Simultaneous determination of zinc and copper(II) with 1-(2-pyridylazo)2-naphthol in micellar media by spectrophotometric H-point standard addition method

The H-point standard addition method (HPSAM) was applied to handling spectrophotometric data for simultaneous determination of Zn²⁺ and Cu²⁺ or selective determination of Zn²⁺ in the presence of Cu²⁺. The ligand 1-(2-pyridylazo)2-naphthol (PAN) and its metal complexes (Zn-PAN and Cu(II)-PAN) were made water-soluble by the neutral surfactant Triton X-100, and therefore, no extraction with organic solvents was required. The method is based on the difference in absorbance of formed complexes between Zn²⁺ and PAN, at two different wavelengths at pH = 9.2. The formation of both the complexes was complete within five minutes. Zn²⁺ can be determined in the range of 0.2–25 μg/mL with satisfactory accuracy and precision in the presence of excess of Cu²⁺ and most other metal ions. Interference effects of common anions and cations were studied. Under working conditions, the proposed method was successfully applied to the simultaneous determination of Zn²⁺ and Cu²⁺ in several real and synthetic mixtures with different concentration ratio of Zn²⁺ and Cu²⁺. The text was submitted by the authors in English.     

H-point standard addition method for simultaneous spectrophotometric determination of Co(II) and Ni(II) by 1-(2-pyridylazo)2-naphthol in micellar media

A very simple and selective spectrophotometric method for simultaneous determination of Co(II) and Ni(II) by 1-(2-pyridylazo) 2-naphthol (PAN), in micellar media, using H-point standard addition method (HPSAM) is described. The ligand and its metal complexes (Co(II)-PAN and Ni(II)-PAN) were made water-soluble by the neutral surfactant Triton X-100, and therefore, no extraction with organic solvents was required. Formation of both the complexes was complete within 10 min at pH 9 (adjusted by ammonia buffer). The linear range was 0.10-2.00 microg ml(-1) for Co(II) and 0.05-1.50 microg ml(-1) for Ni(II). The relative standard deviation (R.S.D.) for the simultaneous determination of 0.50 microg ml(-1) each of Co(II) and Ni(II) was 2.32 and 3.13%, respectively. Interference effects of common anions and cations were studied and the method was applied to simultaneous determination of Co(II) and Ni(II) in alloy samples. The method was compared with derivative spectrophotometric method.     

Zero-crossing second derivative spectrophotometry for simultaneous determination of palladium and nickel using 1-(2-pyridylazo)-2-naphthol in mixed micellar solutions

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous determination of nickel and palladium at trace levels. PAN complexes of nickel and palladium in the pH 1.98 form red and green colored complexes, respectively, which are soluble in aqueous 4:1 Triton X-100 to sodium dodecylsulfate (SDS) micellar media with total detergent concentration of 3.2%. Under optimum conditions, calibration graphs for the simultaneous determination by second derivative spectrophotometry were obtained. Zero crossing second derivative spectrophotometry at 668 and 572 nm, respectively for palladium and nickel was used for the simultaneous determination. The method is able to determine palladium to nickel ratio 70:1 to 1:6 (Wt/Wt), accurately. Accuracy and reproducibility of the determination method on the known various amounts of palladium and nickel in their binary mixtures were tested. Effects of diverse ions on the determination of palladium and nickel to investigate selectivity of the method also were studied.     

Indirect simultaneous kinetic determination of semicarbazide and hydrazine in micellar media by H-point standard addition method

H-point standard addition method (HPSAM) is suggested as a simple and selective method for the determination of semicarbazide and hydrazine. The reduction of Cu²⁺ to Cu⁺ by semicarbazide and hydrazine in the presence of neocuproine (Nc) and the subsequent complex formation between Cu⁺ and Nc produced a sensitive spectrophotometric method for indirect determination of semicarbazide and hydrazine. The difference in the rate of reduction of Cu²⁺ with semicarbazide and hydrazine in cationic micellar media is the basis of this method. Semicarbazide can be determined in the range of 0.5-3.75 μg ml⁻¹ with satisfactory accuracy and precision in the presence of excess hydrazine. The proposed method was successfully applied to the simultaneous determination of semicarbazide (0.5-3.75 μg ml⁻¹) and hydrazine (0.5-5 μg ml⁻¹) and also to the selective determination of semicarbazide in the presence of hydrazine in several synthetic mixtures containing different concentration ratios of semicarbazide and hydrazine.     

