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  • Gas chromatography  (51)
  • AIRCRAFT
  • ASTROPHYSICS
  • Cell & Developmental Biology
  • Chemistry
  • EARTH RESOURCES AND REMOTE SENSING
  • GEOPHYSICS
  • LUNAR AND PLANETARY EXPLORATION
  • Polymer and Materials Science
  • Springer  (56)
  • 1980-1984  (52)
  • 1970-1974  (4)
  • 1965-1969
  • 1925-1929
  • 1920-1924
  • 1984  (19)
  • 1982  (33)
  • 1974  (2)
  • 1972  (2)
  • 1929
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  • 1980-1984  (52)
  • 1970-1974  (4)
  • 1965-1969
  • 1925-1929
  • 1920-1924
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  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of C2−C16 dicarboxylic acids ; Dicarboxylic acid analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary C2−C16 dicarboxylic acids were esterified in aqueous solution in the presence of sulfuric acid. Esterification in water/n-butanol mixtures with mole ratios between 0.02 and 2.53 can be utilized for the quantitative determination of the dicarboxylic acids by gas chromatography. The presence of water does not interfere at water/n-butanol mole ratios below 0.27. For mole ratios above 0.27 anhydrous sodium sulfate has been used for binding the water. The mole ratio range was 0.25–0.75 for anhydrous sodium sulfate/water, and 0.32–1.3 for sulfuric acid/anhydrous sodium sulfate.
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  • 2
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    Chromatographia 18 (1984), S. 663-667 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas solubilities ; Enthalpies of solution ; Polar solutions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas-liquid chromatographic method has been used to determine the solubilities and partial molar enthalpies of solution of the gases H2S, CO2 and COS in four polar solvents. The results agree well with literature values obtained using conventional techniques, with the one exception of H2S in N-methyl-2-pyrrolidinone. In this case there is some evidence for the occurrence of adsorption at the gas-liquid interface.
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  • 3
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aromatic polycarboxylic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The direct esterification and gas chromatographic analysis of aromatic carboxylic acids as n-butyl esters is described. Derivatization is performed in aqueous solution with n-butanol in the presence of sulfuric acid. The butyl esters of benzoic, phthalic, hemimellitic, trimellitic, trimesic and pyromellitic acids permit their gas chromatographic separation from each other and from fatty acids and alipatic dicarboxylic acids. At mole ratios of [H2O]/ [n-BuOH]≤0.04 the water present does not interfere with the esterification reaction. At mole ratios above 0.04 anhydrous sodium sulfate is used for binding the water, at mole ratios of [Na2SO4 anh.]/[H2O]=0.25–0.75.
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  • 4
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    Chromatographia 18 (1984), S. 202-204 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polysiloxane stationary phases ; Heat of adsorption ; Heat of solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The changes in the heat of solution of polar compounds and xylene isomers in methylsilicone fluid OV-101 deposited on Chromosorb W AW DMCS were studied. It was shown that the heat of solution increases with an increase of the percentage loading of the OV-101 up to 10%. Solution and adsorption thermodynamic characteristics of the studied system are briefly discussed.
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Chemically bonded phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Packings consisting of diphenylphosphine complexes with CoCl2 and CoBr2, chemically bonded to the silica surface, were synthesized and their retention parameters determined. The packings are capable of specifically interacting with electron-donating compounds by forming π-complexes. The interaction is considerably stronger in the case of CoBr2-containing packing than in the case of CoCl2-containing packing.
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  • 6
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    Chromatographia 18 (1984), S. 234-238 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular columns ; On-column injection ; Stopped-flow operation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, inexpensive, on-column injector of the septum moving-needle kind is described for quantitative analysis using open-tubular columsn. when operated in the stopped-flow mode an improvement incolumn efficiency is observed combined wit a diminished tendency to produce split-top peaks, particularly for late eluting peaks. Using electronic integration a relative error of about 2.7% was observed for peaks spanning a wide range of sample concentrations and volatilities.
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  • 7
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    Chromatographia 18 (1984), S. 243-248 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas ; Viscosity ; Influence of temperature
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The vicosity-temperature relationship of the three gases (helium, nitrogen and hydrogen) most frequenly used as the carrier gas in gas chromatography is studied. Based on available data, equaitions are derived to describe this relationship. Using these equations viscosity data are tabulated for the chromatographically important temperature range.
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  • 8
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    Chromatographia 18 (1984), S. 260-264 
    ISSN: 1612-1112
    Keywords: Parabens and their dissolution ; Pharmaceutical dosage forms ; Derivatization ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A specific, sensitive and general applicabla gas chromatographic method is described for the determination of parabens in various liquid pharmaceutical preparations: propylparaben and butylparaben in a liquid antacid dosage form (I); methylparaben, ethylparaben and propylparaben in a syrup (II); methylparaben and propylparaben in a solution for injection (III). Each time one of the parabens is used as internal standard. The parabens are extracted with diethylether and derivatized by silylation. Different columns are used for the analysis of the parabens: 3% SE-30 column, a 3% QF-1 column for different selectivity, a 2% OV-1 column for isothermal operation. Special attention is attributed to the standard: the parabens are dissolved in a minimal amount of 0.1 M sodium hydroxide and extracted in the same way as the pharmaceutical dosage form.
