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  • 1995-1999  (289)
  • 1995  (289)
  • crystal structure  (158)
  • Industrial Chemistry and Chemical Engineering
  • Nuclear reactions
  • 1
    ISSN: 1572-8854
    Keywords: Tautomerism ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystals consisting of two distinct chemical entities, tautomers of each other, in exact 1∶1 ratio, have been obtained and their structure determined by X-ray analysis. The crystals of C9H11N3·C9H11N3 are monoclinic,P21/c,a=15.674(3),b=17.085(3),c=13.758(3)Å, β=90.78(2)°,Z=8. There are two hydroxylamine and two aminonitrone molecules in the asymmetric unit. Hydrogen bonds connect those molecules into chiral layers. Layers of opposite chirality alternate andthe crystal is centrosymmetric as a whole. Within those layers chains of tautomers joined by very strong O−H... O and strong N−H... N bonds can be recognized. Proton transfer along those chains with simultaneous rearrangement of π-bonds within the molecules would result in interconversion of tautomers and would affect chirality of the layer.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 57-62 
    ISSN: 1572-8854
    Keywords: phase diagram ; buffered chloroaluminate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The phase diagram of the buffered neutral aluminum chloride + 1-ethyl-3-methyl-1H-imidazolium chloride + sodium chloride (AlCl3-EMIC-NaCl) ternary melt system can be represented by a binary phase diagram composed of (EMI)AlCl4 and NaAlCl4. In the binary phase diagram, the salts are liquid at, or near, room temperature for a wide range of compositions. At the 1∶1 composition, the congruently melting compound (EMI)(Na)(AlCl4)2 with m.p.=36.7°C is formed. Crystals of this mixed organic-inorganic salt were grown for single crystal x-ray diffraction analysis. The compound crystalizes in the space group $$P\bar 1$$ with lattice parametersa=10.321(1) Å,b=10.895(3) Å,c=9.284(4) Å, α=98.31(2)°, β=100.83(4)°, γ=101.95(3)°. Data collected at −120°C gave final residuals ofR=0.037 andR w=0.045 using 2713 observed reflections. The packing diagram reveals Na+ ion zig-zag chains running along thea-axis with each Na+ surrounded by four AlCl 4 − units, reminiscent of NaAlCl4. The AlCl 4 − ions form a distorted square planar coordination sphere around Na+ at an average Na−Al distance of 3.76(4) Å. Using a sodium ionic radius of 1.16 Å, a new AlCl 4 − ionic radius of 2.60 Å is calculated. This radius is 0.21 Å shorter than the reported thermodynamic radius.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 223-226 
    ISSN: 1572-8854
    Keywords: Antifungal alkaloids ; 3-methylsampangine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract 3-Methylsampangine, C16H10N2O, crystallizes in the monoclinic space group P21/c witha=7.260(3),b=10.697(5),c=15.342(6) Å, and β=102.69(4). All nonhydrogen atoms of this potent antifungal agent are planar to within 0.082 Å. The title compound exhibits potentin vitro antifungal activity againstC. neoformans, C. albicans andA. fumigatus.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 219-222 
    ISSN: 1572-8854
    Keywords: Calcium phosphate ; calcium pyrophosphate ; calcium potassium pyrophosphate ; crystal structure ; layer-type structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of Ca10K4(P2O7)6·9H2O has been determined by single crystal X-ray diffraction. Crystals are hexagonal, space group P63cm witha=11.761(1),c=9.770(1) Å, andZ=1. The structure was refined toR=0.028 andR w=0.037 for 468 reflections withI≥3σ(I). The structure consists of a compact assembly of Ca and P2O7 ions arranged in layers perpendicular to thec-axis in a hexagonal array with relatively large open channels along thec-axis. The K ions and the water molecules are located in these open channels and are disordered.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 295-298 
    ISSN: 1572-8854
    Keywords: Cage-diol ; crystal structure ; photooxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract An unusual photooxidation was noted upon photolytic cage closure of a substituted tricyclo[6.2.1.02.7]undecane-exo, exo-diol. The resultant compound, which may be regarded as a mono-reduced pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione, was characterizedvia X-ray crystallography. This species could be reduced to the tricyclo[6.2.1.02,7]undecane-endo, exo-diol under conditions previously shown to be inert for the parent dione.
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  • 6
    ISSN: 1572-8854
    Keywords: Benzonaphthodioxosuberane ; crystal structure ; radermachol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of the title compound (2) C21H16O4 has been determined by an X-ray analysis, by direct methods from diffractometer data and refined by full-matrix least squares. The compound (2) crystallizes in the space group P21/a, with cell parameters:a=36.432(5),b=5.512(3),c=8.269(5) Å, β=108.0(3)°,z=4,D c =1.397 g/cm−3,R=7.8 for 1136 observed reflections. The conformation of the tetracyclic ring system shows a folding of two planar parts of the carbon skeleton about an axis passing thorough C8 and C16 of the seven membered ring C.
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  • 7
    ISSN: 1572-8862
    Keywords: Palladium ; gold ; cluster ; phosphine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract [Au2Pd14(μ3-CO)7(μ2-CO)2(PMe3)11](PF6)2 has been synthesized from [Pd8(CO)8(PMe3)7] and AuCl(PCy3) in the presence of TIPF6. It has been characterised on the basis of mass spectrometry, infrared and NMR spectroscopy, and a single crystal X-ray diffraction study. The structure is based on a palladium-centered Au2Pd11 icosahedron which shares an edge with a Pd5 trigonal bipyramid.
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  • 8
    ISSN: 1572-8862
    Keywords: Cluster carbonyl ; osmium ; gold ; arene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Reduction of the heptaosmium cluster [Os7(CO)21] With [Et4N][NH4) gives the cluster dianion [Os7(CO)20]2−,1, in high yield. The reaction of the dianion with [AuPR 3Cl] (R=Et or Ph) in the presence of TlPF6 forms [Os7((CO)20(AuPR 3)2] [R=Et (2a);R = Ph(2b)] in 80% yield, while the corresponding reaction with (Os(C6H6)(CH3CN)3]2+ gives [Os8(CO)20 (η 6-C6H6)] (3) in reasonable yield (ca. 30%). The dianion,1, and the clusters2 and3 have been fully characterized by bout spectroscopic and crystallographic methods. The crystal structure of the [Ph4P]+ salt of1 shows that the metals in the anion adopt a capped octahedral geometry, with all twenty carbonyl ligands in terminal sites. The metal core geometry in2a is best described as a tricapped octahedron, and is based on the structure of the dianion1 with two adjacent octahedral faces capped by the Au atoms of the two AuPEt3 groups. In a similar fashion, the geometry of3 is related to that of1 with the addition of an Os(C6H6) unit capped to a triangular face, to give a bicapped octahedral framework.
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  • 9
    ISSN: 1572-8862
    Keywords: Undecaosmium carbido cluster ; µ-bridged chlorol preparation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract A chloro-derivative of undecaosmium carbido cluster [Os11C(CO)27(µ-Cl)]-1 anion has been prepared and fully characterized by spectroscopic and crystallographic methods. The structure1 is an important intermediate for the conversion of [Os11C(CO)27]2 2 dianion to [OS10C(CO)24]2-3 dianion.
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  • 10
    ISSN: 1572-8862
    Keywords: Silver ; iron ; carbonyl ; cluster ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The oxidation of the [Fe(CO)4]2− dianion with Ag+ salts occurs through a particularinner-sphere mechanism, which involves an intermediate cascade of silver clusters stabilized by Fe(CO)4 ligands. The last detectable Ag-Fe cluster of the sequence is the [Ag13{μ-Fe(CO)4}8]3− trianion, which has been selectively obtained by using ca. 1.7 equivalents of Ag+ per mole of [Fe(CO)4]2−. The [Ag13{μ-Fe(CO)4}8]3−- trianion has been isolated in a crystalline state with several quaternary cations, and has been characterized by X-ray diffraction studies of its bis(triphenylphosphine)iminium salt. [N(PPh3)2]3 [Ag13{μ 3-Fe(CO)4}8]·2(CH3)2CO, monoclinic, space group P21 (No.4),a = 16.284(2) Å,b =18.767(5) Å,c = 25.905(4) Å,β = 90.46(1)°,V = 7916(3) Å3,Z = 2,R = 0.0324. The molecular structure of the anion consists of a centered cuboctahedron of silver atoms with the triangular faces capped by Fe(CO)4 units. Chemical reduction of ( Ag13{μ 3-Fe(CO)4}8]3− affords the corresponding [Ag13{μ 3-Fe(CO)4)8]4−, which in turn gives [Ag13{μ 3-Fe(CO)4)8]5− and [Ag6{μ 3-Fe(CO)4}4]– upon further reduction. Electrochemical investigations confirm the reversibility of the [Ag13{μ 3-Fe(CO)4}8]3−/4− redox change. Furthermore, in spite of some electrode poisoning effects, evidence of the existence of the [Ag13{μ 3-Fe(CO)4}8]5− pentaanion was obtained. The yet structurally uncharacterized [Ag6{μ 3-Fe(CO)4)4]2− dianion is quantitatively obtained by reaction of [Fe(CO)4]2− with ca. 1.5 equivalents of Ag+ or by addition of one equivalent of Ag+ to solutions of the [Ag5{Fe(CO)4}4]3− trianion. All attempts to isolate its quaternary salts as crystalline materials failed owing to formation of amorphous insoluble precipitates. The above series ofμ 3-Fe(CO)4 octa-capped cuboctahedral Ag13 clusters can be envisioned as the Ag+ . Ag and Ag− cryptates of the [Ag12{μ}3-Fe(CO)4}8]4− cryptand. respectively.
