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  • Column liquid chromatography  (377)
  • Gas chromatography  (280)
  • Springer  (651)
  • American Chemical Society
  • 2005-2009
  • 1985-1989  (516)
  • 1980-1984  (135)
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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Entomologia experimentalis et applicata 34 (1983), S. 20-26 
    ISSN: 1570-7458
    Keywords: Dioryctria abietella ; Cone pyralid ; Lepidoptera ; Pyralidae ; Sex pheromone, (Z,E)-9,11-tetradecadienyl acetate ; Single sensillum recordings ; Electroantennography ; Gas chromatography ; Mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé L'analyse en chromatographie gazeuse associée à une détection électroantennographique a montré que l'acétate (Z,E)-9,11-tétradécadiényle (Z,E)-9,11–14:Ac est l'un des composants de la phéromone de Dioryctria abietella Schiff (Lepid.: Pyralidae). Couplage chromatographie en phase gazeuse spectrometrie de masse a montré la présence d'acétate tétradécadiényle avec un spectre de masse et un indice de rétention identiques au Z,E-9,11–14:Ac Un récepteur cellulaire sensible à la fois au Z,E-9,11–14:Ac et à un extrait de la femelle a été identifié sous l'antenne du mâle. Les analyses des antennogrammes et de la cellule isolée ont étayé la caractérisation du composant de la phéromone comme étant Z,E-9,11–14:Ac. Un récepteur cellulaire additionnel sensible à l'acétate (Z.)-9-tétradécadiényle et à l'acétate (Z.E.)-9,12-tétradécadiényle a été trouvé sur l'antenne du mâle, mais il n'était pas activé par l'extrait de la femelle. Sur le terrain Z,E-9,11–14:Ac, présenté seul, attirait des nombres importants de mâles de D. abietella. L'addition de l'acétate (Z)-9-tétradécényle a inhibé l'attraction des mâles par les pièges.
    Notes: Summary Gas chromatographic analyses coupled with electro-antennographic detection indicated that (Z,E)-9,11-tetradecadienyl acetate (Z,E-9, 11–14:Ac) is a pheromone component of the cone pyralid Dioryctria abietella. Gas chromatographic-mass spectrometric analyses confirmed the presence of a tetradecadienyl acetate with mass spectrum and retention index identical to Z,E-9,11–14:Ac. A receptor cell sensitive to both Z,E-9,11–14:Ac and the female extract was identified on the male antenna. An additional receptor cell sensitive to (Z)-9-tetradecenyl acetate and (Z,E)-9,12-tetradecadienyl acetate was found on the male antenna but was not activated by the female extract. In the field Z,E-9,11–14:Ac presented alone attracted significant numbers of male D. abietella. Addition of (Z)-9-tetradecenyl acetate inhibited the attraction of males to traps.
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  • 2
    ISSN: 1432-1432
    Keywords: Primordial terrestrial atmospheres ; CH4, C2H2, CO2 ; Prebiotic synthesis ; High-frequency discharge ; Hydrocarbons ; Gas chromatography ; Mass Spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Various hydrocarbons were synthesized by high-frequency discharge in a primordial terrestrial model atmosphere. The products were extracted by benzene or methanol and analyzed by GC-MS. The mean carbon chain length of the hydrocarbons formed by the discharge through pure CH4 gas was less than 6. Benzene was also obtained. Some isomers were obtained for each of the hydrocarbons containing a given number of carbons. When a small amount of C2H2 was added to the CH4, longer chain compounds were formed, as compared with discharge in CH4 only. However, when the amount of C2H2 was increased, unextractable high molecular weight compounds were produced. The amounts of products decreased as the mixing ratio of CO2 to CH4 increased. No hydrocarbons were detected when the ratio of CO2/CH4 exceeded 1.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Trees 1 (1987), S. 94-101 
    ISSN: 1432-2285
    Keywords: Monoterpenes ; Abies alba Mill ; Resin ; Seeds ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Using gas-chromatographic methods, the variability of the contents of monoterpene hydrocarbons (α-pinene, β-pinene, Δ3carene and limonene) in the resin of silver fir seeds (Abies alba Mill.) was studied. Resin cavities were characterized according to their position on the seed surface. It was estabilished that the terpene content of the resin of cavities localized on the abaxialadaxial surfaces of the seed differs significantly, creating a gradient of resin composition around the circumference of the seed. The differences between various resin cavities of single seeds were greater than the differences between different seeds of a single cone and between seeds of various cones on a single tree. An accurate definition of the resin cavity location on the seeds appears to be a fundamental condition for the collection of a sample representing the resin composition of individual trees. Resin biosynthesis in the course of organogenesis and the control of terpene contents in the resin of various locations on the seed and the cone are discussed.
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  • 4
    ISSN: 1432-0878
    Keywords: Preputial glands ; Nude mice ; Ultrastructure ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The preputial glands of male nude (nu/nu) mice were analyzed by a combination of electron microscopy and gas chromatography to determine whether or not they are affected, like developing hairs and nails, by the nu/nu genotype. Results of the analyses revealed no differences between the glands of nude and normal male mice in either their ultrastructural characteristics or lipid secretory products.
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  • 5
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    Springer
    Chromatographia 13 (1980), S. 203-206 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas purity ; Sample stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The amount of oxygen which may be present in the gas volume corresponding to a peak is investigated and compared to the sample amounts. It is shown that even with high purity carrier gases one may have a significant excess of oxygen present at low sample amounts. Attention is drawn to the possibility of impurity build-up by diffusion e.g. through the septum.
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  • 6
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    Springer
    Chromatographia 13 (1980), S. 263-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Enantiomers ; Isotopic composition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The high selectivity of complexation gas chromatography has been employed for enantiomer resolution and isotope separation. Thus, a chiral olefin, 3-methylcyclopentene, has been resolved analytically on optically active dicarbonyl-rhodium(I)-3-trifluoroacetyl-1R-camphorate in squalane. The deuterated ethylenes C2H4−nDn have been separated on the same rhodium(I)-containing stationary phase. The chiral aliphatic oxiranes epoxypropane andtrans-2,3-epoxybutane have been resolved on optically active nickel(II)-bis-3-trifluoroacetyl-1R-camphorate in squalane.
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  • 7
    ISSN: 1612-1112
    Keywords: Gas chromatography ; On-column abstraction ; Aliphatic aldehydes ; Amine antioxidants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The selective on-column abstraction of aliphatic aldehydes by gas chromatographic stationary phases containing N-iso-propyl N′-phenyl-p-phenylenediamine is described.
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  • 8
    Electronic Resource
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    Chromatographia 14 (1981), S. 19-22 
    ISSN: 1612-1112
    Keywords: Teflon columns ; Chemically modified teflon ; Gas chromatography ; Capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated open tubular columns prepared from chemically modified teflon tubing have been developed for gas chromatography. Chemical reaction of the inner walls of teflon tubing allows bonding of an adhesive layer on which a variety of stationary phaes can be coated. Test mixtures of alkanes and alcohols were used to investigate the chromatographic properties of these columns and the stability and mixing of the adhesive and stationary phae layers. the results in dicate that mixing of the layers is negligible and that the column is stable for a long period of time.
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  • 9
    ISSN: 1612-1112
    Keywords: Teflon capillary columns ; Chemically modified teflon ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of teflon capillary columns employing direct coating of the stationary phase to the chemically modified teflon surface and the role of the chemically modified teflon in the separation mechanism are described. Two types of contributions from the modified teflon have been observed: nonspecific adsorption of the carbon surface and specific interactions of polar groups in the carbon skeleton. The use of polar liquid phases can eliminate adsorption due to the presence of polar groups in the modified teflon.
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  • 10
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    Chromatographia 14 (1981), S. 55-66 
    ISSN: 1612-1112
    Keywords: Capillary columns, glass ; Gas chromatography ; Column preparation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Kapillar-Gas-Chromatographie ist heute das sich am stärksten entwickelnde Gebiet der Gas-Chromatographie. Es gibt viele komplexe, neue Fragestellungen in der Analytik, welche den Einsatz spezieller Kapillarsäulen erfordem. Glücklicherweise gibt es aber auch eine große Zahl von Herstellungsverfahren für Kapillarsäulen, welche — noch mehr als bei der Herstellung von gepackten Säulen — eine Anpassung an die gestellten Aufgaben ermöglichen. In diesem Artikel werden die Herstellungsverfahren für Kapillarsäulen zusammengestellt und Anregungen gegeben, wie aufgaben-orientierte Säulen erreicht werden.
