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1.
Zusammenfassung Die saure Hydrolyse der Arylazo-Verbindung1 wird beschrieben und interpretiert: Als Zwischenprodukte werden ungeladenes Aryldiazen (Ar–N=N–H) sowie zwitterionisches Aryldiazen (Ar–NH+=N:)und im weiteren Verlauf des Reaktionsgeschehens 1,4-Diaryltetrazenimionen postuliert.
Acid hydrolysis of 2-(4-Chlorophenylazo)-2-(N-carbamidinoureido)-propane
Acid hydrolysis of the arylazo compound1 is described and discussed. As reaction intermediates uncharged aryldiazene (Ar–N=N–H) as well as zwitterionic aryldiazene (Ar–NH+=N:) and subsequently 1.4-diaryltetrazenium ions are postulated.
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2.
A simple, sensitive and selective method for the extraction and trace determination of molybdenum(VI) has been developed; it is based on its reaction with 3-hydroxy-2-(2-thienyl)-4H-chromen-4-one (HTC) in sulphuric acid medium. The 1:2 Mo (VI)-HTC yellow complex is quantitatively extractable into chloroform (max 420 nm) and is stable for more than 4 h. The procedure eliminates the interference of a large number of metal ions and complexing agents. Beer's law is obeyed in the range of 0–2.85 g Mo/mL with a molar absorptivity, Sandell's sensitivity and standard deviation of 5.28×104 L mol–1 cm–1, 0.0018 g Mo/cm2 and ±0.0054, respectively. The method has successfully been used for the spectrophotometric determination of molybdenum in steel samples.  相似文献   

3.
Summary 4-(1H-1,2,4-Triazolyl-3-azo)-2-methylresorcinol reacts with vanadium(V) at pH 8.10 (Tris-HClO4 buffer solution) to produce a pink-violet 11 complex ( max=525 nm,=2.55×104l·mol–1· cm–1) in a 50% (v/v) methanol-water medium, which allows the spectrophotometric determination of 0.1 to 1.51 ppm of vanadium. The method has been applied for the determination of the vanadium content in low alloy steels.
Spectrophotometriscbe Bestimmung von Vanadin mit 4-(1H-1,2,4-triazo-lyl-3-azo)-2-methylresorcin
Zusammenfassung Vanadin bildet bei pH 8,10 (Tris-HClO4-buffer) mit 4-(1H-1,2,4-tri-azolyl-3-azo)-2-methylresorcin ein rosenrot-violettes Chelat, dessen Absorptionsmaximum bei 525 nm in Gegenwart von 50% Methylalkohol gemessen wird. Dieser 11-Komplex entspricht bei einer Vanadin-Konzentration von 0,1–1,51g/ml dem Beerschen Gesetz; seine molare Absorptivität ist 2,55×104l·mol–1·cm–1. Das Verfahren wurde zur Bestimmung des Vanadins in Stahl verwendet.
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4.
A novel chromogenic reagent, 2-(2-sulfo-4-acetylphenylazo)-7-(2,4,6-trichlorophenylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid 1, was prepared by diazo coupling of 4-acetylaniline-2-sulfonic acid and 2,4,6-trichloroaniline to chromotropic acid through –N=N– groups. Based on this reagent, a simple, sensitive and selective spectrophotometric method was developed for the determination of lead. In 0.20M phosphoric acid medium, lead reacts with 1 to form a 1:2 blue complex with an absorption maximum of 654nm. Beers law is obeyed in the range of 0–0.6mgL–1 of lead. The apparent molar absorptivity is 1.25×105Lmol–1cm–1. The detection limit and quantification limit were found to be 0.63µgL–1 and 2.1µgL–1, respectively. The relative standard deviation for eleven replicate measurements was of 2.6%. The interference of foreign ions was also investigated. All the other foreign ions studied did not interfere with lead determination except for Ca(II) and Ba(II). The interference caused by Ca(II) and Ba(II) can be eliminated by prior extraction of lead with potassium iodide-methylisobutylketone (KI-MIBK). The proposed method was applied to the determination of lead in certified samples with satisfactory results.  相似文献   

