Spectrophotometric determination of ruthenium

Zusammenfassung Es wurde festgestellt, daß die Mehrzahl der Amidoxime mit folgenden Ionen reagiert: Hg²⁺, Cu²⁺, Fe³⁺, Co²⁺, UO₂ ²⁺, Cd²⁺, Ag^+;, Pb²⁺, Pd²⁺, Ni²⁺. Von den Malonsäure-bis-amidoximen wurden hergestellt die Silber-, Blei-, Cadmium-, Kupfer- und zwei Quecksilbersalze, von den Amidoximen der Nicotin- und Isonicotinsäure Palladium-, Kupfer-, Cadmium- und Bleisalze. Die Salzbildungsfähigkeit der Amidoximgruppe ist vom Radikal, von den Substituenten an der Amidgruppe und vom Reagens-medium abhängig. Die braunrote Färbung mit Fe³⁺-Ionen ist für alle Amidoxime typisch, diese Reaktion kann zum Nachweis der am Amidstickstoff nichtsubstituierten Amidoxime angewandt werden.IX. Mitteilung: Collect. czechoslov. chem. Commun. 24, 1720 (1959). — X. Mitteilung: Collect. czechoslov. chem. Commun. (im Druck).     

Spectrophotometric determination of ruthenium(III) using diphenylcarbazone

Summary The purple violet ruthenium(III)-diphenylcarbazone complex which is formed at p _h 5–7, and has an absorption maximum at 530 nm with molar absorption coefficient 16.2·10⁴l.cm^–1.mole^–1 is suggested for the estimation of 20–125g ruthenium(III) spectrophotometrically in 30–60% ethanol. The complex is stable over p _h range 3.2–8.4. The limits of interference due to foreign ions have been studied.

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Zusammenfassung Der bei p _h 5 bis7 entstehende Ruthenium(III)-Diphenylcarbazon-Komplex hat ein Absorptionsmaximum bei 530 nm und einen Absorptionskoeffizienten von 16,2·10⁴ l.cm^–1.Mol^–1. Die spektrophotometrische Bestimmung von 20 bis 125g Ruthenium(III) in 30 bis 60%igem Äthanol mit Hilfe dieses zwischen p _h 3,2 und 8,4 beständigen Komplexes wurde vorgeschlagen. Die Störung durch Fremdionen wurde geprüft.

     

Spectrophotometric determination of ruthenium and osmium

The optimum conditions for preparation of stable solutions of ruthenate and osmate, after alkaline fusion of ruthenium(IV) compounds, ruthenium metal and osmium metal in a silver crucible, have been determined. The molar absorptivities of ruthenate and osmate are 1.74 × 10³ 1. mole⁻¹.cm⁻¹ at 465 nm (Ru) and 2.75 × 10³ 1.mole⁻¹.cm⁻¹ at 340 nm (Os) in 2M sodium hydroxide. A differential spectrophotometric method has been developed for determination of ruthenium in ruthenium dioxide, lead ruthenite and bismuth pyroruthenate. Simultaneous spectrophotometric determination is proposed for ruthenium and osmium. The other platinum metals interfere seriously only when present in> 1:1 w/w ratio to Ru.     

Spectrophotometric determination of trace aqueous sulfate using barium-beryllon II

Summary The dibarium salt of beryllon II, 2-(8-hydroxy-3,6-disulfo-1-naphthylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid is the basis of a sensitive (LOD 0.14 ppm) convenient Spectrophotometric procedure for determining trace sulfate through liberation of the dye in a 80% 2-propanol medium at an apparent pH of 4.3. The interferences are negligible and good agreement with ion Chromatographie results are demonstrated for environmental samples.     

Spectrophotometric determination of ruthenium with 8-quinolinol

A spectrophotometric method is described for the determination of 2–80 μg of ruthenium. The method involves oxidation of ruthenium to ruthenate, addition of 8-quinolinol, adjustment of the pH to 4–6.5, digestion of the complex formed at 85° for 30 min, extraction with chloroform, and measurement of absorbance at 430 nm. Almost all other metals and excess of reagent are removed by washing the extract. About 98 % of ¹⁰⁶Ru tracer was recovered.     

