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  • 1995-1999
  • 1985-1989  (1,335)
  • 1988  (1,335)
  • Analytical Chemistry and Spectroscopy  (1,301)
  • Industrial Chemistry and Chemical Engineering
  • Nuclear reactions
Material
Years
  • 1995-1999
  • 1985-1989  (1,335)
Year
  • 101
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 403-410 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: n-Propyl-delta-8-tetrahydrocannabinol (n-propyl-delta-8-THC and n-propyl-delta-9-THC were synthesized by condensation of (1S)-cis-verbenol with 5-n-propyl-1,3-dihydroxybenzene and administered to male Charles River CD-1 mice. Hepatic merabolites were isolated by solvent extraction and chromatography on Sephadex LH-20 and identified by gas chromatography/mass spectrometry. Seven metabolites were identified from each cannabinoid. Metabolism was similar to that previously observed from the pentyl homologues, with the major biotransformation pathway being the production of 11-hydroxy-propyl-THCs and their oxidation to carboxylic acid metabolites. Other metabolites were mainly hydroxylated derivatives of these compounds and the corresponding 11-alcohol. Less hydroxylation at C(8) was found with n-propyl-delta-9-THC than with the pentyl homologue, and the monohydroxy metabolite, 8-alpha-hydroxy-n-propyl-delta-9-THC, was not observed, even though it was a prominent metabolite from delta-9-THC itself. Hydroxylation occurred in the side-chain at C(2′).
    Additional Material: 4 Ill.
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  • 102
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact mass spectra of poly(trimethylsiloxy) derivatives of polyenic long-chain carboxylic acids containing a conjugated diene unit clearly locate all double bonds. Abundant, diagnostic fragment ions arise from cleavage of the bonds at the positions of the original double bonds, combined with loss of a molecule of trimethylsilanol for every two vicinal trimethylsiloxy groups, with the exception of similar ions formed by rupture of an original conjugated double bond and containing the other conjugated double bond, which are weak or absent. The method was applied to several alkadienoic, alkatrienoic and alkatetraenoic acids containing a conjugated diene unit.
    Additional Material: 2 Tab.
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  • 103
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Long-chain unsaturated fatty acids (UFA) can easily be converted on a microgram scale to the corresponding 2-alkenyl-4,4-dimethyloxazolines by condensation with 2-amino-2-methylpropanol (AMP). These modified molecules with a ‘hidden’ carboxyl group have been proved to be a class of useful derivatives for gas chromatography/mass spectrometry (GC/MS) of UFA mixtures. While possessing very good GC characteristics, the title compounds show regular, well-recognizable diagnostic ion peaks of the double bond position in the chain. Detailed description of the method as well as electron impact (E1) mass spectra of derivatives resulting from mono-, di and polyenoic (maximally containing six double bonds) acids are presented.
    Additional Material: 5 Ill.
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  • 104
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 63-66 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A stable isotope assay for the quantification of debrisoquine (1) and its major urinary metabolite 4-hydroxydebrisoquine (2) is described. The method consists of extractive derivatization of 1 and 2 by use of 1,3-diketones, chiral derivatization of the 4-hydroxy group of 2, and gas chromatography/negative ion chemical ionization mass spectrometry in the presence of deuterated analogues of 1 and 2. In comparison with synthetic R-(-)-2 and S-(+)-2 it is shown that in vivo benzylic 4-hydroxylation of 1 is highly stereoselective, leading predominantly to S-(+)-4-hydroxydebrisoquine (enantiomeric excess ≥90%).
    Additional Material: 1 Ill.
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  • 105
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 75-77 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [MH]+ ions of peptides are degraded in one step to acyl ions, indicating the presence of different [MH]+ species. In contrast to protons, cations are added mainly at the carboxylate function of a peptide zwitterion. These species are degraded by loss of the C-terminal amino acid in the form of CO and an imine.
    Additional Material: 3 Ill.
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  • 106
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for qualitative and quantitative analysis of trace amounts of quaternary organoarsenicals such as arsenocholine and acetylarsenocholine has been developed. The method is based on pyrolysis, gas chromatography/mass spectrometry and use of deuterium-labelled internal standards. Arsenocholine and acetylarsenocholine have been estimated in fish from arsenic-polluted brackish water and compared with the same species of fish from unpolluted water. The investigation also includes some fish and crustacea from marine water. The presence of arsenocholine and acetylarsenocholine in different aquatic organisms indicate the existence of a general metabolic pathway for these compounds in aquatic ecosystems.
    Additional Material: 5 Ill.
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  • 107
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 183-184 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 108
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Steviol (ent-13-hydroxykaur-16-en-19-oic acid), the aglycone of various plant-derived glycoside sweeteners consumed by human populations, is known to be mutagenic toward Salmonella typhimurium strain TM677 when metabolically activated using a 9000 × g supernatant fraction derived from the liver of Aroclor 1254-pretreated rats. Mass spectral analysis of this diterpenoid and some analogs revealed characteristic patterns reflecting differential stereochemistry at the C/D rings and variations in the nature of the substituents present. Such information has been used to help identify several in vitro metabolites of steviol in conditions known to produce a mutagenic response, when analyzed by human populations, is known to be mutagenic toward Salmonella typhimurium strain TM677 when metabolically be allylic oxidation and epoxidation. 15-Oxosteviol, a product of oxidation of the major steviol metabolite, 15α-hydroxysteviol, was found to be a direct-acting mutagen.
    Additional Material: 10 Ill.
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  • 109
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive ion fast atom bombardment mass spectra of maltooligosaccharides reductively aminated with 2-aminopyridine (Gn-AP) contain abundant [M + H]+ ions. Determination of G2-AP and G3-AP produced from G5-AP by the action of α-amylases, based on the abundance of their [M + H]+ ions relative to that of cellobiose reductively aminated with 2-amino-6-methylpyridine as the internal standard, allowed rapid and reproducible assay of these enzymes. It was advantageous for clinical investigation that the proportion of pancreatic and salivary α-amylase activities could be determined.
    Additional Material: 4 Ill.
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  • 110
    Electronic Resource
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 111
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of biologically active steroids was analyzed by both, ‘filament on’ thermospray using 100% methanol as the mobile phase with ammonium acetate as buffer, and direct chemical ionization with NH3 gas. The mass spectra obtained were very similar. Addition of pyridine instead of ammonium acetate showed selectivity in adding to the steroid molecule.
    Additional Material: 2 Tab.
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  • 112
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A multi-stage screening and identification scheme for the diagnosis of inborn errors in amino acid, fatty acid, carbohydrate and intermediary metabolism is described. The method is based on a computerized analysis of data obtained with dual-column gas chromatography/FID (GC/FID) and gas chromatography/mass spectrometry (GC/MS) profiling of urinary organic acids. It involves: (1) isolation of the compounds by solvent or solid-phase extraction; (2) conversion into trimethylsilyl (TMS) or TMS-oxime derivatives; (3) GC/FID analysis on SE-52 and OV-1701 capillary columns; (4) tentative identification by comparing the methylene unit (MU) values on both columns with a user-built library of reference compounds; (5) quantitative evaluation of the excretion profile; and (6) analysis by GC/MS of samples with an abnormal profile using an automated peak identification programme.