5.
An extraction-spectrophotometric method for the determination of trace amounts of iron based on its extraction into chloroform with 2-(2-benzothiazolylazo)-4,6-dimethylphenol (BTADMP) from a pH 6.5 medium has been developed. The extracted 12 FeBTADMP complex species allow the determination of 4–30gmg of iron (=3.92×1041·mol–1·cm–1 at 790 nm). The method is highly selective and has been applied to the determination of iron in polymineral-polyvitamin pharmaceutical products.  相似文献   

6.
Reiko Yoda 《Mikrochimica acta》1982,78(3-4):271-278
Summary N,N-Ditnethyl-N-(4-methyl-5-nitro-2-thiazolyl)thiourea A new spectrophotometric method for the determination of palladium with N,N-dimethyl-N-(4-methyl-5-nitro-2-thiazolyl)thiourea (DMNT) is proposed. DMNT instantly forms a yellow chelate with Pd(II) at pH 2 at room temperature, which is readily extracted into organic solvents such as chloroform and shows a higher absorption maximum (=40,400) at 413 nm. The ratio of Pd(II) to reagent in the chelate is 12 as determined by the widely used method and also verified by synthesis of the authentic Pd-chelate. The chelate conforms well with the Lambert-Beer's law over a wide concentration range (3.3–22g in 10 ml chloroform). The optimum concentration range of palladium for spectrophotometry by the Ringbom plot is 5.6–18.6g in 10 ml of chloroform solution. This method gives a good reproducibility, high sensitivity and high accuracy in the presence of many foreign ions.
Spektrophotometrische Bestimmung von Palladium mit N,N-Dimethyl-N- (4-methyl-5-nitro-2-thiazolyl)-thioharnstoff (DMNT)
Zusammenfassung Eine neue spektrophotometrische Methode zur Bestimmung von Palladium mit DMNT wurde vorgeschlagen. Dieses Reagens bildet mit Pd(II) bei pH 2 und Zimmertemperatur ein gelbes Chelat, das mit Chloroform gut extrahierbar ist und bei 413 nm ein hohes Absorptionsmaximum (=40400) zeigt. Dessen Zusammensetzung wurde in üblicher Weise zu 12=Pd: DMNT bestimmt. Im Konzentrationsbereich 3,3–22g/10 ml entspricht das Chelat dem Lambert-Beerschen Gesetz. Die optimale Konzentration für die spektrophotometrische Bestimmung liegt zwischen 5,6 und 18,6g/10 ml Chloroform. Das Verfahren gibt gut reproduzierbare Ergebnisse, ist hoch empfindlich und auch in Anwesenheit vieler Fremdionen sehr genau.
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7.
Summary Manganese forms a red chelate with 4-(2-thiazolylazo)-resorcinol at pH 8.8 (borate buffer), and absorbance is measured after 30 s, at 540 nm in the presence of 20%tert-butyl alcohol (by volume). The 12 complex obeys Beer's law for manganese concentration of 0.04–1.4g per ml, has molar absorptivity 4.176 x 104 and Sandell sensitivity 0.0013g cm–2. The formation constant (logK) is found to be 9.32, and relative standard deviation ±0.22%. Of the 48 ions studied for interference, only Co(II), Zn(II), Cd(II), Pb(II) and EDTA2– are found to interfere. This method has been applied for the determination of manganese content in alloy steels.
Spektrophotometrische Bestimmung von Mangan(II) mit 4-(2-Thiazolylazo)-resorcin
Zusammenfassung Mangan bildet bei pH 8,8 (Boratpuffer) mit 4-(2-Thiazolylazo)-resorcin ein rotes Chelat, dessen Absorbanz nach 30 sec bei 540 nm in Gegenwart von 20% tert. Butylalkohol gemessen wird. Dieser 12-Komplex entspricht bei einer Mangan-Konzentration von 0,04–1,4g/ml dem Beerschen Gesetz; seine molare Absorption beträgt 4,176 x 104, die Empfindlichkeit nach Sandell 0,0013g·cm–2. Die Bildungskonstante (log K) beträgt 9,32, die rel. Standardabweichung ±0,22%. Unter 48 untersuchten Ionen erwiesen sich nur Co(II), Zn(II), Cd(II), Pb(II) und EDTA als störend.-Das Verfahren wurde zur Bestimmung des Mangangehaltes in Stahl verwendet.
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8.
Uranium(VI) reacts with 1-(2-thiazolylazo)-2-naphthol to form a red-coloured chelate in the pH range 5.3–7.2, maintained by 0.04 M acetate buffer. Absorbance of the sparingly soluble complex, solubilized and stabilized by Triton X-100, is measured after 30 min and it is stable for at least 16 hours. The complex exhibits maximum absorbance at 575 and 625–630 nm, but absorbance at longer wavelengths is not stable. The 12 complex obeys Beer's law over the concentration range 0.4–6.4 g of uranium(VI) per cm3, has molar absorptivity 3.36·104 dm3·mol–1·cm–1, Sandell sensitivity 7.0 ng·cm–2, formation constant (log K) 9.32 and coefficient of variation ±0.77%. Effect of 60 ions has been studied and selectivity improved considerably in presence of CDTA. The method has been applied for determination of uranium content in a rock sample.  相似文献   

