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  • 2020-2022
  • 1980-1984  (3,918)
  • 1920-1924  (3,032)
  • Inorganic Chemistry  (6,538)
  • Gas chromatography  (412)
Material
Years
Year
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Naunyn-Schmiedeberg's archives of pharmacology 327 (1984), S. 260-265 
    ISSN: 1432-1912
    Keywords: Amitriptyline ; Imipramine ; Clomipramine ; Demethylated metabolites ; Free fractions ; Serum ; Equilibrium dialysis ; Gas chromatography ; Binding parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The plasma protein binding of amitriptyline, imipramine, clomipramine, and their primary demethylated metabolites were studied by means of a method combining dialysis and gas chromatography. Equilibrium in dialysis of serum containing amitriptyline and its metabolite nortriptyline was attained in about 0.5 h with the drug dissolved in the serum compartment, and in about 2 h with the drug passing from the buffer to the serum compartment. The calculation of free fractions was influenced by variations with dialysis time in the volumes of serum and buffer. Increase of pH in serum increased the protein binding of the weakly basic drugs studied, and made the Donnan distribution effects more pronounced. At pH 7.4, the Donnan effect was negligible. Binding parameters for the 6 tricyclic antidepressant substances studied were estimated for the binding to α1-acid glycoprotein and for total binding in serum. For α1-acid glycoprotein, the k-values ranged from 1·105 to 8·105 M−1, and for pooled serum from 0.4·105 to 8·105 M−1. The determined number of binding sites on the α1-acid glycoprotein was, on average 0.87 for the 6 substances. In serum, the binding capacity was 2–14 times the concentration of α1-acid glycoprotein.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    European journal of pediatrics 142 (1984), S. 165-169 
    ISSN: 1432-1076
    Keywords: Adrenal gland neoplasms ; Urine steroids ; Gas chromatography ; Mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Steroid excretion in urine of 12 infants with virilising adrenal tumours has been determined using gas chromatography. In six children, (Group A, five female, one male) aged 2.8–5.3 years, very high urinary excretions of 17 oxosteroids (〉40 μmol/24 h) were largely accounted for by dehydroepiandrosterone (DHA). In one of the girls, the pattern of steroids excreted in urine was similar to that of newborn infants, with high excretions of 16-oxygenated derivatives of DHA. The histology of this tumour suggested a neoplasia of fetal-type adrenocortical cells. Very large tumours were found in three of the infants, two of whom have died and one has multiple metastases. From the other three children, small, well-encapsulated adenomas were successfully removed. Six children (Group B), had moderately elevated 17-oxosteroid exrretions (8–17 μmol/ 24 h). In five of these cases (four female, one male) aged 0.8–5 years, 11β-hydroxyandrosterone was a consistently prominent urinary steroid. In one boy, aged 7.7 years, 17-oxosteroid excretion was 15 μmol/24 h and the major steroids in urine were metabolites of pregnenolone. These six children have survived with no clinical evidence of recurrent tumour. The in vivo functional activities of the tumours can be deduced from the different profiles of steroids in urine. These have revealed heterogeneous patterns of steroid biosynthesis.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Archives of toxicology 55 (1984), S. 70-75 
    ISSN: 1432-0738
    Keywords: Soman ; Gas chromatography ; Mass spectrometry ; Cholinesterases ; Aliesterase ; Phosphorylphosphatase ; Toxicity ; Stereoselectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The fate of the four stereoisomers of soman [0-(1,2,2-trimethylpropyl)-methyl-fluoro phosphonate] has been studied a) in vivo in mouse blood and liver after IP injection of 0.75 × LD50 Rc- and Sc-soman respectively, and b) in vitro upon incubation wih acetyl- und pseudocholinesterase, aliesterase and phosphorylphosphatase. The analytical method used is based on gas chromatography — mass spectrometry with deuterated internal standard. Most soman disappeared very rapidly from blood and liver. In liver, SCRP and RCRP, the two isomers that preferentially react with cholinesterase, could be detected. The level of SCRP, which was higher than that of RCRP, could be followed for 17–18 h. In blood only SCRP could be detected. The amounts found were fairly constant during the time period 2 min to 4h, and it could even be detected 17–18 h after soman administration.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Archives of toxicology 55 (1984), S. 272-275 
    ISSN: 1432-0738
    Keywords: 2-Ethoxyethanol ; Teratogen ; Adsorption ; Desorption ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A gas Chromatographic procedure for the determination of 2-ethoxyethanol (C2H5OCH2CH2OH) was developed by using the general principles of analysis of solvent vapors. 2-Ethoxyethanol was sampled by adsorbing on activated carbon. It was desorbed with carbon disulfide plus 2-propanol (0.5%). The analytical column was packed with 10% free fatty acid phase on Chromosorb-P AW. The analysis was conducted at 130° C isothermal using a flame ionization detector. Addition of 2-propanol (0.5%) to carbon disulfide improved (P≤0.01) desorption of 2-ethoxyethanol adsorbed on activated carbon. The mean desorption efficiency of carbon disulfide plus 2-propanol (0.5%) was 87.9±2.86% (n=15). Based on a 101 air sample and detector sensitivity of 2×10−10AFS, the calculated limit of detection of 2-ethoxyethanol was 0.1 ppm. The precision (coefficient of variation) for this analytical procedure was 3.34% (n=12). In conclusion, 2-ethoxyethanol adsorbed on activated carbon can be desorbed with carbon disulfide plus 2-propanol (0.5%). Subsequently the desorbed 2-ethoxyethanol can be analyzed by gas chromatographic identification on 10% FFAP using a flame ionization detector.
    Type of Medium: Electronic Resource
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  • 5
    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.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 7
    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.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 9
    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.
    Type of Medium: Electronic Resource
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  • 10
    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.
    Type of Medium: Electronic Resource
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  • 11
    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.
    Type of Medium: Electronic Resource
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 329-332 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Polymethylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 338-339 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Pesticides ; Multidetection ; ECD-NPSD-SSD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 332-333 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Polarity mixtures ; Reaction products ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 370-374 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Trace analysis ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Large sample volume on-column injection (up to 250 μL) of n-pentane solutions of halogenated hydrocarbons has been employed for the direct measurement of both low-boiling and high-boiling compounds in what is essentially a single run. Two-bonded phase, fused-silica capillary columns are joined in series, through which the low-boiling compounds are first chromatographed and detected with an electron capture detector. High-boiling compounds are then trapped in a section joining the two columns, and subsequently chromatographed in the second column, using the same detector. This procedure permits analysis at the ppt level.
    Additional Material: 7 Ill.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 404-410 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Multidimensional capillary columns ; Enantiomeric separations ; Intermediate trapping ; Mixed polarities ; Terpene alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 18
    ISSN: 0935-6304
    Keywords: Low and high resolution liquid chromatography ; Gas chromatography ; Capillary columns ; Alkali flame detection ; Chemical ionization mass spectrometry ; Nitro-PAHs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical procedure is described for the fractionation of organic compounds present in environmental samples and the determination of nitro polyaromatic hydrocarbons (nitro-PAHs). Both low and high resolution liquid chromatography are employed for the prefractionation of the soluble organic fraction (SOF) extracted from particulate matter or gaseous pollutants collected on adsorption traps. High resolution gas chromatography is used to analyze four fractions containing alkanes, PAHs, nitro-PAHs, and other polar PAHs. Nitrogen-containing species are separated by GC and detected specifically using an alkali flame (NPD) detector. Flame ionization (FID) detection, GC-MS of positive ions, and negative ion chemical ionization MS of the whole fraction is used for the identification and quantitation of the various components. The composition of SOF extracted from particulate matter emitted from diesel exhausts is elucidated and a large number of nitro-PAHs identified by the combination of the various techniques.