    Notes: Summary Glass capillary column chromatography is the most rapidly growing part of gas chromatography. There are many complex new analytical tasks and they require special capillary columns, Fortunately there is a wide range of column preparation methods available, and they make the preparation of glass capillary columns a more varied job than that of packed columns. In this paper these methods are reviewed and suggestions are given for making task-oriented columns.
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  • 11
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.
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  • 12
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitised carbon black ; Phenols ; Water pllutants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The fractionation of eleven phenols which may be contaminants in drinking water has been accomplished by using acid-washed graphitised carbon black modified with trimesic acid and PEG 20 M.
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  • 13
    Electronic Resource
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    Chromatographia 14 (1981), S. 447-451 
    ISSN: 1612-1112
    Keywords: Headspace analysis ; Gas chromatography ; Residual analysis of polyethylene terephthalate ; Acetylene reduction assay ; Ethylene evolution in germinating seed ; Acetaldehyde generation in polyester resin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary New application areas for headspace gas chromatography in agricultural and polymer degradation research are described. Specific examples are drawn from the various forms of headspace analysis with emphasis on the automated static equilibrium method.
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  • 14
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    Chromatographia 13 (1980), S. 35-39 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitromethane ; Nitroalkanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Impurities in commercially available nitromethane have been determined by gas-liquid chromatography using six different column packings. Besides nitromethane, 1-nitropropane, 2-nitropropane, acetonitrile, methanol, small amounts of ethanol and acetaldehyde have been detected. The presence of formaldehyde, ethyl acetate and acetone is probable. Mixtures containing comparable amounts of the four nitroalkanes could be separated on all columns, but plots of logarithms of the retention times vs. carbon number or boiling points of the nitroalkanes or column temperatures were linear only in case of columns packed with Porapak R and Q.
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  • 15
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    Chromatographia 16 (1982), S. 60-62 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Amines ; Derivatization ; Chloroformate esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic analysis of amines after conversion to electron capture sensitive carbamates in two-phase systems has been studied. Hydrophilic compounds, for instance methylamine, are reacted with 2,2,2-trichloro-tert. butyl chloroformate. Quantitation below 10−7 M can be made by thermionic or electron capture detection. A hydrophobic amine, namely N,N-dimethyl-n-octylamine, was derivatized with 2,4,6-tribromophenyl chloroformate with addition of iodide ion to the aqueous phase. The favorable effect of iodide ion as well as the choice of pH and chloroformate ester is discussed.
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  • 16
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    Chromatographia 16 (1982), S. 98-102 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Rectangular channel ; Efficiency ; Capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic experiments have been performed in a truly rectangular channel with a 60∶1 cross-sectional aspect ratio, constructed according to the field-flow fractionation technology. It is shown that the peak broadening is controlled by the thickness of the channel while the maximum load is determined by the largest cross-sectional dimension. However, even with its elongated configuration, the side walls contribute significantly to the band broadening of solutes with a high diffusivity. Good agreement is found between the experimental plate height data and the recent theoretical calculations of Golay [13] taking into account the side-wall effect.
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  • 17
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase ; Codeine phosphate drug substance ; Opium alkaloids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid procedure for the evaluation of codeine phosphate drug substance derived from poppy straw or opium concentrate is described. The gradient HPLC procedure employs a pH 2.5 phosphate buffer, methanol and acetonitrile mobile phase at 40°C and a μBondapak C-18 column. Eight opium alkaloids, including the four major alkaloids, are separated from each other. The paper describes details of the assay procedure and presents data documenting the linearity, specificity, precision, and sensitivity of the method.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary liquid, choice of ; Physico-chemical data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A table of data for acidity, basicity, polarity and London potential for stationary phases is given. These provide guidance in choosing a stationary phase for a given task from the 26 substances listed. The indices are calculated from infra-red shifts of 1-chlorobutane and the visible wavelength shifts of l2 when they are dissolved in the stationary phases, from NMR estimates of acidity and basicity and from relative retention data. They replace the less reliable data of Burns and Hawkes. Methods of determining the indices are suggested that require only a gas chromatograph and can be applied by technicians with no specialized understanding of solution parameters. An attempt to add electron donoracceptor indices to the table was unsuccessful. A further table is given of the slopes of the log plots d(logt′)/dC for use in extrapolating from one homologue to another on these stationary phases.
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  • 19
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; External variance determinations ; Column and system compatibility ; Microbore and fast LC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The demand for faster, more economic and convenient high-efficiency LC analyses has led to the development of microbore and fast columns. However, to utilize their benefits, the low column dispersions produced by these new technologies necessitate low external variances in the total system. This paper describes the determination of the external variance of microbore, fast and conventional LC systems by a column method. Compatibility with the relevant column technologies is evaluated by a method involving the comparison of the external and column dispersions. Direct comparison of chromatograms of an 8-component mixture, on a set of columns of various diameters and lengths, shows the relative speed, economy and sensitivity obtainable in practice. The problem of reduced sample loadability is considered and the practical solution of peak compression illustrated.
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  • 20
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention prediction system ; UV multichannel detector ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention prediction system assisted by a micro-computer coupled with an UV multichannel detector has been investigated in the separation of polycyclic aromatic hydrocarbons. The method offered very precise identification of components in NBS-SRM-1647 sample without any standard reference substances. It has been proven that the system makes very precise, non-pollutive and convenient environmental analysis possible.
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  • 21
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    Chromatographia 20 (1985), S. 313-322 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Tetracyclines antibiotics ; Quantitation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of high-performance liquid chromatography (HPLC) for the identification and determination of tetracycline antibiotics is reviewed. HPLC chromatograms provide fast identification by retention time, tR, and precise quantitation by measurement of peak height or peak area. For separation of tetracycline compounds, most HPLC methods use reversed-phase C18 or C8 columns and UV detection. The HPLC solvent system should have a pH of about 6 to prevent steric changes in the tetracycline molecule. For accurate quantitation it is necessary to avoid tailing and this is accomplished by adding a zwitter ion to the solvent system. Methanol and acetonitrile are frequently used as organic modifiers in these solvent systems. In a single analysis, HPLC methods can be used to separate as many as nine or ten commercially used tetracycline compounds and to determine four to five tetracyclines in commercial tetracycline preparations or in biological fluids.
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  • 22
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    Chromatographia 20 (1985), S. 343-346 
    ISSN: 1612-1112
    Keywords: Thermosorb ; Tenax GC ; Environmental Analysis ; Trace Organics ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A preliminary study has been carried out to evaluate a new adsorbent, Thermosorb, for trace level organic contaminants. For this purpose, a comparison was made with a well-characterized adsorbent, Tenax GC, using a prepared aqueous solution of trace organic components. In addition, a comparison was made of chromatograms of air contaminants obtained using both of these adsorbents, under equivalent conditions. The results clearly indicated the potential of this thermally stable, inorganic adsorbent for many trace organic substances of environmental interest.
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  • 23
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    Chromatographia 20 (1985), S. 371-375 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame photometric detector ; Sulphur
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of experimental conditions such as gas flow rates, detector and column temperatures on sulphur response are discussed. It is concluded that the response of the flame photometric detector is affected by the O/H ratio and the total gas flow. Column temperature has an important influence upon S2 emission. It is shown that the sulphur response of the FPD is dependent on the compound containing the sulphur.