Spectrophotometric determination of ruthenium with diphenylthiovioluric acid

Diphenylthiovioluric acid (DPHTVA) reacts with ruthenium(III) to form a complex which has an absorbance maximum at 520 nm. Effects of pH, heating time, buffer and reagent have been studied. DPHTVA has been found to be a sensitive reagent for ruthenium(III) (sensitivity = 0.0044 μg Ru/cm² for log I₀/I = 0.001), and has been made selective by the use of masking agents. The composition of the complex as revealed by different methods is 1:2 (ruthenium:DPHTVA).     

Reaction of 2,6-diamino-4-hydroxypyrimidine with hydrogen peroxide

Conclusions Ammelide and 3-hydroxy-5-amino-s-triazine-1-carboxylic acid are formed respectively by the reaction of 2,6-diamino-4-hydroxypyrimidine with perhydrol and with alkaline H₂O₂ solution.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 3, pp. 655–657, March, 1973.     

Spectrophotometric determination of ruthenium with 3,4-diaminobenzoic acid

Ruthenium(III) chloride and 3,4-diaminobenzoic acid, in aqueous solution at pH 4.0-4.5, react slowly at room temperature, but more rapidly when the mixture is heated, giving solutions that go through colour transitions from amber to purple-red; maximum absorbance of fully developed solutions occurs at 550 nm. The effects of heating temperature and time, pH, reagent concentration, and other variables have been studied. The system conforms to Beer's law; optimum concentration range, for measurement in 10-mm cells, is about 0.5-2 ppm of ruthenium. Interference from foreign ions, especially other platinum elements, is avoided by a distillation separation of ruthenium. The spectrophotometric mole-ratio and continuous-variation methods indicated the presence of complexes of 1:2 and 1:3 ruthenium-to-reagent stoichiometry. Elemental analysis of solid products isolated from solution confirmed the 1:2 reaction ratio. Several other o-diamines gave similar coloured solutions and reaction stoichiometry.     

One-pot syntheses of 6-mercaptopurines (6MP) from 4,5-diamino-6-chloro-pyrimidines

A one-pot synthesis of 6-mercaptopurines from 4,5-diamino-6-chloro-pyrimidine, an aldehyde and elemental sulfur is presented. The key advantage of this procedure is that it utilizes the in situ generated H₂S to convert the chloro to a mercapto group.     

Spectrophotometric determination of tantalum with 4,5-dibromo-o-nitrophenylfluorone

Micro amounts of tantalum can be determined directly by spectrophotometry with 4,5-dibromo-o-nitrophenylfluorone, citric acid, hydrogen peroxide and Triton X-100 in 0.5–5 mol l^?1 sulphuric acid. The apparent molar absorptivity of tantalum at 530 nm is 1.84 × 10⁵ l mol^?1 cm^?1. Beer's law is obeyed for 0–10 μg of tantalum in 25 ml of solution at 530 nm and a large amount of niobium and most foreign ions can be tolerated. Results obtained by applying the proposed method to niobium oxide, ferroniobium, nickel-base alloy and a mineral are satisfactory. The synthesis of the complexing agent is described.     

Spectrophotometric studies of neomycin-copper complex and determination of neomycin sulfate using an auxiliary ligand

Spectrophotometric investigation of the deep blue colored, water-soluble complex of

1. Stability constant and free energy of formation of Cu-NMS complex at 30 ± 1 °C

     

16.

Spectrophotometric studies of kanamycin-copper complex and determination of kanamycin sulfate using an auxiliary ligand     

《Journal of Inorganic and Nuclear Chemistry》1978,40(9):1715-1718

Spectrophotometric investigation of the deep blue, water soluble complex of kanamycin sulphate with bivalent copper in the alkaline medium has been carried out using sodium potassium tartrate as an auxiliary ligand. The complex is found to absorb maximum at 580 nm and pH 8.0. Job's method and mole ratio method have shown the composition of the complex to be 1:2. Conditional stability constant has been determined by Mukherji and Dey method and Raghav Rao's method and the log K_s value by these two methods is found to be 6.69 and 7.59 respectively. The colour of the complex obeys Beer's law within the range 0.3 – 3.0 mg of kanamycin sulphate/ml of the solution. The technique is found to be suitable for the quantitative estimation of kanamycin sulphate.     

17.