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  • 11
    ISSN: 1572-8862
    Keywords: Osmium ; unsaturated cluster ; ortho-metallation ; siloxyl ligand ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of Os3(CO)10(NCMe)[Si(OMe)3](μ-H),1, with PMe2Ph yielded the new complex Os3(CO)10(PMe2Ph)[Si(OMe)3](μ-H),2 by substitution of the MeCn ligand with the phosphine ligand. When heated to 125°C compound2 was decarbonylated and transformed into the new unsaturated cluster complex Os3(CO)8[μ-PMe2(C6H4)][Si(OMe)3](μ-H)2,3 in 54% yield. Compound3 was characterized by a single crystal X-ray diffraction analysis, osmium bonds. The phenyl ring of the phosphine ligand has undergoneortho-metallation by a neighboring metal atom. A terminally coordinated Si(OMe)3 ligand is coordinated to the third osmium atom. The cluster is unsaturated by the amount of 2 electrons, and there is an open coordination site on the siloxyl substituted osmium atom that is partially filled by a weak interaction with one of the π-bonds of theortho-metalled phenyl ring. Complex3 reacts with CO at 1 atm to reform compound2 in 85% yield in 5 h at 40°C. Crystal Data: for3: space group = P21/n,a = 9.911(2) Å,b = 18.451(6) Å,c = 14.872(2) Å,β = 95.64(2)°,Z = 4, 1994 reflections,R = 0.028.
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    Journal of cluster science 6 (1995), S. 549-566 
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; di-μ-oxo bridge ; sexadentate ligands ; asymmetric distortion ; stereoselectivity ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Binuclear oxomolybdenum(V) and oxotungsten(V) complexes of the type, [M 2(O)2(μ-X)(μ-X 1)]”, where M=Mo, W;X.X 1=O, S; L=edta, pdta (n=2-), tpen, tppn (n=2+) (edta4– =ethylenediaminetetraacetate(4–), pdta=R- orR,S-propylenediaminetetraacetate(4–), tpen=N,N,N 1,N1-tetrakis(2-pyridyhnethyl)-ethylenediamine, and tppn=R- orR,S-N,N,N 1,N1-tetrakis(2-pyridylmethyl)-propylenediami ne) are reviewed with respect to their preparation, structure, spectroscopic properties, reactivities, and in particular asymmetric distortion around the bicyclo [4.1.1 ] type core and stereoselectivity related to this distortion,
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  • 13
    ISSN: 1572-8854
    Keywords: Molecular mechanics ; molecular dynamics ; MNDO ; CMPO ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of N,N-diisobutyl-2-(octylphenylphosphinyl)acetamide, or CMPO was recently determined. The compound crystallizes in the space group P21/c witha=13.446(6),b=22.280(7),c=17.217(7) Å, β=92.07(4)°, andD calc=1.05 g/cm3 forZ=8 @20°C). Molecular mechanics, molecular dynamics, and MNDO calculations were also performed on CMPO utilizing the SYBYL1 suite of programs. The results from these calculations are compared to the crystal structure and to similar calculations performed on CMPO using ALCHEMY2,3. In general, the results from the calculations agree fairly well with the parameters from the crystal structure.
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  • 14
    ISSN: 1572-8854
    Keywords: Mercury(II) terpyridine complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [Hg(terpy)2](CF3SO3)2·0.5(CH3)2CO crystallizes in the triclinic $$P\bar 1$$ space group witha=14.631(6),b=15.258(4),c=18.785(7) Å, α=69.66(2), β=70.72(1), γ=88.55(1)°. The crystal structure consists of two independent [Hg(terpy)2]2+ cations, four trifluoromethanesulfonate anions and an acetone molecule in the asymmetric unit. Each mercury atom is coordinated by two tridentate terpyridine ligands forming an irregular six-coordination polyhedron. The Hg−N bond lengths range from 2.27(2) to 2.53(2) Å.
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  • 15
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 463-467 
    ISSN: 1572-8854
    Keywords: 1,3-dithiole-4-carboxamides ; resonance effect ; short intramolecular S...O contact ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The two closely related compoundsN,N-dimethyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide1 andN-(p-methoxy-phenyl)-N-methyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide2 have been characterized by X-ray crystal structure determination. Crystal data for1: triclinic, $$P\bar 1$$ ,a=6.767(1),b=12.594(2),c=6.648(1) Å, α=101.38(1), β=93.37(2), γ=79.62(1)°,V=546.2 Å3,Z=2. Crystal data for2: monoclinic, Cc,a=19.836(4),b=6.057(1),c=15.860(3) Å, β=127.61(3)°,V=1509.5Å3,Z=4. The molecular structures of1 and2 show remarkable differences concerning the conformational behavior. These differences are related to the nature of the substituents at the nitrogen atom. The presence of an aromatic system in2 leads to an almost planar arrangement of the α-oxoketene dithioacetal moiety. This effect is accompanied by a short intramolecular S...O contact of 2.648(2) Å. In the absence of an aromatic system, as is the case for compound1, neither a resonance effect along the α-oxoketene dithioacetal fragment nor a short S...O distance is observed.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 579-582 
    ISSN: 1572-8854
    Keywords: Dibenzo-18-crown-6 ; hetero bimetallic ; crown ether ; crystal structure ; ferric chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Slow evaporation of a solution of ferric chloride and dibenzo-18-crown-6 in 3∶1 CH3CN∶CH3OH produced single crystals of the title complex. This heterobimetallic crown ether complex, [Na(dibenzo-18-crown-6)][FeCl4], crystallizes in the monoclinic space group P2t/n with cell parameters (at 22°C)a=14.608(6),b=10.466(9),c=17.276(9)Å, β=91.47(6)°, andD calc=1.46 g cm−3 for Z=4. The structure consists of discrete ions with the shortest Na ... Cl distance a lengthy contact of 3.56(1)Å. The average Na...O separation is 2.69(3)Å. The [FeCl4]− anion exhibits a distorted tetrahedral geometry with an average Fe−Cl bond length of 2.16(2)Å.
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  • 17
    ISSN: 1572-8854
    Keywords: Amines ; crystal structure ; pentacycloundecane-8,11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structures of three compounds formedvia nucleophilic attack of a heterocyclic secondary amine on PCU-8,11-dione, with the concomitant intramolecular attack of one keto oxygen on the carbon of the other ketone, are presented. In all three compounds, the bridging oxygen contains substantial p-character, and the bonds to the “attacking” nitrogen are significantly shorter than would be expected.
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  • 18
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 25 (1995), S. 765-768 
    ISSN: 1572-8854
    Keywords: Sesterterpene ; scalaran ; crystal structure ; marine compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The molecular geometry of a tetracyclic sesterterpene has been determined by X-ray diffraction. The conformation of the aldehyde group as observed in the crystal structure supports the rationalization for the absence of aldehyde proton coupling in the nmr spectra of the compound. Crystal data: C28H42O5, M.W.=458.6; orthorhombic, P212121;a=10.797(2),b=29.270(9),c=8.033(1)Å,V=2538.7Å3,Dx=1.199 g cm−3;R=0.045 for 2287 observed reflections.
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  • 19
    ISSN: 1572-8854
    Keywords: Calixarene ; complex ; crystal structure ; chirality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound was obtained by treatment ofp-tert-butylcalix[4]arene with (+) camphorsulfonyl chloride in triethylamine and toluene. A (1∶2) complex with toluene has been found. Its structure has been determined by X-ray crystallography. Crystals are triclinic with space group P1,a=16.426(3),b=18.553(3),c=13.661(2) Å, α=94.78(2), β=110.76(2), γ=72.83(2)°,V=3720(2) Å3,d c =1.127 g/cm3 Z=2. Refinement based on 10495 observed reflections led to a finalR value of 0.100. The two independent molecules of calixarene in the asymmetric unit are in the cone conformation and the calixarene cavities are empty. The guest molecule occupies the interhost space. The norborane skelton of (+) camphorsulfonyl group is the same as ones found in literature. Only van der Waals interactions exist between the host and the guest molecules.