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  • 9
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Configuration ; Resolution ; Alcohols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The study of the resolution of sixteen secondary aliphatic alcohols by gas chromatography on (+)-dodecyl (2R, 3R)-tartrate, trapping the ascending part of the peak from a conventional filled column, has allowed the determination in a single operation of the sign and order of emergence of enantiomers. A correlation between the configuration of these secondary alcohols and their order of emergence has been established.
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  • 10
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    Chromatographia 18 (1984), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carboxylic acids ; Acetonyl derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of the acetonyl esters of nine aliphatic carboxylic acids is described, the general formula of the derivatives being RCOOCH2COCH3 where R=alkyl or H. The derivatives show good chromatographic properties on both packed and capillary columns. The electron impact and chemical ionisation mass spectra of the derivatives are discussed.
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  • 11
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermodynamic relationships ; Retention index ; Peak identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A thermodynamic criterion, ΔQ, is suggested which permits to estimate the difference in the functional group energy of interactions for two different stationary phases. The linear dependence of ΔQ on the homolog number m of any series Rm X can be used as the thermodynamic criterion for the identification of substances by GC analysis.
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  • 12
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    Chromatographia 18 (1984), S. 477-488 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Sample capacity ; Column comparison ; Film thickness ; Column diameter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated, open-tubular (capillary) columns prepared from different diameter tubing, with different liquid phase film thickness, are compared with each other and with packed and support-coated open-tubular columns. The comparison is based on the variation of the phase ratio and the capacity factor, and includes column efficiency (HETP, theoretical plate number), resolution, retention time, and sample capacity. Problems associated with the evaluation of the sample capacity are outlined. The influence of temperature on column performance is discussed in detail. Finally, the possibilities of short, wide-bore open-tubular columns prepared with a thick liquid-phase film are demonstrated.
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  • 13
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    Chromatographia 18 (1984), S. 367-368 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Variation of film thickness ; Thick-film columns ; Mass transfer terms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The factors characterizing the influence of the variation of the liquid phase film thickness on the mass transfer terms in the Golay equations describing the performance of open tubular columns are investigated and numerical values are given.
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  • 14
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Cross-linked Stationary phase ; Immobilized Stationary phase ; Packed columns ; Trapping
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A coating of silicone SE-54 on Chromosorb W has been converted to an analytically stable, immobilized stationary phase layer by cross-linking with an organic peroxide. Up to 10% by weight has been applied in this manner. Excellent high temperature qualities are exhibited, such as low bleeding and good base line stability, during typical analyses. Poly (2,6-dimethyl-p-phenylene oxide) has also been crosslinked as a surface coating on Chromosorb W with an organic peroxide. From 3 to 4% by weight has been immobilized in this way. The resultant packing material, following high temperature conditioning, has been examined for use as an adsorbent of trace substances, similar to the applications to which such adsorbents as Tenax GC have commonly been applied, e.g. trace analysis of air. It appears to exhibit satisfactory properties for this analytical purpose.
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  • 15
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    Chromatographia 18 (1984), S. 21-22 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Isopropylidene-glucose ; Glucose ; GC of TMS-derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the gas chromatographic separation of the mixture of di- and mono-O-isopropylidene-D-glucose and D-glucose as their trimethylsilyl derivatives. The use of OV-101 as liquid phase provides a complete separation for the all components in the mixture. Quantative analysis was performed using xylitol as the internal standard for di- and mono-O-isopropylidene-D-glucose, and sorbitol as the internal standard for α-and β-glucose.
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  • 16
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nuclear magnetic resonance ; Terpenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A procedure is described for recording1H NMR spectra of flowing gaseous GC fractions boiling as high as 200°C. The line width of the signals in the NMR spectra is smaller than 2.2Hz.
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  • 17
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    Chromatographia 18 (1984), S. 556-559 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Tetramethrin ; Residues
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the analysis of tetramethrin aqueous formulation and residues of tetramethrin on woolen cloth. The samples were extracted with acetonitrile and partitioned with benzene. Interferences were removed by liquid column chromatography with acid alumina and eluted with 10% ethyl acetate-hexane. Analysis was by gas chromatography with a 10% UCW98 (methylsilicone) column. Detection was made with the flame ionization detector to avoid the repeated dilutions necessary with use of the electron capture detector.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Electric parameters ; Physico-chemical relationships ; Structure-retention study
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new equation is derived relating the retention index to the molecular polarizabilities, ionization potentials and permanent dipole moments of the stationary phase and the solute. Various implications of this equation to quantitative structure-retention relationships are discussed.
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  • 19
    ISSN: 1612-1112
    Keywords: Aldehydes and ketones ; 2,4-dinitrophenylhydrazine-coated silica gel ; Gas chromatography ; Column liquid chromatography ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary After a brief review of several methods described in the literature this paper discusses air-sampling on 2,4-dinitrophenylhydrazine-coated silica gel and identification requirements for aldehydes and ketones most commonly found in industrial pollution. Quantitative analysis of formaldehyde and acetaldehyde either by GC or by HPLC techniques is established using a dynamic system producing test atmospheres and compared with the usual colorimetric determinations.
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  • 20
    ISSN: 1432-0827
    Keywords: Bacterial amphophile ; Purification ; Chemistry ; Resorption ; Ca influx ; Cyclic AMP
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary The bone resorptive factor and amphipathic antigen (AcA) previously identified by us in preparations fromActinomyces viscosus have been partially purified, characterized chemically, and compared. They elute at the same location on chromatography with Ac 22. The fatty acid composition of AcA and the bone resorptive factor is the same. Some differences in carbohydrate composition are observed. TheActinomyces factor does not affect calcium influx or cyclic AMP in isolated bone cells. Therefore it is concluded that AcA stimulates resorption either by gaining entrance into bone cells or by way of a yet undetermined second messenger.