Simultaneous kinetic-spectrophotometric determination of hydrazine and acetylhydrazine in micellar media using the H-point standard addition method.

The H-point standard addition method (HPSAM), based on a spectrophotometric measurement for the simultaneous determination of hydrazine and acetylhydrazine, is described. This method is based on the difference between the rates of their reactions with N,N-dimethylaminobenzaldehyde (DAB) in the presence of sodium dodecyl sulfate (SDS) in acidic media. The results showed that hydrazine and acetylhydrazine could be determined simultaneously in the range of 0.020 - 0.70 and 0.20 - 5.0 mg L(-1), respectively. Under the working conditions, the proposed method was successfully applied to the simultaneous determination of hydrazine and acetylhydrazine in several synthetic mixtures and plasma and water samples.     

Second and first-derivative spectrophotometry for efficient simultaneous and individual determination of palladium and cobalt using 1-(2-pyridylazo)-2-naphthol in sodium dodecylsulfate micellar media.

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous and individual determination of palladium and cobalt at trace levels. PAN complexes of palladium and cobalt at neutral pH form green-color neutral complexes, which are soluble in aqueous SDS micellar media. Under optimum conditions, calibration graphs for individual determinations by zero and first-derivative spectrophotometry, and also for simultaneous determinations by second-derivative spectrophotometry were obtained. A zero-crossing method using second-derivative spectrophotometry at 628 or 578 and 614 nm, respectively, for cobalt and palladium was used for simultaneous determinations. The method is able to determine the cobalt-to-palladium ratio, 5:1 to 1:10 (Wt/Wt), accurately. The accuracy and reproducibility of the determination method for various known amounts of cobalt and palladium in their binary mixtures were tested. The effects of diverse ions on the determination of cobalt and palladium to investigate the selectivity of the method were also studied. The recommended procedures were applied to a synthetic binary alloy, cobalt in vitamin B12 and B-complex ampoules, a Co2O3-Co3O4 laboratorial chemical mixture, some synthetic cobalt-alloy samples, a Pd-charcoal catalyst, and some synthetic palladium alloys.     

H-point standard addition method for simultaneous determination of Fe(II), Co(II) and Cu(II) in micellar media with simultaneous addition of three analytes

H-point standard addition method, HPSAM, with simultaneous addition of three analytes is proposed for the resolution of ternary mixtures. It is a modification of the previously described H-point standard addition method that permits the resolution of three species from a unique calibration set by making the simultaneous addition of the three analytes. The method calculates the analyte concentration from spectral data at two wavelengths where the two species selected as interferents present the same absorbance relationship. These wavelength pairs are easily found, and can be selected to give the most precise results. Diethyldithiocarbomate (DDC) in a cationic micellar solution of cetyltrimethylammonium bromide (CTAB) was used for determination of Fe(II), Co(II) and Cu(II) at pH 5.50. The results showed that simultaneous determination of Fe(II), Co(II) and Cu(II) could be preformed in the range of 0.0–6.0, 0.0–8.0 and 0.0–12.0 μg ml⁻¹, respectively. The proposed method was successfully applied to the simultaneous determination of Fe(II), Co(II) and Cu(II) in several synthetic mixtures containing different concentration of Fe(II), Co(II) and Cu(II).     