    Additional Material: 4 Ill.
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  • 113
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 357-357 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 114
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 359-363 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact (EI) mass spectra (75 eV) of the new carboxylic acid ionophore griseochelin and some of its derivatives are discussed. The mass spectral fragmentation was studied using exact mass measurements and deuterium labelling. Furthermore, the negative ion mass spectra (2-4 eV) of these compounds are compared with their EI mass spectra.
    Additional Material: 4 Ill.
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  • 115
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 399-402 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A fast atom bombardment/collisional activation/linked-scan at constant B/E (tandern mass spectrometric) method is described which can distinguish between α- and β-aspartyl and α- and μ-glutamyl underivatized peptides. The method is based upon differences in loss of CO from aspartyl or glutamyl B-fragment ions (IB) in these isomers which are rationalized from the stability of the resultant A-fragment ions (IA). It was observed that the ratio of IB:IA which was used in this determination was dependent upon the collision cell pressure. The higher the collision cell pressure, the larger the difference between the IB: IA ratios for these linkages.
    Additional Material: 4 Ill.
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  • 116
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 117
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A tandem mass spectrometric method is described which allows the assignment of stereochemistry to fragment ions comprising intact sugar subunits of larger glycosides without chemical degradation and product isolation by chromatography. The approach relies on the mass selection of the ‘sugar ion’ of interest followed by analysis of stereoselective fragmentation induced by low-energy collisional activation. The daughter ion spectra provide configurational fingerprints of the selected sugar ions which can be matched for identity with reference spectra obtained from suitable precursors of known stereochemistry. Glucose, mannose and galactose furnished the required set of the most important reference ions. By using peracetyl (and perdeuterioacetyl) derivatives, galactose was readily identified as the glycosidic sugar constituent of the (known) antibiotic papulacandin B and a further (unknown) congener.
    Additional Material: 5 Ill.
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  • 118
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 473-478 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the calculation of stable isotope enrichments from the mass spectra of organic compounds obtained by gas chromatography/mass spectrometry. Correction factors for the natural abundance of stable isotopes account for the probabilities of observing more than one stable isotope atom in a molecule and these are particularly significant when analysing trimethylsilyl derivatives containing 29Si, 30Si and 13C. It was demonstrated that 15N-labelled molecules, as well as 13C-labelled molecules, elute earlier than their unlabelled analogues in a gas chromatographic peak, and thus enrichment values should be calculated from sample scans taken at regular intervals throughout the peak.
    Additional Material: 3 Ill.
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  • 119
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 495-499 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron ionization mass spectra of 2-amino-4-(5-nitro-2-furyl)thiazole metabolites obtained from microsomal incubations and chemical syntheses were studied. The identities of the metabolites were established by chemical ionization, high resolution, and metastable measurements. The compounds studied showed multiple modes of cleavage, skeletal rearrangements and hydrogen back-transfer.
    Additional Material: 3 Ill.
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  • 120
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary column gas chromatography combined with ion-trap detector mass spectrometry was used in the identification of 85 constituents of the polycyclic aromatic hydrocarbon fraction of diesel fuel. The main constituents are an extensive range of alkylnaphthalenes; alkylated tetrahydronaphthalenes, benzothiophens, dibenzothiophens biphenyls, fluorenes and phenanthrenes were also identified. Chromatographic retention indices for these compounds were determined to calibrate retention data for routine analysis with flame-ionization detection, and to identify positions of alkyl substitution.
    Additional Material: 2 Ill.
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  • 121
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass and ion abundance calibration of gas chromatograph/mass spectrometer responses is essential for the production of good data. In 1975, ion abundance criteria based on the mass spectrum of decafluorotriphenylphosphine (DFTPP) were proposed to standardize quadrupole mass spectra against magnetic sector spectra. This paper reports an investigation of DFTPP ion chemistry with the determination of the effects of some gas chromatograph/mass spectrometer operating parameters on the mass spectrum of DFTPP. New ion abundance criteria are proposed and discussed in relation to the findings of this investigation.
    Additional Material: 8 Ill.
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  • 122
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 447-451 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new method was developed and validated for measuring the CO2 concentration in the breath by mass spectrometric analysis. Argon, an inert gas that is present in air in a constant concentration of 0.923%, was used as an internal standard. By determining the ratio of CO2 (mass 44) to Ar (mass 40) in a breath sample, it was possible to read the CO2 concentration from a standard curve, relating CO2 concentration to CO2: Ar ratio. By combining mass spectrometric determination of CO2 concentration in breath with spirometric measurement of expired volumes, the CO2 production was determined in 67 subjects at rest. The mean value was 8.86 mmol kg-1 h-1, but there was considerable interindividual variation. This new method was applied to glucose oxidation studies in 10 normal subjects, 10 post-gastrectomy patients and 7 obese type II diabetic subjects. Measurement of the 13CO2 exhalation with quantitative determination of CO2 production allowed more accurate determination of the CO2 excretion rate in relation to blood levels of glucose, insulin and free fatty acids than assuming the constant CO2 production of 300 mmol unit body surface-1 h-1 or 9 mmol kg-1 h-1. It also resulted in a better discrimination between normal subjects and diabetics.
    Additional Material: 5 Ill.
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  • 123
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    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 124
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    Biological Mass Spectrometry 15 (1988), S. 501-508 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analysis of doxylamine N-oxide and pyrilamine N-oxide as synthetic standards and biologically derived metabolites by thermospray mass spectrometry (TSP/MS) provided [M + H]+ ions for each metabolite. TSP/tandem mass spectrometry (TSP/MS/MS) of the [M + H]+ ions provided fragment ions characteristic of these metabolites. In addition, TSP mass spectrometry and TSP/MS/MS analysis of ring-hydroxylated N-desmethyldoxylamine, N-desmethylpyrilamine and O-dealkylated pyrilamine is also reported. A fragmentation pathway for analysis by MS/MS of pyrilamine and its metabolites is also proposed. The results demonstrate the utility of TSP/MS for biologically derived metabolites of pyrilamine and doxylamine.
    Additional Material: 10 Ill.
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  • 125
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: γ-Hydroxybutyric acid (GHB) and trans-γ-hydroxycrotonic acid (HCA) together with their respective internal standards were derivatized to give the pentafluorobenzyl esters of the N-tert-butyldimethylsilyl derivatives. These compounds give, under electron capture conditions, very simple negative ion mass spectra. A very sensitive and specific assay for GHB and HCA in brain tissue (detection limit of about 5 pg per injection) using gas chromatography/negative ion mass spectrometry is described. The average levels measured in the whole brain were 1.10 ± 0.18 nmol GHB/g wet weight and 0.18 ± 0.02 nmol HCA/g wet weight.
    Additional Material: 3 Ill.
