941 resultados para Tris(2,3-butanediamine)cobalt(iii)
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Äyräpään–Vuosalmen torjuntataistelu käytiin 20.6.–18.7.1944. Taistelu voidaan jakaa kah-teen vaiheeseen. Taisteluja käytiin Äyräpäässä Vuoksen etelärannalla sekä Vuosalmella Vuoksen pohjoisrannalla, jossa Neuvostoliiton joukkojen hyökkäys pysäytettiin. Suomalaisia taisteluihin osallistui kolmesta divisioonasta ja yhdestä prikaatista. Neuvostojoukoilla oli käytössään kolmen armeijakunnan voimat. Kokonaisuudessaan neuvostojoukkojen käytössä oli siis yhteensä yhdeksän divisioonaa sekä suuri joukko vahvennuksia. Suomalaisten III Armeijakunnan alainen 2. Divisioona osallistui Äyräpään–Vuosalmen torjuntataisteluun tais-teluiden alkamisesta 20. kesäkuuta aina taisteluiden laantumiseen saakka heinäkuun 18. päi-vänä. Tutkimuksessa selvitetään jatkosodan aikana käytössä olleet tiedustelumenetelmät, Äyrä-pään–Vuosalmen torjuntataistelussa toteutettu 2. Divisioonaa koskeva tiedustelutoiminta sekä näiden tietojen käyttö taisteluiden aikana. Tutkimustehtävän vastausten sekä niiden toi-siinsa vertailun ja analysoinnin avulla arvioidaan tiedustelun merkitystä 2. Divisioonan tais-telulle Äyräpään–Vuosalmen torjuntataistelussa. Tutkimuksen päämenetelmänä on kvalitatiivinen analyysi. Pääaineistona tutkimuksessa ovat Kansallisarkiston arkistolähteet, jatkosotaan liittyvä tutkimuskirjallisuus sekä jatkosodan aikana voimassa olleet ohjesäännöt ja oppaat. Arkistolähteistä hyödyllisimpiä ovat 2. Divisi-oonan ja III Armeijakunnan esikuntien tiedustelupäiväkirjat, muut tiedustelua koskevat asia-kirjat sekä 2. Divisioonan ja sen alaisten joukkojen sotapäiväkirjat. Tutkimuskirjallisuusläh-teistä hyödyllisimpiä ovat tiedusteluun, viholliseen sekä 2. Divisioonaan liittyvät teokset. Jatkosodan aikana tiedustelussa käytettyjä päälajeja olivat maatähystys, liikkuva maatiedus-telu eli partiotiedustelu, ilmatiedustelu, vankien, yliloikkareiden ja paikallisten asukkaiden kuulustelu, viholliselta, vangeilta, yliloikkareilta, kaatuneilta, esikunnista ja muualta talteen otettujen asiakirjojen tutkiminen, kuuntelu ja suuntiminen, valon- ja äänenmittaus sekä salai-nen tiedustelu. Tiedustelumenetelmistä 2. Divisioonan kannalta merkityksellisimmiksi mene-telmiksi muodostuivat maatähystys, sotavankien kuulustelu sekä ilmatiedustelu. Muut toteu-tetut tiedustelumenetelmät tukivat ja antoivat oman lisänsä kokonaistiedustelulle. Oman merkittävän osansa tiedustelutoiminnassa muodosti tietojen vaihto. Parhaimpaan lopputulok-seen päästiin keinojen ja tietojen yhdistelemisellä, ja sitä kautta kattavalla tiedustelulla ja analysoinnilla. Selkeät puutteet 2. Divisioonan kokonaistiedusteluverkossa ovat löydettävissä vastustajan etulinjan taakse ulottuvasta tiedustelusta ja tiedustelutietojen käytöstä. Kokonais-tiedustelulla kyettiin luomaan riittävän selkeä kuva taistelualueella olevasta vihollisesta. Ny-kypäivän näkökulmasta katsottuna tiedustelulla ei kuitenkaan kyetty luomaan riittävää ana-lyysia ja arviota tiedustelutiedoista, jotta päätöksenteon tukena olisi ollut joka tilanteessa riittäviä ennakoivia arvioita vihollisen tulevasta toiminnasta.
