Spectrophotometric Studies on the equilibria of vanadium(V)-4-(2-Pyridylazo)-resorcinol-polyaminopolycarboxylate systems

The complexation equilibria in the VO⁺₂-PAR-polyaminopolycarboxylate-(EDTA and CDTA) systems were studied spectrophotometrically in order to establish the action of CDTA in the spectrophotometric determination of vanadium(V) with PAR. Analysis of absorbance-pH curve and ligand exchange equilibria yielded the following values of the constants; K_VO2HR=lO^17.16, K^H_VO2HR=10^-3.95, K_VO2R=10^18.81, K_VO2EDTA=10^17.38 and K_VO2CDTA=10^16.59 at 20°C and ionic strength 0.1 (KCl). Based on these constants, the selective masking behavior of CDTA for the VO⁺₂-PAR system can be quantitatively explained.     

4-(2-Pyridylazo)-resorcin (PAR)

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4-(2-Pyridylazo)-resorcin (PAR)

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Eine spektralphotometrische Tantalbestimmung mit 4-(2-Pyridylazo)-resorcin

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Spectrophotometric determination of lanthanides using 4-(2-Pyridylazo) resorcinol

Summary The formation of red colour produced by the interaction of 4-(2-pyridylazo) resorcinol (PAR) and rare earths has been studied to determine the composition, stability and other characteristics of the chelates formed. The _max of all the chelates was found to be 515 nm atph 6.2 whereas the _max of the PAR reagent at this p_H is 410 nm. The composition of the chelates was found to be 12 (metalPAR) and has been established by two different methods. The stability constant values have been calculated by three different methods. The values of logK, lies in the range of 9.2–10.4 for different rare earth chelates. The chelates are stable over a wide range of p_H. A tentative suggestion has also been made for the position of the chelate ring.

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Zusammenfassung Die rote Farbreaktion von 4-(2-Pyridylazo)-resorcin (PAR) mit Seltenen Erden wurde untersucht, um die Zusammensetzung, die Stabilität und andere Merkmale der dabei entstehenden Chelate zu bestimmen. Beiph 6,2 wurde das Absorptionsmaximum aller Chelate bei 515 nm, das Absorptionsmaximum von PAR bei 410 nm gefunden. Die Zusammensetzung entspricht dem Verhältnis Metall: PAR=12; sie wurde nach zwei verschiedenen Methoden ermittelt. Die Komplexkonstante wurde auf drei verschiedenen Wegen bestimmt. logK liegt bei den verschiedenen Seltenen Erdmetall-Chelaten zwischen 9,2 und 10,4. Die Chelate sind in einem weitenph-Bereich beständig. Die Lage des Chelatrings wurde erörtert.

     

Spektralphotometrische Bestimmung von Gallium mit 4-(2-Pyridylazo)-resorcin

Zusammenfassung 4-(2-Pyridylazo)-resorcin bildet mit Gallium in schwach saurem Medium stufenweise zwei Chelate GaRH⁺ und GaR₂ ⁻, die sich gut als Grundlage für eine empfindliche spektralphotometrische Bestimmung von Gallium (≤ 0,1 μg Ga/ml) bei p_H 3,5–5,0 oder in Formiatpuffer bei p_H 4 eignen. Der Einflu? einiger Ionen, Puffer und der Ionenst?rke der L?sung auf die Bestimmung wird diskutiert.

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Summary Gallium forms by steps two coloured chelates GaRH⁺ and GaR₂ ⁻ with 4-(2-pyridylazo)-resorcinol (PAR) in aqueous solution, which are a convenient basis for the spectrophotometric determination of gallium (≤ 0,1 μg Ga/ml) at p_H 3,5–5,0 or in the presence of formiate buffer at P_H 4. The influence of buffers, ionic strength and some other ions is discussed.

     

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。     

Photometrische Bestimmung von Palladium mit 4-(2-Pyridylazo)-resorcin (PAR)

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Die Verbindung 5-(2-Pyridylazo)-2-monomethylamin-p-kresol(R)

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Selective Spectrophotometric Determination of Palladium (II) With 2-(5-Bromo-2-Pyridylazo)-5-(Diethylamino)-Phenol

Abstract

A spectrophotometric study of the Pd(II) complex of a reagent 2-(5-Bromo-2-Pyridylazo)-5-(diethylamino)-Phenol (5-Br-PADAP) is presented. A violet complex is formed at pH 3.53, and shows maximal absorbance at 585 nm with molar absorptivity of 3.86 × 10⁴ 1. mol^?1 cm^?1. Beer's law is obeyed up to 50 μ of Pd(II). The method offers the advantages of simplicity, high precision, requires no extraction and is very selective, where 5.0 mg Pt(VI) and 0.3 mg Au(III) ions do not interfere.     

Extraction—spectrophotometric determination of copper(II) with 4-(2-pyridylazo)resorcinol and a long-chain quaternary ammonium salt

A simple and highly sensitive extraction—spectrophotometric determination of copper (II) is described. The ion-associate formed between the copper(II)—4-(2-pyridylazo)-resorcinol (PAR) anion and tetradecyldimethylbenzylammonium chloride (TDBA) is extracted with chloroform at pH 9.7. The absorption maximum of the extracted species occurs at 510 nm, the molar absorptivity being 8.05 (± 0.07) × 10⁴ l mol^-1 cm^-1. Beer's Law is obeyed in the concentration range 0.1–0.5 μg Cu ml^-1. The composition of the ion-associate is estimated to be [Cu(PAR)₂(TDBA)₂]. The conditional extraction constant is log K'_ex ≈ 8. The interference of some cations and anions is studied. The method is suitable for analysis of waters.     