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  • 126
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    Biological Mass Spectrometry 15 (1988), S. 525-528 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The negative ion mass spectra of some dihydropyridine analogues of nifedipine are studied; they show a fragmentation which is highly dependent on the position of the nitro group on the phenyl ring: 3′-nitro derivatives give essentially the molecular anion, whereas 2′-nitro derivatives lose successively H2O, RO and O. In addition, (2,1,3-benzoxadiazol-4-yl) derivatives show essentially a [M—ROH]- peak. Possible pathways for these fragmentations are given.
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  • 127
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Paim I, a protein α-amylase inhibitor, is a single-chain polypeptide which consists of 73 amino acids, including 4 half-cystine residues. The positions of disulphide bonds in Paim I have been determined with the combination of enzymatic digestion and fast atom bombardment (FAB) mass spectrometry. Denatured Paim I was digested to peptides with Staphylococcus aureus V8 protease. These peptides were subjected to FAB mass spectrometry, with or without isolation by high-performance liquid chromatography. The positions of disulphide bonds in Paim I were determined from the relative molecular masses of the peptides containing a disulphide bond and by the enzyme specificity of S. aureus V8 protease. It is deduced that Paim I has two disulphide bridges at Cys(8)-Cys(24) and Cys(42)-Cys(70).
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  • 128
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    Biological Mass Spectrometry 15 (1988), S. 577-581 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 129
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A thermospray high-performance liquid chromatography/mass spectrometry method for the separation and quantification of cortisol in human serum has been developed. The technique does not require derivatization, allows for both qualitative and quantitative determinations, provides increased specificity not available from conventional high-performance liquid chromatography, and has a detection limit of 5 pmol on-column. This isotope dilution mass spectrometry method, using d3-cortisol as an internal standard, allows precise determinations even at low isotopic ratios (2%-5 mole%). Evidence that this technique can be applied to the quantification of serum cortisol and to the determination of daily cortisol production in humans is presented.
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  • 130
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    Biological Mass Spectrometry 15 (1988), S. 615-621 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The collisionally activated decomposition of [M + H]+ ions, generated by fast atom bombardment (FAB) of glutathione conjugates, has been studied by tandem mass spectrometry (MS/MS) using hybrid sector/quadrupole instruments. Abundant fragments of diagnostic utility were present in the daughter ion spectra. Common fragmentation modes were observed but their relative importance was strongly dependent on the nature of the conjugated species. As an example of a general approach to the characterization of glutathione conjugates in biological samples, the acetaminophen-glutathione conjugate was identified in rat bile, following coadministration of (2H0)- and (2H3)acetaminophen, using the experimental sequence: (i) conventional FAB mass spectrometric analysis, (ii) MS/MS using constant neutral loss (129 u) scanning to identify parent ions corresponding to glutathione conjugates, (iii) MS/MS to yield daughter ion spectra of parents so identified and corresponding to (2H0)- and (2H3)-labeled conjugates.
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  • 131
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    Biological Mass Spectrometry 15 (1988), S. 411-411 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 132
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of extracts from the South American plant Justicia pectoralis Jacq. permitted the identification, among other compounds, of coumarin, dihydrocoumarin, umbelliferone and 3-(2-hydroxyphenyl)propionic acid by gas chromatography/mass spectrometry (GC/MS); the acids and phenolic compounds were derivatized with diazomethane. GC/MS of simple coumarins, phenylpropionic acids and their hydroxylated isomers was performed after derivatization through methylation and trimethylsilylation; these results may be useful for the identification and quantification of these compounds in other biological materials.
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  • 133
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    Biological Mass Spectrometry 15 (1988), S. 419-427 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fast atom bombardment mass spectra of 24 α-amino acids have been studied. These include the mass spectra as well as the metastable ion MI and collisional activation CA spectra of [M + H]+ and [M - H]- ions. The extent of the common neutral losses as NH3, H2O and CO2H2 in the positive ion spectra is governed by the nature of the side chain. The relationship between the fragmentation behaviour of the negative ions and the presence of particular functional groups is less obvious. Mixtures of amino acids in glycerol show pronounced surface effects.
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  • 134
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    Biological Mass Spectrometry 15 (1988), S. 461-463 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 135
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chlorinated and oxygenated cyclohexene derivatives detected in methylene chloride extracts of chlorinated drinking water were demonstrated to be artifacts produced during sample preparation. Commercial methylene chloride contains cyclohexene as a preservative, and this reacted during the extraction/concentration process to produce microgram amounts of chlorocyclohexene, 2-chlorocyclohexanol, trans-1,2-dichlorocyclohexane, cyclohexenone and cyclohexenol. Quantitative analysis indicated that over 90% of the initial cyclohexene was consumed during the process. Dechlorination of drinking water with sodium arsenite significantly reduced but did not eliminate cyclohexene artifact formation.
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  • 136
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    Biological Mass Spectrometry 15 (1988), S. 465-465 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 137
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    Biological Mass Spectrometry 15 (1988), S. 485-493 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron impact (EI) mass spectra of the permethyl, peracetyl and per(trifluoroacetyl) derivatives of hydroxylated benzo[a]pyrene (B[a]P) metabolites were determined and the fragmentation chemistry producing the spectra elucidated. The metabolites investigated were: 3-hydroxy-B[a]P; 7,8-dihydro-7,8-dihydroxy-B[a]P; 7,8,9,10-tetrahydro-7,8,9-trihydroxy-B[a]P; and 7,8,9,10-tetrahydro-7,8,9,10-tetrahydroxy-B[a]P. In addition, the positive and negative methane chemical ionization spectra were determined for the derivatives of the BP-tetrol. The EI fragmentation patterns of the methylated metabolites that contained partially saturated rings were complex and, in the case of the di- and trimethoxy compounds, included apparent violations of the even-electron rule. The permethylated triol and tetrol cleaved through a retro-Diels-Alder reaction. The EI spectra of the peracetates were dominated by losses of acetic acid and ketene. The per(trifluoroacetyl) species fragmented by losing elements of trifluoroacetic acid, trifluoracetate radical and trifluoroacetyl. The spectra obtained from the permethylated tetrol permitted accurate prediction of the corresponding permethylated derivatives of tetrol metabolites of chrysene and benz[a]anthracene. The ability to predict spectra may be useful in trace analysis of hydrocarbon metabolites in biological samples.
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  • 138
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    Biological Mass Spectrometry 15 (1988), S. 509-516 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved direct chemical ionization (DCI) mass spectrometric technique, using a polyimide-coated fused silica fiber as an extended probe tip, was used to obtain molecular ions and diagnostic fragment ions of underivatized arachidonic acid, 5-hydroperoxyeicosatetraenoic acid, 15-hydroperoxyeicosatetraenoic acid, leukotriene B4 (LTB4) and, for the first time, of leukotriene A4 (LTA4)-free acid. In this technique, sample compounds are coated onto the fused silica fiber and vaporized in the plume of the reagent gas plasma of a chemical ionization source without external heating of the probe. Both ammonia and isobutane DCI spectra were obtained for each compound. A volatile alkaline eluent system was developed that allowed reversed-phase high-performance liquid chromatography of LTA4 to be followed rapidly by DCI mass spectrometry. With these techniques, the conversion of LTA4 to LTB4 during incubation with human liver microsomes was confirmed. Selected ion monitoring (SIM) of preselected ion fragments in the spectrum increases the selectivity of this technqiue and improves quantification in the range 100 ng to 10 pg.