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  • 20
    Electronic Resource
    Electronic Resource
    Springer
    Journal of cluster science 6 (1995), S. 523-532 
    ISSN: 1572-8862
    Keywords: Molybdenum ; reduction ; seven-electron triangular cluster ; bridging sulfide ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The triangular six-electron cluster complex [Mo3S4Cl4(PEt3) x (thf)5] produced by the excision reaction of Mo3S7Cl4 with triethypholsphine is reduced by magnesium at − 20°C. Subsequent addition of dppe (=1,2-his(diphenylphosphino)ethane) to the reduced species affords a seven-electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3)]. The complex crystallizes in the space groupCm witha=17.170(6),b-19.878(6),c = 13.289(5)β = 121.73(2)°,V = 3858(2) A3, andZ = 2. The structure shows an almost equilateral triangle of three molybdenum atoms capped by a Sulfur atom and bridged by three sulfur atoms. The Mo Mo distances, ranging from 2.804(1) to 2.809(1) A are elongated ca. 0.04 A as compared with lose of a six-electron cluster complex with drape ligands. Two molybdenum atoms have a chlorine and a dppe ligands, and the other molybdenum atom bas a chlorine and a triethylphosphine ligands. The UV-Vis spectrum has a characteristic broad hand centered at 1410 n m, which is not observed for six-electron clusters. The ESR spectrum indicates the presence of an unpaired electron consistent with the formulation of the compound as a seven-electron cluster.
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  • 21
    ISSN: 1349-9432
    Keywords: organic crystal ; racemic form ; second-harmonic generation ; refractive index ; nonlinear optical coefficient ; crystal structure ; oriented-gas model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract Linear and nonlinear optical properties of racemic (±)2-(α-methylbenzylamino)-5-nitropyridine ((±)MBANP) single crystals have been comprehensively investigated and compared with those of the enantiomorph (–)2-(α-methylbenzylamino)-5-nitropyridine ((–)MBANP) crystals. (±)MBANP crystal exhibits very high chemical and physical stability, but relatively small nonlinear optical coefficients (d31 = 6.8 pm/V, d32 = 4.7 pm/V, d33 = 0.84 pm/V). A comparison between the nonlinear optical coefficients of (±)MBANP and (–)MBANP demonstrates the validity of the oriented-gas model in molecular crystals that neglects all the contributions from intermolecular interaction.
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  • 22
    ISSN: 1572-9001
    Keywords: MM3 ; PM3 ; MMX ; crystal structure ; norbonadienone ; distorted compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reaction of 4,5-didehydroacenaphthene with phencyclone yields the title compound, a stable dibenzo-fused norbornadienone (8). The X-ray structure of8 is presented and compared with the structure predicted from a MM3, PM3, and a MMX calculation. Thermal decomposition of 8 produces, 7,16-diphenylcyclopenta[d,e]tribenzo[a,h,j]anthracene (9), a hydrocarbon that is computed to have a significantly twisted polycyclic aromatic skeleton with 19 kcal/mole of strain energy.
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  • 23
    Electronic Resource
    Electronic Resource
    Springer
    Structural chemistry 6 (1995), S. 57-63 
    ISSN: 1572-9001
    Keywords: Hydrogen bonding ; carcinogen ; polycyclic aromatic hydrocarbon derivative ; dihydrodiol ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the weak carcinogen 5-methylchrysene-7,8-dihydro-7,8-trans-(e,e)-diol is reported. This molecule contains a distorted bay region as a result of the presence of the 5-methyl group as found in 5-methylchrysene and 5,6- and 5, 12-dimethylchrysene. One torsion angle in this bay region is 20
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  • 24
    ISSN: 1573-9171
    Keywords: resorcinol-based crown ethers ; crystal structure ; intramolecular nonbonded C-H...O contacts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 13- and 26-Membered crown ethers have been synthesized based on resorcinol and 1,8-dichloro-3,6-dioxaoctane. The products with substituents in the benzene ring have been prepared by alkylation of 13-membered crown ether. Complexing properties of the macrocycles have been studied with the use of ion-selective membrane electrodes. The structures of 13- and 26-membered crown ethers have been established by X-ray structural analysis.
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  • 25
    ISSN: 1573-9171
    Keywords: dihydroisoquinoline derivatives ; crystal structure ; electronic, IR, and1H NMR spectra ; quantum-chemical calculation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 3,3-Dimethyl-3,4-dihydroisocarbostyryl azine (2) has been synthesized by oxidation of l-hydrazino-3,3-dimethyl-3,4-dihydroisoquinoline (1). The crystal and molecular structures of compound 2 were determined. It has been established that in the solid state, compound2 exists as an azine tautomer. The IR, electronic, and NMR spectral data indicate that in solution the tautomeric form of2 does not change. A possible mechanism of the oxidation of1 to2 is suggested.
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  • 26
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    Pharmaceutical research 12 (1995), S. 337-341 
    ISSN: 1573-904X
    Keywords: 2-debenzoyl, 2-acetoxy paclitaxel ; docetaxel ; paclitaxel side-chain ; crystal structure ; solid state conformation ; intramolecular hydrogen bonding ; intermolecular hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystals of the C2-acetate analog of paclitaxel, grown from a mixture of isopropyl alcohol and methanol, belong to the space group P2l with a = 9.058(3), b = 18.306(5), c = 15.043(1) Å, β = 97.09(1)°, Z = 2, V = 2475.1(9)Å3, D calc = 1.269 gcm−3 and µ = 0.75 cm−1. The structure was determined by direct methods and refined to R(F) = 0.054 and wR(F) = 0.057 for 605 variables and 3496 observed reflections. The paclitaxel side chain possesses a conformation similar to that observed in the crystal structure of docetaxel (Taxotere®). A three dimensional network of hydrogen bonds is formed through solvent molecules and stabilizes the crystal lattice.
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  • 27
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    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 33-40 
    ISSN: 1573-1111
    Keywords: Calixarene-dye ; crystal structure ; inclusion compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-tetrakis-(4-nitrophenylazo)calix[4]arene-4-picoline (1∶4) complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupC2/c,a=24.9097) Å,b=8.425(6) Å,c=33.81(1) Å, β=101.13(2)°,D c =1.330 g/cm3,Z=4, finalR value =0.067. The cone conformation adopted by this azocalixarene is disturbed by the positions of the picoline molecules. Two of them are inside the macorocycle cavity and the two others are outside.
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  • 28
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    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 119-130 
    ISSN: 1573-1111
    Keywords: Calixarene ; complexation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new method is described for the synthesis of isolatedp-tert-butyldihomooxacalix[4]arene (CALO) with a 24% yield. The ability of CALO to form complexes in the solid state with small neutral molecules has been studied; the potential guests were common solvents bearing various chemical functions. The powder obtained after evaporation of the solvent has been characterized by the X-ray powder diffraction technique. Analysis of the patterns shows the non-complexation of linear alkanes and alcohols, but formation of complexes when the guest is cyclic or when it bears an amine or a ketone function. As illustration of the possible arrangement of molecules in complexes, the structure of the 1:2 complex with tetrahydrofuran (THF) is presented: the crystals are monoclinic, space groupP21/c,a=9.459(2) Å,b=17.286(2) Å,c=30.469(6) Å, β=92.52(2)o,V=4977(2) Å3,Z=4,D c=1.099 Mg m−3, λ=1.54178 Å, μ=5.6 cm−1,R=0.086 for 3590 reflections withF〉4σ (F); one of the THF molecules is inside the cavity of the macrocycle, while the other, in the interhost space, exhibits disorder. In the CALO molecule, three out of the fourtert-butyl groups are disordered which may induce the disorder of the THF molecule.
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  • 29
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    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 187-201 
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; gossypol ; crystal structure ; hydrogen bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the inclusion compound of gossypol withn-valeric acid as a guest molecule has been determined by X-ray structure analysis. The crystals of C30H30O8·(C5H10O2)2, are triclinic, space group $$P\bar 1$$ ,a=6.912(2),b=14.506(3),c=19.387(4) Å, α=78.85(2)°, β=83.92(3)°, γ=86.78(3)°V=1895(1) Å3,Z=2,D x=1.267 g cm−3, μ (CuK α)=0.768 mm−1,T=292 K. The structure has been solved by direct methods on intensity data collected for a twinned crystal and refined to the finalR value of 0.062 for 1606 observed reflections and 470 refined parameters. Gossypol-n-valeric acid (1/2) coordinato-clathrate is not isostructural with any of the previously investigated gossypol inclusion compounds but shows some structural similarities to gossypol-acetic acid (1/1). The host and one of the carboxylic acid molecules are connected via hydrogen bonds into molecular assemblies of a column type which are further bonded to centrosymmetric dimers of the secondn-valeric acid molecule. In effect, host and guest molecules are assembled into layer-type H-bonded aggregates. Structural features common to gossypol-n-valeric acid (1/2) and other earlier reported gossypol inclusion compounds are discussed.