Spectrophotometric Determination of Palladium(II) with n-Hydroxy-N,N-Diphenylbenzamidine and 1 -(2-Pyridylazo)-2-Naphthol

A spectrophotometric method to determine palladium(II) at trace levels is based on the extraction of palladium(II) as a binary complex with N-hydroxy-N,N′-diphenylbenzamidine (HDPBA) in chloroform at pH 5.0 ± 0.2. The complex shows maximum absorbance at 400 nm with molar absorptivity 6.4 × 10³ L mol^?1 cm^?1. The sensitivity of the Pd(II)-HDPBA complex was enhanced by the addition of l-(2-pyridylazo)-2-naphthol (PAN). The green coloured complex shows maximum absorbance at 620 nm with molar absorptivity 1.58 × 10⁴ L mol^?1 cm^?1. Sandell's sensitivity and the detection limit of the method are 0.0067 μg cm^?2and 0.1 μg Pd(II) mL^?1, respectively. Most common metal ions associated with palladium metal do not interfere. The effects of various analytical parameters on the extraction of the metal are discussed.     

Spektralphotometrische Bestimmung von Wismut(III) mit 4-(2-Pyridylazo)-resorcin (PAR)

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铁(Ⅲ)-4-(2-吡啶偶氮)间苯二酚络合物光化学还原反应的研究

在弱酸性溶液中,Fe3 -PAR络合物可发生光化学还原反应生成Fe2 -PAR络合物。研究了溶液酸度、光强度、有机酸、PAR溶液浓度对Fe3 -PAR络合物光化学还原反应的影响,并对反应机理作了初步探讨。在pH4.5HAc-NaAc缓冲溶液中,PAR浓度为1.8×10?4mol/L,125W高压汞灯照射15min,Fe3 -PAR络合物的光化学还原反应趋于完全。Fe2 浓度在0.12～3.2mg/L范围内符合比尔定律;检出限为0.025mg/L。     

M?glichkeiten einer extraktiv-photometrischen Palladiumbestimmung mit 4-(2-Pyridylazo)-resorein

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Spektrophotometrische Untersuchung Der Wechselwirkung Zwischen Rh(III) und 4-(2-Pyridylazo)-Resorzin

Abstract

A detailed investigation has been made of Che pH versus light absorption curves of solutions of PAR and Rh(III) in various concentrations. It has been shown, that depending on tile acidity of the solution, two different substances will be formed; the optimal conditions of the formation of each substance has been found. The molar absorptivities have been determined and the equilibrium and stability constants of the formed substances have been computed from the absorbance versus pH curves.     

Selective Determination of Trace Mercury (II) after Preconcentration with 4-(2-Pyridylazo)-Resorcinol-Modified Nanometer-Sized SiO2 Particles from Sample Solutions

A rapid, selective method that utilize 4-(2-Pyridylazo)-resorcinol (PAR)-modified nanometer SiO₂ (nanometer SiO₂–PAR) as a new solid-phase extractant for preconcentration of trace mercury (II) has been developed. The adsorption property of nanometer SiO₂–PAR for metal ions was studied by selectively extracting different metal ions from aqueous solutions. The results revealed an excellent affinity of the nanometer SiO₂–PAR for mercury (II) in presence of interfering metal ions at pH 4. The main parameters of solid-phase extraction such as shaking time, elution and sample dilution effect were studied. The extractant shows rapid kinetic sorption, and the adsorption equilibrium of mercury (II) on nanometer SiO₂–PAR was achieved in less than 2 min. The adsorbed mercury (II) was easily eluted by 4 mL of 6 mol L⁻¹ HCl. The maximum preconcentration factor was 50. The maximum static adsorption capacity was 276 μmol g⁻¹ at pH 4. The detection limit (3σ) was 0.43 μg L⁻¹ for cold vapor atomic absorption spectrometry (CVAAS), and the relative standard deviation of the eight replicate determinations was 2.4% for the determination of 2.0 μg of Hg(II) in 100 mL water sample. The method was applied to the determination of trace mercury (II) in sample solutions with satisfactory results.     

Effect of Surfactants on the Immobilization of 4-(2-Pyridylazo)resorcinol on Silochroms

The effect of cationic surfactants (cetyltrimethylammonium bromide, cetylpyridinium bromide, and tetrabutylammonium perchlorate) and a nonionic surfactant (OP-7) on the conditions of the immobilization of 4-(2-pyridylazo)resorcinol (PAR) on three types of silica gel (Silochrom S-120 (200–350 m), Silochrom S-120 (315–500 m), and Silochrom S-80 (200–350 m)) was studied. It was found that OP-7 does not affect the adsorption of surfactants. The effect of cationic surfactants increases in the order tetrabutylammonium perchlorate < cetyltrimethylammonium bromide < cetylpyridinium bromide. The adsorption activity of silica gels increases in the order Silochrom S-120 (315–500 m) < Silochrom S-80 (200–350 m) < Silochrom S-120 (200–350 m). Cetylpyridinium bromide provides full immobilization of PAR on silica gel Silochrom S-120 (200–350 m) in the pH range 2–9.