    Additional Material: 7 Ill.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 536-537 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; On-Column injection ; Vaporizing injection ; Decomposition ; α-Ferrocenyl carbinols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 700-701 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary columns ; Immobilization ; 60Co gamma radiation ; Medium-polarity phase ; OV-1701-Vi ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 142-143 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solute focussing ; Solvent effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 22
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 215-217 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Coupled columns ; Halogenated organic pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 222-224 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Interface ; Partition ; Adsorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 282-283 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Gas analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 306-311 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Thermodesorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A commercial thermodesorption and cold trap unit can be used as a large sample volume injection device in high resolution gas chromatography. Volumes of more than 100 μl can be injected. More than 97% of solvents, such as hexane, can be removed by a Tenax TA precolumn without any loss of compounds with volatilities comparable to naphthalene. Experimental conditions, recovery rates of polycyclic aromatic hydrocarbons, and the reproducibility of the method are described in detail. The method was successfully applied for the determination of PAH in air particulate matter extracts.
    Additional Material: 3 Ill.
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  • 26
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 334-335 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused-Silica columns ; Thermal stability ; Dibenzothiophene oxides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 477-479 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary column ; Adsorbent ; Cold trapping ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 28
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 414-422 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Steroid analysis ; Sample pretreatment ; Sample introduction ; Separation speed ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Quantitative analysis of steroids and their metabolites in urine samples calls for increased speed of sample clean-up, of the derivatization procedure, and of separation. A fast procedure for sample pretreatment, which can be performed within 8 hours, is introduced and evaluated. It is shown that use of fast pretreatment in combination with narrow bore columns, which are compatible with existing instrumentation, can considerably increase, laboratory throughput. The effect of different sample introduction techniques (e.g. splitless, on-column, and moving needle) on column efficiency and resolution is demonstrated and discussed.
    Additional Material: 7 Ill.
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  • 29
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 492-494 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Closed loop stripping analysis ; Filter extraction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 30
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 137-139 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Deactivated fused silica tubing ; Zero dead volume union ; Capillary column GC/MS interface ; Test mixture for non-polar columns ; Test mixture of phenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 31
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 144-146 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Cyclopentolate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 32
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 185-190 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Mass spectrometry ; Dynamic headspace ; Deans switching ; Cold trap ; Reinjection ; Polymers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An experimental method for the analysis of volatile organic compounds in polymers is described. The technique involves dynamic headspace sampling, collection, and concentration of the volatiles in a cold trap, followed by capillary column gas chromatography/mass spectometry. Flow switching is carried out by the Deans switching technique. Four technical polymers used as pharmaceutical packaging materials have been analyzed in order to demonstrate the method.
    Additional Material: 6 Ill.
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  • 33
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 212-214 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Trace analysis ; Solvent effect in GC ; Parts per trillion ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 34
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 270-273 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Temperature-programmed analysis ; Retention indices ; Polychclic aromatic hydrocarbons (PAH) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 35
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 340-342 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Sample preparation ; Closed loop stripping analysis ; Charcoal adsorbent filter ; Overcoming contamination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 36
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 487-489 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Multi-dimensional technique ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 37
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 533-536 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Fungicides and insecticides ; Sensitivity limits ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 38
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 140-141 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Narcotics: street samples ; Narcotics, adulterants and diluents: simultaneous determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 39
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    Journal of High Resolution Chromatography 7 (1984), S. 148-150 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; On-column injection/enrichment ; Milliliter sample volumes ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 40
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    Journal of High Resolution Chromatography 7 (1984), S. 191-195 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Saturated hydrocarbons ; Retention indices ; Molar refraction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Kováts retention indices for a series of linear, branched, and cyclic alkanes on squalane at any temperature, and on other stationary phases of different polarity at a given temperature, are related to physicochemical properties of the solutes, such as boiling point and molar refraction, by multiple regression analysis. The equations found permit calculation of the Kováts retention index for all alkanes, with standard deviations close to experimental error. The same equations can also be used for calculating the physicochemical parameters they contain.
    Additional Material: 8 Tab.
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  • 41
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    Journal of High Resolution Chromatography 7 (1984), S. 209-210 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solvent effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 42
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 274-276 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, glass ; Liquid-liquid and liquid-solid extraction ; Serum lipids ; Fatty acids ; Cholesterol and cholesteryl esters ; Triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 43
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 280-281 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Reaction GC ; Iodination reactor ; Electron capture detection ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 44
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    Journal of High Resolution Chromatography 7 (1984), S. 284-285 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Fruit juices ; Amino acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 45
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Thick liquid phase films ; Natural and refinery gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary columns having a thick liquid phase film and a low phase ratio permit the separation of low molecular mass compounds which would have a very small capacity factor on columns with a classical thin film. At the same time, the increased sample capacity allows conventional hot-wire thermal conductivity detectors to be used with such columns. The analysis of natural and refinery gases, containing both inorganic compounds and light (C1—C7) hydrocarbons, utilizing a combination of hot-wire and flame ionization detectors, is demonstrated.
    Additional Material: 10 Ill.
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  • 46
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    Journal of High Resolution Chromatography 7 (1984), S. 382-388 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; HETP equation ; Optimum column parameters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An HETP equation for the capillary column is developed that takes into account the dependence of gaseous diffusion on pressure, the compressibility of the mobile phase, together with the unique relationship between mobile phase velocity, and the resistance to mass transfer in the stationary phase. The equation is used to develop a procedure for column optimization and expressions are derived that allow the optimum column radius and optimum column length to be calculated for a given fixed inlet pressure. It is shown that fast, simple separations are optimally achieved using relatively short small diameter columns. Conversely, optimum performance for the separation of complex mixtures requiring higher efficiencies requires the use of long columns with relatively large diameters.
    Additional Material: 5 Ill.
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  • 47
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    Journal of High Resolution Chromatography 7 (1984), S. 431-432 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 48
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Packed and capillary columns ; Fungicides and insecticides ; Adsorption ; Length of column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 49
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    Journal of High Resolution Chromatography 7 (1984), S. 504-508 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; GC/MS/DS ; Cryotrapping and cryofocussing of organics ; Purgeable compound analysis ; Trace organic analysis ; Priority pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The purge and trap (P&T) method of analysis has been interfaced with fused silica capillary column gas chromatography. This interfacing has been accomplished without splitting the P&T trap desorption carrier gas. Thus, 100% of the purged compounds are transferred to the column. The analytes are cryofocussed on the column using whole column cryotrapping (WCC) at -80°C. The resulting P&T/WCC procedure is extremely well-suited to the analysis of trace purgeable aqueous organic compounds. Samples and standards containing a variety of aromatic standard compounds were analyzed. The standards included benzene, toluene, ethylbenzene, xylenes, C3-C4-benzenes, and naphthalene, as well as three P&T internal standard compounds. Chromatographic peak widths were uniformly less than 6 s at the base and excellent precision was obtained in the relative retention time data for all compounds. The chromatogram of a groundwater sample contaminated with aromatic gasoline compounds is also presented. Since P&T/WCC works well with fused silica capillary columns, the full sensitivity and chromatographic efficiency of capillary gas chromatography is made available to P&T analyses.
    Additional Material: 2 Ill.
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  • 50
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    Journal of High Resolution Chromatography 7 (1984), S. 542-544 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica (capillary) columns ; Bonded (cross-linked) phases ; Hydrocarbon analysis ; Olefinic hydrocarbons ; Retention index data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
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  • 51
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    Journal of High Resolution Chromatography 7 (1984), S. 48-48 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Carrier gas flow controller unit ; On-column injection ; Sample, loading onto column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 52
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    Journal of High Resolution Chromatography 7 (1984), S. 89-92 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Stationary phase ; Polysiloxane ; Autocrosslinkable ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl-2-phenylethylpolysiloxane polymers have been synthesized for comparison with methylphenylpolysiloxane stationary phases for gas chromatography. The 50% 2-phenylethyl polysiloxane was found to be autocrosslinkable at 260°C without addition of free redical initiator. Although the selectivity of this phase appears to be similar to the 50% phenyl polysiloxane, its thermal stability is not as high.
