Synthesis of N-o-methylphenyl-N'-(sodium p-aminobenzene-sulfonate) thiourea and its chromogenic reaction with palladium(II).

A new chromogenic reagent, N-o-methylphenyl-N'-(sodium p-aminobenzenesulfonate)thiourea (MSAT), has been synthesized and characterized by elemental analysis, (1)H-NMR, FT-IR and UV-Vis spectra. Based on the absorption spectrum of the colored complex of MSAT with palladium(II), a novel spectrophotometric method for the determination of palladium has been developed. In a pH 4.0 - 5.5 HAc-NaAc buffer solution, palladium(II) reacted with MSAT to form a stable yellow water-soluble complex with an apparent molar absorptivity of epsilon = 2.04 x 10(5) L mol(-1) cm(-1) at the maximum absorption of 318.0 nm. Beer's law was obeyed in the concentration range of 1.2 - 11.8 microg per 25 mL for palladium(II) with a correlation coefficient of 0.9997. The probable interfering ions and their tolerable limits have also been investigated in detail. The proposed method is simple, rapid, and sensitive, and has been applied to the determination of palladium in anode mud and ore samples with satisfactory results.     

Spectrophotometric determination of palladium after solid-liquid extraction with 1-(2-Pyridylazo)-2-naphthol at 90 degrees C

An effective spectrophotometric determination of palladium with 1-(2-pyridylazo)-2-naphthol (PAN) using molten naphthalene as a diluent has been studied. A green complex of palladium with PAN is formed at 90 degrees C. In the range of pH 1.5-7.5, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in CHCl(3) to be determined spectrophotometrically at 678 nm against the reagent blank. Beer's law is obeyed over the concentration range of 0.5-10 ppm. The molar absorptivity and Sandell's sensitivity are 1.2 x 10(4) l mol(-1) cm(-1) and 0.0070 mg cm(-2), respectively. The optimum conditions for determination are obtained. The interferences of various ions are observed in detail. The method has been applied to the determination of palladium in synthetic samples.     

4-(N,N-diethylamino) benzaldehyde thiosemicarbazone in the spectrophotometric determination of palladium

4-(N,N-diethylamino)benzaldehyde thiosemicarbazone(DEABT) is proposed as a sensitive and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium (II) in a potassium hydrogen phthalate-hydrochloric acid buffer of pH 3.0, to form a yellow complex. Beer's law is obeyed in the concentration range up to 3.60 microgmL(-1). The optimum concentration range for minimum photometric error as determined by Ringbom plot method is 0.36 - 3.24 microg mL(-1). The yellow Pd(II)-DEABT complex shows a maximum absorbance at 408 nm, with molar absorptivity of 3.33 x 10(4) dm3 mol(-1) cm(-1) and Sandell's sensitivity of the complex from Beer's data, for D = 0.001, is 0.0032 microg cm(-2). The composition of the Pd(II)-DEABT complex is found to be 1:2 (M:L). The interference of various cations and anions in the method were studied. The proposed method was successfully used for the determination of Pd(II) in alloys, catalysts, complexes and model mixtures with a fair degree of accuracy.     

Extractive spectrophotometric determination of palladium with N,N,N',N'-tetra(2-ethylhexyl)-thiodiglycolamide T(2EH)TDGA

A precise, sensitive and selective method for the spectrophotometric determination of palladium (II) using N,N,N′,N′-tetra(2-ethylhexyl) thiodiglycolamide T(2EH)TDGA as an extractant is described. Palladium (II) forms yellow colored complex with T(2EH)TDGA which exhibits an absorption maximum at ∼300 nm. The colored complex obeys Beer's law in the concentration range 1.0-15.0 μg ml⁻¹ of palladium with a molar absorptivity of 1.29 × 10⁵ M⁻¹ cm⁻¹. The effects of various experimental parameters have been studied to establish the optimum conditions for the extraction and determination of palladium. The precision of the method has been evaluated and the relative standard deviation has been found to be less than 0.5%. The method has been successfully applied to the determination of palladium in simulated high level liquid waste (SHLW) solution.     

The spectrophotometric determination of thallium(iii)by ternary complex formation

If thallium(III) is added to an aqueous solution of potassium thiocyanate containing a large amount of pyridine in the pH range 5.2–5.5, a yellow solution which is stable in diffuse light is obtained. The yellow colour can be measured at 405 nm for the colorimetric determination of thallium(III) in the range 20–300 μg Tl ml^-1. The complex is a mixed ligand complex with a metal-ligand ratio of 1:2:2. Thallium(I) does not interfere. The interference of various other metal ions and anions is discussed.     