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  • 24
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Resolution of optical isomers ; Chiral column ; Pyrethroids ; Fenvalerate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of the optical isomers of fenvalerate [cyano(3-phenoxyphenyl)methyl 2-(4-chlorophenyl)-3-methylbutyrate] has been carried out by high-performance liquid chromatography (HPLC) on a chiral column with (R)-N-3,5-dinitrobenzoyl-phenyl-glycine (DNBPG) covalently bonded on aminopropyl silica and eluted with mixtures of methanol, 2-propanol, and hexane. The system was applied to the analysis of Pydrin®, an emulsifiable concentrate formulation of fenvalerate, and to the residue analysis of fenvalerate in milk samples. For the analysis of Pydrin® the only requirement was the proper dilution of Pydrin® with hexane. For the analysis of residues in milk, fenvalerate was extracted with hexane after precipitating the milk proteins with acetonitrile and removing the precipitate by filtration; the hexane extract was concentrated to small volume and filtered before being analyzed by HPLC.
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  • 25
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    Chromatographia 17 (1983), S. 269-284 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Phenols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas and high-performance liquid chromatographic methods in the analysis of phenols are reviewed. Among the great number of phenolic compounds analyzed, alkylphenols, chlorophenols, dihydroxy- and trihydroxybenzenes and biphenols are chiefly considered. The advantages and drawbacks of the methods are discussed, quoting the most important work. Relationships between the structural characteristics of phenols, the stationary phase structure, the mobile phase composition and the retention data are treated. Typical examples of the conditions for GC and HPLC analysis are summarized in tables. The literature comprises over 270 references, most of them recent.
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  • 26
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Average molecular polarizability ; Retention index ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The Kováts retention indices of 10 polycyclic aromatic hydrocarbons were determined on SE-30, OV-101, SE-52, OV-7 and OV-17 stationary phases. A significant correlation has been found between the retention indices and the average molecular polarizabilities of the analyzed substances. Equations were derived for the direct determination of the average molecular polarizabilities from the retention index values. The influence of the temperature on this relationship is also indicated.
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  • 27
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    Chromatographia 20 (1985), S. 487-494 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Size-exclusion chromatography ; Controlled-porosity glasses ; Boron-enriched glass surface ; Adsorptive properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Controlled-porosity glasses (CPG) are sieves for macromoleculars, very widely applied in chromatographic columns for the separation of polymers and biopolymers by means of size-exclusion chromatography (SEC) and affinity chromatography. This paper deals with the influence of the thermal treatment of CPG on the elution of polymers in SEC columns. The problem is examined for a few mobile phases and for glasses having different porosities. Additionally, the SEC results obtained are compared with the adsorption properties of the glases investigated.
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  • 28
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrochemical detection ; Cysteinyldopamine ; Tyrosinase ; Autoxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary 5-S-Cysteinyldopamine, a new metabolite of dopamine, was determined in urine by high-performance liquid chromatography with electrochemical detection. The catechol was detected in 14 of 21 melanoma patients and 7 of 21 normal subjects; the highest values were 657 μg/day for melanoma patients and 44 μg/day for normal subjects. These results suggest that the cysteine conjugate may arise from autoxidation of dopamine but tyrosinase may also participate in the oxidation.
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  • 29
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    Chromatographia 21 (1986), S. 136-142 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemical reaction detector ; Carbamate insecticides ; Quantitation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary For the determination of trace amounts of carbamate insecticides in vegetables the combination of liquid chromatography with post column chemical derivatization (chemical reaction detector) is used. In a two step reaction detector the carbamates are firstly saponified in 0.01 M sodium hydroxide at 80°C with a reaction time of 30sec. To this mixture OPA reagent is added to detect the methylamine generated in the saponification. Optimization strategies for this reaction are demonstrated. At a temperature of 80 °C a reaction time of 80 sec is sufficient for quantitative transformation of the methylamine. The peak dispersion can be reduced and hence the detection limit improved by decreasing the diameter of the tubes and by diminishing dilution through the addition of reagent. A 1∶24 ratio of reagent to column (reactor) effluent is possible with cyclone-type mixers. The quantitation of carbamates in different vegetables is demonstrated. The detection limit is 20ppb at a signal to noise ratio of 10∶1.
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  • 30
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame ionisation detection ; Cyanogen ; Cyanogen chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The response of a flame ionisation detector (FID) to cyanogen ((CN)2) and cyanogen chloride (CNCI) has been studied. The lower limits of detection for (CN)2 and CNCl were 6×10−12 moles and 2×10−11 moles respectively. In a comparative study a thermal conductivity detector gave as its lower limit of detection for both (CN)2 and CNCl 4×10−11 moles. Both detectors showed excellent linearity over the range 0 to 10 micromoles. The ratio of the gradients of the FID calibrations (CN)2/CNCI were found to be approximately two suggesting the response depended on the cyanide group. The response and stability of the FID was investigated as a function of air and hydrogen flow-rates. The response increased with increasing air flow-rate for both (CN)2 and CNCI up to 300cm3min−1, thereafter no significant increase was observed. On raising the hydrogen flow from 10 to 25cm3min−1 only a slight increase in the sensitivity of the FID towards both (CN)2 and CNCI was observed. At higher flow rates the response for (CN)2 increased markedly whereas at the same flow rates the response for CNCI increased only slightly.
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  • 31
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    Chromatographia 21 (1986), S. 205-213 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral phases ; Optimization of separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation and properties of chiral bonded phases with amino acid groups are described. These phases were used in non-polar eluents and in aqueous systems in the presence of Cu2+ ions in the ligand-exchange mode. The optimization of chiral resolution is demonstrated for both cases. With non-polar eluents similarity between bonded groups and solutes is required. The elution could be accelerated by non-protonic moderators. Ligand-exchange separation is influenced by the copper content of the eluent and the stationary phase, the organic moderator concentration, the pH and ionic strength of the buffer and by the temperature. Structural requirements of both the bonded groups and of the solutes for chiral separation are discussed.
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  • 32
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    Chromatographia 21 (1986), S. 214-218 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Behaviour of metal acetylacetonates ; Adsorption isotherms ; Heat of solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes, adsorption isotherms, molar heats of solution and changes of the entropy were determined from chromatographic data, which was obtained by the gas chromatographic separation of metal acetylacetonates. The retention data for Cr(III), Co(III) and Al(III) acetylacetonates were measured at different temperatures and different flow rates. From the retention data other values associated with adsorption and solution phenomena were calculated.
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  • 33
    ISSN: 1612-1112
    Keywords: Esterification in aqueous solution ; iso butyl esters of C1–C20 fatty acids ; Gas chromatography ; Fatty acid analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary C1–C20 carboxylic acids have been esterified in aqueous solutions with i-butanol. Gas chromatographic analyses have been performed from a single chromatogram. It has been established that esterification in the concentration range of [H2O]/[i-BuOH]=0.01–10.3 can be utilized for the quantitative determination of these carboxylic acids. The presence of water does not interfere in the range of [H2O]/[i-BuOH]=0.01–1.03. In the cases of [H2O]/[i-BuOH]〉1.03, anhydrous sodium sulfate has been used for binding the water, in an amount of [Na2SO4]anh./[H2O]≥0.2.
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  • 34
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Immobilized stationary phase ; Carbowax-type stationary phase ; Cross-linked polyurethane
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    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of an immobilized stationary phase based on Carbowax 20M is described. The stationary phase cross-linking was carried out with Desmodur N 75 or Desmodur L 75, pluriisocyanates. The properties of the prepared stationary phases are compared.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase capacity factors ; Cavity term ; Molar volumes
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    Topics: Chemistry and Pharmacology
    Notes: Summary Reversed-phase liquid chromatographic capacity factors are well correlated by an equation of the form: $$logk' = (logk')_0 + mV/100 + s\pi ^* + b\beta + a\alpha $$ wheremV/100 measures the cavity term and π*, β, and α are the solvatochromic parameters that measure solute dipolarity/polarizability, hydrogen bond acceptor basicity, and hydrogen bond donor acidity respectively. Liquid molar volume (molecular weight divided by liquid density at 20°C) $$\bar V$$ , and computer-calculated intrinsic (van der Waals) molecular volume, $$\underset{\raise0.3em\hbox{$\smash{\scriptscriptstyle-}$}}{V} _I $$ , are compared as measures of the cavity term in a number of correlations. $$\underset{\raise0.3em\hbox{$\smash{\scriptscriptstyle-}$}}{V} _I $$ leads to more precise correlations as well as to a “cleaner” dissection of the multiple solute/solvent interactions. The opposing exoergic effect of solvent donor/solute acceptor hydrogen bonding, and endoergic cavity term are the main factors influencing HPLC capacity factors.