    Additional Material: 2 Ill.
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  • 53
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    Journal of High Resolution Chromatography 7 (1984), S. 92-94 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Solute focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 54
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    Journal of High Resolution Chromatography 7 (1984), S. 540-541 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary ; SDE enrichment ; Fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 55
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Immobilized capillary columns ; Aqueous solutions ; On-column injection ; Split injection ; Multidimensional separations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Various methods of gas chromatographic analysis at high resolution and low detection limits in aqueous solutions are described with regard to sampling techniques, column technology, and the application of coupled pre-columns, also including multidimensional methods. Immobilized polyethylene glycol (Carbowax 20 M) columns have also been produced and used successfully.
    Additional Material: 11 Ill.
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  • 56
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    Journal of High Resolution Chromatography 7 (1984), S. 13-18 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Biphenyl polysiloxane ; Stationary phase ; Polarizable phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A crosslinkable biphenylmethylpolysiloxane stationary phase was synthesized for capillary column gas chromatography and compared with methyl, phenyl, and cyanopropyl polysiloxane stationary phases for the separation of isomeric polycyclic aromatic compounds. While the new phase gave similar separations of nonpolar isomers when compared to the nonpolar phases, separations of polar isomers were greatly improved because of the induced polarity of the biphenyl group of the stationary phase by the solute molecules. This polarizable stationary phase offers a unique selectivity which is not available in other stationary phases.
    Additional Material: 5 Ill.
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  • 57
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    Journal of High Resolution Chromatography 7 (1984), S. 19-24 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Splitless injection ; Flash derivatization ; Quaternary ammonium compounds ; Acetylcholine ; Biogenic amines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A conventional splitless injector is used as a pyrolysis chamber or chemical reactor for the N-demethylation of acetylcholine and other choline esters. The novel uses of 2-aminoethanol as a N-demethylation reagent in splitless injection and bonded-phase fused silica capillary columns in the separation of the tertiary amine derivatives of choline esters are described. A comparison is made between non-polar and moderately polar fused silica capillary columns in the separation of choline esters.
    Additional Material: 4 Ill.
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  • 58
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    Journal of High Resolution Chromatography 7 (1984), S. 25-32 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; CGC-ECD, CGC-MS ; Chlorophenols ; Chlorophenoxyalkanoic acids ; Neutral chlorinated compounds ; Biological sewage treatment plant ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The environmentally hazardous organic substances in the waste water from the manufacture of chlorophenoxyalkanoic acids have been identified and semiquantified before and after passing through a biological treatment plant for municipal sewage, the secondary effluent of which is discharged into a marine ecosystem. The organics belong to three groups: (i) chlorophenols; (ii) chlorophenoxyalkanoic acids; and (iii) chlorinated neutrals. The removal of chlorophenols and phenoxyalkanoic acids was shown to be good, with a 90% overall reduction of chlorinated substances in the sewage passing through the treatment plant. The lowest reduction occurred for the polychlorinated compounds. Two chlorobenzofurans among the chlorinated neutrals were preliminarily identified.
    Additional Material: 2 Ill.
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  • 59
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mass spectrometry ; Capillary GC ; Fused silica GC ; 6-Nitrobenzo[a]pyrene ; 3-Nitrobenzo[a]pyrene ; 1-Nitrobenzo[a]pyrene ; 3-Nitrobenzo[e]pyrene ; Nitro-PAHs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 60
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    Journal of High Resolution Chromatography 7 (1984), S. 33-37 
    ISSN: 0935-6304
    Keywords: Chlorinated paraffins ; Gas chromatography ; Mass spectrometry ; Negative ion ; Chemical ionization ; Capillary column ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Although chlorinated paraffins (CP) are produced in large amounts (300 000 tonnes per year), little is known about their occurrence in the environment due to the lack of specific and sensitive analytical methods. The present paper describes the GC/MS analysis of different CP's using capillary gas chromatography with on-column injection and negative ion chemical ionization (NCI) mass spectrometry. Chromatographic resolution of groups of isomers and homologues was obtained. The chromatograms and mass spectra are discussed. The suitability of this method for trace analysis of a CP sample using multiple ion detection (MID) is described.
    Additional Material: 3 Ill.
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  • 61
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    Journal of High Resolution Chromatography 7 (1984), S. 68-73 
    ISSN: 0935-6304
    Keywords: MS-MS ; Gas chromatography ; Capillary GC-ECD, GC-MS, GC-MS-MS ; Bleaching ; Chlorine compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatography (GC) with electron capture detection (ECD), GC combined with mass spectrometry (MS), GC with multi-stage mass spectometry (MS-MS), and direct inlet MS-MS have been used to determine 1,1-dichlorodimethyl sulfone (DDS) in aquatic organisms in the receiving waters outside a pulp mill bleach plant. Both GC-MS-MC and direct inlet MS-MS of tissue extracts of fish and mussel appear to be sensitive, selective, and rapid analytical techniques for the determination of DDS.
    Additional Material: 8 Ill.
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  • 62
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; HPLC prefractionation ; MS ; ECD ; Substituted PAHs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described which allows the determination of different substituted polycyclic aromatic hydrocarbons (PAH) such as NO2-PAH, carbazoles, keto-PAH, and aza-arenes in aerosol samples. Liquid CO2-extraction is used to minimize the loss of reactive compounds. High performance liquid chromatography on chemically activated silica is employed to prefractionate the samples into subfractions with a minimum of overlap between different PAH compound classes. Both electron capture detection and negative ion chemical ionization combined with capillary gas chromatography are used for identification and quantification. The latter method also allows distinction between isomers with different toxic properties when N2O/CH4 reaction gas mixtures are used. Selectivity for tetrachlorodibenzo-p-dioxins as against pesticides and polychlorinated biphenyls can be improved by this technique. The applicability of the method is critically discussed and different examples are given.
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  • 63
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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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  • 64
    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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  • 65
    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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  • 66
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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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  • 67
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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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  • 68
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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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  • 69
    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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  • 70
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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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  • 71
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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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  • 72
    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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  • 73
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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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  • 74
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    Zeitschrift für anorganische Chemie 508 (1984), S. 187-190 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Komplexe von Halogeniden der IV. Gruppe mit einzähnigen Schiffschen BasenVerschiedene Komplexe, die bei der Reaktion von N-(phenyl)benzalaldimin und seinen Derivaten mit einer Methylgruppe in verschiedenen Positionen des Anilinringes mit Halogeniden der IV. Gruppe, MX4, (M = Si bzw. Sn und X = Cl bzw. Br) entstehen, wurden hergestellt und mittels UV-, IR- und Raman-Spektren charakterisiert.
    Notes: Coordination compounds resulting from the interaction of N-(phenyl)benzalaldimine and its derivatives containing a methyl group in different positions of the aniline ring and group(IV) halides, MX4 (where M = Si or Sn and X = Cl or Br), have been prepared and characterized by elemental analyses and electronic, infrared and Raman spectra.
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  • 75
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 208-208 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 76
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 38-52 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Phosphorus. 134. On the Triphosphanes H(t-BuP)3H' Li(t-BuP)3Li, and Me3Si(t-BuP)3SiMe3The reaction of 1,3-diiodo-1,2,3-tri-tert-butyltriphosphane, I(t-BuP)3I, with lithium aluminium hydride leads to 1,2,3-tri-tert-butyltriphosphane, H(t-BuP)3H (1). 1 reacts with n-butyllithium to 1,3-dilithium-1,2,3-tri-tert-butyltriphosphide, Li(t-BuP)3Li (2), which reacts further with trimethylchlorosilane yielding 1,3-bis(trimethylsilyl)-1,2,3-tri-tert-butyltriphosphane, Me3Si(t-BuP)3SiMe3 (3). The triphosphanes 1, 2 and 3 could be isolated in a pure state. In solution 1 forms the threo, threo and the threo,erythro configurated diastereomers 1a and 1b in a ratio of about 2:1. 3 predominantly exists in form of the threo,erythro configurated diastereomer 3b by steric reasons.