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  • 30
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    Journal of superconductivity 8 (1995), S. 595-598 
    ISSN: 1572-9605
    Keywords: (Ba/K)BiO3 ; lattice dynamics ; electron phonon coupling ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract The Lattice dynamics of Ba.6K.4BiO3 was investigated by inelastic neutron scattering on a superconducting single crystal (T c =26 K (midpoint)). At low frequencies the dispersion curves are very similar to those observed in BaPb.75Bi.25O3. Differences were found in the bond bending vibrations of the BiO6 octahedra which indicate that the binding in the K-doped compound is more ionic. Rather anomalous features were observed in the high frequency Bi-O bond stretching vibrations which resemble those observed in the high T c cuprates La1.85Sr.15CuO4 and YBa2Cu3O7. The observed frequency shifts are interpreted as the consequence from a strong electron phonon coupling. The data are compared to the results obtained on non superconducting Ba.98K.02BiO3.
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  • 31
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    Proteins: Structure, Function, and Genetics 23 (1995), S. 525-535 
    ISSN: 0887-3585
    Keywords: DNA-protein interaction ; crystal structure ; transcription factor ; gene regulation ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Many transcription factors have an α-helix that binds to DNA bases in a specific fashion. The DNA-binding geometry of these recognition helices varies substantially. We define a set of parameters to describe the binding geometry of recognition helices and analyze specific stereochemical elements that determine particular geometries. Because the convex surface of the helix must fit into the concave surface of the DNA major groove, the number of degrees of freedom of the recognition helix is reduced from a possible six to a single angle, which we call α. The chemically interacting DNA bases and amino acid residues must lie along a common line and have the same spacing along it. This pairing of base positions with residue positions seems to restrict the binding geometry further to a set of discrete values for α. © 1995 Wiley-Liss, Inc.
    Additional Material: 6 Ill.
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  • 32
    ISSN: 1573-904X
    Keywords: HMG-CoA reductase inhibitor ; SQ-33600 ; crystal structure ; hydrates ; solid-state fluorescence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It has been shown previously that the disodium salt of a new HMG-CoA reductase inhibitor (SQ-33600) is capable of existing as a number of hydrate species [1]. Three crystalline solid hydrates and one liquid crystalline phase have been identified, each having a definite stability over a defined range of humidity. These forms have been found to exhibit varying fluorescence properties in their respective solid states, with differences in bandshapes and intensities being noted for each. These spectral variations have been correlated with the known pseudopolymorphism of the compound.
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  • 33
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    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 145-154 
    ISSN: 1573-1111
    Keywords: tert-Butylamine 7.25 H2O ; amine hydrate ; semi-clathrate ; clathrate hydrate ; hydrate ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Of the various hydrates oftert-butylamine, the title compound has been identified as the second-highest, melting incongruently at −19°C. Its crystal structure (orthorhombic, space groupPca21,Z=32 formula units per unit cell,a=24.80,b=16.440,c=25.29 Å) and the exact composition have been determined from X-ray diffraction at −150°C. The hydrate is a rather complex semi-clathrate, with the amine molecules not merely encaged, but also hydrogen-bonded, in a three-dimensional water host structure, which in turn is not fully four-connected. Nevertheless, it bears a clear relationship to the basic and genuine clathrate-hydrate cubic 12 Å type.
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  • 34
    ISSN: 1573-1111
    Keywords: 18-crown-6 ; diaminofurazane ; crystal structure ; host-guest complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray—diffraction study is reported for two molecular complexes containing 3,4-diamino-1,2,5-oxadiazole as guest (G) with 18-crown-6 (18-C-6) andcis-anti-cis-dicyclohexano-18-crown-6 (DCH-6B) as host. Both complexes are of the polymeric-chain structure with the guest molecule bridging two crown neighbours. ComplexI: [18-C-6*G*H2O], 1∶1∶1, monoclinic,P21/n,a=8.171(1),b=15.042(2),c=16.209(6) Å, β=101.15(2)°, finalR-factor 0.068. ComplexII: [DCH-6B*G], 1∶1, monoclinicC2/c,a=21.212(4),b=9.380(2),c=13.049(3) Å, β=108.61(3)°, finalR 0.047.
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  • 35
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    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 211-219 
    ISSN: 1573-1111
    Keywords: (R, R)-Tartaric acid derivatives ; host-guest compounds ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract TheO, O′-dibenzoyl derivative of (R, R)-tartaric acid shows a good inclusion ability for diethyl and di-n-propol ethers. The two crystalline inclusion compounds have 1:1 stoichiometry and reveal isomorphous structures. Hydrogen bonded host molecules form chains running along thez axis of the unit cell and guest molecules join to these chains by short O−H...O hydrogen bonds. Hydrogen bonding in the crystals is characterized by a C(7)D first-order network. The ether molecules are in a fully extended conformation. They are accommodated in channel-like voids running along thex axis. Atomic displacement parameters are significantly larger for diethyl ether than for the di-n-propyl ether molecule reflecting less dense packing for this inclusion compound.
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  • 36
    ISSN: 1573-1111
    Keywords: Bridged calix[4]arene ; caesium complex ; ditopic receptor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures of two binuclear complexes between caesium and 1,3-calix[4]-bis-crowns have been determined. Cs2 Bis-benzoC6(NO3)2. 3CHCl3 (1) in whichBis-benzoC6 is 1,3-calix[4]-bis-benzo-crown-6, crystallizes in the orthorhombic system: space groupPca2 1 a=19.513(10),b=15.382(5),c=23.708(9) Å,V=7116(5) Å3,Z=4. Refinement led to a final conventionalR value of 0.065 for 2321 reflections. The structure of (1) is analogous to those already reported withBis-C6, (in whichBis-C6 is, 1,3-calix[4]-bis-crown-6) and NO 3 − as a counter-ion. Cs2 Bis-C6(NCS)2 (2) crystallizes in the monoclinic system: space, groupC2 a=36.57(2),b=11.47(1),c=13.65(1) Å, β=109.03(5)°.,V=5415(6) Å3,Z=4. Refinement led to a final conventionalR value of 0.063 for 2227 reflections. Compound (2) is made of dimers bridged by a disordered NCS− ion. The crown ether chain conformations are discussed.
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  • 37
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The basic sites of various oxide catalysts for the oxidative dimerisation of methane were studied by FTIR spectroscopy of adsorbed molecular probes (chloroform and CO2). The methods used are compared and the advantage of CO2 as probe for specifying the basic sites is demonstrated. The strengths of the basic sites were seen to correlate with the spectral parameters of the surface carbonates. Differences in spectral responses of carbonates are attributed to the different states of oxygen participating in their formation. The concentration of the strongest sites was estimated. A study of the catalytic activity of this system indicates that the system's activity in oxidative methane coupling depends on the presence and concentration of strong basic sites on the catalyst surface.
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  • 38
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    Chemical Engineering & Technology - CET 18 (1995), S. 425-433 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Turbidimetry has proved to be an efficient method for the quantitative study of powder agglomeration for particle sizes in the region of 1 μm. This work presents a new application of the technique for the agglomeration of α-alumina in water and in n-heptane. The method of determining the kinetic parameters of agglomeration from the initial time-evolution of turbidity is explained.Turbulent flow in the reactor has also been characterised by laser anemometry. From the turbulence intensity, the number of collisions per unit time is calculated and the agglomeration rate can therefore be determined.Good agreement is found between the values obtained respectively from turbidimetric and hydrodynamic measurements. Addition of KOH modifies the zeta potential of alumina in water and influences the agglomeration kinetics. This can also be quantitatively characterised by turbidimetry. The experimental results obtained for alumina particles of diameter 0.3 μm and 1 μm are interpreted according to the DLVO model of interaction between particles.
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  • 39
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    Particle and Particle Systems Characterization 12 (1995), S. 75-80 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In this paper a reconstruction method is presented, which allows the calculation of three-dimensional temperature and velocity fields in an industrial furnace by measuring the propagation times of sound waves. Transceiver systems working in a coal fired power station and reconstructing two-dimensional fields are well known. Referring to these real conditions, the idea was to use two measurement planes situated over each other and projecting the fields in the volume between them. Some simulations show that weak inhomogeneous fields can be well reconstructed, whereas in the presence of turbulent flow and noise a reconstruction is critical.
