphenyl)-2, 2′:6′,2″-terpyridine tetraphenylborate ion-associated complex on microcrystalline naphthalene. This complex is adsorbed on microcrystalline naphthalene in the pH range 0.5-11.0 by shaking for a few seconds. The solid mass so formed is separated by filtration, dissolved in dimethylformamide and the absorbance is measured at 324.7 nm. Beer's law is obeyed in the concentration range 5.0-60.0 μg of copper in 10 ml of the final dimethylformamide solution. The replicate determinations of a sample containing 30 μg of copper gave a mean absorbance of 0.171 with a standard deviation of 0.0019 and a relative standard deviation of 1.11%. The method has been applied to the determination of copper in certain standard reference materials.     

Trace Analysis of Nickel by Extraction-Atomic Absorption Spectrophotometry Determination of its Acenaphthenequinone Dioxime Complex in Molten Naphthalene

A procedure is described for the trace analysis of nickel using the liquid-liquid extraction of nickel acenaphthenequinone dioxime complex with molten naphthalene followed by solid-liquid separation. Nickel complex cannot be extracted into any non-aqueous organic solvents, but can be quantitatively extracted into molten naphthalene. It is very stable at high temperature and is dissolved in the mixed solvent (HNO₃-DMF). The absorbance of the solution was measured at 231.5 nm against a reagent blank. Beer's law is followed in the concentration range of 5–100 μg of nickel in 10 ml of the final solution. The sensitivity for 1% absorption is 0.155 μg/ml nickel. The relative standard deviation is 1.0% for ten replicate determinations of 60 μg of nickel. The interference of various ions has been studied and the method has been applied to the determination of nickel in aluminium alloys.     

Spectrophotometric Determination of Ziram by Coprecipitating the Corresponding Copper(II) or Palladium(II) Complex with Naphthalene

A spectrophotometric method has been developed for the determination of zinc dimethyldithiocarbamate (ziram) by converting it into dimethyldithiocarbamate and coprecipitating its copper(II) and palladium(II) dimethyldithiocarbamate complexes and coprecipitating onto microcrystalline naphthalene. Palladium(II) and copper(II) complexes absorb strongly at 395 nm and 430 nm, respectively. The interference of various ions has been studied and the method has been applied to determine ziram in commercial samples and grains.     

Complex Formation Equilibria of Iron(III) With 2-Hydroxy-3- Pyridinol and 2-Mercapto-3-Pyridinol. Spectrophotometry Determination of Iron(III) In Multivitamins

ABSTRACT

The complex equilibria of iron(III) with 2-hydroxy-3-pyridinol (HHP), and 2-mercapto-3-pyridinol (MHP) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaCIO₄). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance pH-graphs. After considering all the different parameters a simple, rapid, sensitive and selective method for spectrophotometric determination of trace levels of iron(III) was proposed based on the formation of (Fe -MHP) complex at pH 2.5 (λ_max = 640 nm, ? = l×10⁴ L mol^?1 cm^?). The interference of a large number of foreign ions was investigated. The method has been applied successfully for the determination of iron content in some multivitamins with mineral preparations and infant milk products.     

Spectrophotometric Determination of Lead by Extraction of the Mixed-Metal Complex Pb(II)-Ca-Purpurin (1,2,4-Trihydroxyanthraquinone)

Abstract

Mixtures of Lead(II) and Ca(II) form with purpurin (P; 1,2,4-Trihydroxyanthraquinone) the mixed-metal-complex PbCaP₃, which is extracted with isobutyl methyl ketone (IBMK) at pH 7.8. The molar absorptivity of the complex is 2.8 × 10⁴ l.mol^?1.cm^?1 at 575 nm and its conditional extraction constant 2.5 × 10¹⁷ 1⁴.mole^?4. The use of this complex for the spectrophotometric determination of lead up to 40 μg has been investigated. The proposed procedure has been successfully applied to the analysis of this metal in different samples.     

新的含有4-对甲基苯基-3，5-二(2-吡啶基)-1，2，4-三氮唑钴配合物的合成和晶体结构(英)

A new cobalt(Ⅱ) complex, [CoL₂(NCS)₂]·2CH₂Cl₂, [L=4-(p-methylphenyl)-3,5-bis(pyridin-2-yl)-1,2,4-triazole], was synthesized and its crystal structure was determined by X-ray analysis. The complex crystallizes in monoclinic system with space group P2₁/c, a=0.867 40(17), b=1.453 9(3), c=1.781 9(4) nm, β=91.18(3)°, V=2.246 7(8) nm³ and Z=2. The cobalt atom is in a distorted octahedral environment with two bidentate chelating L ligands in the equatorial plane and two NCS^- ions in the axial positions. CCDC: 251658.     