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  • 36
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    Chromatographia 22 (1986), S. 40-42 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pyridate ; CL-9673 ; Reversed phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary The application of a simple reversed-phase, HPLC-UV method for the determination of the contact herbicide pyridate and its main metabolite 3-phenyl-4-hydroxy-6-chloropyridazine-known as CL-9673-in green cereals, grains and straw is described. The method is based on a simple extraction, separation of pyridate from its metabolite, hydrolysis of pyridate to CL-9673, high-performance liquid chromatographic separation of CL-9673 in both fractions using only one reversed phase column and UV-detection. The method is sensitive down to 3 ngg−1 CL-9673 in green plants and grain and 5ngg−1 in straw. In the range 0.05–1.0mgkg−1 recoveries are between 73.7% and 109% from green plants, between 77.7% and 102% from grains and between 77.3% and 87.5% from straw.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Betablocker drugs ; Lipophilicity ; Capacity factors ; Distribution coefficients
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    Topics: Chemistry and Pharmacology
    Notes: Summary The reverse-phase, high-pressure liquid chromatographic capacity factors (k') of a series of 18 betablocking agents were determined in order to establish correlations with their distribution coefficient values (D), obtained from four bibliographic sources. Under the three pH conditions studied (3.5, 6.2 and 7.5) statistically significant linear correlations (p〈 0.002) between log k' and log D values were obtained for the four series studied. In this series it is concluded that the k' factor is a useful and reliable relative lipophilicity parameter.
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  • 38
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    Chromatographia 22 (1986), S. 81-87 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Recycle chromatography ; Pressure dependence ; Capacity factor
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    Topics: Chemistry and Pharmacology
    Notes: Summary It was found experimentally that the potential for routine, rapid high-efficiency separations by alternate column, recycle, reversed-phase chromatography is limited by the increase of capacity factors with pressure.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Aromatic acid isomers ; Low capacity ion-exchange resin ; Microbore packed columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary A low-capacity, anion-exchange, porous-polymer resin was used as the packing material in a microbore column. Using a phosphate buffer containing various organic modifiers, retention behavior of substituted benzoic acid isomers with amino, chloro, methyl, nitro and carboxylic groups was investigated. The effect of ethanol, acetonitrile and sodium dodecylsulfate used as organic modifiers on the retention behavior at various eluent pH values was studies and optimum separations of the positional isomers reported.
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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of C2−C16 dicarboxylic acids ; Dicarboxylic acid analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary C2−C16 dicarboxylic acids were esterified in aqueous solution in the presence of sulfuric acid. Esterification in water/n-butanol mixtures with mole ratios between 0.02 and 2.53 can be utilized for the quantitative determination of the dicarboxylic acids by gas chromatography. The presence of water does not interfere at water/n-butanol mole ratios below 0.27. For mole ratios above 0.27 anhydrous sodium sulfate has been used for binding the water. The mole ratio range was 0.25–0.75 for anhydrous sodium sulfate/water, and 0.32–1.3 for sulfuric acid/anhydrous sodium sulfate.
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  • 41
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    Chromatographia 18 (1984), S. 663-667 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas solubilities ; Enthalpies of solution ; Polar solutions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gas-liquid chromatographic method has been used to determine the solubilities and partial molar enthalpies of solution of the gases H2S, CO2 and COS in four polar solvents. The results agree well with literature values obtained using conventional techniques, with the one exception of H2S in N-methyl-2-pyrrolidinone. In this case there is some evidence for the occurrence of adsorption at the gas-liquid interface.
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  • 42
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    Chromatographia 18 (1984), S. 668-672 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mixed eluents ; Preferential sorption of eluents ; Pressure effects
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    Topics: Chemistry and Pharmacology
    Notes: Summary Pronounced base line perturbations were repeatably observed in LC both in alternating recycling and in backflushing experiments when binary eluents and refractometric detectors were used. The perturbations which we call eigenzones appeared immediately after operating the recycling or the backflushing valve, and their size and shape depended on the nature of both the column filling and the mixed mobile phase as well as on the pressure drop across the column. Experimental results presented confirm that the primary causes of the eigenzones were the pressure changes in the columns which influenced the sorption equilibrium of mixed eluent components within the column packing. Some practical consequences of this effect are briefly discussed.
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  • 43
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aromatic polycarboxylic acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The direct esterification and gas chromatographic analysis of aromatic carboxylic acids as n-butyl esters is described. Derivatization is performed in aqueous solution with n-butanol in the presence of sulfuric acid. The butyl esters of benzoic, phthalic, hemimellitic, trimellitic, trimesic and pyromellitic acids permit their gas chromatographic separation from each other and from fatty acids and alipatic dicarboxylic acids. At mole ratios of [H2O]/ [n-BuOH]≤0.04 the water present does not interfere with the esterification reaction. At mole ratios above 0.04 anhydrous sodium sulfate is used for binding the water, at mole ratios of [Na2SO4 anh.]/[H2O]=0.25–0.75.
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  • 44
    ISSN: 1612-1112
    Keywords: Polycyclic aromatic hydrocarbons ; Column liquid chromatography ; Polyphenyl bonded phases ; Retention and carbon content
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    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the retention of PAHs having various molecular sizes and the carbon contents (%) of bonded stationary phases with various types of ligands were investigated. The examined stationary phases were phenyl, diphenyl, triphenyl and benzyl-bonded silicas. The data indicated that sometimes it is not true that the retention of any solute relates linearly to the carbon content of the stationary phase. As the result, it is suggested that the pore size distribution of the silica support, the bulkiness of the ligand bonded to the silica and the molecular size of solute should also be considered before any precise statement can be made.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Metalloporphyrins ; 5,10,15,20-Tetraphenylporphine
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    Topics: Chemistry and Pharmacology
    Notes: Summary The Co(II), Ni(II), Fe(III) and V(IV) complexes of tetraphenylporphine (TPP) can be eluted at short retention times from a LiChrosorb RP-18 column with pure ethanol. However, both Mn(III) and Co(III) complexes of metal TPP chloride type are so strongly retained on the column that they cannot be eluted. While the retention of other metal teraphenylporphine complexes was not affected, that of the metal(III) complexes of the TPP chloride type especially MnTPPCl and CoTPPCl, decreases dramatically with an increase in the concentration of NH4Cl added into the mobile phase; a linear relationship between logk' and log[NH4Cl], with the slope of about−1, has been observed for these two metal(III) complexes in the NH4Cl concentration range from 2.5×10−4 to 1.3×10−2 mol/l. Thus, the specific control of the retention of the metal(III) complexes is enabled by conditioning the NH4Cl content of the mobile phase, and the chromatographic separation is demonstrated.
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  • 46
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    Chromatographia 22 (1986), S. 55-58 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; 1-Octanol/water partition coefficient ; Cellulose acetate ; Reverse osmosis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The adsorption properties of esters, aldehydes, ethers and amides on cellulose acetate, which is commonly used as a reverse osmosis membrane material, in an aqueous solution system were measured by high-performance liquid chromatography. The adsorption property was characterized with the specific retention volume. For a noncyclic homologous series the logarithm of the specific retention volume was linearly correlated with the logarithm of the partition coefficient between 1-octanol and water. The fact that the slopes of these regression lines are almost identical confirms that the dominant effect on adsorption is the hydrophobic interaction between cellulose acetate and the solute molecule. The intercept represents the effect of the polar groups on adsorption. The effect of the polar group decreases as follows: ―C(O)O―, ―CO―, HCON〈 〉 CH3CON〈 〉 ―OH, ―O―.