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  • 21
    ISSN: 1612-1112
    Keywords: Teflon capillary columns ; Chemically modified teflon ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of teflon capillary columns employing direct coating of the stationary phase to the chemically modified teflon surface and the role of the chemically modified teflon in the separation mechanism are described. Two types of contributions from the modified teflon have been observed: nonspecific adsorption of the carbon surface and specific interactions of polar groups in the carbon skeleton. The use of polar liquid phases can eliminate adsorption due to the presence of polar groups in the modified teflon.
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  • 22
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    Chromatographia 16 (1982), S. 60-62 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Amines ; Derivatization ; Chloroformate esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic analysis of amines after conversion to electron capture sensitive carbamates in two-phase systems has been studied. Hydrophilic compounds, for instance methylamine, are reacted with 2,2,2-trichloro-tert. butyl chloroformate. Quantitation below 10−7 M can be made by thermionic or electron capture detection. A hydrophobic amine, namely N,N-dimethyl-n-octylamine, was derivatized with 2,4,6-tribromophenyl chloroformate with addition of iodide ion to the aqueous phase. The favorable effect of iodide ion as well as the choice of pH and chloroformate ester is discussed.
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  • 23
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    Chromatographia 16 (1982), S. 98-102 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Rectangular channel ; Efficiency ; Capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic experiments have been performed in a truly rectangular channel with a 60∶1 cross-sectional aspect ratio, constructed according to the field-flow fractionation technology. It is shown that the peak broadening is controlled by the thickness of the channel while the maximum load is determined by the largest cross-sectional dimension. However, even with its elongated configuration, the side walls contribute significantly to the band broadening of solutes with a high diffusivity. Good agreement is found between the experimental plate height data and the recent theoretical calculations of Golay [13] taking into account the side-wall effect.
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  • 24
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    Chromatographia 15 (1982), S. 704-706 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Isopropyliden-sorboses ; TMS-derivatives ; GC-MS combined technique ; Mass spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method has been developed using gas chromatography — electron impact mass spectrometry for the determination of the di-0-isopropylidene-sorbofuranose and mono-0-isopropylidene-sorbofuranose. The compounds are separated as their trimethylsilyl derivatives on a capillary column coated with the stationary phase SE-52. The mass spectra show that the silylation reaction is quantitiative and that the isopropylidene groups does not change.
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  • 25
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    Chromatographia 15 (1982), S. 183-185 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Analysis of ethylbenzene hydroperoxide ; Time normalization method
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method, based on the time normalization technique, is described for the analysis of ethylbenzene hydroperoxide in mixtures containing ethylbenzene, acetophenone, 1-phenylethanol, benzaldehyde and phenol. Different liquid phases were tested and the best results were obtained with tricresyl phosphate and neopentyl glycol sebacate. The influence of the support, the liquid loading and the gas velocity are discussed.
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  • 26
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    Chromatographia 15 (1982), S. 625-630 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular (capillary) columns ; Comparison of liquid phases ; Influence of temperature ; Retention index data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The influence of temperature and liquid phase film thickness of open-tubular (capillary) columns on the retention index values of hydrocarbons on methylsilicone liquid phases is discussed. Data obtained on methylsilicones and squalane are compared. Retention index values of 43 hydrocarbons between 40 and 70 °C on OV-101 liquid phase are listed.
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  • 27
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    Chromatographia 15 (1982), S. 351-354 
    ISSN: 1612-1112
    Keywords: Supported catalysts ; Reserved-flow GC ; Drying step ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Application of reversed-flow gas chromatography to study the drying step in the preparation of supported catalysts is proposed. It is demonstrated that this technique can be applied to investigate the kinetic law followed, as well as to obtain kinetic parameters of drying (rate constants, activation energies and frequency factors). Amaterial illustrating this application is γ-Al2O3 impregnated with usual organic solvents (n-C5H12,n-C6H14,n-C7H16, CH3COCH3 and CH3CH2OH). It was found that in all cases above a simple first-order law based onone kind of active site is followed. Moreover, it was observed that the activation energyE a of the drying process increases almost linearly with the relative molecular mass of the solvent, whereas for the same solventE a increases with the amount used. The operation of a kinetic compensation effect suggests “similar” activated complexes of the various solvents used.
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  • 28
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused silica capillaries ; New polar phases: OV-1701 and RSL-310 ; Immobilization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities of OV-1701 and RSL-310, two new stationary phases, have been evaluated for capillary gas chromatography in fused silica columns. OV-1701 is a cyanopropylphenyldimethyl polysiloxane of moderate polarity possessing excellent chromatographic characteristics. The phase exhibits high coating and chromatographic efficiencies, high temperature stability and is suitable for cross-linking. RSL-310 is a polar liquid stationary phase yet to be permanently bonded in a capillary column. The selectivity of both phases extends the applicability of fused silica columns.
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  • 29
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    Chromatographia 15 (1982), S. 241-244 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Monosaccharides ; Polyols ; GC of TMS derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the gas chromatographic separation of the mixture of isopropylidene monosaccharides, and their trimethylsilyl derivatives. Based on the total analysis time and resolution the best stationary phase was SF-96 using Chromosorb G as the solid support and temperature programming.