    Notes: Die Umsetzung von 1,3-Diiod-1,2,3-tri-tert-butyltriphosphan, I(t-BuP)3I, mit Lithiumaluminiumhydrid führt zu 1,2,3-Tri-tert-butyltriphosphan, H(t-BuP)3H (1). 1 reagiert mit n-Butyllithium zu 1,3-Dilithium-1,2,3-tri-tert-butyltriphosphid, Li(t-BuP)3Li (2), das mit Trimethylchlorsilan weiter zu 1,3-Bis(trimethylsilyl)-1,2,3-tri-tert-butyltriphosphan, Me3Si(t-BuP)3SiMe3 (3), umgesetzt werden kann. Die Triphosphane 1, 2 und 3 konnten in reiner Form isoliert werden. In Lösung bildet 1 die threo, threo- und threo,erythro-konfigurierten Diastereomere 1 a und 1 b im Verhältnis von etwa 2:1. 3 liegt aus sterischen Gründen hauptsächlich in Form des threo, erythro-konfigurierten Diastereomers 3 b vor.
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  • 77
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 145-152 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Oxidation Products of Intermetallic Compounds. III. Low Temperature Forms of K2Sn2O3 and Rb2Sn2O3 and a Notice about K2Ge2O3By controlled oxidation of KSn (at 320°C) and RbSn (at 410°C) with O2 the hitherto unknown low temperature forms of K2Sn2O3 (a = 8.4100(8) Å) and Rb2Sn2O3 (a = 8.6368(8) Å) are obtained, which are isotopic with cubic K2Pb2O3. Oxidation at higher temperatures (at 510-5207°C) leads to the well-known HT-forms. The Madelung Part of Lattic Energie, MAPLE, is calculated for both compounds.K2Pb2O3, Rb2Pb2O3, Cs2Pb2O3, and Cs2Sn2O3 have been prepared too by oxidation of KPb, RbPb, CsPb, and CsSn.Oxidation of KGe (at 400°C) leads to the first oxogermanate(II), K2Ge2O3 (cubic a = 8.339(1) Å, isotypic with K2Pb2O3) together with K6Ge2O7.
    Notes: Aus KSn bzw. RbSn entstehen durch direkte Oxydation K2Sn2O3 bzw. Rb2Sn2O3 bei 320°C bzw. 410°C die bislang unbekannten „Tieftemperaturformen“ (a = 8,4100(8)Å bzw. a = 8,6368(8)Å), isotyp mit kubischem K2Pb2O3. Bei höherer Temperatur (510 bzw. 520°C) entstehen die bekannten Hochtemperaturformen.Der Madelunganteil der Gitterenergie, MAPLE, wird berechnet und diskutiert.Ebenso erhält man durch direkte Oxydation von KPb, RbPb, CsPb und CsSn die Oxide K2Pb2O3, Rb2Pb2O3, Cs2Pb2O3 und Cs2Sn2O3. Durch Oxydation von KGe wurde bei 400°C erstmals K2Ge2O3 (kubisch a = 8,339(1) Å; isotyp mit K2Pb2O3) neben K6Ge2O7 erhalten.
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  • 78
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 174-182 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion des SnCl2 mit Br2 und I2 in schwachen Donor-LösungsmittelnEs wurden die Verbindungen SnCl2Br2(MeCN)2, “Sn3Cl8Br4(THF)6” und “Sn3Cl10Br2(OEt)6” durch Reaktion zwischen SnCl2 und Br2 in Acetonitril (MeCN), Tetrahydrofuran (THF) und Diethylether (OEt2) gewonnen. Die zwei letzten Verbindungen sind feste Lösungen von SnCl4L2 und SnCl2Br2L2 (L = THF, OEt2) jeweils im Verhältnis 1:2 und 2:1. Die Verbindungen wurden mit Hilfe von IR-, Raman- und Mößbauer-Spektroskopie charakterisiert. Es wurde C1-Symmetrie für SnCl2Br2(MeCN)2 und C2v mit den Liganden in trans-Position für SnCl2Br2L2 (L = THF, OEt2) gefunden. Das bisher nicht bekannte Mößbauer-Spektrum des SnBr4(THF)2 wurde gemessen und ebenfalls die Reaktion zwischen SnCl2 und I2 in denselben Lösungsmitteln studiert. Die Bildung des SnCl4L2 (L = MeCN, THF, OEt2) SnI4 und einer kleinen Menge des SnI3Cl wurde beobachtet und Raman-spektroskopisch identifiziert.
    Notes: The compounds SnCl2Br2(MeCN)2, “Sn3Cl8Br4(THF)6”, and “Sn3Cl10Br2(OEt2)6” were obtained by reaction between SnCl2 and Br2 in acetonitrile (MeCN), tetrahydrofuran (THF) and diethyl ether (OEt2). The two last are solid solutions of SnCl4L2 and SnCl2Br2L2 (L = THF, OEt2) in the proportions 1:2 and 2:1, respectively. The compounds are characterized by IR, Raman, and Mössbauer spectroscopy, a C1 symmetry being found for SnCl2Br2 (MeCN)2 together with a C2v symmetry, with the ligands in trans positions, for SnCl2Br2L2 (L = THF, OEt2). The Mössbauer spectrum of SnBr4(THF)2 was also obtained, which has not previously been reported. The reaction between SnCl2 and I2 has also been studied in the same solvents, and the formation of SnCl4L2 (L = MeCN, THF, OEt2), SnI4, and a small amount of SnI3Cl was observed, which have been identified by Raman spectroscopy.
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  • 79
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 192-200 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Einige Cobalt(II)-Komplexe von 4,6-Dimethylpyrimidin-2(1H)-on (HL) wurden dargestellt und mittels IR- und Elektronenspektren magnetochemisch und konduktometrisch untersucht. Der Ligand wird über das nicht protonierte N-Ringatom angelagert und in einem Fall auch über das O-Atom der Carbonylgruppe. Die “blauen” Komplexe [CoX2 · 2HL] (X2 = Cl2, CBr, Br2, (NCS)2) und [CoX2 · 2HL] · 2HL (X = Cl, Br) haben eine verzerrte C2v-Anordnung [CoX2N2]; die Thiocyanate sind über die N-Atome an das Metall gebunden. Die „grünen“ Komplexe CoX2 · 2HL (X = Cl(4H2O), Br) besitzen eine quadratisch-pyramidale Anordnung [CoX2N2O]. Die „rosa“ Komplexe CoX2 · 4HL · nH2O (X = ClO4, n = 2, X = BF4, n = 8, CF3CO2, n = 4) und die „cremefarbigen“ CoX2 · 4HL · 6H2O (X = J, ClO4) zeigen oktaedrische Anordnung; nur CF3CO2- ist koordiniert. Die „veilchenfarbenen“ Komplexe CoAcL · 2HL · 2H2O und Co3Ac4L2 · 2HL · 2H2O haben eine mehrkernige Struktur; das Acetation betätigt sich als zweizähniger Ligand.