9.
A selective Spectrophotometric method has been developed for the trace determination of copper after adsorption of its 1-phenyl-4,4,6-trimethyl(1H, 4H)-pyrimidine-2-thiol (PTPT) complex onto microcrystalline naphthalene. The complex is quantitatively adsorbed on naphthalene in the pH range 7.5–11.5, separated by filtration, dissolved in dimethylformamide (DMF) and determined spectrophotometrically at 400 nm. Beer's law is obeyed in the concentration range 2.5–37.5 g of copper in 10 ml of DMF. The molar absorptivity and Sandell's sensitivity are 1.30 × 1041 · mol–1 · cm–1 and 0.0048g cm–2, respectively. Ten replicate analyses of a solution containing 20.0 g of copper gave a mean absorbance of 0.410 with a relative standard deviation of 0.91 %. The interferences of various ions have been studied and the method has been validated by the determination of copper in various standard reference materials, beers, wines, human hair, goat liver and environmental samples.On leave from St. Stephen's College, Delhi 110 007, India  相似文献   

10.
Summary It has been established that 1-(2-phenyl-2-hydroxyiminoethyl)-1-quinolinium chloride, 1-(2-phenyl-2-hydroxyiminoethyl)-1-isoqui-nolinium chloride, 1-(2-phenyl-2-hydroxyiminoethyl)-1-(4-methyl)-quinolinium chloride and 1-(2-phenyl-2-hydroxyiminoethyl)-1-(6-methyl)quinolinium chloride react with palladium(II) chloride in the pH range 3.3–7.1 and form yellow water-soluble 11 complexes with maximum absorbance at 413 nm. The conditional stability constants of the complexes at the optimum pH of 6.5 are all about 104.7, and the molar absorptivities are in the range 2.2–2.6×103 l·l mole–1·cm–1 at pH 6.5 and 413 nm. Beer's law is obeyed up to 3–4×10–4 M oxime concentration, depending on the oxime determined.  相似文献   

11.
We have synthesized the organic conductor (BEDT-TTF)AgXIY (X 1.8 and Y 2.9). This compound has, in addition to high electronic conductivity (300 k 5–10 –1 · cm–1), significant ionic conductivity connected with the motion of silver ions. The value of this ionic conductivity at room temperature is 10–3 –1 · cm–1. The activation energy for diffusion of Ag ions is equal to 0.2 eV.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 247–249, March–April, 1989.  相似文献   