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  • 30
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    Chromatographia 15 (1982), S. 312-314 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Injection-port modification ; Oxygen and nitrogen traces
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The paper presents a new device modifying normal injection port of a gas chromatograph for eliminating air contamination thus enabling determination of traces of oxygen or nitrogen. Further modification is also proposed which enables the analysis to be carried out with a limited quantity of sample gas. Potential application of this device in the analysis of reactive gases like florine has been indicated.
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  • 31
    ISSN: 1612-1112
    Keywords: Phthalides ; Gas chromatography ; Chromosorb W ; Isomerization ; Ligustilide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary During GLC of naturally occurring mixtures of phthalides on packed columns an artefact was sometimes detected that originated from Z-ligustilide. Active sites of Chromosorb W were responsible for the formation of the artefact, that was assumed to be E-ligustilide as GC-MS revealed that its mass spectrum was identical with that of Z-ligustilide. No isomerization was observed when freshly coated Chromosorb W was used or the support was deactivated by benzoyl chloride or melamine. The identity of the artefact was confirmed by UV irradiation experiments.
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  • 32
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    Chromatographia 15 (1982), S. 30-32 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Arsenic ; Inorganic materials
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the quantitative chlorination and extraction of arsenic as arsenic trichloride from a number of alloys. The conditions for the quantitative gas chromatographic measurement of the volatile chloride have been studied. The proposed method for inorganic materials is very fast giving results within 10 min; sensitive, 1.5·10−13 g As can be detected, simple and accurate. At the ng level of As the error is about 20% with a standard deviation less than 20%, and at the 10pg level the error is about 36% with a standard deviation of 44%.
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  • 33
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    Chromatographia 15 (1982), S. 765-768 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale chromatography ; Capacity ; Dual-stage separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The capacity of different versions of single- and dual-stage separation of mixtures on a preparative scale is considered. It has been shown that dual-stage separation with intermediate condensation considerably enhances the capacity of the installation as compared with a single-stage process.
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  • 34
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    Chromatographia 15 (1982), S. 117-124 
    ISSN: 1612-1112
    Keywords: Various packed GC column ; Gas chromatography ; Porous layer beads ; GC/MS analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Theoretical comparisons of various packed GC column types are presented with respect to analysis time, efficiency, sample dilution, and sample capacity for a given maximum inlet pressure. In particular, totally porous particles, porous layer beads, and glass beads are compared with one another. It is shown that 30 μm porous layer beads offer a useful compromise between analysis time and plate count with relatively good sample capacity. Moreover, when using 1 mm i.d. columns (microbore), outlet flow rates that are reasonable for direct coupling to magnetic sector mass spectrometers are achieved making these columns suitable for GC/MS. Using 30 μm Zipax porous layer beads, columns yielding 8,000 to 10,000 plates/meter have been produced with inlet pressures of 13 to 26 atm. A simple modification of the injection port converts the maximum inlet pressure of a commercial gas chromatograph to 26 atm. With such pressures, columns in excess of 20,000 plates can be achieved. Chromatograms are presented illustrating the promise of these microbore columns for GC and GC/MS analysis.
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  • 35
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    Chromatographia 15 (1982), S. 245-248 
    ISSN: 1612-1112
    Keywords: Chromatoscopy ; Gas chromatography ; Graphitized carbon black ; Molecular structure and retention ; Aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A molecular-statistical calculation of the retention volumes at zero sample size on graphitized thermal carbon black is carried out for quasi-rigid molecules of fluorene, indene, 1-methylindene, 2-methylindene and three dimethylindenes. A reasonable agreement is observed between the calculated and the available experimental gas chromatographic data. The potential barrier to internal rotation and the torsional angle in styrene molecules are estimated by comparing theoretically calculated and measured retention volumes.
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  • 36
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silicone liquid phases ; Oxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The on-column oxidation of apolar and polar silicones used as gas chromatographic stationary phases is investigated. Even at 225° the effects of oxidation are found to be slight. Of the materials investigated the methylphenylsilicones are the most stable.
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  • 37
    ISSN: 1612-1112
    Keywords: Glass capillary ; Gas chromatography ; Methyl chloroacetates ; Methyl chloropropanoates ; Methyl chlorobutanoates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatography of all chlorinated methyl acetates, methyl propanoates and methyl mono- and dichlorobutanoates has been studied on Carbowax 20M and SE-30 glass capillary columns under various running conditions. The order of elution on a non-polar column was largely determined by the boiling point of esters, whereas on a polar column it was much influenced by the structure of compounds. Complete separation of the combined mixture of all 27 compounds could not be achieved, however, methyl 3,3-dichlorobutanoate was the only ester overlapped on both columns in spite of the various column temperatures used. The best separation of the mixture was on Carbowax 20M with a temperature program from 50°C at 8°C/min, isothermal running conditions leading either to poor separation of volatile components or long analysis time and broad peaks of higher chlorinated esters. The relative retention times for compounds at the various column temperatures are given and the retention order on a polar and on a non-polar column discussed.
