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Statistical comparisons of heavy-metal concentrations in river sediments (1996)

Murray, K. S.

Springer

Environmental geology 27 (1996), S. 54-58

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ISSN: 1432-0495

Keywords: Heavy metals ; Statistics ; River sediments

Source: Springer Online Journal Archives 1860-2000

Topics: Geosciences

Notes: Abstract Statisticalt tests were used to determine lead, copper, and chromium enrichment in sediments from the Lower Branch of the Rouge River in southeast Michigan, USA. Both absolute metal concentrations and ratios of trace metal to conservative metal concentrations were used to compare sampled sites along the Lower Branch of the Rouge River to background sites in the headwaters region. Concentration ratios were used to reduce the effects of certain chemical and physical characteristics on the level of metal contained in a given sediment. Results from the comparison of sample sites to the background reveal metal enrichment at several sites, particularly along the highly urbanized, downstream section of the river. This section of the Lower Branch of the Rouge River exhibits significant lead and copper contamination, as well as measurable chromium enrichment when using either concentrations alone or ratios as methods of comparison. The areas of metal enrichment appear to coincide closely with areas of known anthropogenic activities. Of particular interest, however, is the enrichment of lead and copper at two upstream sites where the statistical tests suggest an anthropogenic source for the enrichment, but where no previously known cultural activities existed. These data prompted a historical search of records, which discovered several abandoned landfills immediately upstream of the metal enrichment sites.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00770602

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Applied field Mössbauer spectra of low-spin mononuclear and binuclear iron(III)phthalocyanines (1988)

Bakshi, E. N. ; Murray, K. S.

Springer

Hyperfine interactions 40 (1988), S. 283-286

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ISSN: 1572-9540

Source: Springer Online Journal Archives 1860-2000

Topics: Physics

Notes: Abstract Well characterized low-spin Fe(III)phthalocyanine complexes have recently been synthesized. Two six-coordinate examples, a binuclear μ-oxo bridged complex [((γ-picoline)FePc)2O],1, and a mononuclear bis-azido complex (PNP)[FePc(N3)2],2, display typical S=1/2 Fe(III) parameters (1, δ=0.20 mm/s, ΔEQ=1.79 mm/s;2, δ=0.22 mm/s, ΔEQ=2.47 mm/s at 4.2K). As an applied longitudinal magnetic field is increased to 32kOe the corresponding splittings in1 and2 indicate very small effective fields at the Fe nuclei. This is due to an S=O ground state in the weakly antiferromagnetically coupled complex1. The small hyperfine splitting in2 contrasts with the well resolved hyperfine splitting reported for various S=1/2 Fe(III)porphyrins and Fe(III)heme proteins.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF02049098

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High-spin Mangan(II)-Phthalocyanine: Darstellung und spektroskopische Eigenschaften von Acidophthalocyaninatomanganat(II) (1994)

Sievertsen, S. ; Moubaraki, B. ; Murray, K. S. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 682-690

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ISSN: 0044-2313

Keywords: Phthalocyanines ; MnII complex ; Uv-vis-n.i.r., m.i.r., f.i.r., resonance Raman, ESR spectra ; magnetism ; cyclovoltammetry ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: High Spin Manganese(II) Phthalocyanines: Preparation and Spectroscopical Properties of Acidophthalocyaninatomanganate(II)Acidophthalocyaninatomanaganese(III) is reduced by boranate, thioacetate or hydrogensulfide to yield acidophthalo-cyaninatomanganate(II) ([Mn(X)Pc2-]-; X = Cl, Br, NCO, NCS) being isolated as tetra(n-butyl)ammonium salt. In the cyclovoltammogram of [Mn(NCO)Pc2-]- the halv-wave potential for the redoxcouple MnII/MnIII is at -0.13 V, that of the first ring reduction at -0.99 V. The magnetic moments are indicative of high-spin 6A1 ground states: μMn = 5.84 (NCO), 5.78(Cl), 5.65 (Br), 5.68 μB (NCS). A Curie-like temperature dependence of μMn is observed in the region 300-30 K. Below 30 K an increase in μMn occurs due to weak intermolecular ferromagnetic coupling. The ESR spectra confirm the S = 5/2 ground state with a strong g = 6 resonance observed (AMn = 80 G) as expected for an axially distorted ligand-field. Besides the typical π-π* transitions of the Pc2--ligand several weak bands are observed in the Uv-vis-n.i.r. spectra at ca. 7.5, 9.1, 14.0 and 19.0 kK that are assigned to trip-multiplet transitions. In resonance with the band at 19.0 kK the Mn—X stretching vibration (v(MnX)) is resonance Raman enhanced: X = NCO: 319, Cl: 286, SCN: 238, Br: 202 cm-1. These vibrational frequencies are confirmed by the f.i.r. spectra. In the case of the thiocyanato-complex probably both forms of bonding of the ambident NCS-ligand are present (v(Mn—NCS): 274 cm-1). The frequencies of the vibrations of the inner (CN)8 ring are reduced by up to 20 cm-1 as compared with those of low spin MnII phthalocyanines.

