Spectrophotometric determination of microamounts of yttrium with 1-amino-4-hydroxyanthraquinone

Summary 1-amino-4-hydroxyanthraquinone (AMHA) is proposed as a spectrophotometric reagent for the determination of yttrium. The solution equilibria ofAMHA complexes with Y(III) have been studied spectrophotometrically in 50% (v/v) ethanol at 25°C and an ionic strength ofI=0.1 mol·dm^–3 (NaClO₄). The complexation reactions were investigated and characterized using graphical logarithmic analysis of the absorbance graphs. The composition, molar absorptivities, and stability constants of the chelates ofAMHA with Y(III) have been determined spectrophotometrically. A simple, rapid, selective, and sensitive method for the spectrophotometric determination of microamounts of Y(III) is developed based on the formation of the violet YLH⁺ complex with _max=580nm atpH 6.2(=0.98×10⁴l·mol^–1·cm^–1). Interferences and their elimination have been studied. Many foreign ions are tolerated in considerable amounts; 45–60 fold amounts of rare earths do not interfere with the determination of yttrium. In the determination of yttrium in synthetic polymetallic samples the relative error and relative standard deviation of the method were found to be better than 1 and 0.5%, respectively.

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Spektrophotometrische Bestimmung von Mikromengen Yttrium mit 1-Amino-4-hydroxyanthrachinon

Zusammenfassung 1-Amino-4-hydroxyanthrachinon (AMHA) wird als spektrophotometrisches Reagens zur Bestimmung von Yttrium vorgeschlagen. Die Gleichgewichte von Komplexen ausAMHA und Y(III) in Lösung wurden in 50% (v/v) Ethanol bei 25°C und einer lonenstärke vonI=0.1M (NaClO₄) untersucht. Die Komplexierungsreaktionen wurden durch graphische logarithmische Analyse der Extinktionskurven charakterisiert. Die Zusammensetzungen, die molaren Extinktionen und die Stabilitätskonstanten der Chelate vonAMHA mit Y(III) wurden spektrophotometrisch bestimmt. Eine einfache, schnelle, selektive und empfindliche Methode zur spektrophotometrischen Bestimmung von Mikromengen Y(III) wurde entwickelt. Sie basiert auf der Bildung des violetten YLH⁺-Komplexes mit _max=580 nm beipH 6.2 (=0.98×10⁴l·mol^–1·cm^–1). Störungen und ihre Beseitigung werden ebenfalls diskutiert. Viele Fremdionen werden in beträchtlichen Mengen toleriert; 45–60 facher Überschuß an Seltenen Erden stört die Bestimmung von Yttrium nicht. Der relative Fehler und die relative Standardabweichung der Methode bei der Bestimmung von Yttrium in synthetischen polymetallischen Proben waren besser als 1 bzw 0.5%.

     

Fluorimetric determination of vanadium based on its reaction with 1-amino-4-hydroxyanthraquinone

A fluorimetric method for the determination of vanadium(V) (0.06–0.36 ppm) is described. The 1-amino-4-hydroxyanthraquinone is oxidized by this ion which yields a product exhibiting an intense yellow fluorescence in acidic solution. The experimental variables and interferences in this determination have been studied.     

Complexation equilibria and spectrophotometric determination of iron(III) with 1-amino-4-hydroxyanthraquinone

The complex equilibria of iron(III) with 1-amino-4-hydroxyanthraquinone (AMHA) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaClO(4)). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance-pH graphs. A simple, rapid, selective and sensitive method for the spectrophotometric determination of trace amounts of Fe(III) is developed based on the formation of Fe(AMHA) complex at pH 2.5 (lambda(max) = 640 nm, epsilon approximately = 2.1 x 10(4) L. mol(-1) . cm(-1)) in the presence of a large number of foreign ions. Interferences caused by palladium(II) was masked by the addition of cyanide ions. The method has been applied to the determination of iron in some synthetic samples and polymetallic iron ores.     