    Abstract: CoII-Komplexe von 4,6-Dimethylpyrimidin-2(1H)-on
    Notes: Some cobalt(II) complexes of 4,6-dimethylpyrimidine-2(1H)-one (HL) have been prepared and studied by infrared and electronic spectra and by magneto-chemical and conductometric measurements. The ligand is coordinated through the unprotonated ring-nitrogen atom and in one case also through the carbonylic oxygen atom. The “blue” complexes [CoX2 · 2HL] (X2 = Cl2, ClBr, Br2, (NCS)2) and [CoX2 · 2HL] · 2HL (X = Cl, Br) have a distorted C2v [CoX2N2] coordination; the thiocyanate ion is N-bonded to the metal. The “green” complexes CoX2 · 2HL (X = Cl(4H2O), Br) have a square-pyramidal [CoX2N2O] coordination. The “pink” CoX2 · 4HL · nH2O (X = ClO4, n = 2; X = BF4, n = 8; X = F3Ac, n = 4) and “cream” CoX2 · 4HL · 6 H2O (X = I, ClO4) complexes have an octahedral coordination; only the F3Ac- ion is coordinated. The “cyclamen” CoAcL · 2HL · 2 H2O and Co3Ac4L2 · 2HL · 2H2O complexes have a polynuclear constitution; the Ac- ion behaves as bidentate ligand.
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  • 80
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 31-36 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Raman Spectroscopic Investigations of Coordination Polymeric Metal TricyanmethanidesThe Raman spectra of 3d-metal tricyanmethanides M{C(CN)3}2 as well as of [Ni{C(CN)3}2py2] are investigated. The observed Raman lines are assigned, characteristic variations of position and intensity of these lines are discussed.
    Notes: Es werden die Ramanspektren der koordinationspolymeren 3d-Metalltricyanmethanide M{C(CN)3}2 (M = Mn, Fe, Co, Ni, Zn) sowie von [Ni{C(CN)3}2py2] untersucht. Die beobachteten Ramanlinien werden zugeordnet, charakteristische Variationen der Lage und Intensität dieser Linien werden diskutiert.
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  • 81
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    Zeitschrift für anorganische Chemie 510 (1984), S. 51-60 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry and Structural Chemistry of Phosphides and Polyphosphides. 34. Vapor Pressure Measurements in the Europium-Phosphorus SystemThe vapor pressure of the europium phosphides EuP7, α-EuP3, ß-EuP3, EuP2 and Eu3P4 were measured using the Knudsen-Effusion technique. These compounds were vaporized incongruently according to the general reaction a EuPm, (s) = a EuPn, (s) + P4, (g) where a (m - n) = 4. The following enthalpies and entropies of reaction were calculated (δH)kJ · mol-1/δS (J · K-1 mol-1)/ T(K). [δH/δS/T]: EuP7 → ß-EuP3 [191/215/698]; α-EuP3 → EuP2 [212/162/847]; ß-EuP3 → EuP2 [261/212/847]; EuP2 → Eu3P4 [209/144/868]; Eu3P4 → EuP [240/131/1110]. The temperature and pressure ranges over which these phosphides exist were determined from the above values. Standard enthalpies of formation relative to EuP(s) were calculated by combining different reaction enthalpies. The results demonstrate the relatively high stability of ß-EuP3, EuP7 and the instability of EuP2.
    Notes: Für die Europiumphosphide EuP7, α-EuP3, ß-EuP3, EuP2 und Eu3P4 wurden die Dampfdrucke der inkongruenten Verdampfungsreaktionen a EuPm, (f) = a EuPn, (f) + P4, (g) mit a(m - n) = 4 mit der Knudsen-Methode gemessen. Zur Abspaltung von einem Mol P4,(g) wurden bei den mittleren Temperaturen T(K) die folgenden Reaktionsenthalpien δH(kJ · mol-1) und Reaktionsentropien δS(J · K-1 · mol-1) erhalten: [δH/δS/T]: EuP7 β ß-EuP3 [191/215/698]; α-EuP3 → EuP2 [212/162/847]; ß-EuP3 → EuP2 [261/212/847]; EuP2 → Eu3P4 (209/144/868); Eu3P4 → EuP [240/131/1110]. Hierdurch wurden die Existenzfelder der verschiedenen Europiumphosphide in Abhängigkeit von Druck und Temperatur festgelegt. Durch Kombination der verschiedenen Reaktionsenthalpien werden die Standardbildungsenthalpien der Phosphide relativ zu EuP berechnet. Sie zeigen die hohe Stabilität von ß-EuP3 und EuP7 sowie die Instabilität von EuP2.
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  • 82
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    Zeitschrift für anorganische Chemie 508 (1984), S. 86-92 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of (PPh4)2[Mo2Cl10]The title compound is obtained in the reaction of [MoCl4(Ph—C≡C—Ph)]2 with tetraphenylphosphonium chloride in dichloro methane, forming brown crystals. It is characterized by the i.r. spectrum and a crystal structure analysis by the aid of X-ray diffraction data. The complex crystallizes triclinic in the space group P1 with one formula unit per unit cell. The cell dimensions are a = 1122 pm, b = 1137 pm, c = 1283 pm; α = 63.4°, β = 69.1°, γ = 86.5°. The crystal structure determination (2959 observed, independent reflexions, R = 4.5%) shows the constants of the unit cell to consist of on centrosymmetric anion, two cations and one disordered molecule of dichloro methane. The distance Mo—Mo in the anion is 380 pm, which excludes direct magnetic interaction between the molybdenum atoms.
    Notes: Die Titelverbindung entsteht in Form brauner Kristalle durch Umsetzung von [MoCl4(Ph—C≡C—Ph)]2 mit Tetraphenylphosphoniumchlorid in Dichlormethan; sie wird durch das IR-Spektrum und durch eine Kristallstrukturbestimmung charakterisiert. Der Komplex kristallisiert triklin in der Raumgruppe P1 mit einer Formeleinheit pro Elementarzelle. Die Zellparameter betragen a = 1122 pm, b = 1137 pm, c = 1283 pm, α = 63,4°, β = 69,1°, γ = 86,5°. Die röntgenographische Kristallstrukturbestimmung (2959 beobachtete, unabhängige Reflexe, R = 4,5%) zeigt, daß die Struktur aus zentrosymmetrischen, dimeren Anionen, isolierten Kationen, und einem fehlgeordneten Molekül Dichlormethan pro Elementarzelle besteht. Der Mo—Mo-Abstand im Anion beträgt 380 pm, was eine direkte magnetische Wechselwirkung zwischen den Mo-Atomen ausschließt.
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  • 83
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal and Molecular Structure of Tris(diethyldithiocarbamato)dimethylphenylphosphinetechnetium (III)The title compound Tc(S2CNEt2)3(Me2PhP) I has been prepared by the reaction of TcCl3(Me2PhP)3 with NaS2CNEt2. The crystal structure of I has been determined by single-crystal X-ray diffraction methods at room temperature. Crystals are rhombic, space group P212121, with a = 8.708(1), b = 12.012(1), c = 29.626(3) Å and Z = 4. The compound consists of discrete I molecules. The technetium atom has a seven-coordinated environment which is best described as a distorted pentagonal bipyramid. The Tc - P distance (2.330(3) Å) is remarkably short compared with other technetium complexes with mono-dentate phosphine ligands.
    Notes: Die Titelverbindung Tc(S2CNEt2)3(Me2PhP) I wurde durch Reaktion von TcCl3(Me2PhP)3 mit NaS2CNEt2 dargestellt und ihre Kristall- und Molekülstruktur durch Röntgenstrukturanalyse ermittelt. Die Kristalle sind rhombisch, Raumgruppe P212121, mit a = 8,708(1), b = 12,012(1), c = 29,626(3) Å und Z = 4. Die Verbindung besteht aus diskreten monomeren Molekülen. Das Technetiumatom hat siebenfache Koordination, die am besten als geringfügig verzerrte pentagonale Bipyramide beschrieben werden kann. Die Tc - P-Bindungslänge (2,330(3) Å) ist bemerkenswert kurz im Vergleich zu anderen Technetiumkomplexverbindungen mit einzähnigen Phosphanen.