Simultaneous determination of cobalt and palladium in micellar media using H-point standard addition method and partial least square regression

A simple, sensitive and selective spectrophotometric method for the simultaneous determination of Co(II) and Pd(II) using partial least square (PLS) calibration and H-point standard addition method is described. The method is based on the complex formation of Co(II) and Pd(II) with 4-(2-pyridylazo) resorcinol (PAR) in acidic media and in the presence of sodium dodecyl sulfate (SDS) as a micellizing agent. Acidic media and the presence of a micellar system improve selectivity and sensitivity, respectively. By applying PLS calibration, Co(II) and Pd(II) can be determined in the range of 0.20-2.0 and 0.40-4.0 microg ml(-1), respectively. The relative errors of prediction for the determination of Co(II) and Pd(II) in the 10 prediction samples were 1.69 and 1.72%, respectively. The results of applying H-point standard addition method show that Co(II) and Pd(II) can be determined simultaneously with concentration ratio of Co(II) to Pd(II) varying between 7:1 and 1:8 in the mixed samples. Both proposed methods (PLS and HPSAM) were applied to the determination of Co(II) and Pd(II) in several alloy solutions with satisfactory results.     

H-point standard addition method for simultaneous determination of cobalt(II) and zinc(II) ions

The H-point standard addition method (HPSAM) was applied to the simultaneous determination of zinc(II) and cobalt(II). This method is based on the difference in the absorbance of methylthymol blue complexes of Zn(II) and Co(II) at pH 6 buffered solution in different wavelength pairs. The results showed that Zn(II) and Co(II) can be determined simultaneously with concentration ratios of 20:1 and 1:7.5. Under working conditions, the proposed method was successfully applied to the simultaneous determination of zinc and cobalt in synthetic and real samples.     

H-point standard addition method for simultaneous determination of cobalt(II) and zinc(II) ions

The H-point standard addition method (HPSAM) was applied to the simultaneous determination of zinc(II) and cobalt(II). This method is based on the difference in the absorbance of methylthymol blue complexes of Zn(II) and Co(II) at pH 6 using different wavelength pairs. The results showed that Zn(II) and Co(II) can be determined simultaneously with concentration ratios of 20:1 and 1:7.5. Under working conditions, the proposed method was successfully applied to the simultaneous determination of zinc and cobalt in synthetic, drinking water and vitamin samples.     

Spectrophotometric determination of uranium with 1-(2-pyridylazo)-2-naphthol

1-(2-Pyridylazo)-2-naphthol (PAN) rcacts with uranium to form a deep red precipitate in ammoniacal solutions, this can be extracted with chloroform if sodium chloride or sulfate is added and it has a maximum absorption at 560 mμ The color is stable and follows Beer's law. Trace amounts of uranium may be determined in the presence of many metals without prior separation if strong complexing agents, such) as EDTA or cyanide, are added     

Colorimetric determination of zirconium with 1-(2-pyridylazo)-2-naphthol

A method is described for the determination of as little as 50 ppm of zirconium in uranium-fission element alloys and zinc magnesium-uranium-fission element alloys. Zirconium is extracted from a nitric acid-aluminium nitrate medium with dibutyl phosphate in toluene. The uranium co-extracted with the zirconium is removed by scrubbing with hydrochloric acid-ammonium thiocyanate solution. A portion of the organic phase is mixed with pyridine-toluene solution of 1-(2-pyridylazo)-2-naphthol to develop the colour.     

Mass spectrometric investigation of copper chelates with 1-(2-pyridylazo)-2-naphthol

The mass spectra of copper chelates of 1-(2-pyridylazo)-2-naphthol, HX, prepared by different methods, are discussed. Peaks due to Cu(2)X(2)(+), CuX(2)(+) and CuXCl(+) have been positively identified and all copper-containing species have the expected isotopic ratios. The significance of probe temperature and impurities are discussed and it is concluded that the spectra are more in accordance with the known chemical facts than those reported earlier by Betteridge and John.     

Spectrophotometric determination of hafnium(IV) with 1-(2-pyridylazo)-2-naphthol

Summary The red complex formed between hafnium(IV) and 1-(2-pyridylazo)-2-naphthol (1 2) at pH 4.0 is used for Spectrophotometric determination of hafnium., the absorbance being measured at 545 nm. Beer's law is obeyed for hafnium concentration of 0.2 to 3.6g per ml. Molar absorptivity is 3.86×10⁴ and Sandell sensitivity is 0.0046g per cm². Hafnium has been determined in the presence of 6-fold amounts of zirconium. The relative standard deviation is ± 1.0%.