Complexation and determination of palladium (II) ion with para-Cl-phenylazo-R-acid spectrophotometrically

The complexation of para-Cl-phenylazo-R-acid azo dye with Pd(II) has been studied spectrophotometrically. Protonation constant (pK(a)) of the ligand has been calculated and the stability conditional constants of para-Cl-phenylazo-R-acid ligand with palladium ion has been determined at a constant temperature (25.0 degrees C), where the molar ratio of this complex is 1:1 (metal:ligand) with logbeta(1)=3.75, and 1:2 with logbeta(2)=8.55. Solid complex of para-Cl-phenylazo-R-acid has been prepared and characterized on the basis of elemental analysis and FTIR spectral data. A procedure for the spectrophotometric determination of Pd(II) using para-Cl-phenylazo-R-acid as a new azo chromophore is proposed where it is rapid, sensitive and highly specific. Beer's law was obeyed in the range 0.50-10.00 ppm at pH 5.0-6.0 to form a violet-red complex (epsilon=7.7 x 10(4) l(-1) mol(-1) cm(-1) at lambda(max)=560 nm). Metal ions such as Cu(II), Cr(III), La(III), Yb(III), Y(III), and Rh(III) interfere with the complex. Ammonium salt of trimellitic acid is used to precipitate some of the interfering ions and a scheme for separation of Pd(II) from a synthetic mixture similar in composition to platinum ore or deposit was made.     

Extractive spectrophotometric determination of palladium using 2-(2-hydroxyimino-1-oxoethyl)furan

A rapid, simple, selective and sensitive method for the determination of palladium in trace amounts has been developed, based on the reaction of 2-(2-hydroxyimino-1-oxoethyl)furan [-isonitroso-2-acetyl-furan] with the metal ion in acetic acid. The intense yellow complex is quantitatively extractable into chloroform, whose absorbance is measured at 425 nm. The method is free from the interference of a large number of other metal ions. It obeys Beer's law in the range 0.0–3.8 g Pd mL^–1 with Sandell's sensitivity of 0.003 g Pd cm^–2. The ratios of metal to ligand in the extracted complex are 1:1 and 1:2. The analysis of various samples has been carried out with satisfactory and reproducible results.     

Extraction and spectrophotometric determination of Pd(II) with 3,4,4a,5-tetrahydro-3,3,4a-trimethyl-7-(substituted)-pyrimido(1,6-a)-benzimidazole-1-thiol (PBT)

A method for the extraction-spectrophotometric determination of palladium with 3,4,4a,5-tetrahydro-3,3,4a-trimethyl-7-(substituted)-pyrimido(1,6-a)benzimidazole-1-thiol (PBT) is described. PBT-Pd(II) complex is extracted from an acidic aqueous solution (0.01-0.5M HClO(4)) into a chloroform layer. The absorbance is measured at 438 nm and the molar absorptivity found to be 1.033 x 10(4)M(-1) cm(-1). The complex system conforms to Beer's law over the range 1.9-28.5 mug/ml palladium(II). The effects of pH (2-6), HClO(4) concentration, PBT concentration and shaking time were studied. The ratio of metal ion to ligand molecules in the coloured complex was found to be 1:4. The tolerance limit for many metals have been determined. Finally, the method has been applied successfully to the determination of palladium in synthetic mixtures and in the standard palladium carbon powder (palladium catalyst).     

Analytical study of the phenyl-2-pyridyl ketone azine-palladium system. Photometric determination of palladium

Phenyl-2-pyridyl ketone azine reacts with palladium(II) to produce a yellow 1:1 complex (λ_max = 425 nm, ? = 10.4 × 10³M^?1 cm^?1 in aqueous ethanolic solution) and a red-violet 3:1 complex (λ_max = 530?540 and 380?390 nm). The yellow complex in aqueous ethanolic solution has been used for the spectrophotometric determination of trace amounts of palladium. The method has been applied to the determination of palladium in some catalysts and one mineral.     

Spectrophotometric determination of cobalt with phenanthrenequinone monoxime

Phenanthrenequinone monoxime reacts with cobalt to form a yellow-orange insoluble 1:3 (cobalt:ligand) complex which is extractable into chloroform in the pH range 4.45-8.0. The determination of cobalt is carried out at 470 mmu. Beer's law is obeyed over the concentration range 0-3.0 ppm of cobalt. The sensitivity is 0-00336 mug of Co/cm(2) for 0.001 absorbance. The effect of a number of foreign ions has been studied.     

Spectrophtometric determination of tungsten(VI) with rutin and cetyltrimethylammonium bromide

Tungsten-(VI) reacts with rutin in the presence of cetyltrimethylammonium bromide to form a soluble yellow complex having maximum absorbance at 416 nm. The molar ratio of tungsten to rutin in the complex is 1:2. The molar absorptivity is 5.01 x 10(4) 1.mole(-1).cm(-1). Beer's law is obeyed over the range 1 x 10(-7)(-1) x 10(-5)M tungsten (VI). Optimum solution conditions for the determination of tungsten in various sample matrices have been found and the interference of diverse ions has been examined.     

Picolinaldehyde 4-phenyl-3-thiosemicarbazone as a spectrophotometric reagent for the selective determination of small amounts of cobalt in the presence of iron

The characteristics and analytical applications of picolinaldehyde 4-phenyl-3-thiosemicarbazone are described. This compound gives coloured reactions with cobalt(II), iron(II) and (III), nickel(II), copper(II), palladium(II) and other ions, that are much more sensitive than those with picolinaldehyde thiosemicarbazone. The 1:2 yellow cobalt(II) complex has been used for the spectrophotometric determination of cobalt in the presence of iron, and applied to steel analysis.     