Determination of manganese by flame atomic absorption spectrometry after its adsorption onto naphthalene modified with 1-(2-pyridylazo)-2-naphthol (PAN)

A system for determination of manganese, after preconcentration with 3% (w/w) 1-(2-pyridylazo)-2-naphthol (PAN), adsorbed on microcrystalline naphthalene is proposed. An amount of 200 mg of this complexing mixture is placed in a glass column and conditioned with a NH₄Cl/NH₄OH buffer solution (pH 9.5). The aqueous sample, containing manganese, is treated with an ammonium tartrate solution, then with a hydroxylammonium chloride solution and, finally, with a buffer solution. The resulting solution is passed through the column containing microcrystalline naphthalene modified with 1-(2-pyridylazo)-2-naphthol (PAN) where Mn(II) is retained. The column is first washed with deionized water and then with 10.0 ml of dimethylformamide to dissolve the Mn(II)-PAN/naphthalene complex. Manganese is determined by air-acetylene flame atomic absorption spectrometry. About 1 μg of manganese can be concentrated from 200 ml of aqueous sample, allowing a preconcentration factor of 20, a limit of quantification of 5 ng ml⁻¹ and R.S.D. of 3.8%. The accuracy was ascertained using certified reference materials, including samples of urine and glass. Water samples were also analysed and the results are in good agreement with those obtained by graphite furnace atomic absorption spectrometry.     

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。     

钯的PAR-氯化四苯鉮的萃取光度法测定

本文报道了钯与4-(2-吡啶偶氮)间苯二酚(PAR=H_2R,下同)和四苯钟离子形成离子缔合物的化学条件,经氯仿萃取后,建立了一种测定微量钯的萃取光度法。萃取的最佳pH为4.4,络合物的化学式为[(C_6H_5)_4As~+,PdClR~-],其最大吸收峰波长为532nm,表观摩尔吸光系数e_(532)=3.3×10~4L·mol~(-1)·cm~(-1),10mL萃取液中钯量在0～25μg内遵守比耳定律。方法简便,选择性好,用于催化剂中钯的测定,结果满意。     

用2-QADN2,7-金属络合物示波极谱法同时测定铜镍钴镉

本文研究了2-QADN2,7-金属络合物的极谱特性。在pH9.60的缓冲溶液中,Cu(Ⅱ)、Ni(Ⅱ)、Co(Ⅱ)和Cd(Ⅱ)与2-QADN2,7的络合物在-0.37、-0.69、-0.77和-0.82V产生灵敏的极谱波,利用这些波可测定痕量的铜、镍、钴和镉。铜的检测下限为2.0×10~(-8)mol/L,镍、钴及镉的检测下限为5.0×10~(-8)mol/L。提出的方法用于同时测定头发和茶叶中的痕量铜、镍和钴,结果满意。     

Atomic Absorption Spectrophotometric Determination of Copper(II) after Adsorption of its Oxinate on Microcrystalline Naphthalene

A New Atomic Absorption Spectrophotometric Procedure Has Been Developed For The Microdetermination Of Copper(Ii) As Its Oxinate By Its Adsorption On Micro-Crystalline Naphthalene And Dissolution In 1 N Nitric Acid. Copper(Ii) Oxinate Is Quantitatively Adsorbed In The PH Range Of 3.2–10.1 And Trace Amounts Of Copper Can Be Determined. The Effect Of Variables Such As Reagent And Naphthalene, Shaking Time, Digestion Time, And Diverse Ions Are Studied. The Proposed Method Has Been Applied To The Determination Of Copper In Standard Reference Material (Zinc Alloy), And Metallic Zinc And Lead.     

Spectrophotometric Determination of Molybdenum(VI) as a Ternary Complex with 4-Nitrocatechol and Benzalkonium Chloride

A new liquid—liquid extraction system for molybdenum(VI) was studied. It contains 4-nitrocatechol (4NC) as a complexing chromogenic reagent and benzalkonium chloride (BZC) as a source of heavy cations (BZ⁺), which are prone to form chloroform-extractable ion-association complexes. The optimum conditions for the determination of trace molybdenum(VI) were found: concentrations of 4NC and BZC (7.5 × 10⁻⁴ mol dm⁻³ and 1.9 × 10⁻⁴ mol dm⁻³, respectively), acidity (3.75 × 10⁻² mol dm⁻³ H₂SO₄), extraction time (3 min), and wavelength (439 nm). The molar absorptivity, limit of detection, and linear working range were 5.5 × 10⁴ dm³ mol⁻¹ cm⁻¹, 5.6 ng cm⁻³, and 18.6–3100 μg cm⁻³, respectively. The effect of foreign ions was examined, and the developed procedure was applied to the analysis of synthetic mixtures and real samples (potable waters and steels). The composition of the extracted complex was 1:1:2 (Mo:4NC:BZ). Three possible structures of its anionic part [Mo^VI(4NC)O₂(OH)₂]²⁻ were discussed based on optimizations at the B3LYP/3-21G level of theory, and simulated UV/Vis absorption spectra were obtained with the TD Hamiltonian.     