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  • 139
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Self-chemical ionization Fourier transform ion cyclotron resonance (FT-ICR) mass spectra are reported for bases, nucleosides, and alkylated and exocyclic adducts of bases and nucleosides. The technique always produces a protonated molecular ion and in the majority of cases this is a single, intense peak. Analysis of a base mixture and a nucleoside mixture demonstrates the technique as an excellent method to identify the constituent compounds qualitatively. The high resolution capabilities and tandem mass spectrometric techniques (msn) in FT-ICR are discussed with respect to developing the technique as a future method to identify and characterize nucleic acid constituents, specifically adducts.
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  • 140
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    Biological Mass Spectrometry 15 (1988), S. 357-357 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 141
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    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 142
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    Biological Mass Spectrometry 15 (1988), S. 369-374 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 13C enrichment of the carboxyl carbon of leucine was measured by isotope ratio mass spectrometry after conversion to CO2 by reaction with ninhydrin in a Vacutainer and cryogenic purification using the Finnigan MAT Breath Gas Analysis System designed for processing 13C breath test samples. The sources of error which arise with submicromole samples are examined and corrections provided for suboptimal mass spectrometer signals and contamination of the evolved CO2 with CO2 from the reaction medium. The main limitations to the accuracy and precision of the method are not instrumental but arise from the contamination with residual CO2 in the reaction medium, and this sets a lower limit of around 0.25 μmol leucine on the practical sample size. This is an improvement of about five-fold on the previous manual method of CO2 isolation.
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  • 143
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fragmentation pathways of methyl abscisate and its 2E isomer in methane positive ion chemical ionization (PICI) and methane negative ion chemical ionization (NICI) mass spectrometry have been elucidated using isotopically labelled analogues. It is shown that in PICI the most abundant ions are formed by the loss of water, methanol, both methanol and water and of methyl formate. The PICI mass spectrum of methyl 2E abscisate differs significantly in that the loss of water is much less important. In NICI, the most abundant ions from methyl abscisate are due to the molecular anion, [M - H2O]- and [M - CH3OH]-. It is shown, however, that the methyl ester methyl is not lost in this last fragmentation. Two other significant ions contain the side chain and the ring of methyl abscisate, respectively. In contrast, the NICI mass spectrum of methyl 2E abscisate differs principally in showing an abundant loss of a hydrogen atom.
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  • 144
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    Biological Mass Spectrometry 15 (1988), S. 389-398 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl-delta-8-tetrahydrocannabinol (methyl-delta-8-THC), methyl-delta-9-THC and abn-methyl-delta-8-THC were synthesized by condensation of orcinol and (1S)-cis-verbenol and were administered to male Charles River CD-1 mice. Extracted hepatic metabolites were isolated by chromatography on Sephadex LH-20 and examined by gas chromatography/mass spectrometry as trimethylsilyl (TMS), (2H9)TMS and methyl ester/TMS derivatives. In addition, metabolic fractions were reduced with lithium aluminium deuteride to convert carboxylic acids to alcehols for structural correlation. Metabolites from methyl-delta-8-THC were similar with respect to the positions substituted to those produced by higher homologues; the major metabolite was methyl-delta-8-THC-11-oic acid. abn-Methyl-delta-8-THC was metabolized in a different manner. The location of the aromatic methyl group at the position adjacent to ring fusion appeared to inhibit metabolism at C(11) to a considerable extent and also to reduce the amount of the resulting alcohol from being oxidized to a carboxylic acid. This caused other metabolic pathways to become dominant, with the result that a compound containing a hydroxy group at the gem-methyl position was the major metabolite. Hydroxylation at this position has not been confirmed with any other cannabinoid, although it is thought to result in trace concentrations of hydroxy metabolites from some compounds. Metabolism of methyl-delta-9-THC was also similar to that of the higher homologues, with the exception that less metabolism occurred at C(8) and a higher percentage of the total metabolic fraction was accounted for by the 11-oic acid metabolite. Minor metabolites were mainly dihydroxy compounds and hydroxylated derivatives of delta-9-THC-11-oic acid.
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  • 145
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    Biological Mass Spectrometry 15 (1988), S. 459-460 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 146
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    Biological Mass Spectrometry 15 (1988), S. 465-465 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 147
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    Biological Mass Spectrometry 15 (1988), S. 467-472 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Stable isotope ratio mass spectrometry was used for the analysis of 13C and 18O in CO2 of human breath collected in evacuated serological tubes (Vacutainer® and Venoject®) and in gas sample bottles. There was a 1-2‰0 difference between the δ13CPDB values obtained from breath CO2 collected in gas bottles and that collected in two batches of Vacutainer. δ18OPDB differed between Vacutainers and gas bottles by as much as 14%0 and standard deviations within the two batches of Vacutainer were 0.7 and 1.8%0. The poor reproducibility and accuracy for the δ18OPDB values was caused by the presence of a contaminant which originated from the rubber septa of the Vacutainers. The results show that it is not possible to obtain δ18OPDB values with a high degree of accuracy or precision for breath samples collected in Vacutainers. However, with selection of less contaminated or re-evacuated batches, δ13CPDB analysis of breath CO2 in Vacutainers may provide acceptable accuracy and precision. δ13CPDB and δ18OPDB values measured in breath collected in non-sterile Venoject tubes were also significantly different from those obtained with gas bottles. However, the accuracy and precision of these determinations were considerably better than in sterilized Vacutainer tubes. As a result of these comparisons it is concluded that gas bottles are necessary for the full accuracy and precision of stable isotope ratio analysis mass spectrometers to be exploited in breath CO2 analysis. However, automated analysis of breath CO2 collected in non-sterile Venoject tubes will provide an accuracy and precision that is suitable for most biological studies.
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  • 148
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Prednisolone, dexamethasone and betamethasone were labelled with deuterium via a simple synthetic procedure and used as internal standards in the gas chromatographic/mass spectrometric analysis of the corresponding undeuterated compounds. The mass spectrometer was used in the negative chemical ionization mode, which gave fragmentation of the methoxime trimethylsilyl ether derivatives favourable for their quantification. The method was applicable to the quantification of synthetic corticosteroids contained in human aqueous humour in the 0.1-10-ng range.
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  • 149
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    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 150
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    Biological Mass Spectrometry 15 (1988), S. 553-564 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary column isobutane chemical ionization was found to be an excellent method for the mass spectral characterization of mustard, other sulfur vesicants and related compounds. Interpretation of [M + H]+ and fragmentation ion information afforded by this technique enabled the identification of many previously unreported mustard impurities. The developed methodology was applied to the analysis of an Iran/Iraq soil sample suspected to have been contaminated with mustard. Mustard and 17 other mustard related impurities were identified and characterized in this sample under electron impact and isobutane chemical ionization conditions.