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  • 40
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    Particle and Particle Systems Characterization 12 (1995), S. 95-104 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A tutorial review of diffraction tomography is given along with an overview of recent advances of this technique in borehole geophysics, ultrasonic imaging, and optical microscopy. First, the basic principles of diffraction tomography are presented. Then, we discuss a generalized inversion algorithm, valid for irregularly spaced data and a non-uniform background, and present reconstructions based on ultrasonic water tank data and underground georadar data. Next, we discuss a hybrid filtered backpropagation algorithm for ultrasonic and optical imaging. Quantitative images, based on experimental data, are presented of objects embedded in water or in biological tissue and probed by ultrasound, and of fibers embedded in an index matching liquid and probed by laser light.
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  • 41
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    Particle and Particle Systems Characterization 12 (1995), S. 194-197 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Flow agents are widely used in industry, such as the plastics and pharmaceutical industry, to promote the flow of cohesive powders. Few studies of the quantitative effects of the flow agents on the flow of the powder have been reported. In this communication the effect of silica flow agents on the flow of a plastic powder is studied by means of avalanching behaviour. The avalanching behaviour of the powder as modified by the silica flow agents is summarized using descriptive parameters based on the calculation of fractal dimensions in data space and phase-space strange attractors. The structure of the strange attractors are shown to be statistically self-similar and-effective descriptors of the change of rheology caused by the presence of the flow agents.
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  • 42
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    Particle and Particle Systems Characterization 12 (1995), S. 212-212 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 43
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    Particle and Particle Systems Characterization 12 (1995) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 44
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    Particle and Particle Systems Characterization 12 (1995), S. 213-213 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 45
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    Particle and Particle Systems Characterization 12 (1995), S. 148-157 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Among the most important characteristic properties of disperse systems such as latices, pigments, ceramic materials or drug formulations are the particle size and the particle size distribution. To measure these quantities, several methods and measuring instruments based on different physical principles are available. These include turbidimetry, dynamic and static light scattering, electron microscopy with image analysis, ultra- and disc centrifugation, light diffraction and the electrical sensing zone method. All these measuring techniques are doubtless necessary because of the large product variety and the broad particle size range. However, some problems arise if different techniques are used and the results are compared uncritically without considering to the application range and the resolution of the methods. An extensive comparative test was therefore carried out using seven latices in the submicron range with defined monomodal, bimodal and hexamodal particle size distributions. The most important methods of determining average particle size values and particle size distributions were tested and compared. Of the methods to determine only average particle sizes, turbidimetry is the most efficient, followed by dynamic light scattering with cumulants evaluation. Static light scattering only yields accurate results for small particles with narrow particle size distributions. Of the methods to determine particle size distributions, ultracentrifugation and, somewhat less, disc centrifugation and electron microscopy with image analysis are the most efficient. Dynamic light scattering only yields reliable results in the case of small particles with narrow distribution curves. Light diffraction and the electrical sensing zone method are less suitable for the submicron range.
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  • 46
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    Particle and Particle Systems Characterization 12 (1995), S. 170-170 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 47
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    Particle and Particle Systems Characterization 12 (1995) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 48
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    Particle and Particle Systems Characterization 12 (1995), S. 179-187 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The dynamic shape of coarse particles was determined by catastrophic tumbling studies performed in a rotating cylinder. Here, the dynamic shape was defined as the deviation from ideally regular and predictable tumbling behaviour.The data suggested that even with a comprehensive description of a static particle its transport properties cannot be accurately predicted.The fractal dimension in data space of the time series of events presents a method that can identify limits of predictability, and thus show regions that should be avoided to- minimise the emergence of chaotic behaviour.
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  • 49
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    Particle and Particle Systems Characterization 12 (1995), S. 188-193 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The paper reports on the particle. sampling efficiency of the inlet system for the Aerodynamic Particle Sizer (TSI, Inc., St. Paul MN). Large particles are depleted from the sampled aerosol by two mechanisms: super-isokinetic sampling at the entrance of the inlet, and inertial impaction on the inner nozzle. A fluorometric technique was used to separately characterize these mechanisms. Numerical studies were also performed. The experimental results show that the inlet's overall efficiency drops from around 90% for 3 μm particles to less than 45% for particles larger than 10 gm. Several high efficiency inlets were developed and tested. These inlets provide higher sampling efficiencies, but reduce the instrument's sizing resolution. Measurements of 7.3 μm oleic acid particles with a high efficiency inlet showed a 5% spread in measured diameter at 50% count, while less than a 1076 spread was observed using the standard inlet. It was also found that the super-isokinetic condition reduces particle losses on the inner nozzle. The standard inlet is recommended for verifying test aerosol monodispersity. An alternative to the standard inlet is suggested for measurement of size distributions.
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  • 50
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    Particle and Particle Systems Characterization 12 (1995), S. 204-206 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Small quantities of Larostat 519, an anti-static agent, were added to four samples of a commercial organic powder which was giving flowability problems believed to be caused by electrostatics. The effects on standardised bulk densities, on the Hausner Ratio, and on the behaviour of the samples when exposed to various controlled relative humidities in an experimental rotating inclined pan, were significant, and are reported and interpreted.
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  • 51
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    Particle and Particle Systems Characterization 12 (1995), S. 198-203 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A simple technique is presented for determining the zeta potential of large particles ( 〉 20 μm) by streaming current measurements. The method has the advantage of not requiring correction for surface conductivity. The theory involves a description of pore space by either Darcy's law or the Kozeny-Carman equation. The simplifications introduced by assimilating the pore space to a bundle of capillary tubes are discussed. Results are presented for the variation of zeta potential with pH and ionic strength for a sieve cut of spherical glass beads and two different samples of irregular particles of silicon carbide.
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  • 52
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    Particle and Particle Systems Characterization 12 (1995), S. 295-298 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Concerning the use of air classifiers with cut sizes in the micron range and lower, it is necessary to disperse the feed material properly in an air flow to avoid agglomerates larger than the desired cut size. Commonly used dispersing devices such as injectors use large amounts of air. To reduce the size and costs of the subsequent air classifiers, two new types of dispersing systems were developed, one design being related to a brush feeder and the other to a pin mill. Both apply mechanical rather than fluid mechanical forces in the dispersion process. The brush disperser achieves the same size distributions as the pin mill disperser with much less machinery. Its properties as a feeding and dispersing system are shown and its ability to disperse particles in the submicron range is confirmed by two independent particle size analysis systems: a new diffraction spectrometer and an impactor.
    Additional Material: 7 Ill.
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  • 53
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    Particle and Particle Systems Characterization 12 (1995), S. 304-308 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The calibration of an optical particle counter (OPC) by means of the Aerodynamic Particle Sizer APS (TSI, Model 3310) was investigated. The pulse-height distribution and the aerodynamic size distribution were measured by parallel use of an OPC and the APS. A calibration curve was obtained by comparison of the two different cumulative distribution curves. First calibration results are presented for spherical particles (water droplets and glycerine droplets): A comparison of these results with Mie calculations and aerodynamic calibrations by means of sampling cyclones shows good agreement. Furthermore, measurements were carried out with non-spherical particles. Quartz dust was used for these measurements. In order to calibrate the OPC by means of the APS, the behaviour of both devices was investigated.
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  • 54
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    Particle and Particle Systems Characterization 12 (1995), S. 324-326 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 55
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A simple design of an adiabatic reactor for the production of hydrogen from methanol without external heating has been explored. Heat and steam are generated by oxidising part of the methanol and are removed in the process of reforming methanol to hydrogen. The reactor design emphasises the degree of control that can be achieved in a two-bed system by controlling the air to methanol and water to methanol ratios in the feed. Predictions of the model are compared with experimental testing to allow optimisation of the process. Up to 75% of methanol can be converted to hydrogen.
    Additional Material: 9 Ill.
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  • 56
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Two vanadia/titania catalysts, containing 1 and 8 wt% vanadia on anatase, have been investigated for the selective oxidation of o-xylene to phthalic anhydride. In a comparative study, activity and selectivity in o-xylene oxidation were measured using an integral reactor and a reactor with external product recirculation, with the objective of studying the influence of backmixing in the latter on the reaction behaviour. Adsorbed surface species were investigated by means of in-situ diffuse reflectance FT-IR spectroscopy, using an environmental chamber which corresponds to an integral reactor. No difference in activity and selectivity in o-xylene oxidation was observed between the two catalysts. FT-IR studies showed adsorbed o-xylene, benzoate and a high concentration of phthalic anhydride on the surface of both catalysts. o-Xylene oxidation follows a sequential reaction path, with o-tolualdehyde as the first intermediate and phthalide, phthalic anhydride and maleic anhydride as sequential products. No evidence was found for a direct oxidation-path of o-xylene to phthalic anhydride. Total oxidation products CO and CO2 are formed by direct oxidation of the o-xylene and by oxidation of the reaction products. Due to greatly reduced concentration and temperature gradients, the recycle reactor proved to be highly suitable for studying the extremely exothermic oxidation of o-xylene.
    Additional Material: 5 Ill.