Spectrophotometric determination of ruthenium after extraction of perruthenate with benzyltributylammonium chloride     

M. S. El-Shahawi  A. Z. Abu Zuhri  S. M. Al-Daheri 《Fresenius' Journal of Analytical Chemistry》1994,350(12):674-677

A simple and convenient extractive spectrophotometric method for the determination of ruthenium has been developed. It is based on the oxidation of the different ruthenium (II, III or IV) species to perruthenate with potassium periodate at pH 7.8. The perruthenate is then extracted with benzyltributylammonium chloride in chloroform followed by direct spectrophotometric measurements at 342 and 380 nm. The optimum concentration range was found to be 0.1–5 mg l^–1, the standard deviation ±2.1%. The method has been successfully applied to the determination of ruthenium in organoruthenium compounds.     

18.

Reaction of 4,5-diamino-1,6-dihydropyrimidin-6-ones with two equivalents of chalcones     

Braulio Insuasty  Monica Ramos  Rodolfo Moreno  Jairo Quiroga  Adolfo Snchez  Manuel Nogueras  Norbert Hanold  Herbert Meier 《Journal of heterocyclic chemistry》1995,32(4):1229-1233

The reaction of 4,5-diamino-1,6-dihydropyrimidin-6-ones 1 with two equivalents of the chalcones 2 leads in an acidic medium to the formation of the 2,3,6,7-tetrahydro-1H-pyrimido[4,5-b][1,4]diazepin-6-one derivatives 3a-d . The structure elucidation of the products is based on nmr measurements and an X-ray diffraction.     

19.

Spectrophotometric determination of carbon monoxide with ruthenium(II) octaethylporphyrin     

Corsini A  Chan A  Mehdi H 《Talanta》1984,31(1):33-38

A novel spectrophotometric method for the estimation of carbon monoxide at levels from 2 to 250 ppm is presented. The method is empirical and based on formation of a carbonyl complex of ruthenium(II) octaethylporphyrin and measurement of the difference in absorbance at 393.5 nm between this complex and the porphyrin reagent. Oxygen and nitrogen do not interfere and up to 300 ppm of sulphur dioxide and about 1500 ppm of carbon dioxide can be tolerated in determination of carbon monoxide at the 4 and 10 ppm levels. Hydrogen sulphide interferes and must be removed before the determination. The method has been tested over the range 2-45 ppm of carbon monoxide with 16 synthetic and 2 commercial standard air samples. The average error was +/- 3%. Application to urban-air samples and car-exhaust gases yielded acceptable results. The main disadvantages are the tedious preparation of the initial ruthenium(III)-porphyrin compound and the decomposition of the reagent in the presence of hydrazine.     

20.

Spectrophotometric determination of 6-aminopenicillanic acid using bromophenol blue and bromothymol blue     

Alaa S. Amin  Yousry M. Issa 《Mikrochimica acta》1995,117(3-4):187-194

Two simple, selective and sensitive spectrophotometric methods are described for the determination of 6-aminopenicillanic acid (6-APA). The methods are based on the reaction of 6-APA with either bromophenol blue (BPB) or bromothymol blue (BTB), to give orange-red and green species, respectively. The coloured products are quantified spectrophotometrically at 625 and 616 nm for BPB and BTB, respectively. The optimization of the different experimental conditions is described. No interferences from different -lactams and common degradation products were observed in the determination of 6-APA using BTB, while flucloxacillin, dicloxacillin, adrenaline, vitamin C, urea and common degradation products in any percentage interfere on using BPB only. The BTB method was better than the BPB method, because of its wider range of determination (0.4–20 g ml^–1 vs. 0.4–7.2 g ml^–1 on using BPB), higher molar absorptivity and Sandell sensitivity (3.27 × 10³l mol^–1 cm^–1 and 0.099 g cm^–2 vs. 2.82 × 10³lmol^–1 cm^–1 and 0.115 g cm^–2), greater stability (3 and 10 days on using BTB and BPB, respectively) and better selectivity. The results were compared with those given by the Official United States Pharmacopeial XXI method.     