12.
The three copper(II)-arsenates were synthesized under hydrothermal conditions; their crystal structures were determined by single-crystal X-ray diffraction methods:Cu3(AsO4)2-III:a=5.046(2) Å,b=5.417(2) Å,c=6.354(2) Å, =70.61(2)°, =86.52(2)°, =68.43(2)°,Z=1, space group ,R=0.035 for 1674 reflections with sin / 0.90 Å–1.Na4Cu(AsO4)2:a=4.882(2) Å,b=5.870(2) Å,c=6.958(3) Å, =98.51(2)°, =90.76(2)°, =105.97(2)°,Z=1, space group ,R=0.028 for 2157 reflections with sin / 0.90 Å–1.KCu4(AsO4)3:a=12.234(5) Å,b=12.438(5) Å,c=7.307(3) Å, =118.17(2)°,Z=4, space group C2/c,R=0.029 for 1896 reflections with sin / 0.80 Å–1.Within these three compounds the Cu atoms are square planar [4], tetragonal pyramidal [4+1], and tetragonal bipyramidal [4+2] coordinated by O atoms; an exception is the Cu(2)[4+1] atom in Cu3(AsO4)2-III: the coordination polyhedron is a representative for the transition from a tetragonal pyramid towards a trigonal bipyramid. In KCu4(AsO4)3 the Cu(1)[4]O4 square and the As(1)O4 tetrahedron share a common O—O edge of 2.428(5) Å, resulting in distortions of both the CuO4 square and the AsO4 tetrahedron. The two Na atoms in Na4Cu(AsO4)2 are [6] coordinated, the K atom in KCu4(AsO4)3 is [8] coordinated by O atoms.Die drei Kupfer(II)-Arsenate wurden unter Hydrothermalbedingungen gezüchtet und ihre Kristallstrukturen mittels Einkristall-Röntgenbeugungsmethoden ermittelt:Cu3(AsO4)2-III:a = 5.046(2) Å,b = 5.417(2) Å,c = 6.354(2) Å, = 70.61 (2)°, = 86.52(2)°, = 68.43(2)°,Z = 1, Raumgruppe ,R = 0.035 für 1674 Reflexe mit sin / 0.90 Å–1.Na4Cu(AsO4)2:a = 4.882(2) Å,b = 5.870(2) Å,c = 6.958(3) Å, = 98.51(2)°, = 90.76(2)°, = 105.97(2)°,Z = 1, Raumgruppe ,R = 0.028 für 2157 Reflexe mit sin / 0.90 Å–1.KCu4(AsO4)3:a = 12.234(5) Å,b = 12.438(5) Å,c = 7.307(3) Å, = 118.17(2)°,Z = 4, Raumgruppe C2/c,R = 0.029 für 1896 Reflexe mit sin / 0.80 Å–1.Die Cu-Atome in diesen drei Verbindungen sind durch O-Atome quadratisch planar [4], tetragonal pyramidal [4 + 1] und tetragonal dipyramidal [4 + 2]-koordiniert; eine Ausnahme ist das Cu(2)[4 + 1]-Atom in Cu3(AsO4)2-III: Das Koordinationspolyeder stellt einen Vertreter des Übergangs von einer tetragonalen Pyramide zu einer trigonalen Dipyramide dar. In KCu4(AsO4)3 haben das Cu(1)[4]O4-Quadrat und das As(1)O4-Tetraeder eine gemeinsame O—O-Kante von 2.428(5) Å, was eine Verzerrung der beiden Koordinationsfiguren CuO4-Quadrat und AsO4-Tetraeder bedingt. Die zwei Na-Atome in Na4Cu(AsO4)3 sind durch O-Atome [6]-koordiniert, das K-Atom in KCu4(AsO4)3 ist [8]-koordiniert.
Zur Kristallchemie dreier Kupfer (II)-Arsenate: Cu3(AsO4)2-III, Na4Cu(AsO4)2 und KCu4(AsO4)3
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13.
2-Amino-3-(-phthalimidoalkyl)indoles have been obtained by the rearrangement of -phthalimido acid -phenylhydrazides under the action of POCl3. The possibility has been studied of eliminating the phthalyl protective group from these compounds and a convenient method has been developed for obtaining 2-amino-3-(-aminoalkyl)indole dihydrochlorides. The behavior of the 2-amino-3-(-phthalimidoalkyl) indoles in alkylation reactions has been investigated.Deceased.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 484–488, April, 1980.  相似文献   