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  • 38
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    Chromatographia 15 (1982), S. 517-520 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carbon-silica adsorbents ; n-Octadecanol film ; Phase transitions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of the n-octadecanol film on carbon-silica adsorbent (Carbosil) were investigated. It was found that n-octadecanol forms an oriented film on the Carbosil's surface. If the surface of the basic silica gel is not completely covered with carbon, then the phase transition takes place in this film at a temperature higher than the melting temperature of n-octadecanol. One may distinguish two forms of this film, characterised by the different structures and the temperatures of the phase transitions. The first exists on the surface of silica gel unblocked by carbon. This part of the film is a monolayer, in which the alcohol molecules are vertically oriented. The solid compact-liquid expanded type phase transition at the well-defined temperature occurs in this film. In the second part of the film formed on the carbon surface, there is a multilayer of n-octadecanol. Its molecules are probably parallely oriented in relationship to the adsorbent surface. This film desintegrates progressively when the temperature increase. Maximum temperature of this phase transition is lower than the temperature of its analogue on pure silica gel surface.
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  • 39
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    Chromatographia 15 (1982), S. 546-558 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Quantitative analysis ; Sample inlet systems ; High-speed analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The attainment of precise quatitative analytical data using open-tubular (capillary) columns in standard, commercially available gas chromatographic instrumentation is demonstrated. Key elements in the design and proper utilization of the instrumentation are discussed. The function of the various sample introduction systems is elaborated and their quantitative performance demonstrated. The extra-column contribution to band-spreading is determined and the resultant data is used assessing the suitability of commercial instrumentation for highspeed capillary gas chromatography. The quantitative analysis of a sample containing some eleven components in less than thirty seconds is shown.
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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crystal hydrates as stationary phases ; Mobile Phases containing water ; Selective retentions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of crystallohydrates, crystallohydrate solutions and melts as stationary phases in gas chromatography has been proposed. Crystallohydrates have been shown to display high selectivity in the separation of polar organic compounds when use is made of water vapours as the mobile phase. Some aspects of gas-liquid chromatography in water vapours and with the stationary phase comprising crystallohydrates have been studied, and the preliminary results obtained point to the desirability of further progress in this field.
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  • 41
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    Chromatographia 16 (1982), S. 201-203 
    ISSN: 1612-1112
    Keywords: Phenols ; Whisky ; Gas chromatography ; Aroma compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Twelve volatile phenols were identified in whisky by combined gas chromatography-mass spectrometry. Of these phenols 2,4-dimethylphenol was found for the first time in the aroma of whisky. The content of phenol, o-, m-, and p-cresol, guaiacol, p-ethylphenol, p-ethylguaiacol and eugenol in whiskies originating from different countries was determined by gas chromatography as their 2,4-dinitrophenyl ethers using electron capture detection. The results show that Scotch whiskies differ from others in the content of o-, m-, and p-cresol. The odour threshold values of phenols studied were determined in a 10% (v/v) ethanol-water mixture and in some cases also in the whiskies. Cresols have been found to make contribution to the aroma of Scotch whisky.
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  • 42
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    Chromatographia 16 (1982), S. 26-31 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ionization detectors ; Gaia
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper is an account of the development of the gaia hypothesis as seen through the eyes of a gas chromatographer. Gaia is a radical notion about the Earth which postulates the climate and chemical composition to be regulated at an optimum by and for life. Gas chromatography played an important role in the gathering of evidence for the hypothesis but most significantly the art of inventing detectors lead to the developement of a planetary life detector through which gaia was revealed.
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  • 43
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    Chromatographia 16 (1982), S. 282-285 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Naphtha analysis ; Gasoline analysis ; Hydrocarbon type analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two different gas chromatographic methods are used for the determination of hydrocarbon type distribution in naphtha and gasoline samples with final boiling points up to 275 °C. The methods are based either on a single capillary column or on a valve-switched packed column system. Both methods give extensive information on paraffins, olefins, naphthenes and aromatics in total as well as by carbon-number. In each case the analysis is fully automated with a computer controlling the entire analysis from injection to results presentation. The advantages and limitations of both methods are discussed.
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  • 44
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    Chromatographia 16 (1982), S. 322-324 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitized carbon black supports ; Determination of hydroxyacids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Acid-washed graphitized carbon black (Carbopakc B) modified with trimesic adic and PEG 20M has proved to be effective for quantitative analysis of underivatized low molecular weight hydroxyacids. Calibration data revealed good linear relationships between relative peak area and concentration for lactic and 3-hydroxybutyric acids down to 0.05 mmol/l. The packing material was suitable for the analysis of aqueous solutions of hydroxyacids as it is tolerant to injections of water over a prolonged period of use. The GC system developed has been applied to the analysis of some hydroxyacids of biomedical interest in blood plasma and lactic acid contained in wine and beer.
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  • 45
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified thermal energy analyzer ; Selective detection of nitrogen compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary A modification to the TEATM Analyzer is described, which allows it to be used as a highly selective GC detector for nitrogen compounds as well as for N-nitrosamines and nitro compounds. The modified Analyzer is as sensitive as the AFID, but has a much higher selectivity towards nitrogen compounds than the AFID. Its response appears to be molar, with an output that is dependent only on the number of nitrogen atoms present. The performance of the modified Analyzer for the analysis of ammonia, amines,N-nitrosamines, nitriles and organonitro compounds is reported and discussed, as is its application to the detection of these compounds in bacon and beer samples.