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  • 47
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Volatile nitrosamines ; Fused silica capillary columns ; Linear indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary Fused silica capillary columns of different diameters and polarities are linked to a thermal energy analyzer and a flame ionisation detector for comparison. Extra column effects are discussed. Unsymmetrical homologue nitrosamines are applied in order to assign the volatile nitrosamines most often to be determined by their linear indices rather than by their overall retention times.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Dihydroartemisine ; Interconversion equilibrium ; Multiple-peaks
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    Topics: Chemistry and Pharmacology
    Notes: Summary The interconversion between the α- and β-isomers and the multiple-peaks of dihydroartemisinine (dihydroqinghaosu) were investigated in reversed-phase, highperformance liquid chromatography. A convenient method using the Gaussian distribution function instead of the Schmidt graphical method for the theoretical calculation of the “diffuse” probability curves versus the fraction of the dead time on column as β form was introduced. Based on the theoretical probability curves and the experimental multiple-peak chomatograms, the effects of temperature and flow velocity on the accuracy and precision of analysis of dihydroartemisinine are indicated and the activation energy of the interconversion between α- and β-isomers of dihydroartemisinine is estimated.
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  • 49
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermionic detector ; Flame-forming agents ; CO2 and water gas
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of carbon monoxide were suggested as the flame-forming agent in the thermionic detector (TID). The main characteristics of this detector were studied. It was shown that the optimum flow rate of carbon monoxide is 40 ml/min at an air flow rate of 400–550 ml/min. The response increases twice with the positive potential on the collector. Molar responses of TID were compared with those obtained when using carbon monoxide and hydrogen. For instance, for phosphorus containing compounds they are approximately the same (∼102), while for nitrogen containing compounds in the case of carbon monoxide, there is a 2–5 fold increase in the response. The linear dynamic range for methaphose and azobenzene is 103.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Nucleotides ; Mytilus edulis ; Smooth muscle
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the analysis of the 5′ mono-, di- and triphosphates of adenosine, guanosine, uridine and cytidine, as well as uridinediphosphate-glucose and cyclic AMP. Separation is achieved by reversed-phase ion-pair chromatography with linear gradient elution. Application of this method to the analysis of nucleotides in smooth molluscan muscles is described, including the determination of cAMP-levels and the calculation of energy charges for all of the four nucleotide systems.
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  • 51
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porphyrin ; Metalloporphyrin ; Hematoporphyrin IX
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    Topics: Chemistry and Pharmacology
    Notes: Summary The feasibility of reversed-phase high-performance liquid chromatography for the separation of metal complexes of hematoporphyrin IX (Hp) is described. The retention order, Zn-complex〈Hp (free acid)〈 Ni-complex〈Cu-complex, is regular on an octadecylbonded stationary phase with different compositions of an aqueous methanol mobile phase. These four compounds can be successfully separated within about 8 min on a LiChrosorb RP-18 column (250×4-mm i.d.) with a 85:15 (vol/vol) mixture of methanol and phosphate buffer (pH 3) at a flow rate of 1 ml/min.
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  • 52
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Chemically bonded phase ; Specific interactions
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    Topics: Chemistry and Pharmacology
    Notes: Summary Packings consisting of chemically bonded diphenylphosphine complexes with CuCl2 and CuBr2 were synthesized and their retention parameters determined. The packings investigated are capable of specific interactions with electron-donating compounds and are characterized by particularly high selectivity in relation to cis and trans isomers allowing their complete separation.
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  • 53
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    Chromatographia 22 (1986), S. 157-159 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flavonol aglycones ; Isocratic elution ; Wine phenolics
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    Topics: Chemistry and Pharmacology
    Notes: Summary An HPLC isocratic elution procedure which allows the separation of flavonol aglycones in wine without interference from other phenolics of low molecular weight is described. The method has been applied to the separation, identification and quantitative estimation of flavonol aglycones in ether extracts of different Spanish wines (red and white table wines and Sherry finos). The results suggest that these determinations, associated with other analyses, would permit the chemical characterization of wines.
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    Chromatographia 23 (1987), S. 796-802 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Steroids ; Rat tissue ; Purification by extraction
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic method for analysis of steroids in the tissue of laboratory animals is described. A two-stage solid extraction procedure, utilizing Sep-pak C18 and graphitized carbon black, gives a purified product. Steroids in this extract were separated by multistep gradient elution with a reversedphase liquid chromatography system, using acetonitrilewater as solvent. Several columns with different geometry and phase loading were investigated. Optimum resolution was obtained with a medium covered and spherical particle. The applicability of this method was successfully demonstrated in the analysis of the testis and adrenal gland of rat.
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    Chromatographia 23 (1987), S. 814-817 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin layer chromatography ; Ammonium tungstophosphate ; Aminoacids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of aminoacids on columns of silica coated with different percentages of ammonium tungstophosphate at several buffer phosphate concentrations is reported. The stationary phase shows a high selectivity towards aminobutyric acids and methyl derivatives of tryptophan due to the distance between the carboxylic group and the −NH 3 + group involved in the cation-exchange process and/or to the steric hindrance by a methyl substituent. A relationship between HPLC and HPTLC data has been verified and applied to the prediction of the separation of six aminoacids.
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  • 56
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    Chromatographia 23 (1987), S. 818-824 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective sampling ; On-line fractionation ; Essential oil analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper describes the possibilities of on-line selective sampling as an on-line fraction technique for the analysis of essential oils. Selective sampling is a micro-separation method, on-line with on-column injection, carried out directly in the syringe body by means of a selective elution of the sample through a fraction cartridge. The paper reports a method of both preparing and standardizing silica gel cartridges, and illustrates through some examples the results of some elution series of solvents on different essential oils.
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  • 57
    ISSN: 1612-1112
    Keywords: Organic pollutants determination ; Gas chromatography ; Thermal desorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary The problem of the separation of 34 volatile organic chlorinated compounds is solved by using three different GC columns selected according to the needs of the particular separation required. The effect of water vapor contained as moisture in the trapped air on the retention of some characteristic compounds is studied. The influence of dead volumes on trap injection is also studied.
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    Chromatographia 23 (1987), S. 888-892 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Calculation of temperature programmed ; Retention indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is presented for the calculation of the retention indices under linear temperature programming with or without an initial isothermal period. The data calculated by the method are in good agreement with the isothermal retention indices.
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  • 59
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Propyl esters of aromatic polycarboxylic acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The direct esterification and gas chromatographic analysis of aromatic carboxylic acids as n-propyl esters is described. Derivatization is performed in aqueous solution with n-propanol in the presence of sulfuric acid. The n-propyl esters of benzoic, phthalic, trimellitic and pyromellitic acids permit their gas chromatographic separation from each other and from fatty acids and aliphatic dicarboxylic acids. At mode ratios of [H2O]/[n-PrOH]≤0.03 the water present does not interfere with the esterification reaction. At mole ratios above 0.03 anhydrous sodium sulfate is used for binding the water, at mole ratios of [Na2SO4anh.]/[H2O]=0.51–1.52 and of [H2SO4]/[Na2SO4anh.]=0.43–1.28, respectively.
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    Chromatographia 23 (1987), S. 934-938 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Calibration ; Confidence interval ; Limit of determination ; Limit of calibration
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    Topics: Chemistry and Pharmacology
    Notes: Summary In HPLC calibration the expressions lowest calibration limit and determination limit are defined in statistical terms. The lowest calibration limit is the minimum mass in the measured series of calibration points. It is calculated from the confidence interval of the inverse of the calibration function as the lowest mass limit that may be differentiated from zero mass with a preset probability of error. If the calculated lowest calibration limit is lower than the actual data, points at lower concentration may be measured. The determination limit is the smallest concentration of an analysis that is differentiated from the concentration zero or an apparent blind value in the calibration curve with a given probability of error. Using two different UV-detectors (variable wavelength and photodiode-array) the lowest calibration limit is experimentally evaluated and compared with specific data for the detectors.
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  • 61
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Quantitation ; Fermentation products
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is proposed for the analysis by gas chromatography of volatile compounds found in alcoholic and acetic fermentation samples. The method represents a suitable choice for the accurate and precise determination of 19 compounds (including Methanol) by direct injection onto a single column. Chromatograms of synthetic mixtures as well as actual samples show the capabilities of the micropacked column used.
