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  • Analytical Chemistry and Spectroscopy  (4,318)
  • 1980-1984  (4,318)
Collection
Publisher
Years
Year
  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1984), S. 573-576 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A detailed energy-resolved study of the fragmentation of CH2=CHCH(OH)CD2CD3 (1-d5) has been carried out using metastable ion studies and charge exchange techniques, combined with collision-induced dissociation studies to establish the structures of fragment ions. At low internal energies (metastable ions) the molecular ion of 1-d5 rearranges to the 3-pentanone structure and fragments by loss of C2H5 or C2D5 leading to the acyl structure, [CH3CH2C≡O]+ or [CD3CD2C≡O]+, for the fragment ion. However, with increasing internal energy of the molecular ion this rearrangement process decreases rapidly in importance and loss of C2D5 by direct cleavage, leading to [CH2=CHCH=OH]+, becomes the dominant fragmentation reaction. As a result the [C3H5O]+ ion seen in the electron impact mass spectrum of 1-penten-3-ol has predominantly the protonated acrolein structure.
    Additional Material: 2 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 312-315 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is shown that under field desorption conditions some less volatile or non-volatile compounds such as oligosaccharides, sulphonic acids and fatty acids can be ionized below the threshold of field electron emission by clustering with anions. In all cases the sample, together with polyethylene oxide 4000, is dissolved in water. The source of the clustering anion is provided either by a small amount of a salt added to this solution (sugars) or by the compounds themselves (sulphonic and fatty acids). The solution is applied to unactivated and/or slightly activated 10 μm tungsten wire cathodes. Suitable clustering ions for the sugars appear to be [Cl]-, [NO3]- and to a lesser extent [Br]- and [I]-. Most of the sulphonic acids studied give rise to the formation of [Mn - H]- ions (n≤5), but their potassium salts yield only unclustered sulphonate anions. However, the addition of a small amount of LiCl to the mixture of benzene sulphonic acid and polyethylene oxide 4000 promotes the formation of clustered anions, [(M - H)2Li]- being by far the most abundant if activated cathodes are used. This addition of some LiCl is essential in the case of fatty acids: without LiCl no anions may be desorbed at all from activated wires, but with the presence of LiCl both [M - H]- and the most abundant [(M - H)2Li]- anions are easily generated.
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 525-529 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The positive ion field desorption (FD) spectrum of arginine taken at the best anode temperature only contains a peak due to [M+H]+ ions. At higher emitter temperatures a considerable amount of fragmentation is induced and the [M+H—NH3]+ ions become most abundant. Specific 15N labelling reveals that the eliminated ammonia molecule, exclusively, contains one of the terminal nitrogen atoms of the guanidyl group. This also applies to the ammonia loss from metastably decomposing [M+H]+ ions. The positive ion fast atom bombardment (FAB) spectrum shows more fragmentation than the FD spectrum. In contrast with the FD results, the [M+H]+ ions generated upon FAB with ion lifetimes 〈10-6 s eliminate both ammonia containing one of the terminal nitrogen atoms of the guanidyl group and ammonia containing the α-amino group in the ratio of 1.35, as found by 15N labelling. The metastably decomposing [M+H]+ ions, however, eliminate only the former ammonia molecule. In the negative ion FD and FAB spectra no other peak than that corresponding to the [M—H]- ion is observed. Some attention has been paid to the thermal degradation of arginine on the basis of a few Curie-point pyrolysis experiments.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 169-171 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary columns ; Trimethylsilyl derivatives ; Pregnant mares' urine estrogens ; Estrone-equilin separation ; OV-225, Silar 10C stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Glass capillary columns coated with OV-225 and Silar 10C were used to analyze estrogens (as their trimethylsilyl derivatives) present in pregnant mares' urine. Such columns provide better resolution in a shorter time than the corresponding packed columns, as exemplified by the separation of estrone from equilin.
    Additional Material: 2 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 21 (1983), S. 315-318 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of the 1H NMR spectra of 2,8-dithia-1,5-diphosphabicyclo[3.3.0]octane, 2,8-dithia-1-phospha-5-azabicyclo[3.3.0]octane and 2,8-dithia-1-arsa-5-phosphabicyclo[3.3.0]octane is supported by means of 2D- J-resolved NMR measurements. The spectra suggest a preferred conformer with strong puckering of the fused five membered rings.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 6-10 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Retention index calculation by correlation techniques ; Use of n-dialkyl sulphides as standards ; Use of selective detectors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Retention indices were determined for a homologous series of n-dialkyl sulphides on three stationary phases (SE-30, OV-17 and XE-60) under isothermal and linear temperature programming conditions. Under these two different GC conditions, equations were derived for each of the three stationary phases which showed the dependence of retention index on the number of carbon atoms and the boiling points for a homologous series of n-dialkyl sulphides. The equation for the correlation isothermal retention index was shown to be applicable to the identification of n-dialkyl sulphides using linear temperature programming. It was found that the GC behaviour of n-dialkyl sulphides makes these compounds suitable for use as a standard series instead of n-alkanes for the calculation of retention indices in GC analysis in which detectors insensitive to n-alkanes are employed. The use of the homologous series of n-dialkyl sulphides for the calculation of sulphide retention indices can be great practical importance in the microanalysis of natural compounds. We have used this method successfully in the analysis of pesticides containing S-atoms.
    Additional Material: 1 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 306-309 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for separation of low amounts of DHETX m. s. from human plasma, based on extraction and determination by high performance liquid chromatography with fluorimetric detection.
    Additional Material: 4 Ill.
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  • 8
    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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  • 9
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 74-78 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fragmentation pathways of RDX in chemical ionization mass spectrometry have been rationalized, using data from different reagent gases, including CD4 and iso-C4D10. The dependence of spectra taken with different gases on the acid strength of the reactant ions in the gases is accounted for.
    Additional Material: 1 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 440-446 
    ISSN: 0935-6304
    Keywords: High performance thin-layer chromatography ; β-adrenoceptor blocking drugs ; Continuous development ; Multiple development ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High performance thin-layer chromatography was used for the separation of nine therapeutically important and structurally similar β-adrenoceptor blocking drugs on silica gel plates. In situ scanning of the plate in the reflectance mode gave detection limits in the low nanogram range depending on the individual drug and the wavelength selected for its determination. Scanning the HPTLC plate at several wavelengths can be used to aid the identification of partially resolved components. Continuous development and continuous multiple development techniques are compared for the simultaneous separation of the drug mixture.
    Additional Material: 7 Ill.
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