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  • 46
    ISSN: 1612-1112
    Keywords: Graphizized carbon black traps ; Organic air pollutants ; Work areas ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of traps containing graphitized carbon black for the collection and pre-analysis of atmospheric pollutants in industrial areas is presented. The working conditions, in terms of trapping capability and effectiveness of release by thermal desorption are discussed. Some practical applications are also given.
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  • 47
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Van der Waals' volume ; Polarity of stationary phase ; Retention index
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    Topics: Chemistry and Pharmacology
    Notes: Summary Equations for Retention Index (I) versus Van der Waals, volume (Vw) on squalane are studied for alcohols, carbonyls, esters and ethers. Each equation includes linear and branching substances with different positions of the functional group in the carbon chain. The study is extended to stationary phases with polarities from 4.29 to 91.54 on the Tarjan et al. scale. Variations of the slope and origin ordinate values with the polarity of the stationary phase are discussed.
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  • 48
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    Chromatographia 15 (1982), S. 125-132 
    ISSN: 1612-1112
    Keywords: Capillary columns ; Fast analysis ; Gas chromatography ; Instrumental effects ; Optimization
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    Topics: Chemistry and Pharmacology
    Notes: Summary The efficiency of fast GC columns depends largely on the quality of the chromatograph. A theoretical and experimental study shows the relative importance of the various phenomena involved and permits the optimization of a GC System. Extremely good performances, exceeding 2,500 plates per second have been routinely obtained.
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  • 49
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    Chromatographia 15 (1982), S. 180-182 
    ISSN: 1612-1112
    Keywords: Acidic fermentation products ; Characterisation ; Gas chromatography ; Methyl esters
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    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and simple method for the identification of acidic fermentation products is described. Methyl esters of volatile and non-volatile acids are separated on a single chromatographic column. Retention time data for a number of acids are tabulated.
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  • 50
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    Chromatographia 15 (1982), S. 521-524 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Connectivity index ; Van der Waals' volume ; Alkanes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The relationships between retention index and Van der Waals' volume and between retention index and connectivity index have been studied for 58 different alkanes (C1−C9) on squalane. The correlation coefficient for the former is higher than for the latter. From these equations a linear relationship between Van der Waals' volume and connectivity index is obtained which indicates that the two parameters are equivalent. A simple method for calculating the Van der Waals' volume of alkanes is proposed.
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  • 51
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Fused silica capillaries ; Capillary drawing ; Glass capillaries
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    Topics: Chemistry and Pharmacology
    Notes: Summary A compact description is given of a simple and reliable method of drawing flexible fused silica capillary for gas chromatography. Some emphasis is given to the fact that the practices of drawing optical fibres should not be followed too slavishly so this leads to unnecessarily complicated and expensive equipment. Satisfactory capillary column silica tubing can be made with straightfoward extension of the method developed earlier for drawing thick walled capillary. A simple glass/silica hydrogen oxygen diffusion flame bumer is described for fusing the preform tubing at the draw point which is enclosed by a water cooled glass enclosure to trap evaporated silica and maintain the operation under dust free conditions. The uniformity of the capillary diameter is better than 5% which is adequate for most gas chromatographic purposes. The second part of the paper yet to be published will cover the methods developed for coating the capillary both internally and externally.
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    Chromatographia 16 (1982), S. 107-111 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermionic ionization ; Catalytic flame ionization
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    Topics: Chemistry and Pharmacology
    Notes: Summary A newly designed thermionic detector was operated in two modes of thermionic ionization detection (TID), and a third mode of catalytic flame ionization detection (CFID). Operating modes were varied by changing the composition of the electrically-heated thermionic/catalytic source, and the composition of gases supplied to the detector. A TID-2 source activated by a low concentration of Cs/ceramic was operated in a dilute H2/air environment and provided specific responses to nitrogen and phosphorus compounds. A TID-1 source activated by a high concentration of Cs/ceramic was operated in a N2 environment and provided very high specificities and picogram detectivities to compounds containing electronegative functional groups such as the NO2 group. A CFID source formed from Ni/ceramic was operated in a H2/air flame environment and provided universal responses to all organics with enhanced responses to some heteroatom compounds.
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    Calcified tissue international 16 (1974), S. 145-152 
    ISSN: 1432-0827
    Keywords: EHDP ; Bone ; Chemistry ; Serum ; Rabbits
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    Topics: Biology , Medicine , Physics
    Notes: Abstract The effects of disodium ethane-1-hydroxy-1,1-diphosphonate (EHDP) on bone and serum chemistry were investigated in adult rabbits. EHDP was administered by subcutaneous injection at doses of 0.25, 2.5 and 10 mg/kg body weight/day for of 28 days. Blood samples were obtained weekly from each rabbit and serum levels of total calcium, ionized calcium, inorganic phosphate and alkaline phosphatase were determined. At the end of the treatment period all rabbits were sacrificed and the tibiae removed for chemical analysis and histological evaluation. The effect of EHDP administration on serum chemistry was both dose- and time-related. The highest of the three doses, 10 mg/kg/day, resulted in a time-related decrease in total serum calcium. This dose also caused a rapid but transient reduction in serum ionized calcium. The effect of EHDP on serum inorganic phosphate was biphasic. Administration of 2.5 mg/kg/day resulted in a time-related elevation in this parameter, whereas the 10 mg/kg/day dose resulted in a time-related hypophosphatemic response. There were no significant drug-related changes in tibial fat-free dry weight, ash weight, total calcium or total phosphorus values. However, administration of 2.5 and 10 mg/kg/day EHDP resulted in increased osteoid tissue as measured histologically. These results are compared with data from other EHDP studies, and discussed in relation to the maturity and growth-state of the experimental animals.