Notes: Acidophthalocyaninatomanagan(III) wird mittels Boranat, Thioacetat oder Hydrogensulfid zum Acidophthalocyaninatomanganat(II) ([Mn(X)Pc2]; X = Cl, Br, NCO, NCS) reduziert und als Tetra(n-butyl)ammoniumsalz isoliert. Im Cyclovoltammogramm von [Mn(NCO)Pc2-]- liegt das Halbstufenpotential für das Redoxpaar MnII/MnIII bei -0,13 V, das der ersten Ringreduktion bei -0,99 V. Die magnetischen Momente der Komplexe weisen auf einen high-spin 6A1-Grundzustand hin: μMn = 5,84 (NCO), 5,78 (Cl), 5,65 (Br), 5,68 μB (NCS). Die Temperaturabhängigkeit der magnetischen Suszeptibilität μMn zeigt zwischen 300 und 30 K Curie-Verhalten. Unterhalb von 30 K steigt μMn wegen schwacher intermolekularer ferromagnetischer Kopplungen an. Die ESR-Spektren bestätigen den S = 5/2-Grundzustand mit einem starken g = 6 Resonanzsignal (AMn = 80 G), wie es für ein axial verzerrtes Ligandenfeld erwartet wird. In den UV-VIS-NIR-Spektren treten neben den typischen π-π*-Übergängen des Pc2--Liganden weitere schwache Banden bei ca. 7,5, 9,1, 14,0 und 19,0 kK auf, die Trip-Multiplett-Übergängen zugeordnet werden. In den Resonanz-Raman-Spektren werden in Resonanz mit der Bande bei 19,0 kK bevorzugt die Mn—X-Valenzschwingungen (v(MnX)) angeregt: X = NCO: 319, Cl: 286, SCN: 238, Br: 202 cm-1. Die Schwingungsfrequenzen stimmen mit entsprechenden FIR-Absorptionen gut überein. Im Falle des Thiocyanato-Komplexes sind eventuell beide Bindungsformen des ambidenten NCS-Liganden präsent (v(Mn—NCS): 274 cm-1). Die Schwingungsfrequenzen des inneren (CN)8-Ringes liegen um bis zu 20 cm-1 tiefer als die von low-spin MnII-Phthalocyaninen.

Additional Material: 8 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19946200417

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Darstellung und Eigenschaften anionischer Fluoro-Komplexe von Mg-, Zn- und Al-Phthalocyanin(2-) (1984)

Homborg, H. ; Murray, K. S.

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 517 (1984), S. 149-160

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ISSN: 0044-2313

Keywords: Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Preparation and Properties of Anionic Fluoro Complexes of Mg-, Zn-, and Al-Phthalocyanine(2-)By treatment of a suspension of MgPc(2-) · 2H2O, ZnPc(2-), or XAlPc(2-) (X=F—I) in dichloromethane with TBAF · 3H2O the crystalline salts TBA[MFPc(2-)] (M=Mg, Zn) and TBA[AlF2Pc(2-)] · 2H2O · O.3HF are isolated. Solutions of the pure salts are instable against hydrolysis. In the case of Al the complex anion [(AlFPc(2-))2O]2- is formed. The properties, cyclic voltammograms, i.r., Ra, and u.v.-vis-spectra are discussed.

Notes: Bei der Einwirkung von TBAF · 3H2O auf eine Suspension von MgPc(2-) · 2H2O, ZnPc(2-) oder XAlPc(2-) (X=F—I) in Dichlormethan werden die Komplexasalze TBA[MFPc(2-)] (M=Mg, Zn) und TBA[AlF2Pc(2-)] · 2H2O · O,3HF kristallin erhalten. Lösungen der reinen Komplexsalze sind hydrolyseempfindlich. Im Falle von Al bildet sich das Komplexanion [(AlFPc(2-))2O]2-. Die Eigenschaften, zyklischen Voltammogramme, IR-, Ra. und UV-Vis-Spektren werden diskutiert.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19845171014

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Dimere low-spin Eisen(III)-Phthalocyanine: Synthese und Eigenschaften ferromagnetisch gekoppelter μ-Oxodi(acidophthalocyaninatoferrate(III))Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)