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    Chromatographia 18 (1984), S. 175-182 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fourier transform IR ; Polar compounds ; Coal products
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fourier-transform infrared spectrometry (FTIR) was utilized as a detection system for high-performance liquid chromatography of polar compounds on a normal bonded-phase system. In addition to FTIR, UV (254 nm) and refractive index detection were employed in the separation of model compounds containing oxygen and nitrogen atoms in their molecules (phenols, alcohols, neutral and weakly basic nitrogen compounds). A polar amino-cyano (PAC) bonded-phase column was employed with a binary mobile phase (98:2 CDCl3:CH3CN). The separations and the information gained from each detector is discussed, including interactions between sample material and mobile phase. A polar fraction of a coal-derived product is also chromatographed under identical conditions. The results based on FTIR detection and chromatographic retention behavior suggest the exclusive presence of hindered and unhindered phenols.
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  • 63
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    Chromatographia 18 (1984), S. 202-204 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polysiloxane stationary phases ; Heat of adsorption ; Heat of solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary The changes in the heat of solution of polar compounds and xylene isomers in methylsilicone fluid OV-101 deposited on Chromosorb W AW DMCS were studied. It was shown that the heat of solution increases with an increase of the percentage loading of the OV-101 up to 10%. Solution and adsorption thermodynamic characteristics of the studied system are briefly discussed.
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  • 64
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Chemically bonded phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary Packings consisting of diphenylphosphine complexes with CoCl2 and CoBr2, chemically bonded to the silica surface, were synthesized and their retention parameters determined. The packings are capable of specifically interacting with electron-donating compounds by forming π-complexes. The interaction is considerably stronger in the case of CoBr2-containing packing than in the case of CoCl2-containing packing.
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    Chromatographia 18 (1984), S. 211-215 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Alkylbenzenes ; PAHs ; Retention prediction ; Microcomputer
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The microcomputer-assisted retention prediction system in C18 reversed-phase HPLC is described. The system is based on the use of the hydrophobic parameter and the correlation factor of alkylbenzenes and polycyclic aromatic hydrocarbons (PAHs) which are highly correlated to their retention in reversed-phase HPLC. The system is evaluated by comparing the retention data between measured and predicted values. One of the typical examples applied for PAH analysis in the extracts of diesel particulate matter shows the high potential of the system investigated.
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    Chromatographia 18 (1984), S. 216-220 
    ISSN: 1612-1112
    Keywords: Cation exchangers ; Column liquid chromatography ; Exchange capacity, determination ; Organic peroxidation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two oxidation procedures for the synthesis of silicabased aliphatic sulfonic acid cation-exchangers for HPLC are described. Several reaction conditions for oxidizing a terminal-bonded thiol with organic peroxides are provided along with their yields, capacities, reproducibility, and chromatographic behavior. Also, three methods for determining exchange capacity are discussed, and their relationship to the capacity factors of charged solutes is compared. The maximum capacity determined by the titration of the bonded silica was 0.34 meq/gram. The general problems of synthesizing cation-exchangers, measuring their efficiencies and exchange capacities, and evaluating their overall performances are outlined.
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  • 67
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    Chromatographia 18 (1984), S. 234-238 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular columns ; On-column injection ; Stopped-flow operation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, inexpensive, on-column injector of the septum moving-needle kind is described for quantitative analysis using open-tubular columsn. when operated in the stopped-flow mode an improvement incolumn efficiency is observed combined wit a diminished tendency to produce split-top peaks, particularly for late eluting peaks. Using electronic integration a relative error of about 2.7% was observed for peaks spanning a wide range of sample concentrations and volatilities.
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  • 68
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    Chromatographia 18 (1984), S. 243-248 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas ; Viscosity ; Influence of temperature
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The vicosity-temperature relationship of the three gases (helium, nitrogen and hydrogen) most frequenly used as the carrier gas in gas chromatography is studied. Based on available data, equaitions are derived to describe this relationship. Using these equations viscosity data are tabulated for the chromatographically important temperature range.
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  • 69
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    Chromatographia 18 (1984), S. 260-264 
    ISSN: 1612-1112
    Keywords: Parabens and their dissolution ; Pharmaceutical dosage forms ; Derivatization ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary A specific, sensitive and general applicabla gas chromatographic method is described for the determination of parabens in various liquid pharmaceutical preparations: propylparaben and butylparaben in a liquid antacid dosage form (I); methylparaben, ethylparaben and propylparaben in a syrup (II); methylparaben and propylparaben in a solution for injection (III). Each time one of the parabens is used as internal standard. The parabens are extracted with diethylether and derivatized by silylation. Different columns are used for the analysis of the parabens: 3% SE-30 column, a 3% QF-1 column for different selectivity, a 2% OV-1 column for isothermal operation. Special attention is attributed to the standard: the parabens are dissolved in a minimal amount of 0.1 M sodium hydroxide and extracted in the same way as the pharmaceutical dosage form.
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  • 70
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Configuration ; Resolution ; Alcohols
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    Topics: Chemistry and Pharmacology
    Notes: Summary The study of the resolution of sixteen secondary aliphatic alcohols by gas chromatography on (+)-dodecyl (2R, 3R)-tartrate, trapping the ascending part of the peak from a conventional filled column, has allowed the determination in a single operation of the sign and order of emergence of enantiomers. A correlation between the configuration of these secondary alcohols and their order of emergence has been established.
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  • 71
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    Chromatographia 18 (1984), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carboxylic acids ; Acetonyl derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of the acetonyl esters of nine aliphatic carboxylic acids is described, the general formula of the derivatives being RCOOCH2COCH3 where R=alkyl or H. The derivatives show good chromatographic properties on both packed and capillary columns. The electron impact and chemical ionisation mass spectra of the derivatives are discussed.
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  • 72
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pre-column derivatization ; Ultraviolet detector sensitivity ; Dihydroartemisinin ; Diacetyldihydrofluorescein
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of diacetyldihydrofluorescein (DADF) for derivatization of dihydroartemisinin (dihydroqinghaosu, DHQHS) is proposed. The reaction between DHQHS and this reagent in the presence of 4-dimethylaminopyridine (DMAP) and N,N′-dicyclohexylcarbodiimide (DCC) was complete in 8 hours at room temperature giving about 80 per cent theoretical yield. The derivative showed intense UV absorption, thus providing a sensitivity of 0.1 nanogram by UV detection after column separation. The influences of the ratio of the reagents, reaction temperature, chromatographic conditions and the extent of detection linearity were investigated. The reaction gave consistent results and chromatographic separation was not affected by an excess of the reagent or side products.
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  • 73
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    Chromatographia 23 (1987), S. 195-198 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention relationships ; Polarity parameters ; Retention index
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    Topics: Chemistry and Pharmacology
    Notes: Summary The possibility of evaluation of the parameters representing the dispersive solute-solvent interactions is presented. BN and Bs values can be used to describe the liquid phase polarity and to predict the retention indices of alcohols when the model polyxyethylene glycol dialkyl ethers and their sulphur analogs are used as stationary phases. The possibility of the first ionization potentials estimation is also presented.
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  • 74
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    Chromatographia 18 (1984), S. 369-373 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion exchange ; dynamic ; Metal ions ; Equilibria effects
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    Topics: Chemistry and Pharmacology
    Notes: Summary Equilibria occurring during the dynamic ion exchange separation of metal ions were examined, and their effect on the chromatography of the metal ions was evaluated. Bonded reversed-phase silica, pure organic reversed phase, and silica columns were used to differentiate between the role of silica and the reverse phase. The results show that system peaks had the most important influence on the applicability of dynamic exchangers to quantitative metal ion determinations. The response of system peaks to sample composition (pH, ionic strength, matrix effects) was complicated and could not be predicted easily. Equilibria effects that can cause analytical errors were identified and recommendations for elimination of such errors are given.
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  • 75
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Amines ; Phenols ; Fourier transform I.R.
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    Topics: Chemistry and Pharmacology
    Notes: Summary Several chromatographic parameters have been examined as to their effect on detectability for microbore high-performance liquid chromatography coupled with Fourier-transform infrared spectrometry. Detection limits for several compound classes are presented as amount injected. Improvements in detectability for this technique are discussed.