14.
E-4-(2-(4- tert - butylphenyl) ethen-1- yl)benzoate, E-1, photoisomerizes to the Z-1 isomer and vice versa in the free state and in the binary complexes 2·E-1, 2·Z-1, 3·E-1 and 3·Z-1 where 2 is the urea-linked cyclodextrin N-(6 A -deoxy--cyclodextrin-6 A - yl)-N-(6 A -deoxy--cyclodextrin-6 A - yl)urea and 3 is N,N- bis(6 A -deoxy--cyclodextrin-6 A - yl)urea. In 2·E-1and 3·E-1 the stilbene occupies both cyclodextrin (CD) components of 2 and 3, whereas in 2·Z-1 and 3·Z-1 it only occupies one CD component while the other CD component is unoccupied. 4- tert - Butylphenolate, 4, and its carboxylate, 5, and sulfonate, 6, analogues form the ternary complex 2·Z-1·4 and its analogues and also 3·Z-1·4 and its analogues. These photoisomerize to 2·E-1and 3·E-1 and either free 4, 57 or 6 and thereby function as molecular devices.  相似文献   

15.
Summary Thiazolylazophenols containing a methyl or a phenyl group in the thiazole ring were synthesized and their potential for the spectrophotometric determination of iron were studied. These dyes react with iron(II) to form brownish complexes, which show a characteristic absorption in near-infrared region. Among them, 2-(2-benzothiazolylazo)-4-methoxyphenol is most suitable and the iron(II) complex has the absorption maximum at 815 nm in chloroform. The optimum pH for iron extraction lies between 5.5–9.5 and Beer's law holds up to 6 ppm of iron, with a molar absorptivity of 1.47×104 1 mol–1 cm–1. The composition and the extraction constant of the complex was found to be FeBTAMP=12 and log Kex=–0.76±0.12, respectively. Many kinds of ions can be tolerated even in the presence of large amounts. The method has been applied to the determination of iron in mixtures containing 3d type metal ions, natural waters and native sulfurs with satisfactory results.
Komplexbildende Eigenschaften von Thiazolylazophenol und spektro-photometrische Bestimmung von Eisen(II) mit 2-(2-Benzothiazolylazo)-4-methoxyphenol
Zusammenfassung Thiazolylazophenol mit einer Methyl- bzw. Phenylgruppe am Thiazolring wurde synthetisiert und seine Eignung für die spektrophotometrische Bestimmung von Eisen(II) studiert. Diese Farbstoffe bilden mit Fe(II) bräunliche Komplexe, die charakteristische Absorption im nahen IR zeigen. Unter ihnen ist 2-(2-Benzothiazolylazo)-4-methoxyphenol am besten geeignet. Der Fe(II)-Komplex hat ein Absorptionsmaximum bei 815 nm in Chloroform. Das optimale pH für die Eisenextraktion liegt zwischen 5,5 und 9,5; das Beersche Gesetz ist bis zu 6 ppm Fe erfüllt, der molare Extinktionskoeffizient beträgt 1,47×104 l·mol–1·cm–1. Fe(II)BTMP=12. Die Extraktionskonstante ist log Kex=–0,76±0,12. Zahlreiche Ionen stören auch in größerer Menge nicht. Die Methode wurde zur Eisenbestimmung in Gemischen mit 3d-Typ-Metallen, in natürlichen Wässern und in inländischem Schwefel angewandt.
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16.
A simple, rapid method for the spectrophotometric determination of niobium in trace amounts is presented, employing 3-hydroxyflavone as a ligand for the complexation of the metal ion and extracting the coloured complex into chloroform from 4M HClO4 solution. Beer's law is obeyed in the range 0.0 to 3.2 g ml–1 Nb(V), with a lower working limit of 0.1 g ml–1 Nb(V). Molar absorptivity and Sandell's sensitivity of the complex at 395 nm are 4.088 × 104l mol–1 cm–1 and 0.002g Nb(V) cm–2, respectively. The stoichiometry of the complex is established as 12 by Job's and mole ratio methods. The method is free from the interference of a large number of analytically important elements. The proposed system handles satisfactorily the analysis of several samples of varying complexity. The results are highly reproducible with a relative standard deviation of 0.34% for 20 g of Nb.  相似文献   