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  • 84
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    Zeitschrift für anorganische Chemie 510 (1984), S. 152-162 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermodynamics and Structure of Molten Mixtures Alkali Halide-Alkaline Earth HalideThermodynamic quantities ai, fi, GE, and SE were calculated on the basis of vapour pressures of molten mixtures of the type alkali halide-alkaline earth halide. Negative deviations from ideality were found in all systems. The influence of cations or anions on the properties of mixtures is discussed. There is a good correlation between GE and the change of polarization energy δEp. Strong ionic interactions were found in molten mixtures, especially in the system RbBr - CaBr2. The existence of stable complex ions in melts could not be shown by Raman spectroscopy.
    Notes: Aus den Dampfdrücken der geschmolzenen Mischungen vom Typ Alkalimetallhalogenid-Erdalkalimetallhalogenid wurden die thermodynamischen Daten ai, fi, GE sowie Orientierungswerte für SE berechnet. In allen Systemen treten z. T. beträchtliche negative Abweichungen von der Idealität auf. An ausgewählten Beispielen wird der Einfluß der Kationen bzw. Anionen auf die Mischungseigenschaften diskutiert. Für die GE-Werte ergibt sich eine gute Korrelation mit der Änderung der Polarisationsenergie δEp. Ramanspektroskopische Untersuchungen konnten die Existenz stabiler komplexer Ionen nicht belegen, weisen aber besonders bei den Mischungen RbBr - CaBr2 auf starke interionische Wechselwirkungen hin.
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  • 85
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    Zeitschrift für anorganische Chemie 510 (1984), S. 189-193 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die binären und ternären Gleichgewichte im System MoO3 - TeO2 - Al2O3 wurden rötgenographisch untersucht. Bei 750°C in Luft wurden in diesem System die im Abstract angegebenen koexistierenden Bereiche gefunden. Eine Bildung ternärer Verbindungen konnten im untersuchten Temperaturbereich (450 - 750°C) nicht beobachtet werden.
    Notes: The binary and ternary equilibrium reactions of Al2O3 with TeO2 and MoO3 were studied by X-ray diffraction methods and the following compatibility ranges were determined in the TeO2 - MoO3 - Al2O3 system at 750°C in air: TeO2, Te2MoO7, Al2TeO6; Te2MoO7, MoO3, Al2TeO6; MoO3, Al2(MoO4)3, Al2TeO6; Al2(MoO4)3, Al2O3, Al2TeO6. Ternary compound formation was not observed in the temperature range investigated (450 - 750°C).Phasengleichgewichte im System MoO3 - TeO2 - Al2O3.
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  • 86
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N.M.R. Spectroscopic Studies of 15N Labelled N-Phosphorylphosphazenes and Imidodiphosphoric Acid Derivatives15N labelled compounds were prepared and investigated by means of 31P- and 15N-NMR spectroscopy. The chemical shift values δP and δN, and the coupling constants 1JPN and 2JPP are discussed and interpreted qualitatively by semiempirical quantumchemical calculations (CNDO/2) using POPLE'S ΔE-model.
    Notes: 15N-markierte Verbindungen der Substitutionsreihen wurden synthetisiert und mit Hilfe der 31P- und 15N-NMR-Spektroskopie untersucht. Die chemischen Verschiebungen δP und δN sowie die Kopplungskonstanten 1JPN und 2JPP werden diskutiert und qualitativ mit Hilfe halbempirischer quantenchemischer Rechnungen (CNDO/2) im Rahmen des POPLE-schen ΔE-Modells interpretiert.
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  • 87
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of the Two-component System Triethylphosphite/Carbon Tetrachloride with Nucleophiles Containing Hydrogen. 1. Reaction with Acyl AmidesAcyl amides react with the two-component system triethylphosphite/carbon tetrachloride yielding N-acyl phosphazenes, (EtO)3P=N—Ac. In this way (EtO)3P=N—P(O)(OEt)2, (EtO)3P=N—CN, (EtO)3P=N—C(O)Ph, and (EtO)3P=N—SO2Ph were prepared. Ethyl esters of phosphoric acid and trichloromethane phosphonic acid were obtained as by-products.
    Notes: Säureamide reagieren mit dem Zweikomponentensystem Triethylphosphat/Tetrachlorkohlenstoff zu N-Acylphosphazenen, (EtO)3P=N—Ac. Auf diese Weise wurden aus entsprechenden Amiden (EtO)3P=N—P(O)(OEt)2, (EtO)3P=N—CN, (EtO)3P=N—C(O)Ph und (EtO)3P=N—SO2Ph dargestellt. Als Nebenprodukte werden Phosphorsäureethylester und Trichlormethanphosphonsäureester erhalten.
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  • 88
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Discrete Polynuclear Metal Complexes from Polysulfide Solutions: [Cu6S17]2-, a Novel Binary Polynuclear CuI Complex with Several Remarkable Structural FeaturesThe complex [Cu6S17]2-, obtained from Cu(acac)2 and an ethanolic polysulfide solution, contains an unusual arrangement of the metal atoms and novel types of ligand coordination, particularly of polysulfido (S42- and S52-) ions. The relevance of the synthesis with respect to the “dilemma of transporting metals together with sulfur” for the process of metal sulfide rock formation is evidenced. (PPh4)2[Cu6S17] crystallizes in the space group C2/c with Z = 4 (for further details see Inhaltsübersicht).
    Notes: Der Komplex [Cu6S17]2-, der als Tetraphenylphosphonium-Salz (1) aus Cu(acac)2 und einer ethanolischen Polysulfidlösung erhalten wurde, zeigt eine ungewöhnliche Anordnung der Metall-Atome und eine neuartige Koordination von Polysulfidoliganden (S42- und S52-). Auf die Relevanz der Synthese bezüglich der Problematik der Entstehung von Metall-Sulfid-Mineralien wird hingewiesen. 1 kristallisiert monoklin in der Raumgruppe C2/c mit Z = 4 (Gitterdimensionen a = 20,270(7), b = 11,605(5), c = 26,331(9) Å, β = 109,68(4)°).
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  • 89
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    Zeitschrift für anorganische Chemie 511 (1984), S. 108-131 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Organosilicon Compounds. 97. About the Influence of the Si-Substituents (Me, Cl) upon the Formation and the Reactions of Ylides1,3-disilapropanes with different grade of chlorination or methylation at the silicon atoms and containing a CCl2 group cleave the Si—P bond of Me3SiPMe2. By subsequent rearrangement ylides with = PMe2Cl group are formed. The reactivity of the CCl2 group depends on the grade of Si-chlorination resp. Si-methylation. Si-methylation decreases the reactivity of the CCl2 group. The reaction of 1,3-disilapropanes and Me3SiPMe2 (molar ratio 1:1) runs in a sequence shown in “Inhaltsübersicht”. Ylid C is able either to react with the initial compound A forming B, or in competition decomposes forming D. Reacting Si-perchlorinated carbosilanes, the decomposition forming D is not to be observed. In Si-methylated ylides like (Me3Si)2C=PMe2—PMe2 and (Me3Si)2C=PMe2—P(Me)SiMe3 the ylid carbon atom is able to abstract a proton of the P—CH3 group resp. P—H groups of the trivalent phosphorus forming (Me3Si)2C(H)PMe2. The rearrangement is proved by deuterated derivatives. The different behaviour is due to the increased basicity of the ylid-C atom in Si-methylated phosphorus ylides. Quite the same behaviour show the phosphorus ylides of 1,3,5-trisilacyclohexane.