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Gestión del conocimiento
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Gestión del conocimiento
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Gestión del conocimiento
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Gestión del conocimiento
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Modifications to the commercial hydride generator, manufactured by Spectrametrics, resulted in improved operating procedure and enhancement of the arsenic and germanium signals. Experiments with arsenic(III) and arsenic(V) showed that identical reiults could be produced from both oxidation states. However, since arsenic(V) is reduced more slowly than arsenic(III), peak areas and not peak heights must be measured when the arsine is immediately stripped from the system (approximately 5 seconds reaction). When the reduction is allowed to proceed for 20 seconds before the arsine is stripped, peak heights may be used. For a 200 ng/mL solution, the relative standard deviation is 2.8% for As(III) and 3.8% for As(V). The detection limit for arsenic using the modified system is 0.50 ng/mL. Studies performed on As(V) standards show that the interferences from 1000 mg/L of nickel(II), cobalt(II), iron(III), copper(II), cadmium(II), and zinc(II) can be eliminated with the aid of 5 M Hel and 3% L-cystine. Conditions for the reduction of germanium to the corresponding hydride were investigated. The effect of different concentrations of HCl on the reduction of germanium to the covalent hydride in aqueous media by means of NaBH 4 solutions was assessed. Results show that the best response is accomplished at a pH of 1.7. The use of buffer solutions was similarly characterized. In both cases, results showed that the element is best reduced when the final pH of the solution after reaction is almost neutral. In addition, a more sensitive method, which includes the use of (NH4)2S208' has been developed. A 20% increase in the germanium signal is registered when compared to the signal achieved with Hel alone. Moreover, under these conditions, reduction of germanium could be accomplished, even when the solution's pH is neutral. For a 100 ng/mL germanium standard the rsd is 3%. The detection limit for germanium in 0.05 M Hel medium (pH 1.7) is 0.10 ng/mL and 0.09 ng/mL when ammonium persulphate is used in conjunction with Hel. Interferences from 1000 mg/L of iron(III), copper(II), cobalt(II), nickel(II), cadmium(II), lead(II), mercury(II), aluminum(III), tin(IV), arsenic(III), arsenic(V) and zinc(II) were studied and characterized. In this regard, the use of (NH4)ZS20S and Hel at a pH of 1.7 proved to be a successful mixture in the sbppression of the interferences caused by iron, copper, aluminum, tin, lead, and arsenic. The method was applied to the determination of germanium in cherts and iron ores. In addition, experiments with tin(IV) showed that a 15% increase in the tin signal can be accomplished in the presence of 1 mL of (NH4)2S20S 10% (m/V).
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The reaction of tris(pentafluorophenyl)phosphine [5] with the nucleophiles dimethyl formamide (DMF), hexamethylphosphoric triamide (HMPA), diethyl formamide (DEF), hexaethylphosphoric triamide (HEPA), hydrazine, N,N-dimethyl hydrazine (in presence and/or absence of KF), phenylhydrazine, ammonium hydroxide, formamide, aniline, sodium hydrogen sulfide, and hexaethylphosphorous triamide was investigated. The reaction of [5] with DMF and HMPA gave the same product, namely tris-[4-(N,N-dimethylamino)-2,3,5,6-tetrafluorophenyl]phosphine [12] but in higher yield in the case of HMPA. Compound (5] also reacted with DEF to give tris[4-(N,N-diethylamino)-2,3,5,6-tetrafluorophenyl] phosphine [14]. When [51 was treated with HEPA, it gave a mixture of bis(pentafluorophe~yl)-(N,N-diethylamino-tetrafluorophenyl)phosphine, pentafluorophenyl-bis-(N,N-diethylamino-tetrafluorophenyl)phosphine and tris (N,N-diethylamino-tetrafluorophenyl)phosphine. Treatment of [5] with aqueeus hydrazine solution in excess ethanol gave tris(4-hydrazo-2,3,4,6-tetrafluorophenyl)phosphine [1s1 in high yield while reaction with aqueous hydrazine led to C-P cleavage and production of tetrafluorophenyl hydrazine. With N,N-dimethyl hydrazine, [5] gave tris(4-N,N-dimethylhydrazine-2,3,5,6-tetrafluorophenyl) phosphine {20j. The latter could be obtained in higher yield and shorter reaction time, by the addition of KF. The reaction of compound {51 with phenylhydrazine in THF gave bis(pentafluorophe~yl)-4-S-phenylhydrazino- 2,3,5,6-tetrafluorophenyl phosphine [22] in low yield. Reaction of [5] with ammonium hydroxide in THF at high pressure in the presence of KF gave tris-~4-amino-2,3,5,6-tetrafluorophenyl)phosphine [25]. Similarly, formamide led to a mixture of (C6F4NHZ)3P, (C6F4NHZ)ZPC6FS, (C6F4NHZ)ZPC6F4NHCHO, and C6F4NHZP(C6Fs)(C6F4NHCHO). When [5] was treated with aniline, a mixture of mono-, di-, and tri-substituted products was obtained. Sodium hydrogen sulfide in ethylene glycol/ pyridine led to C-P cleavage and the isolation of pentafluorobenzene and tetrafluorothiophenol. Reaction of [5] and its oxide [35] with different alkoxides in the corresponding alcohols led mainly to C-P bond cleavage products, with the exception of one case where sodium methoxide was used in ether, and which led to tris-(4-methoxy-2,3,9,6-tetrafluorophenyl)phosphine [37]. On the basis of various spectroscopic data, it was concluded that the para position in compound [5] was generally the favoured site of attack.