Method	$\text{log}\text{K}{}_{\mathrm{s}}$	ΔF (Kcal/mole)
Mukherji and Dey (4)	4.11	?5.70
Subhrana and Raghavrao (6)	4.80	?6.66

Spectrophotometric studies of kanamycin-copper complex and determination of kanamycin sulfate using an auxiliary ligand

Spectrophotometric investigation of the deep blue, water soluble complex of kanamycin sulphate with bivalent copper in the alkaline medium has been carried out using sodium potassium tartrate as an auxiliary ligand. The complex is found to absorb maximum at 580 nm and pH 8.0. Job's method and mole ratio method have shown the composition of the complex to be 1:2. Conditional stability constant has been determined by Mukherji and Dey method and Raghav Rao's method and the log K_s value by these two methods is found to be 6.69 and 7.59 respectively. The colour of the complex obeys Beer's law within the range 0.3 – 3.0 mg of kanamycin sulphate/ml of the solution. The technique is found to be suitable for the quantitative estimation of kanamycin sulphate.     

Spectrophotometric determination of ruthenium after extraction of perruthenate with benzyltributylammonium chloride

A simple and convenient extractive spectrophotometric method for the determination of ruthenium has been developed. It is based on the oxidation of the different ruthenium (II, III or IV) species to perruthenate with potassium periodate at pH 7.8. The perruthenate is then extracted with benzyltributylammonium chloride in chloroform followed by direct spectrophotometric measurements at 342 and 380 nm. The optimum concentration range was found to be 0.1–5 mg l^–1, the standard deviation ±2.1%. The method has been successfully applied to the determination of ruthenium in organoruthenium compounds.     

Reaction of 4,5-diamino-1,6-dihydropyrimidin-6-ones with two equivalents of chalcones

The reaction of 4,5-diamino-1,6-dihydropyrimidin-6-ones 1 with two equivalents of the chalcones 2 leads in an acidic medium to the formation of the 2,3,6,7-tetrahydro-1H-pyrimido[4,5-b][1,4]diazepin-6-one derivatives 3a-d . The structure elucidation of the products is based on nmr measurements and an X-ray diffraction.     

Spectrophotometric determination of carbon monoxide with ruthenium(II) octaethylporphyrin

A novel spectrophotometric method for the estimation of carbon monoxide at levels from 2 to 250 ppm is presented. The method is empirical and based on formation of a carbonyl complex of ruthenium(II) octaethylporphyrin and measurement of the difference in absorbance at 393.5 nm between this complex and the porphyrin reagent. Oxygen and nitrogen do not interfere and up to 300 ppm of sulphur dioxide and about 1500 ppm of carbon dioxide can be tolerated in determination of carbon monoxide at the 4 and 10 ppm levels. Hydrogen sulphide interferes and must be removed before the determination. The method has been tested over the range 2-45 ppm of carbon monoxide with 16 synthetic and 2 commercial standard air samples. The average error was +/- 3%. Application to urban-air samples and car-exhaust gases yielded acceptable results. The main disadvantages are the tedious preparation of the initial ruthenium(III)-porphyrin compound and the decomposition of the reagent in the presence of hydrazine.     

Spectrophotometric determination of 6-aminopenicillanic acid using bromophenol blue and bromothymol blue

Two simple, selective and sensitive spectrophotometric methods are described for the determination of 6-aminopenicillanic acid (6-APA). The methods are based on the reaction of 6-APA with either bromophenol blue (BPB) or bromothymol blue (BTB), to give orange-red and green species, respectively. The coloured products are quantified spectrophotometrically at 625 and 616 nm for BPB and BTB, respectively. The optimization of the different experimental conditions is described. No interferences from different -lactams and common degradation products were observed in the determination of 6-APA using BTB, while flucloxacillin, dicloxacillin, adrenaline, vitamin C, urea and common degradation products in any percentage interfere on using BPB only. The BTB method was better than the BPB method, because of its wider range of determination (0.4–20 g ml^–1 vs. 0.4–7.2 g ml^–1 on using BPB), higher molar absorptivity and Sandell sensitivity (3.27 × 10³l mol^–1 cm^–1 and 0.099 g cm^–2 vs. 2.82 × 10³lmol^–1 cm^–1 and 0.115 g cm^–2), greater stability (3 and 10 days on using BTB and BPB, respectively) and better selectivity. The results were compared with those given by the Official United States Pharmacopeial XXI method.