    Notes: Die am Si-Atom unterschiedlich chlorierten und methylierten 1,3-Disilapropane mit der CCl2-Gruppe ermöglichen die Spaltung von Me3Si—PMe2 unter Bildung der P-halogenierten Phosphorylide, wobei mit steigendem Methylierungsgrad die Reaktivität abnimmt. Die Umsetzungen verlaufen in folgender Reaktionsfolge: Das Ylid C kann mit der nicht umgesetzten Ausgangsverbindung A zu B zurückreagieren oder es zersetzt sich in einer Konkurrenzreaktion zu D. Bei Si-chlorierten Yliden wird die Bildung von D nicht beobachtet. In Si-methylierten Yliden wie (Me3Si)2C=PMe2—PMe2 und (Me3Si)2C=PMe2—P(Me)SiMe3 vermag das Ylid-C-Atom ein H-Atom aus der P—CH3-Gruppe oder der PH-Gruppe des dreibindigen Phosphors zu abstrahieren unter Bildung von (Me3Si)2C(H)PMe2. Die Umlagerung wird anhand deuterierter Derivate belegt. Das unterschiedliche Verhalten wird auf die erhöhte Basizität des Ylid-C-Atoms in den Si-methylierten Phosphoryliden zurückgeführt. Ganz entsprechend verhalten sich die Phosphorylide 1,3,5-Trisilacyclohexans.
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  • 90
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 176-184 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polymorphism of SrTa2O6Orthorhombic SrTa2O6 is a new low temperature modification related to orthorhombic CaTa2O6. SrTa2O6(orh.) was obtained when the wellknown modification SrTa2O6(TTB) which is related to the tetragonal tungsten bronzes was heated in the presence of a transporting agent (chlorine) or a mineralizer (melt of B2O3) at temperatures below 1150°C. It could be prepared by the reaction of a 1:1 mixture of Sr(NO3)2 or SrCO3 with Ta2O5 in a sealed quartz glass tube as well. SrTa2O6(orh.) also occurred as an intermediate phase of the reaction of the corresponding 1:2 mixture at temperatures below 900°C (e. g. 840°C). Indexing of Guinier powder patterns led to the following unit cell: a = 11.006 Å, b = 7.638 Å, c = 5.622 Å. At temperatures above 1220°C SrTa2O6(orh.) changes (in air) to SrTa2O6(TTB). A reversal of this transition could not be achieved without the presence of a mineralizer or a transporting agent. CaxSr1-xTa2O6 solid solutions of the low temperature form could not definitely be established. However, at 1300°C solid TTB solutions of CaxSr1-xTa2O6 were formed. For x 〉 0.05 the TTB unit cells are orthorhombically distorted. For x ≥ 0.85 the x-ray powder patterns of the solid solutions looked like the one of CaTa2O6(orh.) and no TTB-structure was observed at 1300°C.
    Notes: Von SrTa2O6 wurde eine neue, mit orthorhombischem CaTa2O6 strukturverwandte Tieftemperatur-Modifikation erhalten. SrTa2O6(orh.) ließ sich bei Temperaturen unter 1150°C sowohl aus der bisher bekannten, den tetragonalen Wolframbronzen verwandten Modifikation SrTa2O6(TWB) in Gegenwart eines Transportmittels (Chlor) bzw. eines Mineralisators (B2O3-Schmelze), wie auch durch Umsetzen von Gemengen (1:1) aus SrCO3 oder Sr(NO3)2 und Ta2O5 in geschlossenen Quarzglasampullen erhalten. Auch als Zwischenprodukt der Umsetzung entsprechender 1:2-Gemenge bei Temperaturen unter 900°C (z. B. 840°C) tritt diese Modifikation auf. Die Gitterkonstanten von SrTa2O6(orh.) sind aufgrund von Pulverdaten: a = 11,006 Å, b = 7,638 Å, c = 5,622 Å. Beim Erhitzen auf etwa 1 220°C (an der Luft) wandelt sich SrTa2O6(orh.) in SrTa2O6(TWB) um. Eine Rückumwandlung von SrTa2O6(TWB) in SrTa2O6(orh.) ohne Mineralisator- oder Transportmittelzusatz war nicht zu erreichen. Mischkristalle CaxSr1-xTa2O6 der Tieftemperaturform ließen sich nicht sicher nachweisen. Die bei Mischkristallen mit 0,05 〈 x ≤ 0,20 (1300°C) vorliegende TWB-Struktur ist orthorhombisch verzerrt. CaTa2O6(orh.) zeigte dagegen ab x ≥ 0,85 (1300°C) keine Entmischung.
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  • 91
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 167-173 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Isolation, and Characterization of Mixed Thiocyanato(1.3-diaminopropane) -chromium(III) ComplexesThe complexes [Cr(NCS)4dap]- and trans-[Cr(NCS)2(dap)2]+ (dap = 1.3-diaminopropane) are prepared for the first time, isolated as salts and characterized by CHN analysis, chromium contents, the electrophoretic behaviour in dimethylformamide, and by UV, VIS, and IR spectra.
    Notes: Die Komplexe [Cr(NCS)4dap]- und trans-[Cr(NCS)2(dap)2]+ (dap = 1,3-Diaminopropan) werden erstmals dargestellt, als Salze isoliert und durch CHN-Analyse, Chrombestimmung, elektrophoretisches Verhalten in Dimethylformamid sowie Spektren im UV, VIS und IR charakterisiert.
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  • 92
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 201-208 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Schwefel-Stickstoff-Chelatbildner. IV. Einige Kupfer(II)-Komplexe von Thioaminopyridinen. IR- und ReflexionsspektroskopieEine Reihe von CuII-Komplexen sind dargestellt und charakterisiert worden. Die angenommenen Strukturen beruhen auf ihren IR -und VIS-Spektren. Die Thioaminopyridine können in verschiedener Weise koordiniert sein. Im Gegensatz zu unseren Befunden an aliphatischen Thioaminen ergab sich kein Zusammenhang zwischen der Struktur der CuLX2-Verbindungen und der Art des X--Anions. Ein Hinweis auf die Struktur der CuL2+-Komplexe in wäßriger Lösung kann aus festem CuLX2 nicht erhalten werden.
    Notes: A series of solid state CuII complexes with thia-aminopyridines . S(CH2)mNH2 have been prepared and characterized. The postulated structures of these CuLX2 (X = OAc-, NO3-, ClO4- or Cl-) compounds were based on their I.R. and electronic spectra. It was found that the thiaaminopyridines may coordinate in quite different ways. In contrast with what was found for the aliphatic thiadiamines, no relation was stated between the structure of the CuLX2 compounds and the nature of the X- anion.Moreover the solid state compounds do not give a clear indication for the structure of the CuL2+ species in aqueous solution.
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  • 93
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 199-207 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermochemische Eigenschaften und Aufwachsen von Hg1-xCdxTe auf CdTeNach thermodynamischen Rechnungen enthält die Gasphase des epitaktischen Hg1-xCdxTe - HgI2 - CdTe Systems vorwiegend Hg(g) und HgI2(g) durch die andere Moleküle vom Ausgangsstoff zum CdTe Substrat wandern. Transportversuche im Temperaturgradienten 590° → 535°C zeigten, daß man dünne Schichten von Hg1-xCdxTe auf CdTe von einem ternären Ausgangsmaterial in Gegenwart von HgI2 erhält.
    Notes: Based on a thermodynamic analysis, the vapor phase of the Hg1-xCdxTe - HgI2 - CdTe epitaxy system consists predominantly of Hg(g) and HgI2(g) through which nutrient species migrate from the source to the CdTe substrate. Growth experiments in the 590° → 535°C temperature gradient showed that Hg1-xCdxTe layers can be grown on CdTe substrates using a preannealed, ternary source material in the presence of HgI2.
    Additional Material: 3 Ill.
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  • 94
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical Transport Reactions of Ni-Sulfides and Some Relationships in C.T.R. of Complex Solids in the Case of Sulfides of Fe, Co, NiCrystals of α-Ni3S2, NiS, and NiS2 as well as solid solutions Fe1-yNiySx were grown by C.T.R. The coexistence equilibrium pressure of the solution equilibrium pressure p(S2), the activity of the metal component, the stability of gaseous metal halides concerning decomposition as well as their stability related on the transport agent have to be taken into account to choose a suitable transport agent, which have a sometimes opposite influence on the transport behaviour. Halogenes, hydrogen halides, and GeI2 were used as transport medium.