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  • 151
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    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 152
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of ion-molecule reactions with NH3 for selected reaction monitoring (SRM) in gas chromatographic/tandem mass spectrometric analysis is demonstrated for 2-methoxyethanol and chlorobenzene in methanol and urine. In the former, the reaction [CH3OC2H4]+ + NH3 → [H2NC2H4]+ + CH3OH was followed; in the latter, the reaction [C6H5Cl]+· + NH3 → [C6H5NH3]+ + Cl·. Increased selectivity and an improvement in sensitivity by factors of up to five were observed when compared to conventional SRM analyses that used collisionally activated decompositions on NH3. SRM analyses with a triple quadrupole tandem mass spectrometer using ion-molecule reactions rather than collisionally activated decompositions have been found to be more sensitive and more selective in two model systems.
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  • 153
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    Biological Mass Spectrometry 15 (1988), S. 89-98 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of 35 steroid conjugates (sulfates and glucuronides) and bile salts were investigated by using fast atom bombardment and tandem mass spectrometry. Collisional activation of the [M - H]- anions of sulfate conjugates and bile salts predominantly yields fragment ions arising by reactions occurring remote from the charge site. These reactions are sometimes sensitive to differences in stereochemistry at positions remote from the charge site and are useful for positional isomer differentiation. On the other hand, collisional activation of the [M - H]- anions of the glucouronide conjugates leads primarily to charge-driven fragementations.
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  • 154
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    Biological Mass Spectrometry 15 (1988) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 155
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    Biological Mass Spectrometry 15 (1988), S. 183-183 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 156
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    Biological Mass Spectrometry 15 (1988) 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 157
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    Particle and Particle Systems Characterization 5 (1988), S. 13-15 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The size distributions of carefully screened √2 size fractions of ground materials were determined using a Microtrac laser diffractometer. The size distributions were fitted to the empirical function P(x) = 1/[1 + (x50/x)λ] where P(x) is cumulative mass fraction less than Microtrac size, x. The standard deviation of λ for a 50 second test time was approximately 0.5, so that seventeen test times give a mean with an estimated error within ± 0.25 (95% confidence level). Values of λ were 5.44, 4.82, 4.40 for a coal ground under different conditions, indicating statistically different shape distributions; the average value for mica was 2.91 owing to the high aspect ratio of the particles. The ratio of x50 to the geometric mean sieve size was 1.2 for the coal and 0.70 for mica.
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  • 158
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: When a particle crosses a laser beam out of the focal plane, the light attenuation signal occuring on the beam axis contains some information regarding the particle size and trajectory.These attenuation signatures are analysed and predicted with a simplified model based on Fraunhofer diffraction. Numerical and experimental results are found to be in good agreement.A modified laser Doppler velocimeter using this sizing method is able to perform simulataneous measurement of size and velocity of spherical particle in the range 10 μm-500 μm.
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  • 159
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    Particle and Particle Systems Characterization 5 (1988), S. 29-37 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The limiting resolution of Coulter size measurements, the size within which two separate populations can be distinguished, is discussed in relation to the standard aperture.Electronic pulse editing, by comparing pulse height to width, enables small particles to be resolved from baseline instrument noise, but can give incomplete resolution of ultra-narrow distributions from artefactually produced peaks using the standard aperture. Improvements in the minimum measurable size and in sizing resolution of narrow size ranges are also shown to be possible by improving the signal quality from the Coulter aperture.A novel mathematical approach is described for the derivation of true size spectra for narrow particle size distributions by deconvolution of the composite spectra resulting from the effect of the inhomogeneous electric field in the Coulter aperture. Simple empirical equations are used derived from the location and amplitude of the spurious peaks observed in such composites relative to the genuine peaks.The method is applied to three “industrial” materials (wide size range samples) to determine the likelihood that such size ranges are affected by the spurious or artefactual peaks. A fresh blood sample deconvoluted by this method is shown to be apparently composed of more than one population of cells.
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  • 160
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A model for the direct problem of calculating the forward scattering signature of a multiple scattering medium is presented. The new formulation is optimized for integration into schemes for reconstructing the particle size distribution from laser diffraction (forward scattering) signatures obtained from optically thick media. The analysis is valid for media where the particle sizes and interparticle spacings are large (relative to the wavelength and the particle size, respectively) such that Fraunhofer diffraction theory adequately describes the properties of the forward scattered light from individual scattering events. The simulated performance of laser diffraction particle sizing instruments was then studied using predictions of the scattered light signatures which would be measured by laser diffraction instrument under multiple scattering conditions. The results were compared with experimental data and theoretical calculations based on other models.
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  • 161
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    Particle and Particle Systems Characterization 5 (1988), S. 85-86 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This note deals with the Fourier representation of particle shape. A frequency distribution pn, n = 1,2, …, expressing the contribution of the different harmonics to the dispersion of the position vector is defined. The Meloy law of morphological coefficients may be derived by optimizing the value of the informational entropy which is attached to pn.
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  • 162
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    Particle and Particle Systems Characterization 5 (1988), S. 47-49 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 163
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper describes new progress obtained with an optical technique called V.I.D.E. (Visible Infra-red Double Extinction) which simultaneously measures mean particle size in the range of 10-120 μm and mean number density in densely laden media (up to 0.1% volume fraction). The underlying theory, taking account of multiple light scattering, is recalled. Simultaneous size and concentration measurements are obtained by simultaneously recording transmittances of the medium at two well chosen wavelengths. Experimental results for suspensions of glass particles in air, are described and discussed. The size of particles given by the technique agrees with that given by optical microscopy and Malvern diffractometry. The V.I.D.E. technique is shown to be very suitable to investigate dense media whose optical thickness is up to nine and for which other techniques fail.
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  • 164
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    Particle and Particle Systems Characterization 5 (1988), S. 77-84 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper is based on the development of the Moza-Austin technique for characterizing thousands of coal particles by approximate analysis of the major inorganic constituents Ca, Al, Si, K, Na, Fe and S in each particle. The technique has sufficient sensitivity to work on small volumes, is fast enough to handle large number of particles within a reasonable period of time, and consists of scanning electron microscopy combined with energy dispersive x-ray spectrometry (SEM-EDS). A computerized SEM-EDS system that allows the automated analysis of hundreds of particles per hour is described. The analysis is based on the location and tracing of exposed areas of particles embedded in a polished specimen, the selection of sampling points on the traced sections, the collection of an x-ray spectrum from each sampled point for a defined period of time, and the processing of the x-ray intensity to calculate point composition using ZAF corrections. Procedures for correcting for dead time, spectrum background, x-ray detector efficiency and spectrum overlap are described. Problems and future work are discussed.