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  • 57
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    Chemical Engineering & Technology - CET 18 (1995), S. 63-67 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Influences of different parameters on diameter and height of RDC column and on mass transferred from unit column volume were investigated. The results of the calculation can assist designers in making proper choice for the operating range of RDC columns.
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  • 58
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    Chemical Engineering & Technology - CET 18 (1995) 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
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  • 59
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    Chemical Engineering & Technology - CET 18 (1995), S. 110-117 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The octane enhancer tertiary amyl methyl ether (TAME) is produced by liquid phase synthesis from methanol and a mixture of isoamylenes, namely 2-methyl-1-butene and 2-methyl-2-butene, using a sulfonic acid ion exchange resin as catalyst. Three reactions take place simultaneously in TAME synthesis: etherification of the two methylbutenes and their isomerisation. In order to study the equilibrium of the multiple reactions in TAME synthesis, the thermodynamic properties of the compounds in the liquid phase and equilibrium constants were calculated using a modified UNIFAC method to describe the nonideality of the system. Four parameters influencing the equilibrium conversion were derived and discussed in detail. Supplemental experiments were performed at three temperatures in the range from 303 to 343 K and at different initial molar ratios of educts. Equilibrium conversions of methanol were determined from these experiments and compared with calculated values. At 298 K the predicted activity based equilibrium constant was 22.9 for TAME synthesis from 2-methyl-1-butene and 1.6 for TAME synthesis from 2-methyl-2-butene; for isomerisation of 2-methyl-1-butene to 2-methyl-2-butene a value of 14.3 was obtained.
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  • 60
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    Chemical Engineering & Technology - CET 18 (1995) 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
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  • 61
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: An approach to feedforward distillation control based on inverse computation of nonlinear stage models is presented. The feedforward model calculates dynamic trajectories of manipulated variables from measured disturbances and product purity set points independently of the control configuration. Because the model includes the dominant dynamics and nonlinearities of the column, dynamic decoupling of the control loops is achieved. A superimposed linear controller only has to compensate model uncertainties and disturbances that cannot be measured. The proposed approach improves the control performance. Simulation studies show the applicability of the method to multicomponent distillation as well as to distillation trains. Experiments on a pilot plant scale binary distillation column verify the simulation results.
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  • 62
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    Chemical Engineering & Technology - CET 18 (1995), S. 210-215 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper describes an original system for automated solid-phase peptide synthesis (SPPS) that was developed in our laboratories. The synthesizer is equipped with separate activator and batch reactors, and was designed to operate under either manual or computer control. Two metering pumps, which constitute the core of the entire apparatus, provide for the delivery and transfer of reagents and solvents in the appropriate quantities and in the correct sequence, and permit simultaneous condensation and activation operations that result in considerable time saving. Various applications to the synthesis of biologically important peptides, utilizing the most widely used strategies in SPPS, are presented as examples of this improved technology.
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  • 63
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    Chemical Engineering & Technology - CET 18 (1995), S. 248-255 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In this work a Sulzer structured packing, Mellapak 250Y, was studied for applications in the field of absorption. A new model was proposed which makes it possible to estimate the packing surface that actually takes part in the process. In the course of these studies, new experimental data were obtained relating to the absorption of 1,1,1-trichloroethane using Genosorb 300, a mixture of polyethylene glycol dimethyl ethers produced by Hoechst S.p.A., as absorption liquid. The results obtained with the proposed model are in agreement both with the experimental measurements made in the course of the work and with experimental absorption measurements reported by other authors on water systems.
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  • 64
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    Chemical Engineering & Technology - CET 18 (1995), S. 278-283 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Deactivation kinetics and coke removal kinetics were derived from experimental studies on the disproportionation of ethylbenzene with a protonated Y-faujasite (Z-14) in a loop reactor under supercritical conditions. Derivation of the steady state kinetics of ethylbenzene disproportionation permitted determination of the catalyst activity. At small educt mole fractions of ethylbenzene, owing to the modest removal of coke the deactivation kinetics can be described by a power relationship. The rate of coke removal can be correlated with the activity and the deactivation rate of the catalyst.
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  • 65
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    Chemical Engineering & Technology - CET 18 (1995) 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
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  • 66
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    Chemical Engineering & Technology - CET 18 (1995), S. 337-342 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Neural networks can be an attractive alternative to mathematical modelling of complex and poorly understood processes if input/output data can easily be obtained. Woodchip refining falls into this category. The mechanism of the refining process is still being studied and no thorough models have yet been developed. A feed-forward neural network is proposed for modelling of woodchip refiners. The outputs predicted by the neural network are compared with industrial refiner data. It is also shown that a modified neural network structure can be used to optimize refiner operation and product quality. The advantages and disadvantages of neural network model application in simulation and optimization of industrial processes are discussed.
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  • 67
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    Chemical Engineering & Technology - CET 18 (1995), S. 364-369 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Fluid catalytic cracking, a common secondary process employed in the petroleum industry, is used to convert heavier feedstocks into products such as liquefied Petroleum Gas (LPG), motor gasoline, diesel etc. The present study focuses on developing a three lump fraction kinetic model to estimate the yield of C5 up to 370°C cut (motor gasoline and middle distillates). A Micro Activity Test (MAT) apparatus was used to estimate the parameters in the kinetic model. The study is useful in evolving a procedure to simulate plant performance using experimental data obtained in the MAT apparatus for a particular catalyst and feedstock in terms of the product yield pattern.
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  • 68
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    Chemical Engineering & Technology - CET 18 (1995), S. 414-419 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Ethane was converted into aromatic hydrocarbons on H-ZSM-5 and Zn-ZSM-5 at 773 K in a flow reactor system using nitrogen and hydrogen as carrier gases. Residence time was varied by changing catalyst weights to obtain information about primary and secondary reaction steps. On H-ZSM-5 ethane conversion proceeds via formation of ethene and subsequent oligomerization. Oligomers undergo fast isomerization, cracking and cyclization leading to a broad spectrum of aromatics. Methane is a secondary product. Dehydrogenation reactions proceed irreversibly. Introduction of zinc species significantly enhances the aromatization activity of H-ZSM-5 on the one hand and causes a change of reaction mechanism on the other. Oligomerization of olefinic intermediates can take place at zinc sites. In nitrogen, aromatization of C6 olefins is faster than isomerization and cracking of these oligomers. Dehydrogenation steps proceed reversibly. On using hydrogen as the carrier gas over Zn-ZSM-5, the conversion of ethane as well as the formation of aromatics decrease. Furthermore, aromatics richer in hydrogen (especially C8 aromatics) are then formed preferentially.
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  • 69
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    Particle and Particle Systems Characterization 12 (1995) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 70
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    Particle and Particle Systems Characterization 12 (1995), S. 10-15 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The performances of three ambient PM10 samplers were studied at three monitoring stations in Taiwan. It was found that differences in the daily measured PM10 concentrations of the SA 1200 and Wedding high-volume samplers are now within ± 10% since the former now has a closer cut-point to the latter than in the earlier SA 321 A model. The Wedding beta gauge automatic sampler was found to be applieable in rainy and humid weather conditions in Taiwan. Its daily PM10 concentrations are typically within ± 10% of those of the Wedding highvolume sampler. The particle loading effect of Wedding highvolume and beta gauge samplers was found to be important. To avoid sampling errors due to the loading effect with ambient PM10 samplers, they must be cleaned regularly at an interval depending on the ambient particulate level.
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  • 71
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    Particle and Particle Systems Characterization 12 (1995), S. 28-37 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A method is described for mapping the perimeter of shapes as a sequence of connected X & Y coordinates. It operates by tracking, in tandem, along a dilated outline of the shape and the true outline, maintaining contact between both tracks. This combination permits the complete mapping of binary shapes regardless of their complexity. The resulting sequence of X & Y coordinates form an 8-connected map of the outline, which can then be used to obtain fractal dimensions using structured walks. The method requires a digitised image that has been converted into a binary form and the ability to read the values of individual pixels from the digitised binary image. In addition a number of approaches for increasing the efficiency of the twin tracking algorithm are outlined.Obtaining fractal dimensions from a structured walk based on a fully mapped perimeter increases the accuracy of the measured fractal dimensions, extends the range of step sizes over which measurements can be made and permits a highly detailed examination of the perimeter.
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  • 72
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    Particle and Particle Systems Characterization 12 (1995), S. 38-41 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The possibilities of applying specific turbidity and turbidity theoretical computations of light-scattering characteristics, the ratio methods in the distributional analysis of PVC and SiO2 exact Lorenz-Mie theory was applied. A good correlation with dispersions with spherical particles are discussed. The calculation of the best estimates of distribution function parameters was found were performed numerically using the simplex method. For theoretical computations of light-scattering characteristics, th exact Lorenz-Mie theory was applied. A good correlation with the results of angular light scattering and electron microscopy was found.