17.
Summary p-Sulphobenzeneazo-4-(2-amino-3-hydroxypyridine) reacts with vanadium to form an orange-red coloured complex having maximum absorbance at 530 nm. The reaction is slow at room temperature, it is complete at 40–45° C in 5 min. The effects of temperature, time, pH, reagent concentration, and other variables have been studied. The system obeys Beer's law over the concentration range of 1–12g vanadium(V) ml–1. The molar absorptivity is 5.453 x 103l·mole–1·cm–1. The metal:ligand ratio of 12 was confirmed by Job's continuous variation and mole ratio methods.
Spektrophotometrische Bestimmung von Vanadin(V) mit p-Sulfobenzolazo-4-(2-amino-3-hydroxypyridin)
Zusammenfassung p-Sulfobenzolazo-4-(2-amino-3-hydroxypyridin) bildet mit Vanadin(V) einen orange-roten Komplex, dessen Absorptionsmaximum bei 530 nm liegt. Bei Zimmertemperatur verläuft die Reaktion langsam, bei 40–45° ist sie in 5 min vollständig. Der Einfluß von Temperatur, Zeit, pH, Reagenskonzentration und anderer variabler Faktoren wurde untersucht. Im Konzentrationsbereich 1–12g Vanadin/ml entspricht die Reaktion dem Beer-schen Gesetz. Die molare Absorptivität ist 5,453 x 103l·mol–1·cm–1. Das Verhältnis Metall:Ligand wurde nach Job bestimmt und beträgt 12.
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18.
Summary 4(5)-D-Arabinotetrahydroxybutylimidazoline-2-thione, THBIT, is proposed as a new reagent for the spectrophotometric determination of Pd(II). Pd(II) forms 11, 12 and 14 complexes with THBIT. The system conforms to Beer's law up to 5g/ml palladium concentration in aqueous medium (molar absorptivity, 1.99×104 l· mole–1·cm–1 at 338 nm). The most serious interference is from Hg(II), Os(VIII), Ru(IV), Cr(VI), V(V) and S2O3 2–. The method has been used successfully for the determination of palladium in catalysts and synthetic samples.  相似文献   

19.
4-(21-Thiazolylazo) resacetophenone oxime forms a pink colored soluble complex with uranium(VI) in buffer solutions of pH 6.0. The colored complex has a maximum absorbance at the wavelength 572 nm and the color is stable for about 48 h. The system obeys Beer's law over the concentration range 0.2–6.0 g of uranium cm–3. The molar absorptivity and the Sandell sensitivity of the complex are 6.2×104 dm3.mol–1.cm–1 and 0.0038 g cm–2, respectively. Effect of various diversions has been studied and the method was successfully applied for the determination of uranium in rock samples.  相似文献   

20.
There are two molecules in the asymmetric unit (I and II). The structure consists of a 2-pyrazoline ring and three aromatic rings two of which are free and the third one is condensed with a 3-methyl-4(3H)-pyrimidine ring (4(3H)-Quinazolinone). While the pyrazoline ring is in the distorted envelope conformation, the free aromatic rings are planar and the pyrimidine ring deviates from the planarity. The crystal structure is stabilized by C–HO inter and intramolecular bonds.  相似文献   

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