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  • 165
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    Particle and Particle Systems Characterization 5 (1988), S. 100-102 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 166
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    Particle and Particle Systems Characterization 5 (1988), S. 109-115 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Inversion of the Laplace transform, used in the laser scattering measurement of colloidal particle size distributions, presents severe numerical difficulties. In the presence of noise the variance of the inversion integral is infinite, indicating maximum uncertainty in the inversion. This paper applies the method of minimum variance, or “optimal”, filtering to the eigenfunction spectrum of the Laplace transform, giving an inversion which has finite variance.Spectral decomposition using the eigenfunctions of the Laplace transform gives a representation of the noise and desired signals analogous to the Fourier spectrum used in linear system theory. It is possible to obtain a filtered estimate of the unknown linewidth distribution. The requirement that the variance of this filtered estimate is minimum leads to a Wiener-Hopf integral equation defining the optimal filter.The results of this paper provide a basis of comparison of all methods of inversion of the Laplace transform, including the extensive literature of colloidal particle sizing by laser scattering or photon correlation.
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  • 167
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    Particle and Particle Systems Characterization 5 (1988), S. 130-138 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The adhesivity of fresh coal fly ashes from two Australian power stations on Dralon-T monofilaments has been experimentally analysed. It was found that one of the dusts was more adhesive to the fiber and its particles were also more strongly electrostatically charged. These obervations explain the reported large differences in the pressure loss across the fabric filters at the two stations. By precharging the particles, the technique can also be utilized in determining the adhesivity of fly ashes which carry relatively small natural electrostatic charging.
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  • 168
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    Particle and Particle Systems Characterization 5 (1988), S. 153-164 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The paper provides a description of the local drop-size distributions in a liquid spray issuing from a 60° oil-burner nozzle obtained experimentally using a phase-doppler anemometer. The details of the optical system and the signal processing electronics of the phase-Doppler anemometer are included.Details have also been given concerning the use of the log-hyperbolic distribution and in particular of a procedure for determining the four defining parameters from a given experimental distribution, in this case that of drop size. Analytical formulae to compute moments of the distribution and the mean diameters are also given.All size distributions are shown to be well described by the log-hyperbolic distribution involving four parameters. The variation of these parameters along the axis of the jet clearly reveals a developing region of the spray followed by a fully developed state, for which physical reasons are given. The parameters can also be used to predict the local drop-size distribution at any intermediate location on the spray axis.
    Additional Material: 14 Ill.
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  • 169
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    Particle and Particle Systems Characterization 5 (1988), S. 179-185 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Conventional shape parameters have serious limitations because of their inability to capture finer surface morphology as well as to regenerate the particle form. This problem has been successfully circumvented by applying Fourier analysis technique to the projected image of the particle profile to obtain Fourier coefficients which have been shown to be size inveriant and insensitive to starting point for digitization. Synthesis technique to regenerate the particle profile from Fourier coefficients has revealed that gradual addition of higher order harmonics brings the regenerated form very close to its original counterpart. The regeneration of the form of particles of different shapes as well as application of few strategy to harmonic amplitudes have amply demonstrated the capability of the technique as a potential tool for characterization of powders.
    Additional Material: 12 Ill.
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  • 170
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    Particle and Particle Systems Characterization 5 (1988), S. 103-108 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper presents some characteristics of the light scattered by one spherical particle illuminated by a Gaussian beam. The basic theory is a generalization of the Lorenz-Mie Theory. The fact that the computations can be easily carried out on a micro-computer is pointed out.
    Additional Material: 11 Ill.
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  • 171
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    Particle and Particle Systems Characterization 5 (1988), S. 139-143 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The method described is based on the fact that the measurement of particles in the gaseous phase is generally easier than that in the liquid phase for fine particles smaller than 1 μm in diameter. The system consists of a liquid nebulizing unit, evaporator, condenser, mixing diluter and two different aerosol sizing instruments. It has been found that this method can continuously detect particulate impurities in ultrapure water in situ and can measure the size distribution of fine powders in the submicron particle size range down to about 0.05 μm.
    Additional Material: 11 Ill.
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  • 172
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    Particle and Particle Systems Characterization 5 (1988), S. 186-192 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The progress of the compaction process to produce from an assembly of particles a coherent mass can be achieved by the application of shear and normal stress. The achievement of a densified coherent mass necessitates, together with the yielding of material, the movement of particles over and between each other. In uniaxial compaction the angle of internal friction, δE, is a projection of the unique critical state line which divides a three dimensional relationship between volume change (V), shear stress (φ) and normal stress (σ) into yield domains and surfaces. There is one region for failure and flow (the Hvorslev surface) and another region for failure and consolidation (the Roscoe surface).In this paper the concepts of the Roscoe and Hvorslev surfaces together with the Coulomb yield criterion have been applied to the uniaxial compaction, over a range of compactable stresses, of titanium dioxide (20-2000 kPa). The characteristics of applied and shear stress, angle of internal friction (δE), angle of shearing resistance (φ) and surface area (SBET) were measured and correlated with the compaction stress (σc) and diametral strength (σf) of the compacts to investigate the phenomena of uniaxial compaction.
    Additional Material: 9 Ill.
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  • 173
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    Particle and Particle Systems Characterization 5 (1988), S. 165-169 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A method based on the measurement of scattered light intensity distributions is demonstrated to be able to determine directly the particle size of monodisperse supermicron-size particles. In all other cases of a particle cloud, information about the size distribution can be acquired from comparison of measured and calculated intensities as a function of scattering angle. This indirect method is only applicable if the assumptions made in the theory used for comparison are fulfilled. Therefore, the method is limited to spherical particles with known refractive index. The type of size distribution also has to be known. In the cases considered a log-normal size distribution was assumed. The uncertainty of the result increases with increase in the number of parameters that have to be determined. The method seems to be limited to unimodal distributions described with two parameters.
    Additional Material: 11 Ill.
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  • 174
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    Particle and Particle Systems Characterization 5 (1988), S. 193-193 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 175
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A complete theory of Gaussian beam scattering by a sphere is exposed. It is a generalization of the Lorenz-Mie Theory to the case of Gaussian beam illumination. The spherical, isotropic and homogeneous scatterer may be located anywhere with respect to the beam. The Bromwich Scalar Potentials are used to solve the scattering problem and expressions are obtained for the scattered field (both in the near field and far field regions), the scattered intensities and the phase angle. In the limit of special cases the expressions agree with previous works restricted to more particular problems.
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  • 176
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    Particle and Particle Systems Characterization 5 (1988), S. 23-28 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Experiments with common powder laboratory apparatus are used to illustrate the problems of sampling a poorly mixed quantity of glass ballotini. The use of known and easily sieved mixtures permits the quantitative analysis of the results to show how bias in samples may be detected.