Sievertsen, S. ; Murray, K. S. ; Moubaraki, B. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 1203-1212

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ISSN: 0044-2313

Keywords: μ-Oxodi(acidophthalocyaninatoferrates(III)) ; spectroscopic, magnetic and Mößbauer properties, ferromagnetic coupling ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Dimeric Low-Spin Iron(III) Phthalocyanines: Synthesis and Properties of Ferromagnetically Coupled μ-Oxodi(acidophthalocyaninatoferrates(III))μ-Oxodi(phthalocyaninatoiron(III)) ([(FePc2-)2O]) dissolved in pyridine reacts with different Tetra(n-butyl)ammonium salts yielding partly solvated Di(tetra(n-butyl)ammonium)-μ-oxodi(acidophthalocyaninatoferrates(III)) ((nBu4N)2[(Fe(X)Pc2-)2O]; X- = CN-, Im-, NCO-, NCS-, NO2-). The uv-vis. spectra show the typical B, Q, N and L regions of the Pc2- ligand scarcely influenced by the axial ligands X. In comparison with [(FePc2-)2O] mainly the B region is hypsochromically shifted due to strong excitonic coupling (〉 3 kK). Two regions of weak absorbance at ca. 7.6-8.7 and 11.4-13.0 kK are assigned to trip-doublet transitions. The m.i.r. and resonance Raman spectra are dominated by the fundamental vibrations of the Pc2- ligand being characteristic for hexa-coordinated low-spin FeIII phthalocyanines. Internal vibrations of the ambident axial ligands X are in accordance with the proposed Fe—X bond. The i.r. active asym. (Fe—O—Fe) stretching vibration is observed in the region 631-690 cm-1. Fe—X stretching vibrations are only present in the f.i.r. spectra. The magnetic properties and Mößbauer spectra are interpreted in terms of an electronic model which assumes that a S′ = 1 ground state arises from strong ferromagnetic coupling of the low-spin FeIII centres. Both spin-Hamiltonian and ligand-field models have been employed to fit the variable temperature susceptibility data. These low-spin μ-oxo FeIII dimers are rare compared to the many known examples of coupled high-spin species including the parent, [(FePc2-)2O].

Notes: In Pyridin gelöstes μ-Oxodi(phthalocyaninatoeisen(III))([(FePc2-)2O]) reagiert mit verschiedenen Tetra(n-butyl)ammoniumsalzen unter Bildung von teilweise solvathaltigen Di(tetra(n-butyl)ammonium)-μ-oxodi(acidophthalocyaninatoferraten(III)) ((nBu4N)2[(Fe(X)Pc2-)2O]; X- = CN-, Im-, NCO-, NCS-, NO2-). In den UV-Vis-Spektren heben sich die für den Pc2--Liganden typischen B-, Q-, N- und L-Regionen, wenig vom axialen Liganden X beeinflußt, deutlich heraus. Wegen der starken Excitonen-Kopplung (〉 3 kK) ist insbesondere die B-Region gegenüber der von [(FePc2-)2O] hypsochrom verschoben. Schwache Absorptionsbereiche bei ca. 7,6-8,7 und 11,4-13,0 kK werden Trip-Dublett-Übergängen zugeordnet. Die MIR- und Resonanz-Raman-Spektren werden von den Fundamentalschwingungen des Pc2--Liganden dominiert, die für hexakoordinierte low-spin FeIII-Phthalocyanine charakteristisch sind. Ausgewählte interne Schwingungen der ambidenten Axialliganden X stützen die angenommene Art der Fe—X-Bindung. Die ir-aktive, asym. (Fe—O—Fe)-Valenzschwingung tritt ligandabhängig zwischen 631 und 690 cm-1 auf. Fe—X-Valenzschwingungen werden nur im FIR-Spektrum beobachtet. Die magnetischen Eigenschaften und die Mößbauer-Spektren werden anhand eines elektronischen Modells diskutiert, welches auf der Annahme eines (S′ = 1)-Grundzustandes basiert, der aus der starken ferromagnetischen Kopplung der beiden low-spin FeIII-Zentren resultiert. Für die Anpassung der Temperaturabhängigkeit der magnetischen Suszeptibilitäten sind sowohl das Modell des einfachen Spin-Hamilton-Operators als auch Ligandenfeld-Modelle verwendet worden. Diese low-spin μ-Oxo-Eisen(III)-Dimere sind angesichts der vielen bekannten Beispiele gekoppelter high-spin Spezies, [(FePc2-)2O] eingeschlossen, eine Rarität.

Additional Material: 9 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19946200713

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