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  • 73
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    Particle and Particle Systems Characterization 12 (1995) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 74
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    Particle and Particle Systems Characterization 12 (1995), S. 58-58 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 75
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    Particle and Particle Systems Characterization 12 (1995), S. 3-9 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A method is described by which the angular orientation distribution of fibrous particles carried in a gaseous stream may be investigated. The method is based upon the interpretation of the spatial intensity distribution or scattering profile of laser light scattered by individual fibres. The scattering instrument used to capture the profiles is described, and the mathematical computation required to ascertain the orientation of each particle at the measurement point is detailed. Illustrative results are given for a study of airborne micromachined silicon particles of 12 μm length and 1.0 μm by 1.5 μm cross-section. The method is currently being employed by the authors to investigate ways of improving the orientation control over nonspherical particles in systems such as aerodynamic particle sizers and particle shape classifiers, since lack of particle orientation control is known to adversely affect the measurement accuracy of both these types of instrument.
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  • 76
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A biaxial tester was utilized in order to characterize mechanical powder behaviour. Tests were aimed at characterizing the virgin consolidation behaviour of CRM 116 limestone powder, standardized by the Community Bureau of Reference (BCR). The tests indicated that the virgin consolidation behaviour of the powder can be represented by means of topographic maps and surface plots in the principal stress space irrespective of the consolidation stress paths. Resulting strains and bulk densities can also be represented in the same manner. Reloading tests were also carried out on samples consolidated by following different stress paths (consolidation procedures). By applying stresses to the previously consolidated samples and determination of points of initial plastic deformations, the yield surface for each specific type of consolidation was drawn. These tests revealed anisotropic behaviour of the powder, depending on the type of consolidation.
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  • 77
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    Particle and Particle Systems Characterization 12 (1995), S. 42-45 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The use of a compact cylindrical piezoelectric transducer in the jet dispersion unit of the sorting system of an optical or electrical particle size analyser is discussed. Solving two equations for the shift distribution in a piezoelectric transducer with a running fluid chamber, important expressions for the vibrational velocity of acoustic terminal, mechanical impedance, of the stable part of the jet are obtained. The practical application of this technique is illustrated by the calculation of desi parameters for an industrial dispersion unit used in an H.cytophotometer (Ortho Instruments, USA). Good agreement between theoretical and experimental results is shown.
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  • 78
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    Particle and Particle Systems Characterization 12 (1995), S. 54-54 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 79
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    Particle and Particle Systems Characterization 12 (1995), S. 46-53 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The efficiency of reactors fed with particulate mixtures is often reduced by segregation of solids. Placing continuous mixers directly ahead of a reactor may be a solution to this problem. The performance of such mixers can be monitored for appropriate binary solids systems with an optical in-line measuring system. The tracer concentration (SiC or Irgalite) in Al(OH)3 was registered with high time resolution, thus making possible an extended statistical analysis of mixing processes using the power density spectrum. Experimental mixers with a maximum -throughput of 300 kg/h were fed with a fluctuating tracer concentration and the variance reduction ratios were determined. A model was developed that takes into account feeding constancy, residence time distribution and the limited homogeneity of particulate mixtures. Diagrams for continuous solids mixing processes are derived therefrom. They demonstrate the importance of high-accuracy feed-rate control.
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  • 80
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    Particle and Particle Systems Characterization 12 (1995), S. 59-67 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: During the past decade, the application of Nuclear Magnetic Resonance (NMR) imaging techniques to problems of relevance to the process industries has been identified. In the context of particle technology, NMR imaging, in addition to the more routinely used techniques of Pulsed Gradient Spin Echo (PGSE) NMR and NMR spectroscopy, offer new methods of characterising pore structure, adsorption and diffusion processes within particles and packed beds of particles, as well as enabling time-resolved in-situ study of processes such as twophase flow, aggregation, polymerisation, crystallisation and phase separation phenomena. This paper reviews recent work in these areas, and also highlights the new insights NMR imaging can give us regarding the characterisation of porous materials, and the influence of the structure of the pore space on the transport processes occuring within a given porous solid.
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  • 81
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    Particle and Particle Systems Characterization 12 (1995), S. 68-74 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: An overview of Electro-Magnetic Tomography (EMT) using mutual inductance measurements is presented. The paper reviews the technique and principle of operation and gives a description of three case studies, which cover some of the generic design considerations and which illustrate the potential variety for inductive EMT systems. Results from the systems are described. These systems are presently experimental and possible future developments and applications are discussed.
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  • 82
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    Particle and Particle Systems Characterization 12 (1995), S. 232-236 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The use of a rotating disc to study the avalanching behaviour of a powder is discussed. It is shown that the strange attractor plotted in discreet time maps summarizes useful information on the rheological behaviour of powders and powder mixtures. In particular it is shown that the avalanching behaviour is related to the particle size distribution of the powder and that one can study the changes in rheological behaviour as another powder is mixed with it. The strange attractor patterns generated are dependent upon the environmental conditions under which the experiments are carried out. For this reason the measurements are referred to as an assessment of the holistic powder rheology. The potential use of the disc to study the holistic rheology of powder systems is outlined.
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    Particle and Particle Systems Characterization 12 (1995), S. 264-266 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 84
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    Particle and Particle Systems Characterization 12 (1995), S. 242-256 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The theory of scattering of a first-order Gaussian beam by an infinite cylinder with arbitrary location and arbitrary orientation is presented. A component of the theory is the use of the theory of distributions.
    Additional Material: 3 Ill.
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  • 85
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    Particle and Particle Systems Characterization 12 (1995), S. 268-268 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 86
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 274-278 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In this paper, a new approach using small angle light scattering to study the structure of large micron sized flocs is described. The flocs were made up from uniformly sized, approximately spherical hematite particles, induced to aggregate using 250 mM KCl to ensure that growth was governed by diffusion limited aggregation alone. The fractal dimensions of the hematite aggregates changed from 1.73 to 2.23 ± 0.05 as the aggregation proceeded, indicating that restructuring occurred during aggregation. The fractal dimensions obtained from the small angle light scattering technique are compared with those obtained from the combination of volume fraction and floc size measurement. The steady state fractal dimensions (2.23 ± 0.05) obtained by small angle light scattering are comparable to the fractal dimensions obtained from determining the slope of the relationship between floc volume fraction and floc size (2.09 and 2.14 ± 0.05). The discrepancy between the fractal dimensions obtained by these techniques during the initial stages of aggregation is due to the fact that the latter method measures the average fractal dimensions, whilst the former method measures the fractal dimensions at any particular instant.
    Additional Material: 4 Ill.
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  • 87
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 279-283 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: It is generally recognized that fundamental limitations make data analysis for dynamic light scattering (DLS) not straightforward. In addition to experimental problems such as multiple scattering, number fluctuation and noise, there are intrinsic problems. Data analysis is a so-called reverse problem which, owing to the mathematical equations, becomes “allergic” to noise (an ill-posed inverted problem). In an attempt to overcome at least some of these limitations, a software solution was developed. This mainly aimed to implement a tool that makes it easy to evaluate physically plausible solutions, rather than to determine many (less accurate) parameters related to the size distribution. One of the major goals was to create a “white-box” program. The software is in essence an easy-to-use graphical interface between user and computer. The most important motivation to apply the concept of on-line simulation is the limited information content of DLS autocorrelation functions. In the present approach, the user, rather than the software, has to evaluate the physically plausible solutions and select the most appropriate one. The computer becomes a mirror that calculates but leaves the decision making to the user. Using this software environment, the resolving power of the technique in ideal and noisy conditions was investigated. Results were obtained for monomodal samples where the mean diameter seems to be far more reliable than the polydispersity. For bimodal samples, the convergence of the solution to a monomodal distribution was observed when the noise level increased. The goal is to put into perspective the results as obtained in most “black-box” software without having to use heavy mathematical approaches. One of the major applications is the use of the program as an interactive introductory tool to become acquainted with the power and, above all, with the limitations of DLS.
    Additional Material: 6 Ill.
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  • 88
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 207-211 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: To reduce errors when measuring sizes of particles in light-scattering counters and phase-Doppler analysers, the hydrodynamic focusing of particle trajectories in relation to the centre of the measurement zone is used. This focusing is effected in a special running-type chamber. Equations describing the mechanical energy of liquid flows running through a running-type chamber have been compiled. By solving a system of such equations, relatively simple equations for engineering calculations of the coefficient of hydrodynamic compression of particle trajectories in relation to the centre of the measurement zone have been obtained. Results of experimental research are given and the application of the proposed technique for designing improved running-type chambers with one and two “sheaths” is demonstrated.
    Additional Material: 5 Ill.