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  • 177
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    Particle and Particle Systems Characterization 5 (1988), S. 72-76 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Photon correlation spectroscopy (PCS) has been applied to various systems of particles suspended in a fluid. Computer simulations were used to analyse CONTIN, a program for the numerical inversion of the experimental data. Measurements were performed on a spectrometer equipped with a digital correlator. Various suspensions of polysterene latex spheres differing both in size and size distribution were prepared in double distilled water. Further some samples provided by an external institution without prior specification were analysed. Diffusivity measurements on submicron DES (di-2-ethylhexyl sebacate) particles in nitrogen were also performed. The results obtained demonstrate the strengths and the limitations of PCS as a method of determining particle size distributions in particle fluid systems.
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  • 178
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    Particle and Particle Systems Characterization 5 (1988), S. 170-173 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Computerized tomography (CT) means reconstruction of pictures from projections taken at different angles. This method is well known in fields such as medical diagnostics and nondestructive testing. The application of CT to gas/liquid flow measurement results in a non-intrusive method for measuring the spatial distribution of the gas phase in a cross-section of the flow. In our application the projection data are obtained from measurement of the extinction along a set of ultrasonic rays in this cross-section, using piezo-ceramic ultrasonic transducers. The transducers are arranged in a circular sensor array which is directly integrated in the pipe wall of the flow; instead of mechanical rotation, the sensors are sequentially switched.
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  • 179
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    Particle and Particle Systems Characterization 5 (1988), S. 50-50 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 180
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: We try to evaluate the level of confidence that can be placed in the optical methods available for sizing cometary dust (and, at the same time, deriving all its other characteristics). We use for this purpose the new informations provided by the in-situ sampling of Comet Halley dust. We try to determine whether data from this origin are compatible with visible and I. R. spectra of this comet acquired from the Earth, and with earlier interpretations of such spectra. We find that, as happens frequently when remote sensing and local sampling techniques data can be compared, none of these techniques can claim to be fully satisfactory. In the case of cometary dust, current estimates based on optical sizing only may be much less accurate than precedingly assumed. Improvements in the observational approaches appear needed, as well as new laboratory investigations and theoretical developments to improve the capabilities of the optical studies of cometary dust.
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  • 181
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    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Simultaneous size and velocity measurements can be obtained by using photodetector positions of different off-axis-angles. But not for all of these positions one receives unambiguous results for the correlation between the phase difference and the particle diameter. This can be clearly demonstrated by the plots of the numerical calculations of the complete Mie's scattering equations. These plots show that for transparent particles which exceed the continuous phase in density at special off-axis-angles the situation of light refraction changes into a situation of additional light reflection or vice versa. On the other hand for transparent particles which are less dense compared with the continuous phase and for totally absorbing materials these plots confirm the simplified equations for reckoning the particle diameter by the laws of geometrical optics. The good agreement between these results can also be verified for the backscatter mode for measurements of metallic spheres with an imaginary refractive index.
    Additional Material: 6 Ill.
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  • 182
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    Particle and Particle Systems Characterization 5 (1988), S. 94-99 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper attempts to answer the question of whether a measurement of the relative flow rate of a suspension of spheres, flowing under constant pressure drop through gaps of precisely determined geometry, may be utilised to measure the concentration and size distribution of the particles. A positive answer is possible only if several restrictions are imposed on the character of the flow, a maximum ratio of sphere diameter to gap height and a maximum number of captured particles. This answer is based on a model of the filtration process taking place in the gap and the consequent relationship between the flow characteristics of the gap and the number and diameter of the captured particles.
    Additional Material: 7 Ill.
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  • 183
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    Particle and Particle Systems Characterization 5 (1988), S. 116-121 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Aspects of measuring the particle size distribution and median diameters of fine boron powders have been investigated. It has been demonstrated that high concentrations, typically 20 w/o, of wetting agent are necessary in a predispersion stage, especially if the material has a wide range of particle size. Measurements were made with both Coulter counting and a light scattering technique from which it has been demonstrated that for particles of median diameter in the range 10-30 μm, the latter oversizes with respect to the former by as much as 30%.
    Additional Material: 8 Ill.
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  • 184
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    Particle and Particle Systems Characterization 5 (1988), S. 150-151 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 185
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    Journal of High Resolution Chromatography 11 (1988), S. 20-24 
    ISSN: 0935-6304
    Keywords: Capillary column liquid chromatography ; Laser-induced fluorescence ; Serum bile acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the determination of individual free and conjugated bile acids in serum using microcolumn liquid chromatography coupled with a laser-induced fluorescence detector is described. Bile acids are separated into free/glycine-conjugate and taurine-conjugate fractions using a Sep-Pak SIL cartridge. The taurine-conjugated bile acid fraction is subjected to enzymatic hydrolysis. Subsequently, free and conjugated bile acids are labeled using 4-(bromomethyl)-7-methoxycoumarin as a fluorogenic reagent, producing stable derivatives that can be excited by the 325 nm line of a He/Cd laser. Prior to their fluorimetric detection, the individual components of a bile acid serum profile are separated by reversed-phase microcolumn liquid chromatography.
    Additional Material: 5 Ill.
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  • 186
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    Journal of High Resolution Chromatography 11 (1988), S. 25-29 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Mixed mobile phases ; Practical aspects ; Equilibration times ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Studies of mixed mobile phases in supercritical fluid chromatography must include consideration of a number of factors. Phase equilibria and critical parameters of a mixed fluid are very important in both the solvent delivery system and in the chromatographic column. The effects of pressure and temperature on retention with mixed mobile phases were studied and compared to estimated density values. System equilibration times with regard to pressure, temperature, and composition were studied. A mixed mobile phase was applied to the analysis of a high-molecular-weight metalloporphyrin.
    Additional Material: 5 Ill.
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  • 187
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    Journal of High Resolution Chromatography 11 (1988), S. 29-32 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Injection techniques ; Reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analysis of the precision obtained using commercially available microvalve injectors is reported for three modes of injection: conventional split; timed-split; and direct. Results from this study show that good precision (〈 3% RSD for external standard and 〈 1% RSD for internal standard methods) can be obtained with capillary supercritical fluid chromatography (SFC). However, particular attention must be paid to the type of valve used, the orientation of the column relative to the valve, the mode of interfacing or connecting the column to the valve, and the type of pressure or density programming used for the analysis as all of these factors will affect the reproducibility.
    Additional Material: 1 Ill.
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  • 188
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    Journal of High Resolution Chromatography 11 (1988), S. 38-42 
    ISSN: 0935-6304
    Keywords: SFC ; Fluid extraction ; FID detection ; Packed columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of fluid extraction in combination with fluid chromatography with packed column and flame ionization detection is described. Fluid chromatographic equipment is shown. Applications of this system to drug characterization are demonstrated.
    Additional Material: 8 Ill.
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  • 189
    ISSN: 0935-6304
    Keywords: Large PAH ; Retention prediction ; Reversed-phase ; Microcolumn LC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The retention behavior of condensed large polycyclic aromatic hydrocarbons has been investigated with diphenylsilica stationary phases in reversed-phase microcolumn liquid chromatography. The results were correlated with two parameters which indicate size and shape of the molecules. Since the resulting equation can be used for retention prediction of large polycyclic aromatic hydrocarbons, computer-assisted “standardless” identification is accomplished for “unknown” compounds contained in the standard.