Complexes of some rare earth metals with 1-amino-4-hydroxyanthraquinone

La, Ce(III), Pr, Nd and Sm(III) form very stable reddishviolet 1:1 complexes with 1-amino-4-hydroxyanthraquinone in methanol. The stability constants are very similar.     

Tautomerism of anthraquinones: XI. 1-amino-4-hydroxyanthraquinone

The disperse dye red 2C regarded as 1-amino-4-hydroxy-9,10-anthraquinone is not a 9,10-anthraquinone derivative. It is characterized by a keto-enol and amino-imine tautomerism, and it consists of equilibrium mixtures of tautomers and conformers containing 4-amino-9-hydroxy-1,10-, 9 amino-4-hydroxy-1,10-, 9 amino-10-hydroxy-1,4-anthraquinones, 9 hydroxy-1,10-anthraquinone 10-imine, and also their conformers with a single intramolecular hydrogen bond. The significant differences in the absorption spectra known for this dye originate from the dissimilar isomeric composition of the samples of this dye prepared or purified by various procedures     

Spectrofluorimetric determination of beryllium based on the inclusion complex of 1-amino-4-hydroxyanthraquinone with β-cyclodextrin as ligand

The use of the inclusion complex of 1-amino-4-hydroxyanthraquinone (AHA) in the internal cavity of β-cyclodextrin is compared with AHA alone as a ligand for the spectrofluorimetric determination of beryllium. The organizing ability of the cyclodextrin medium and the protection of the ligand from the micro-environment confers increased sensitivity, selectivity and detection limit, and allows the determination of 10–70 ng ml^?1 beryllium, compared to 60–500 ng ml^?1 in the absence of the cyclodextrin.     

Quantum-chemical and correlation study of deprotonation and complexation of 1-amino-4-hydroxyanthraquinone

Existing views on the deprotonation and complexation of 1-amino-4-hydroxyanthraquinone are wrong. This compound, its anions, and complexes with metals are not individual substances, but they form a dynamic equilibrium mixture of keto-enol (keto-oxide) and amino-imine tautomers. Different samples of the same compound differ by the tautomeric composition, the respective information is contained in their electron absorption spectra. In weak alkaline solutions the deprotonation occurs exclusively at the hydroxy group. Most typical structure of 1-amino-4-hydroxyanthraquinone anions is 1,10-quinoid, its metal complexes have 9,10-and 1,10-quinoid structures. The ground states of molecules are more responsible for the tautomeric transformations than the excited states. Quantum-chemical calculations of tautomeric anthraquinones by semiempirical PPP methods are more reliable than modern ab initio calculations.     

Kinetic-fluorimetric determination of magnesium in micellar medium

A simple method for the kinetic determination of magnesium(II) is described. The method is based on the reaction of 2-fluorenaldehyde 2-pyridylhydrazone with magnesium ion to originate a strong green fluorescence that decreases with time. The reaction is monitored at 520 nm, when excited at 375 nm, and the initial rate method is applied to perform the analytical procedure. Magnesium contents between 0.36 and 1.22 μm ml^?1 can be determined. The method is free from interferences of alkaline earth ions.     

Kinetic-fluorimetric determination of microamounts of cerium(IV) by means of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2,6-disulphonate

Summary A kinetic method for determination of traces of Ce(IV), based on the oxidation of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2, 6-disulphonate is described. The reaction is monitored by means of the fluorescence of the oxidation product ( _ex=525nm, _em=585 nm), and allows determination of 0.02–0.37 ppm Ce(IV). The proposed method has few interferences.

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Kinetisch-fluorimetrische Bestimmung von Mikromengen Cer(IV) mit Natnum-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat

Zusammenfassung Eine kinetische Methode zur Bestimmung von Spuren Cer(IV) mit Hilfe von Natrium-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat wurde beschrieben. Dabei wird ein fluoreszierendes Oxydationsprodukt gebildet, das bei 525 nm angeregt mit einer maximalen Emission bei 585 nm fluoresziert. Die Reaktion ermöglicht die Bestimmung von 0,02–0,37 ppm Cer(IV). Die vorgeschlagene Methode wird nur durch wenige Störungen eingeschränkt.