    Notes: Durch chemische Transportreaktionen wurden Kristalle der Phasen α-Ni3S2, NiS und NiS2 sowie Mischkristalle Fe1-yNiySx erhalten. Bei der Auswahl des Transportmittels sind der Koexistenzzersetzungsdruck bzw. Löslichkeitsdruck p(S2) und die Metallaktivität im Bodenkörper, die Stabilität der gasförmigen Metallhalogenide bezüglich Zerfall und ihre Stabilität relativ zum Transportmittel zu beachten, die z. T. gegenläufigen Einfluß haben. Geeignete Transportmittel sind Halogene, Halogenwasserstoffe und GeI2.
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  • 95
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 57-71 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical Transport of Zinc Oxide and the Estimation of its Phase WidthThe chemical transport behaviour of zinc oxide using different transport agents and the influence of the transport conditions (T, ΔT, p) on transport rate and deposition form was studied. The range of homogeneity of ZnO is very narrow. The best agents for deposition of ZnO with the upper phase boundary are Cl2 and Br2, for the deposition of the lower phase boundary HBr and NH4Br are more suitable. The deviation from stoichiometry depends on the deposition temperature and amounts to 10 till 250 ppm in the range of 1073 up to 1373 K.
    Notes: Das chemische Transportverhalten von Zinkoxid mit Cl2, Br2, HCl, HBr, NH4Cl und NH4Br und der Einfluß der Transportbedingungen (T, ΔT, p) auf die Abscheidungsgeschwindigkeit und Abscheidungsform wurde studiert. ZnO weist ein sehr schmales Homogenitätsgebiet auf. Zur Abscheidung von ZnO der oberen Phasengrenzzusammensetzung sind Cl2 und Br2 am besten geeignet. Für die Abscheidung von ZnO der unteren Phasengrenzzusammensetzung sind am besten HBr und NH4Br geeignet. Die Abweichung von der Stöchiometrie hängt von der Präparationstemperatur der Kristalle ab und liegt zwischen 10 und 250 ppm im Temperaturbereich 1073 bis 1373 K.
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  • 96
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 89-94 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXXVIII. Reactions of Dibenzyl Manganese with Oxygene(C6H5CH2)2Mn · C4H8O2 reacts with oxygen forming an unstable deep violet compound which changes in a stable unsoluble yellow peroxide of the formula C6H5CH2MnO—OMnCH2C6 H5. With excess oxygen a polynuclear complex of 3 valent manganese is formed with the composition Mn4O4(OH)4(OCHC6H5)2.The compounds isolated were characterized by the products of hydrolyses and thermolyses, anaerobic reaction with iodine, magnetic moments, i.r. and e.s.r. spectra.
    Notes: Dibenzylmangan-1,4-dioxan reagiert mit Sauerstoff zu einer tiefvioletten instabilen Substanz. Diese wandelt sich in ein stabiles gelbes, schwerlösliches Peroxid der Formel C6H5CH2MnO—OMnCH2C6H5 um. Mit überschüssigem Sauerstoff entsteht daraus ein Mehrkernkomplex des 3wertigen Mangans der Zusammensetzung Mn4O4(OH)4(OCHC6H5)2.Die isolierten Verbindungen wurden durch ihre Hydrolyse- und Thermolyseprodukte, anaerobe Iodierung, magnetischen Momente sowie IR- und ESR-Spektren näher charakterisiert.
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  • 97
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984) 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 98
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 19-25 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Antimony (III) Tris (thiophosphinates)The title compounds are formed by the reaction of Sb(CH3COO)3 with thiophosphinic acids R2P(=S)OH (R = CH3 cyclo-C6H11, C6H5). The crystal and molecular structures of Sb((cyclo-C6H11)2POS)3 and Sb((C6H5)2POS)3 have been determined by single crystal X-ray methods. SbIII is pyramidally coordinated to the oxygen atoms of the R2POS ligands through short (primary) bonds with a mean length of 203 pm. The Sb—S distances of the mainly chelating ligands vary between 300 and 320 pm (secondary bonds). The lone electron pair is stereochemically active.
    Notes: Die Umsetzung von Sb(CH3COO)3 mit Thiophosphinsäuren R2P(=S)OH (R = CH3, cyclo-C6H11, C6H5) führt zu Verbindungen der Formel Sb(R2POS)3. Die Strukturen der Verbindungen mit R = cyclo-C6H11 und C6H5 wurden an Einkristallen röntgenographisch bestimmt. SbIII ist über kurze (primäre) Bindungen mit der mittleren Länge von 203 pm pyramidal an die Sauerstoffatome der R2POS-Liganden gebunden. Die Sb—S-Abstände (sekundäre Bindungen) sind ungefähr 320 pm lang. Das freie Elektronenpaar ist stereochemisch aktiv.
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  • 99
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 43-49 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: I.R. and Mass Spectroscopic Investigations on α,ω-Dihydrochloro Silanes H(SiCl2)nH with n = 3-7Mass spectra of α,ω-dihydrochlorosilanes H(SiCl2)nH were analyzed respecting to their fragmentation. This shows, that the cleavage starts with the break of SiSi bonds, by preference in the middle of the chain. This is in accordance to the results of IR spectra which show very similar frequencies like perchlorooligo silanes. Thus, the lowest force constants of SiSi bondings in α,ω-dihydrochloro silanes, can be also expected in the middle of the chain.
    Notes: Die Massenspektren der α,ω-Dihydrochlorsilane H(SiCl2)nH mit n = 3-7 werden bezüglich ihrer Fragmentierung analysiert. Es zeigt sich, daß die Spaltung mit einem Zerbrechen der SiSi-Bindung, vorzugsweise in der Mitte der Kette beginnt. Dies steht im Einklang mit den Ergebnissen der IR-Spektren, die sehr ähnliche Frequenzen zeigen, wie bei den Perchlorsilanen gefunden. Daraus kann geschlossen werden, daß auch bei den α,ω-Dihydrochlorsilanen die mittleren SiSi-Bindungen die kleinsten Kraftkonstanten zeigen.
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  • 100
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phase Determinations by X-rays on the Thermal Dissociation and the Hydrolysis of Alkali Hexafluorogermanates at Higher TemperaturesFor a better understanding of the thermal dissociation of alcaline hexafluorosilicates investigations have been done on hexafluorogermanates. In these systems the formation of new phases has been studied by x-rays in dependence of temperature. Thermal behaviour of the substances strongly depends on the starting structure. Phase transformations taking place at lower temperatures are strongly determine the reaction at higher temperature. Therefore, we found differences to the analogous thermal reactions of hexafluorosilicates.There is a high sensitivity to hydrolysis of hexafluorogermanates above 600°C. We discuss the difference in reaction of thin powder layers and of powder samples in the volume.
    Notes: Zum besseren Verständnis des thermischen Verhaltens von Alkalihexafluorosilicaten wurden Vergleiche mit analogen Germanium-Verbindungen angestellt. Die Phasenneubildung wurde als Funktion der Temperatur röntgenographisch untersucht. Es ergab sich eine starke Abhängigkeit des thermischen Verhaltens von der Ausgangsstruktur. Phasentransformationen, die bei niederen Temperaturen ablaufen, beeinflussen bei höherer Temperatur das Reaktionsgeschehen (thermische Vorgeschichte der Substanz). Deshalb resultieren gegenüber den Hexafluorosilicaten differierende Reaktionsabläufe. Durch Heizguinieraufnahmen unter getrocknetem, strömendem Inertgas wurde die enorme Hydrolysenempfindlichkeit der Hexafluorogermanate oberhalb 600°C bewiesen.Das unterschiedliche Verhalten von dünnen Pulverschichten und kompakten Pulverproben wird diskutiert.
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