    Additional Material: 4 Ill.
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  • 190
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    Journal of High Resolution Chromatography 11 (1988), S. 42-46 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Packed precolumn ; Sampling reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The peculiarities of the flow splitting technique for sample injection into a capillary column have been discussed. A comparative investigation of reproducibility of the analytical results obtained for two gas chromatographic systems using flow splitting [1) sample injector-packed predolumn-splitter-open tubular capillary column and (2) sample injector-splitter-open tubular capillary column] has been carried out. It was experimentally shown that the first system ensures considerably better reproducibility for the results concerning the composition of the analyzed mixtures. Other advantages of the first system are also discussed.
    Additional Material: 2 Ill.
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  • 191
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    Journal of High Resolution Chromatography 11 (1988), S. 46-50 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Dynamic headspace ; Multivariate data analysis ; Pattern recognition ; Polymers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatographic profiles have been generated from different batches of a polypropylene/polyethylene copolymer. The profiles generated from polymer pellets have been obtained by dynamic headspace/capillary gas chromatography analysis. Initially 10 to 40 peaks were chosen at random from the quantitative reports and transferred to a data table. After appropriate scaling the table has been analyzed by a multivariate statistic program, SIMCA (Soft Independent Modeling of Class Analogy) a pattern recognition technique. The method has been used to differentiate batches according to sensory qualities of the final packaging product and changes in polymer peilet production.
    Additional Material: 6 Ill.
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  • 192
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    Journal of High Resolution Chromatography 11 (1988), S. 51-56 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Air analysis ; Airborne halocarbons ; Chlorocarbons ; Electron capture detector ; Forest decline ; Halocarbons ; Thermodesorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The atmospheric levels of C1- and C2-halocarbons are determined by trapping on an adsorbent, thermodesorption, cryofocussing, gas chromatographic separation on a thick-film capillary, and electron-capture detection. The various aspects relevant to reliability and accuracy are discussed, such as type of adsorbent, range of detector response, and levels of contaminants present in blanks. These in turn have implications for optimum sample size and amount of adsorbent. The adopted method is suitable for routine analysis of airborne halocarbons at variable locations. The air concentrations of C1- and C2-halocarbons on the ground of mountain forests are similar to those in cities, a fact which supports the hypothesis that chlorocarbons are involved in the initiation of a phytotoxicological phenomenon commonly referred to as “forest decline”.
    Additional Material: 5 Ill.
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  • 193
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    Journal of High Resolution Chromatography 11 (1988), S. 56-60 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; On-column injection ; Dual column analysis ; Essential oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system to analyze a complex mixture simultaneously on two different columns after one single on-column injection is described. The splitting device, the possibilities of component identification by searching in a data base for Kovats indices on two different polarity stationary phases, and a practical example of an essential oil analysis are presented.
    Additional Material: 2 Ill.
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  • 194
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    Journal of High Resolution Chromatography 11 (1988), S. 65-69 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Temperature/pressure programming ; Density/temperature programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The theoretical and practical implications of simultaneous temperature/pressure and synchronized density/temperature programming are considered. Examples are shown for separations of dimethylpolysiloxanes where these techniques provide superior separation over their analogous isothermal programming methods.
    Additional Material: 4 Ill.
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  • 195
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    Journal of High Resolution Chromatography 11 (1988), S. 61-64 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography/Mass spectrometry ; Packed column ; Capillary column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A frit restrictor interface for capillary column supercritical fluid chromatography/mass spectrometry (SFC/MS) has been constructed and used for the analysis of high boiling point alkanes. Packed column SFC/MS is described using both a moving belt liquid chromatographic/mass spectrometric interface and a thermospray source in the filament-on mode.
    Additional Material: 4 Ill.
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  • 196
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    Journal of High Resolution Chromatography 11 (1988), S. 73-75 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; 100 μm i.d. capillary column ; High speed separations ; Lemon oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Narrow bore columns (100 μm) have successfully been applied in the analysis of commercial lemon oils. On these columns, high resolution is obtained in a short analysis time. Different Brazillian lemon oils are characterized qualitatively and quantitatively.
    Additional Material: 2 Tab.
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  • 197
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    Journal of High Resolution Chromatography 11 (1988), S. 69-72 
    ISSN: 0935-6304
    Keywords: Ultra-high resolution GC ; Reduced diameter capillary columns ; Capillary direct GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For clinical and environmental analyses utilizing capillary gas chromatography/mass spectrometry (GC/MS), increased sensitivity and speed of analysis are highly desirable. These performance advantages are realized using a WCOT column of 100 μm i.d. as compared to the more conventional 200 μm i.d. capillary columns. The improved sensitivity of capillary direct GC/MS with the 100 μm i.d. column for the confirmation of drugs of abuse will be demonstrated. For environmental analysis, the superior efficiency and resolution of the 100 μm i.d. column can be employed for the separation of priority pollutants. This approach is more amenable to capillary direct GC/MS providing a more effective interface to the mass spectrometer. As a result improved sensitivity and a considerable decrease in analysis time is achieved over that obtained with the larger diameter environmental specialty phase columns.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 198
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 81-84 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Packed fused silica column ; Direct sample injection ; Extraction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A direct sample injection technique was developed for supercritical fluid chromatography in a packed capillary column, with carbon dioxide as mobile phase and a flame ionization detector. The method allowed solutions, neat liquids, and even solids to be introduced as samples. Also, extraction with supercritical carbon dioxide was combined with this method to separate polymer additives.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 199
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 75-81 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Element selective detection ; Radio frequency plasma ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A radio frequency plasma detector for element specific detection in gas chromatography is described. The detector is comprised of a radio frequency (300 kHz) discharge between electrodes in helium, and utilizes a low-resolution emission spectrometer to monitor selected spectral emission lines produced when the helium discharge decomposes and excites the atomic constituents in the chromatographic column effluent. The spectrometer is tuned to an atomic emission line in the near-infrared portion of the spectrum, and the emission intensity from the discharge region of a selected line is used to monitor the concentration of the element producing that line. Acceptable detector sensitivity was achieved by the use of a high-throughput optical system. Selectivity was achieved by a combination of correct line selection, plasma and carrier gas purification, and plasma gas doping.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 200
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 85-89 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Two-dimensional system ; Mechanical switching valve ; Heart-cutting ; Grob test ; Aroma fractions ; GC-GC/sniffing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A commercially available mechanical micro switching valve has been tested for inertness. The test mixtures used were a modified Grob test and a solution consisting of eight typical aroma compounds, both at the 2-ng level. Cryogenic focusing of the sample after chromatography including one passage through the valve revealed that irreversible interaction of some test substances with valve components was rather small. A composite main peak of a chromatogram from a fruit juice aroma exhibiting a “mixed odor” was selectively transferred (heart-cutting) to a second column and resolved into three peaks. GC-GC/sniffing assigned a minor peak to a substance formerly hidden under the composite peak. Separate heating of the valve during temperature programming of the column was found to be unnecessary.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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