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The preparation and characterization of two families of building blocks for molecule-based magnetic and conducting materials are described in three projects. In the first project the synthesis and characterization of three bis-imine ligands LI - L3 is reported. Coordination of LI to a series of metal salts afforded the five novel coordination complexes Sn(L4)C4 (I), [Mn(L4)(u-CI)(CI)(EtOH)h (II), [CU(L4)(u-sal) h(CI04)2 (sal = salicylaldehyde anion) (III), [Fe(Ls)2]CI (IV) and [Fe(LI)h(u-O) (V). All complexes have been structurally and magnetically characterized. X-ray diffraction studies revealed that, upon coordination to Lewis acidic metal salts, the imine bonds of LI are susceptible to nucleophilic attack. As a consequence, the coordination complexes (I) - (IV) contain either the cyclised ligand L4 or hydrolysed ligand Ls. In contrast, the dimeric Fe3+ complex (V) comprises two intact ligand LI molecules. In. this complex, the ligand chelates two Fe(III) centres in a bis-bidentate manner through the lone pairs of a phenoxy oxygen and an imine nitrogen atom. Magnetic studies of complexes (II-V) indicate that the dominant interactions between neighbouring metal centres in all of the complexes are antiferromagnetic. In the second project the synthesis and characterization two families of TTF donors, namely the cyano aryl compounds (VI) - (XI) and the his-aryl TTF derivatives (XII) - (XIV) are reported. The crystal structures of compounds (VI), (VII), (IX) and (XII) exhibit regular stacks comprising of neutral donors. The UV -Vis spectra of compounds (VI) - (XIV) present an leT band, indicative of the transfer of electron density from the TTF donors to the aryl acceptor molecules. Chemical oxidation of donors (VI), (VII), (IX) and (XII) with iodine afforded a series of CT salts that where possible have been characterized by single crystal X -ray diffraction. Structural studies showed that the radical cations in these salts are organized in stacks comprising of dimers of oxidized TTF donors. All four salts behave as semiconductors, displaying room temperature conductivities ranging from 1.852 x 10-7 to 9.620 X 10-3 Scm-I. A second series of CT salts were successfully prepared via the technique of electrocrystallization. Following this methodology, single crystals of two CT salts were obtained. The single crystal X-ray structures of both salts are isostructural, displaying stacks formed by trimers of oxidized donors. Variable temperature conductivity measurements carried out on this series of CT salts reveal they also are semiconductors with conductivities ranging from 2.94 x 10-7 to 1.960 X 10-3 S em-I at room temperature. In the third project the synthesis and characterization of a series of MII(hfac)2 coordination complexes of donor ligand (XII) where M2+ = Co2+, Cu2+, Ni2+ and Zn2+ are reported. These complexes crystallize in a head-to-tail arrangement of TTF donor and bipyridine moieties, placing the metal centres and hfac ligands are located outside the stacks. Magnetic studies of the complexes (XV) - (XVIII) indicate that the bulky hfac ligands prevent neighbouring metal centres from assembling in close proximity, and thus they are magnetically isolated.
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Coordination chemistry of schiff bases is of considerable interest due to their various magnetic, catalytic and biological applications. Here it describes the spectral characterization of schiff bases and its Mn (II), Cu (II) and Ni (II) complexes. Then synthesis and spectral characterization of Zn (II), Cd (II) and Co (II) complexes of schiff base derived from 3-Formylsalicilic Acid and 1,3-diaminopropane. Then it discusses the synthesis and spectral studies of Copper (II) complexes of 2-Hydroxyacetophenone N-phenyl semicarbazone. Finally it discusses the synthesis and spectral characterization of Co (III) complexes of salicylaldehyde N-phenyl semicarbazone. The preparation and characterization of Cobalt (III) complexes of salicylaldehyde, N-phenylthiosemicarbazone containing hetrocyclic bases phenalthroline and bipyridine. Thiocyanate, azide and perchlorate ions act as coligands. Elemental analysis suggests +3 state for Cobalt. HNMR, IR and UV-visible spectra characterize the complexes.