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  • 76
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polystyrene packings ; Pre-column derivatization ; Thiamine compounds ; UV and fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatography of thiochrome and related phosphate esters was studied on two different polystyrene packing materials. The adsorbents were compared with respect to capacity factors, plate heights and resolution factors measured with different mixtures of phosphate buffer (pH 8.5) and methanol. In contrast with derivatized silica, these phases were found to be stable using an alkaline mobile phase and sample. Fast separations were possible with good peak symmetry at all organic modifier concentrations.
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  • 77
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    Chromatographia 18 (1984), S. 445-448 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Amino-bonded stationary phase ; Ion-exchange ; Fermentation solution ; Biomass
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    Topics: Chemistry and Pharmacology
    Notes: Summary In this work the analytical separation of biomass hydrolysis and fermentation products is described. Aminobonded phase and ion exchange materials (HPX 87H, HPX 42A, μ Spherogel Carbohydrate) were used as HPLC stationary phases for the determination of monomeric and oligomeric carbohydrates, carbohydrate degradation and fermentation products. The HPX 42A and the amino-bonded phase columns are especially suitable for the analysis of the gluco oligomers. The HPX 87H column separates the monomeric sugars and their degradation and fermentation products (e.g. furfurals and ethanol) very well. Using the μ Spherogel Carbohydrate column the lower gluco-oligomers as well as the monomeric sugars and their degradation and fermentation products, can be determined within 35 minutes.
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  • 78
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermodynamic relationships ; Retention index ; Peak identification
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    Topics: Chemistry and Pharmacology
    Notes: Summary A thermodynamic criterion, ΔQ, is suggested which permits to estimate the difference in the functional group energy of interactions for two different stationary phases. The linear dependence of ΔQ on the homolog number m of any series Rm X can be used as the thermodynamic criterion for the identification of substances by GC analysis.
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  • 79
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral bonded phase ; Racemate resolution
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    Topics: Chemistry and Pharmacology
    Notes: Summary A chiral stationary phase with an immobilized, optically active diamine was prepared for the separation of enantiomers. The synthesis of the phase was carried out by bonding (−)trans-1,2-cyclohexanediamine to microparticulate silica gel through the coupling agent 3-glycidoxypropylsilane. The resolution of the racemic compounds catechin, 2,2′-dihydroxy-1,1′binaphthyl and trans-1,2-cyclohexandiol, is reported.
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  • 80
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    Chromatographia 18 (1984), S. 477-488 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Sample capacity ; Column comparison ; Film thickness ; Column diameter
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    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated, open-tubular (capillary) columns prepared from different diameter tubing, with different liquid phase film thickness, are compared with each other and with packed and support-coated open-tubular columns. The comparison is based on the variation of the phase ratio and the capacity factor, and includes column efficiency (HETP, theoretical plate number), resolution, retention time, and sample capacity. Problems associated with the evaluation of the sample capacity are outlined. The influence of temperature on column performance is discussed in detail. Finally, the possibilities of short, wide-bore open-tubular columns prepared with a thick liquid-phase film are demonstrated.
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  • 81
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    Chromatographia 18 (1984), S. 495-498 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; PAHs ; Molecular shape recognition
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    Topics: Chemistry and Pharmacology
    Notes: Summary The molecular-shape recognition of polycyclic aromatic hydrocarbons has been studied on various stationary phases in reversed-phase high-performance liquid chromatography. The examined stationary phases were phenyl-, diphenyl-, triphenyl- and benzyl-bonded silicas. The results of regression analysis inidcated that triphenylsilica is the best packing material to recognize the difference in the molecular-shape of structural isomers. This fact was confirmed by the separation of 4-ring isomers.
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  • 82
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention data ; Substituted benzene derivatives ; Correlations
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    Topics: Chemistry and Pharmacology
    Notes: Summary The capacity factors of substituted benzene derivatives on bonded phases of various chain lengths in the reversed-phase mode have been measured and correlation of retention data between four stationary phases has been investigated by linear regression analysis. As a result, a difference in the retention mechanism between phases of shorter chain length and octadecylsilica was observed. In addition, it is also apparent that the multicombination treatment between retention data and descriptors such as π, HA, HD and σ promises the possibility of predicting the retention of substituted benzene derivatives on various reversed-phase stationary phases.
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  • 83
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polyamines ; Dansyl derivatives ; Peak compression
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    Topics: Chemistry and Pharmacology
    Notes: Summary Analytical conditions for the high-speed, reversed-phase, liquid chromatographic of a diamine (putrescine) and polyamines (spermine and spermidine) were determined. Various elution modes were employed using the same mobile phase constituents: 20mM sodium heptane sulfonate and 20mM acetic acid as solvent A and, pure acetonitrile as solvent B. Samples were derivatized with dansyl chloride before injection. Under isocratic conditions, the separation of the three polyamines was achieved in 7 min. The use of a linear elution gradient led to the same analytical time but with a better resolution of the putrescine peak from non-polyamine frontal peaks. For these measurements, the sample size was 5μl. This volume was increased to 20μl and the use of a steep gradient combined with the peak-compression technique allowed a fast analysis in 2–3 minutes, which may be compared with a 30 min run time necessary when a conventional column is used.
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  • 84
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    Chromatographia 23 (1987), S. 395-400 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Photokinetic data ; Reaction mechanism ; (E)-1-phenylpropene
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    Topics: Chemistry and Pharmacology
    Notes: Summary A combined method of high-performance liquid chromatography and UV-absorption spectroscopy is described for use in dynamic systems. It provides a way of obtaining detailed mechanistic information as well as quantitative data (rate constants, quantum yields), even though neither mechanism nor photoproducts are known. The kinetic treatment of the photoreaction of (E)-1-phenylpropene was successful, showing a photo-isomerization and a parallel step. Information on this additional step is obtained by using HPLC to observe the changes in the concentrations of the reactants' selectivity. The necessity of process control is demonstrated.
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  • 85
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    Chromatographia 23 (1987), S. 419-422 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acid esters ; Particulate material in seawater
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the determination of fatty acids of the molecular weight range of propionic to erucic acid is reported. The acids are converted to either p-bromophenacyl-or p-phenylphenacylesters and the esters are separated by HPLC and detected by UV-absorption. Twentytwo esters, including saturated, monoolefinic and polyunsaturated ones were separated within one HPLC-run. The detection limit is about 5 pmol per fatty acid. The application of the method to particulate material is described.
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  • 86
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange stationary phases ; Polymer coating ; Cross-linking
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    Topics: Chemistry and Pharmacology
    Notes: Summary PHEB=POLY(2-hydroxy, 3N-ethylenediamino)butadiene has been synthesized. This unsaturated pre-polymer can be immobilized on different, preferably inorganic supports of suitable porosity such as silica or alumina by cross-linking. Weak anion-exchange phase are obtained. Such phases do not have the disadvantages of organic polymeric phases, regarding pressure stability and swelling by solvent influence. The ion-exchange capacity and the retentivity of IE-separations can deliberately be varied via the thickness of the cross-linked polymer layer. Alumina can also be coated with PHEB applying the same cross-linking procedure. Such phases exhibit an exceptional chemical stability even when operated with mobile phases at very high pH-values. Separations of excellent selectivity are achieved for inorganic anions, as well as with mixtures of aliphatic and aromatic free acids also including hydroxy- (mono- or poly)carboxylic acids.
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  • 87
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase systems ; Stationary phase-solute interactions ; Polycyclic aromatics
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    Topics: Chemistry and Pharmacology
    Notes: Summary Capacity factors of peropyrene-type polycyclic aromatic hydrocarbons were measured using 15 different liquid chromatographic reversed phase systems. On the basis of the retention data the electric interaction indices have been calculated. Application of these indices for structure-retention studies on peropyrene-type polycyclic aromatic hydrocarbons is demonstrated.