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Zusammenfassung Der rote, bei pH 4,0 sich bildende Komplex mit 1-(2-Pyridylazo)-2-naphthol (1 2) dient zur Bestimmung von Hafnium (IV). Seine Extinktion wird bei 545 nm gemessen. Zwischen 0,2 und 3,6g Hf/ml ist das Beersche Gesetz gültig. Hafnium läßt sich in Gegenwart der sechsfachen Menge Zirkonium bestimmen. Die relative Standardabweichung beträgt ± 1,0%.

     

Spectrophotometric determination of cobalt with 1-(2-pyridylazo)-2-naphthol and surfactants

A simple and highly selective spectrophotometric method for the determination of cobalt based upon the rapid reaction with PAN in the presence of surfactants and minute amounts of ammonium persulphate at pH 5.0 is described. The cobalt(III) chelate is made water-soluble by a neutral surfactant. Triton X-100, combined with sodium dodecylbenzene sulphonate (DBS). Iron(III), bismuth, tin(IV) and aluminium are masked with oxalate or citrate. Iron(II) must be absent. The other metal-PAN chelates, except that of nickel, are readily decomposed by EDTA. Up to 150 microg of nickel does not interfere. When larger amounts up to 625 microg are present, the absorbance can be corrected by measurements at two wavelengths. In a strongly acid medium (below pH 0.5) the nickel and other metal chelates are completely and instantaneously decomposed, while the cobalt(III) chelate remains unchanged. When, in place of EDTA, several ml of 6M hydrochloric acid are added after the colour development, nickel in quantities up to 1250 microg can be tolerated. A several hundredfold excess of zinc and manganese does not interfere. At 620 nm Beer's law is obeyed over the cobalt concentration range 0.4-3.2 microg/ml. The precision (95% confidence) is +/- 1.0 microg for 100 microg of cobalt. The molar absorptivity is 1.90 x 10(4) l. mole(-1) .cm(-1).     

Spectrophotometric determination of rare earth metals with 1-(2-pyridylazo)-2-naphthol

1-(2-Pyridylazo)-2-naphthol (PAN) reacts very sensitively with rare earth metals to form a deep red precipitate in alkaline solution; this can be extracted with ether, except in the case of lanthanum, cerium and scandium. Absorption maxima occur at 530 and 560 mμ. Traces of rare earth metals may be determined in the presence of many foreign metals.     

A study of the spectrophotometric method for the determination of uranium(VI) in trialkylamine/kerosene extracts using 1-(2-pyridylazo)-2-naphthol

Summary The Spectrophotometric method for the determination of uranium(VI) in trialkylamine extracts using 1-(2-pyridylazo)-2-naphthol (PAN) as a colorimetric reagent has been examined. The Job and Mole Ratio methods suggest that the coloured product is a 11 complex of uranium and PAN. The method can be applied to cover the concentration range 0 to 5 g uranium per litre of extract. Sulphate interference is eliminated in the method by removal with calcium ions before colour development. Interferences from other ions likely to be present in the aqueous liquor appear to arise largely from inhibition of the uranium partition into the amine phase.

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Untersuchung der spektralphotometrischen Uran(VI)-Bestimmung in Trialkylamin/Kerosin-Extrakten mit Hilfe von 1-(2-Pyridylazo)-2-naphthol

Zusammenfassung Das Verfahren, bei dem ein Uran-PAN-Komplex der Zusammensetzung 11 gebildet wird, kann für einen Konzentrationsbereich von 0 bis 5 g U pro l Extrakt eingesetzt werden. Eine Störung durch Sulfat wird durch dessen Entfernung mit Calciumionen vor der Farbentwicklung verhindert. Störungen durch andere Ionen werden hauptsächlich durch Beeinflussung der Uranextraktion hervorgerufen.