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  • 89
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    Particle and Particle Systems Characterization 12 (1995), S. 216-216 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 90
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 237-241 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The finely stratified sphere model was used to calculate electromagnetic fields inside homogeneous and radially inhomogeneous spheres which are illuminated by electromagnetic plane waves. A complete picture of the internal fields is given for spheres whose diameters are comparable to the wavelength (α = 1.5 and 5, where α = 2 πa/γs is the size parameter of the sphere) and spheres whose diameters are much larger than the, wavelength (α as high as 150), for coated spheres (spheres composed of a homogeneous core and a homogeneous shell) and gradient-index spheres (spheres with a continuous of refractive index), for spheres at states of morphology-dependent resonances (MDRs) and those at non-resonant states.
    Additional Material: 10 Ill.
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  • 91
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    Particle and Particle Systems Characterization 12 (1995), S. 225-231 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A method has been developed to increase the sensitivity of phase Doppler interferometry-based particle sizing systems to small particles in the presence of a spray containing large and small droplets; an important consideration when using seed particles to track the gas-phase velocity in multi-phase flows. The method, applicable to PDPA systems configured to operate in first and higher order refraction mode, involves doping the sprayed liquid with a dye that is strongly absorbing at the incident laser wavelengths. This results in greatly diminished scattered intensity from larger droplets, thus allowing the photomultiplier gain to be set to a level sufficient to easily detect small particles without saturation. Tests conducted indicate that, at a collection angle of 30° and droplet absorptivity of γ = 0.014/μm, the PDPA can accurately size absorbing droplets up to approximately 200 μm. This upper limit can be extended by changing selection angle. Tests performed with an actual spray demonstrated that the method allowed detection of 1 μm to 235 μm droplets; more than four times the instrument's usual range of 50: 1. A data correction scheme to determine the effective probe volume radius for each particle size class has been developed for absorbing particles, as standard correction schemes derived for non-absorbing droplets excessively weigh distributions toward smaller particles.
    Additional Material: 10 Ill.
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  • 92
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 93
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 257-263 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Perimeter data, obtained from structured walks performed upon straight chains of circles and displayed in Richardson plots, reveal two distinct classes of discontinuities: textural and structural. Textural discontinuities contain information about the surface features of the profile, while structural discontinuities reveal the profile's overall shape. The origins of both types of discontinuities have easy explanations. The highly predictable behavior of the structural discontinuities serves as the basis of a newly proposed method of analysis for perimeter data. The number of structural discontinuities is equal to N, the number of circles in the chain; furthermore, the value of the step size \documentclass{article}\pagestyle{empty}\begin{document}$ \underline {\lambda} $\end{document} * associated with the first structural discontinuity is inversely related to N. These properties seem is be retained when the circles slightly intersect and also when the circles vary in diameter. Analysis of the structural discontinuities may provide a new method suitable for automated examination of chain-like agglomerate particles.
    Additional Material: 10 Ill.
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  • 94
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    Particle and Particle Systems Characterization 12 (1995), S. 269-273 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Based on technology described in a Du Pont patent for an offline system, we have developed a prototype in-line ultrasonic cell for measuring particle size distribution. We have used this cell to verify the Allegra-Hawley model of ultrasonic attenuation in dilute (〈 5 % vol) slurries of sub-micron ceramic particles, and we are developing a model that can cope with the multiple scattering effects occuring at higher concentrations.In this paper we present the results of attenuation measurements for ultrasound (2-50 MHz) in slurries with concentrations ranging from 0.5 010 to 38 010 (vol). The attenuation is proportional to slurry concentration up to 5 010 (vol) and is predicted by single scattering models. Above approximately 100% concentration, the attenuation is actually lower than expected. For the dilute slurries we find excellent agreement between our measurements and the Allegra-Hawley calculations, and the effects of the particle size distribution are evident in the ultrasonic attenuation spectrum. These ultrasonic data can be inverted to determine the particle size and concentration in aqueous slurries of sub-micron particles.
    Additional Material: 5 Ill.
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  • 95
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    Particle and Particle Systems Characterization 12 (1995), S. 284-288 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Measurements on paint components have been conducted with symmetrical flow field-flow fractionation (sym flow FFF) and asymmetrical flow FFF (asym flow FFF). Both methods are based on the same principle of separation, but they differ in the construction of the fractionation channel and the configuration of the channel flow and crossflow. On the basis of the good selectivity and resolution of these techniques, it was possible to determine the particle size of each individual constituent of a three-component mixture of a paint binder, pigment and filler, characterized by relatively broad and overlapping distributions, and to follow the changes on mixing them. In the case of sym flow FFF, it was possible to use thinner fractionation channels, with no system peaks and good selectivity in both the normal and steric-hyperlayer mode. The main features of asym flow FFF are the simpler construction of the fractionation channel and the possibility of focusing the sample in the channel better and of following visually the separation. This variant should be preferably used in the normal mode of operation.
    Additional Material: 13 Ill.
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  • 96
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    Particle and Particle Systems Characterization 12 (1995), S. 289-294 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A theory has been developed for spectral photosedimentation in a centrifuge. The use of several wavelengths allows particle size analyses in the submicron range without a knowledge of the optical material properties and is not restricted to spherical particles. As a result of this theory the extinction efficiency and the particle size distribution of the analysed particles can be calculated even for non-spherical particles from an experiment.A photocentrifuge has been built according to the developed theory. The theory has been verified by the measurement of spherical particles for which Mie theory is applicable. The experimentally obtained extinction efficiency agrees well with computations according to Mie theory. The accuracy of measured particle size distributions is comparable to those measured with other sedimentometers.
    Additional Material: 9 Ill.
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  • 97
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 299-303 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In most multi-phase flow problems, the particulate phase is exposed to an external field which causes dispersion. Therefore, local velocity measurements of the disperse phase are no longer equivalent with respect to averaging in time and averaging in volume. While the local time-averaged velocity still characterizes the transport of the ensemble in the Eulerian sense, one has to be be careful in modeling this velocity average by considering the ensemble's composition. It is shown for different particle ensembles that the conventional particle velocity average M1,0 calculated with respect to the dispersion relationship and a particle size number density distribution is far below the measured ensemble average; the deviation depends on the width of the particle size distribution. It is deduced that Eulerian particle velocity values referring to a certain time interval can be modeled by a ratio of velocity moments M2,0/M1,0 calculated with particle size number distributions referring to a certain probe volume. This relationship was confirmed by measurements.
    Additional Material: 5 Ill.
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  • 98
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    Particle and Particle Systems Characterization 12 (1995), S. 314-317 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The average local velocity of the upward of particles motion was determined in a dense fluidized bed by the means of a fibre optical probe. The probe consists of two independent light gates. The particles passing in front of the light gates reflect the light, generating sign sequences that are analysed by computer. From the average time difference of the sign sequences and from the distance of the light gates, the average local velocity can be calculated. The average local velocity of the particles along the height and diameter of the fluidized bed and also as a function of the fluidization air velocity was examined. It was concluded that the average local velocity is closely correlated with the local porosity of the dense fluidized bed and depends mainly on the fluidization air velocity. Using a fibre optical probe, the optimum range of the fluidization air velocity can be determined.
    Additional Material: 9 Ill.
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  • 99
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    Particle and Particle Systems Characterization 12 (1995), S. 309-313 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In-process measurement of particle size and concentration distributions provides continuous analysis, quality control, and optimization of product yield. As process production rates continue to improve, the delay between laboratory analysis and process correction of the product stream becomes more significant and costly in many commercial applications. Elimination of sample handling and operator manipulation is now possible for most pneumatic flows using optical methods which are properly interfaced with the process stream. Insitec has developed such an instrument based on ensemble laser-diffraction that has been successfully applied to a wide range of research and industrial process applications.As part of the adaptation of instrumentation to the specific needs of different process applications, we have developed several different interface arrangements, including a direct inline system and an eductor bypass instrument. A specific window purge design has been developed and shown to operate for extended time periods (exceeding one month and more) without maintenance. To address the wide range of operating concentrations that occur in practice, a variable pathlength interface has been developed along with a deconvolution algorithm that corrects multiple scattering effects for light transmissions down to 20%. Distribution update rates are computed and displayed in less than 5 seconds. This methodology is described along with measurements in a non-steady pharmaceutical powder processing application. Results show uniform size measurement for ten-fold concentration variations. Real time measurements allowed diagnosis and correction of non-steady feed rates to a classifier-mill.
    Additional Material: 7 Ill.
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  • 100
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 12 (1995), S. 318-323 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The guidelines which are at the base of the definition of a system capable of operating on a slurry containing the solid particulate for its characterization are described. All the considerations have been developed with particular reference to the case of a granular heterogeneous material in particular, the different research problems, making a comparison with the case of static images, acquired under laboratory conditions, are pointed out. Attention was focused on problems of acquisition and digital image processing to obtain information which is clean from noise and errors. The considerations and procedures analysed show general validity and can be applied to a large number of problems linked to the “on-line” morphological characterization of particulate solids materials. Some results for morphological characteristics of lead sulphide (PbS) samples are reported.
    Additional Material: 6 Ill.
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