     

Fluorimetric determination of cerium with paracetamol

A simple, sensitive and selective method for determination of cerium(IV), based on the oxidative reaction between cerium(IV) and paracetamol, has been developed. The fluorescent species is an oxidation product of paracetamol and has excitation and emission maxima at 265 and 360 nm, respectively. The fluorescent intensity of the system is linear over the range 2.0 x 10(-7)-8.0 x 10(-6)M Ce(IV). The method has been applied in the determination of Ce(IV) in synthetic mixtures and ores with good accuracy being achieved.     

Spectrophotometric determination of cerium with sulphanilic acid

In the presence of other rare earths, cerium(IV) can be determined spectrophotometrically by its reaction with sulphanilic acid with which it produces a red colour. Solutions containing 28-210 ppm of cerium absorb at 495 mmicro according to Beer's law. Other rare earths, except neodymium, and many common ions do not interfere. Strong oxidising agents and neodymium in greater than fifty times the concentration of cerium interfere with this method. The precision depends on the control of pH and time. Cerium alloys have been analysed by this method and the results are compared with those obtained by another spectrophotometric method.     

Preparation of 1-amino-4-methylpiperazine

The selectivity of the formation of N-di(2-chloroethyl)methylamine in reactions with various chlorinating agents has been investigated and the optimum chlorinating agent has been found. 1-Amino-4-methylpiperazine has been obtained for the first time by the cyclization of N-di(2-chloroethyl)methylamine with aqueous hydrazine. A possible mechanism has been proposed for the cyclization reaction.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1794–1797, December, 2004.     

Tautomerism of the metal complexes with 1-amino-4-hydroxyanthaquinone

Diversity of electronic absorption spectra of the metal complexes with 1-amino-4-hydroxyan-thraquinone is a consequence of the fact that they exist as equilibrium mixtures of tautomers with the isomeric quinoid structure of the ligand. These complexes are characterized by keto-oxide and amino-imine tautomerism, and samples of the complexes differ by composition of the tautomers.     

Gravimetric determination of thorium and cerium with n-benzoylphenylhydroxylamine

Benzoylphenylhydroxylamine has been used for the precipitation of thorium and trivalent cerium; the precipitates are ignited to the corresponding metal dioxide and weighed. Ceric ions are reduced before precipitation. The gravimetric separation of thorium and cerium is effected by precipitation at different pH values.     

双硫腙褪色光度法测定痕量铈

研究了Ce(Ⅳ)在H2SO4介质中和溴化十六烷基吡啶存在下催化H2O2氧化双硫腙的褪色反应及其动力学条件,测定了反应级数和表观活化能,建立了测定痕量铈的新方法。双硫腙的最大吸收波长为450nm,该方法的检出限为1 9×10-9g/mLCe(Ⅳ),线性范围为0～150ng/mLCe(Ⅳ),方法可用于人发中痕量铈的测定。     

Spectrophotometric determination of nickel in vegetable oil with ammonium 2-amino-1-cyclohexene-1-dithiocarboate

The reaction between nickel and ammonium 2-amino-1-cyclohexene-1-dithiocarboate in aqueous acetone medium at pH 3.0-8.0 results in a stable dark red complex. The ratio of reagent to nickel in the complex is 2:1 and the formation constant is 7.38 +/- 0.12 x 10(10). Beer's law is obeyed up to 4 microg/ml nickel at the absorption maximum at 535 nm. The apparent molar absorptivity is 2.8 x 10(4) l.mole(-1). cm(-1), and the detection limit is 10 ng/ml nickel. The method is applied to the determination of nickel in vegetable oil.