Application of the Ion Pair of 2-(5-Bromo-2-pyridylazo)-5-diethylaminophenol and Ammonium Tetraphenylborate for Preconcentration of Trace Vanadium and Determination by Third Derivative Spectrophotometry

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New Insights into the Catalytic Activity of Cobalt Orthophosphate Co3(PO4)2 from Charge Density Analysis

An extensive characterization of Co₃(PO₄)₂ was performed by topological analysis according to Bader‘s Quantum Theory of Atoms in Molecules from the experimentally and theoretically determined electron density. This study sheds light on the reactivity of cobalt orthophosphate as a solid-state heterogeneous oxidative-dehydration and -dehydrogenation catalyst. Various faces of the bulk catalyst were identified as possible reactive sites given their topological properties. The charge accumulations and depletions around the two independent five- and sixfold-coordinated cobalt atoms, found in the topological analysis, are correlated to the orientation and population of the d-orbitals. It is shown that the (011) face has the best structural features for catalysis. Fivefold-coordinated ions in close proximity to advantageously oriented vacant coordination sites and electron depletions suit the oxygen lone pairs of the reactant, mainly for chemisorption. This is confirmed both from the multipole refinement as well as from density functional theory calculations. Nearby basic phosphate ions are readily available for C−H activation.     

Cobalt(II) and copper(II) complexes of (2-thiophene)-(5,6-diphenyl-[1,2,4]-triazin-3-yl)hydrazone

New complexes having the formulae [L₂CoX₂] and [LCuCl₂], [LCuCl] and [LCu](ClO₄)₂ where L?=?(2-thiophene)-(5,6-diphenyl-[1,2,4]-triazin-3-yl)hydrazone TDPTH; X?=?Cl, OAc or ClO₄ have been synthesized and characterized on the basis of elemental analyses, conductance, magnetic moments and infrared, electronic and ESR spectral data. The IR spectra indicate that TDPTH is a neutral bidentate ligand, coordinating via a triazine-N and azomethine-N in [L₂CoX₂] and [LCuCl₂] with the thiophene-S not coordinated but is tridentate in [LCuCl] and [LCu](ClO₄)₂ through the same two nitrogen atoms and thiophene-S. The magnetic moment and electronic spectral data suggest a distorted octahedral structure for Co(II) complexes, a dimeric square pyramidal geometry for [LCuCl₂] through chloride bridges and a dimeric diamagnetic, four-coordinate copper in [LCu](ClO₄)₂ through thiophene-S bridges. The X-band ESR spectra of Co(II) complexes, in the solid state, are rhombic with three g values consistent with a high-spin distorted octahedral structure. The X-band ESR spectrum of the powdered sample of both [LCuCl₂]·2H₂O and [LCu](ClO₄)₂ at room temperature and at 77?K showed only one broad signal due to?ΔM _s?=?±?1 transition and a weak signal due to the forbidden?ΔM _s?=?±?2 transition, indicating an antiferromagnetic interaction between copper(II) centers whereas [LCuCl] is ESR silent, indicating a monovalent copper ion in this complex.     

强碱性SO_4~(2-)型阴离子交换树脂吸附分离-分光光度法测定痕量铅

提出了离子交换柱上吸附的分离技术，结合水相分光光度法测定痕量铅。实验表明，采用SO~(2-)_4型阴离子交换位吸附铅离子，可以消除基体金属在内的全部阳离子的干扰；测定方法的灵敏度ε为2.3×104L·mol-1·cm－1，铅含量在0～7.2mg·L－1范围内符合Beer定律．方法用于黄河水和碳酸镉样品中痕量铜的测定，结果较满意。     

流动注射-速差动力学分析研究meso-四(3-氯-4-磺基苯)卟啉光度法同时测定铜锌

本文研究了多种金属离子与meso-四(3-氯-4-磺基苯)卟啉的显色反应动力学特性。利用Cu(Ⅱ)、Zn(Ⅱ)与其它金属离子之间反应速率上的差异,建立了一种选择性同时测定Cu(Ⅱ)、Zn(Ⅱ)的流动注射分析法,不经分离同时测定桃叶样品中的铜、锌,结果满意。