Direct photometric determination of cobalt(II) with N-methylaminothioformyl-N'-phenylhydroxylamine

N-Methylaminothioformyl-N'-phenylhydroxylamine forms a 1:2 (metal:ligand) greenish yellow complex with cobalt(II). This complex has maximum absorption at 470 nm with a molar absorptivity of 1.65 x 10(4) 1.mole(-1).cm(-1). Beer's law is obeyed over the concentration range 6 x 10(-6)-6 x 10(-5)M. The effect of diverse ions is described.     

Spectrophotometric Determination of Palladium with Methylthymol Blue

A new, sensitive spectrophotometric method for the determination of palladium(II) with methylthymol blue has been developed. The palladium methylthymol blue complex has an absorption maximum at 530 nm. The colour reaction has a sensitivity of 0.005 µg of palladium/cm² and obeys Beer's Law over the range 0.4 to 3.24 ppm of palladium. The effects of concentration of perchloric acid, reagent, heating, stability of colour and diverse ions have been investigated. The ratio of metal: ligand in the complex is 1:1 and the formation constant was calculated to be 1.18×10⁴.     

Spectrophotometric investigation of the reaction of CU(II) and Cu(I) with 1-isonitroso-(1,2,3,4)-tetrahydrophenazine

The reactions of Cu(II) and Cu(I) with 1-isonitroso-(1,2,3,4)-tetrahydrophenazine (HITF) have been studied spectrophotometrically. Both ions form complexes with metal/ligand ratio 1:2. The complex of Cu(I) and ITF can be used for copper determination in the range 2-50 x 10(-6)M, and has been separated as the perchlorate in crystalline form. The spectrophotometric characteristics and the equilibrium constants for the ligand and for the complexes are reported.     

Sorption of radiocalcium on human hair

The possibility of determination of microgram quantities of palladium by radiochemical displacement of labelled Zn from Zn: 1-/2-pyridylazo/-2-naphthol comples has been explored. Conditions for quantitative displacement, a calibration in the range of 40–140 g of palladium and the effects of diverse ions have been reported.     

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。     

N,N（二甲庚基）乙酰胺萃钯机理研究

本文研究了N,N二甲庚基乙酰胺(N_(s03))从氯化物体系中萃取钯的机理。应用等摩尔系列法和斜率法确定萃合物组成为:(CH_3CONR_2H)_2PdCl_4。通过紫外-可见光谱法研究,证实N_(503)萃取钯的机理属阴离子交换反应,其萃取方程式为: 2CH_3CONR_2HCl_((o)) PdCl_4~(2-)(a)?(CH_3CONR_2H)_2PdCl_4(o) 2Cl~-(a)     

Comparative studies of ONNO-based ligands as ionophores for palladium ion-selective membrane sensors

Palladium sensors based on two neutral ionophores, N,N′-bis(acetylacetone) cyclohexanediamine (L₁) and N,N′-bis(o-hydroxyacetophenone)-1,2-cyclohexanediamine (L₂) for quantification of palladium ions are described. Effect of various plasticizers (o-NPOE, DBP, DEP, DOP, TBP, and CN) and anion excluder, sodium tetra phenyl borate (NaTPB) has been studied. The best performance is obtained with a membrane composition of PVC:o-NPOE:ionophore (L₁):NaTPB of 150:300:5:5 (%, w/w). The sensor exhibits significantly enhanced selectivity towards palladium ion over the concentration range 1.0 × 10⁻⁸ to 1.0 × 10⁻¹ M with a lower detection limit of 4.0 × 10⁻⁹ M and a Nernstian compliance (29.1 ± 0.3 mV decade⁻¹ of activity) within pH range 2.0-6.0 and fast response time of 10 s. Influence of the membrane composition and possible interfering ions has also been investigated on the response properties of the electrode. Fast and stable response, good reproducibility and long-term stability of the sensor are demonstrated. The sensor has been found to work satisfactorily in partially non-aqueous media up to 20% (v/v) content of methanol, ethanol and acetonitrile and could be used for a period of 4 months. Selectivity coefficients determined with fixed interference method (FIM) indicate high selectivity for palladium. The proposed electrode shows fairly good discrimination of palladium from other cations. The application of prepared sensor has been demonstrated in determination of palladium ions in spiked water sample.     

o-Hydroxyacetophenone thiosemicarbazone as a reagent for the rapid spectrophotometric determination of palladium

o-Hydroxyacetophenone thiosemicarbazone has been synthesized and employed as a new reagent for the spectrophotometric determination of palladium(II), which forms two complex species with it in aqueous dimethylformamide at pH 6.0, these having 1:1 and 1:2 metal-ligand ratios. The Job and molar-ratio plots have an unusual shape that is due to the stepwise conversion of the 1:1 complex into the 1:2 species. The molar absorptivity at 370 nm is 9 x 10(3) l.mole(-1).cm(-1). Beer's law is obeyed over the range 0.42-10.6 mug/ml palladium.