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    Calcified tissue international 14 (1974), S. 3-14 
    ISSN: 1432-0827
    Keywords: Hydroxyapatite ; Mineral ; Phase ; Chemistry ; Synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Description / Table of Contents: Résumé Des diagrammes de phase d'équilibre ont été déterminés pour le système CaO-P2O5-H2O en utilisant des techniques de synthèse hydrothermique au cours de variatio nsde température allant de 300–600° et 2 Kb H2O de pression. De l'hydroxyapatite bien cristallisé a été synthétisé et caractérisé. De faibles variations de paramètres de la maille cristalline, liées à la température de synthèse et composition globale du matériel initial, ont été déterminées. Des conditions chimiques précises sont nécessaires pour obtenir de l'apatite, en tant que seule phase solide en équilibre dans la solution. Les résultats de diagramme de phase d'équilibre sont comparés avec ceux obtenus dans des milieux synthétiques.
    Abstract: Zusammenfassung Es wurden Gleichgewichts-Phasendiagramme für das System CaO-P2O5-H2O bestimmt, indem hydrothermale Synthese-Techniken im Temperaturbereich von 300–600° und bei einem Druck von 2 Kb H2O verwendet wurden. Es wurde gut-kristallisiertes Hydroxyapatit erzeugt und charakterisiert. Es wurden geringe Unterschiede in den Parametern der Zelleinheiten festgestellt, welche von der angewandten Temperatur und der Zusammensetzung des Startmaterials abhingen. Es waren genaue chemische Bedingungen nötig, um Apatit als die einzige feste Phase im Gleichgewicht mit der Lösung zu erhalten. Die Resultate der Gleichgewichts-Phasendiagramme werden mit früheren Untersuchungen mit der Synthesetechnik verglichen.
    Notes: Abstract Equilibrium phase diagrams have been determined for the system CaO-P2O5-H2 using hydrothermal synthesis techniques in the temperature range 300–600° and 2 Kb H2O pressure. Well-crystallized hydroxyapatite has been produced and characterized. Small variations in unit cell parameters dependent on temperature of synthesis and bulk composition of the starting materials have been determined. Precise chemical conditions were required to obtain apatite as the only solid phase in equilibrium with solution. Equilibrium phase diagram results are compared with previous synthetic investigations.
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    Calcified tissue international 10 (1972), S. 82-90 
    ISSN: 1432-0827
    Keywords: Calcium ; Phosphate ; Precipitation ; Kinetics ; Chemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Description / Table of Contents: Résumé La cinétique de la formation et de la transformation des précipités de phosphate de calcium, obtenus en mélangeant de volumes égaux de solutions à 6×10−3 M de calcium total et/ou phosphate total est étudiée à 25°C. Les solutions de phosphate sont préajustées à un pH de 7.4. Les changements de pH et de turbidité des solutions sont suivis simultanément en fonction du temps. Les précipités sont isolés à des intervalles de temps variables et caractérisés par diverses méthodes physico-chimiques. Initialement un précipité avec un rapport molaire Ca/P de 1.5, amorphe aux rayons X et en diffraction électronique, est formé. Le spectre IR indique la présence de PO 4 3− et de HPO 4 2− . Après une période métastable, on observe la précipitation d'un matériel cristallin dans ou sur la phase amorphe. Vingt quatre heures après préparation de l'échantillon les précipités présentent surtout les caractères du phosphate octocalcique.
    Abstract: Zusammenfassung Die Kinetik der Bildung und Transformation von Calciumphosphat-Niederschlägen wurde bei 25°C untersucht. Es wurden dazu gleiche Volumen von Lösungen gemischt, bei einer Konzentration von 6×10−3M totales Calcium und/oder totales Phosphat. Die Phosphatlösungen wurden zuerst auf pH 7,4 eingestellt. Veränderungen des pH und Trübung der Lösungen wurden gleichzeitig als eine Funktion der Zeit aufgezeichnet. Niederschläge wurden in verschiedenen Zeitintervallen isoliert und mit verschiedenen physiko-chemischen Methoden charakterisiert. Am Anfang wurde ein Niederschlag mit einem molaren Ca/P-Verhältnis von 1,5, im Röntgenbild und in der Elektronendiffraktion amorph, gebildet. Infrarotspektren deuteten die Anwesenheit von PO 4 3− - und HPO 4 2− -Ionen an. Nach einer metastabilen Periode erfolgte ein Niederschlag aus kristallinem Material innerhalb oder auf der amorphen Substanz. 24 Std nach der Herstellung der Proben zeigten die Niederschläge in der Hauptsache die Charakteristiken von Octocalciumphosphat.
    Notes: Abstract The kinetics of the formation and transformation of calcium phosphate precipitates obtained by mixing equal volumes of solutions, 6×10−3 M in total calcium and/or total phosphate was investigated at 25°. The phosphate solutions were preadjusted to pH 7.4. Changes of the pH and turbidity of the solutions were followed simultaneously as a function of time. Precipitates were isolated at various time intervals and characterized by different physicochemical methods. Initially a precipitate with a molar Ca/P ratio of 1.5, amorphous to X-ray and electron diffraction was formed. IR spectra indicated the presence of PO 4 3− and HPO 4 2− ions. After a period of metastability, precipitation of a crystalline material within or upon the amorphous matter occurred. Twenty four hours after sample preparation the precipitates showed mainly the characteristics of octacalcium phosphate.
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    Calcified tissue international 10 (1972), S. 171-197 
    ISSN: 1432-0827
    Keywords: Amorphous ; Crystalline ; Calcium phosphate ; Chemistry ; Composition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Description / Table of Contents: Résumé Des échantillons non lavés de phosphate de calcium amorphe (ACP) contiennent une fraction labile, non remplaçable, riche en phosphate acide avec un rapport Ca/P faible: cette fraction est perdue de façon irréversible au cours du lavage. De l'ACP frais, précipité entre pH 6.6–10.6, varie dans un rapport molaire Ca/P de 1.18 à 1.50 et dans un rapport HPO 4 2− /P total de 33.0% à 10.1%. A pH 7.40, de l'ACP frais a un rapport molaire Ca/P de 1.36±0.02 et contient 22.8 (±2.2)% HPO 4 2− . Les résultats obtenus avec du précipité non lavé ne peuvent s'expliquer par du Ca2+ emprisonné et de l'HPO 4 2− ou du Na+, Cl− et CO 3 2− exogènes. Les phosphates de calcium amorphes constituent une classe de sels ayant des caractères chimiques variables et des propriétés physiques identiques, comparables au verre. Le CaHPO4·xH2O non cristallin peut être un ACP, surtout au cours des phases précoces de formation. A des pH physiologiques, l'ACP se transforme en petits cristaux applatis contenant de fortes quantités de phosphate acide facilement remplaçable. Le fait de laver la couche de surface produit un changement chimique dans les nouveaux cristaux: des cristaux non lavés donnent des diagrammes de diffraction d'apatite peu cristallins, ainsi que des spectres infra-rouges peu nets, intermédiaires entre des apatites et du phosphate octocalcique. Des explications structurales sont proposées et les compositions minérales amorphe/cristalline de l'os et du cartilage sont recalculées.
    Abstract: Zusammenfassung Ungewaschene Proben von amorphem Calciumphosphat (ACP) enthalten eine unersetzliche labile Fraktion, welche reich an saurem Phosphat ist und ein niederes Ca/P-Verhältnis hat und welche während des Waschprozesses unwiderruflich verloren geht. Natives ACP, welches im pH-Bereich 6,6–10,6 ausgefällt wurde, variierte im molaren Ca/P-Verhältnis zwischen 1,18 und 1,50 und in HPO 4 2− /totales P zwischen 33,0 und 10,1%. Bei pH 7,40 hatte natives ACP ein molares Ca/P-Verhältnis von 1,36±0,02 und enthielt 22,8 (±2,2)% HPO 4 2− . Die Werte beim ungewaschenen Niederschlag rühren weder von aus dem Überstand aufgenommenem Ca2+ und HPO2−, noch von außen kommendem Na+, Cl− und CO 3 2− her. Die amorphen Calciumphosphate werden als eine Klasse von Salzen erkannt, welche veränderliche chemische, aber identische glasartige physicochemische Eigenschaften haben. Nicht kristallines CaHPO4·xH2O kann auch ein ACP sein, besonders in den frühen Bildungsstadien. Bei physiologischem pH verwandelt sich ACP in kleine plattenförmige Kristalle, welche große Mengen von leicht ersetzbarem saurem Phosphat enthalten. Das Waschen dieser Oberflächenschicht erzeugte chemische Veränderungen in den resultierenden Kristallen; ungewaschene Kristalle zeigten ein Diffraktionsmuster, das nur schwach demjenigen des kristallinen Aspatites glich, aber ein schlecht aufgelöstes Infrarotspektrum, welches zwischen Apatit und Octocalciumphosphat war. Es werden strukturelle Erklärungen für alle diese Phenomena diskutiert, und revidierte amorph/kristalline Mineralzusammensetzungen von Knochen und Knorpel wurden neu berechnet.
    Notes: Abstract Unwashed samples of amorphous calcium phosphate (ACP) contain an irreplaceable labile fraction, rich in acid phosphate and low in Ca/P ratio, which is irreversibly lost during the washing process. Native ACP precipitated in the pH range 6.6–10.6 varied in Ca/P molar ratio from 1.18 to 1.50 and in HPO 4 2− /total P from 33.0% to 10.1%. At pH 7.40, native ACP had a Ca/P molar ratio of 1.36±0.02 and contained 22.8 (±2.2)% HPO 4 2− . Unwashed precipitate data could not be attributed to either trapped supernatant Ca2+ and HPO 4 2− or extraneous Na+, Cl−, and CO 3 2− . The amorphous calcium phosphates are recognized as a class of salts having variable chemical but identical glass-like, physicochemical properties. Non-crystalline CaHPO4·xH2O may also be an ACP, especially during early formative stages. At physiological pH, ACP transforms to small platy crystals containing large amounts of readily-replaceable acid phosphate. Washing this surface layer produced chemical alterations in the resultant crystals; unwashed crystals had poorly-crystalline apatitic diffraction patterns but exhibited poorly-resolved infrared spectra intermediate between apatite and octacalcium phosphate. Structural explanations for all these phenomena are discussed, and revised bone and cartilage amorphous/crystalline mineral compositions have been re-calculated.
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