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  • 88
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Prediction of retention volume ; Porous polymers coated with liquid phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new expression which permits the prediction of the net retention volumes in gas chromatography with column packings of coated porous polymers is reported. The porous polymers Chromosorb 101 and Chromosorb 102 were used as supports and squalane, Ethofat and Carbowax 20M as stationary phases at three different column temperatures of 80°C, 100°C and 150°C. Several organic compounds of various polarity were used as test compounds and the net retention volumes, VNtheor, have been calculated according to this new expression. The VNtheor values were compared with the experimental net retention volumes, VNexp, and it was found that the difference between these two values is dependent on the type of compound and column packing. Nevertheless, the elution order could be predicted in most cases.
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  • 89
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    Chromatographia 23 (1987), S. 499-501 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Packed+capillary GC switching system ; Precolumn construction, oven and connector
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    Topics: Chemistry and Pharmacology
    Notes: Summary The constractional details of precolumns, its oven and connector have been given with two types of multiflow control modules. Two types of phases made in China, a silanized pellicular beads and a non silanized pellicular silica beads, with an optimum particle size of 20μm to 30μm were packed in the precolumn 20mm in length with the column efficiency of 4620 plates/meter at column temperature of 49°C. A 25m×0.22mm i.d. capillary column coated with bonded methylsilicone phase from Chrompack connected with the precolumn (250°C) has an efficiency of 5376 plates/meter for n-octane. But it decreased to 3149 plates/meter by decreasing the precolumn temperature to 130°C.
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  • 90
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Immobilized Carbowax-type stationary phases ; Free fatty acids analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Capillary columns coated with acid-modified poly-(ethylene glycol)-type immobilized stationary phases have been studied. The thermostability and chromatographic behaviour of the columns and the stability of the coated films after washing with different solvents were investigated.
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  • 91
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fourier transform IR detection ; Headspace sampling ; Solvents of abuse
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    Topics: Chemistry and Pharmacology
    Notes: Summary After experimental intoxication of rats, gas chromatography — Fourier transform infrared spectrometry with headspace sampling (HS/GC/FT-IR) was used to identify solvents of abuse in biological material (blood, liver, lungs and brain). Limits of detection were measured for acetone, 2-butanone, ether, toluene and trichlorethylene with standard solutions. All the solvents have been identified in the organs of the intoxicated rats. For blood samples a salting-out effect was obtained with potassium carbonate. HS/GC/FT-IR allowed the identification of metabolites of acetone (isopropanol) and of 2-butanone (2-butanol) in blood and organs.
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  • 92
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    Chromatographia 25 (1988), S. 31-36 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Radioactivity detector ; Solid scintillator ; Fibre-packed flow cells
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new type of flow-cell radiation detector for use in liquid chromatography which is packed with aligned scintillator fibers is described. A primary advantage of the fiber packed cell is that light generated by the scintillator is absorbed to a much less extent by the fibers than by the powder scintillator used in conventional flow cells. A detection efficiency of 55% has been obtained for carbon-14 using 0.1-mm diameter hand-pulled glass fibers. Computer modeling has shown that even better results can be obtained by using smaller and more uniform diameter fibers which will allow better packing. The fiber cell also demonstrates back pressures which are a factor of 50 less than the conventional cell and much less susceptibility to absorption of compounds because of its lower surface area.
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  • 93
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    Chromatographia 25 (1988), S. 854-860 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polystyrene ; Gradient elution ; Turbidimetry
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    Topics: Chemistry and Pharmacology
    Notes: Summary Polystyrene samples of narrow molecular-weight distribution have been eluted according to their molecular weight from columns packed with bare silica Si50, phenyl, or C18 bonded phase by gradients of methanol and tetrahydrofuran (THF) or ofiso-octane and THF. Among the six combinations investigated,iso-octane/THF with a silica column formed a proper normal-phase system whereas methanol/THF with a C18 column formed a proper reversed-phase system. The combinations of C18 column andiso-octane/THF or of Si50 column and methanol/THF gradient did not correspond to the approved polarity rules in high-performance liquid chromatography but were nevertheless effective in separating polystyrene mixtures by molecular weight. Methanol andiso-octane are nonsolvents for polystyrene whereas THF is a solvent. The solubility of polystyrene as a function of molecular weight and concentration was determined by means of turbidimetric titration of solutions in THF with the nonsolvents used in the gradients. The solubility and elution characteristics were almost identical on C18 columns or in methanol/THF combinations. The elution from phenyl bonded phase and Si50 columns usingiso-octane/THF gradients required more THF than the solubility experiments. Information is also given on the occurrence of multimodal elution patterns.
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  • 94
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polycyclic aromatic compounds ; Alkylated PAC ; Retention characteristics ; Normal phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention characteristics of series of polymethyl and mono-n-alkyl derivatives of benzene and pyrene, and also of parent polycyclic aromatic hydrocarbons (PAH), were studied using silica and aminopropyl- and cyanopropyl-modified silica. Differences in the selectivities for the studied compound groups were found between the three phases. Deviations from linear behaviour in plots of log (k′)vs. carbon number were observed for the methyl series. These are explained in terms of differences in π-electron delocalisation within the aromatic ring systems. Further, the effect of methyl substitution on selectivity decreased with an increasing number of aromatic rings. Results were obtained which indicated that the primary adsorption site in a cyano column used in normal phase mode, at least for PAH molecules, is the cyano group.
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  • 95
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    Chromatographia 25 (1988), S. 43-50 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phase ; Void volume ; Adsorption isotherms
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    Topics: Chemistry and Pharmacology
    Notes: Summary In reversed-phase liquid chromatography with n-alkyl bonded silica, the dead volume (V0) of the column is theoretically indeterminate owing to adsorption of organic modifier on n-alkyl chains and of water on silanol groups. With binary mobile phases, retention volumes of the mobile phase components and of their deuterated species are relaeed to the adsorption isotherms and V0 by equations which can be solved with some assumptions on the adsorbed layer composition. Methanol-water and acetonitrile-water systems are studied. As the experimental excess isotherm shows a linear part in the concentration range 50–80% in organic modifier, the hypothesis of an adsorbed layer of constant composition in this range is possible. When increasing the water content of the mobile phase, adsorption of water occurs up to saturation of silanol groups. Then the assumption of a constant water content for a mobile phase having more than 50% of water is applied. With the hypothesis of a constant adsorbed content of organic modifier when the eluent has more than 80% of organic modifier, V0 and the absolute isotherms are calculated over the entire range of mobile phase composition. Experimental retention behavior of the mobile phase components are totally explained by these V0 determinations. The retention times of commonly used V0 markers are compared with V0 values. It is shown that, when buffering the eluent, no visible effect on the distribution equilibrium is observed, so that injection of concentrated potassium nitrate is a convenient method to measure V0. With a few solutes with are UV detectable it is possible to measure V0 whatever the mobile phase composition in methanol-water and acetonitrile-water systems.
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  • 96
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stationary phase solubility parameters ; Cyano-silica ; Amino-silica ; Diol-silica
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Extended solubility parameters have been determined for aminopropyl, cyanopropyl and 1,2-dihydroxypropyl propyl ether (diol) normal bonded-phase HPLC columns. Parameters were calculated from both the retention data of solutes (partition model) and empirically determined solvent strengths (adsorption-displacement model). The use of solvent strengths to calculate solubility parameters for these silica-based bonded stationary phases appears to be superior, since this technique avoids many of the problems that arise from their inherent heterogeneity. Normalized solubility parameters were also used to position these columns on a stationary phase selectivity triangle. The amino and cyano phases appear in regions of the tringle expected based on the properties of the pure liquids, but an ether linkage in the diol apparently neutralizes some of the acidity expected from this phase.
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  • 97
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Simultaneous distillation-extraction ; Cheese volatiles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simultaneous distillation-extraction apparatus proposed by Godefroot has been used for the GC study of volatile components of cheese. 5–10 g of cheese provide a fraction that can be directly injected into a GC or a GC/MS. Two capillary columns (SE-30 and SP-1000) were evaluated, the second one being adequate for quantitative determinations. Camphor was used as internal standard. The coefficients of variation ranged from 1.4 to 11.8. The technique can be used as a fast method for the characterization of cheeses from their volatile component concentrations.
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    Chromatographia 25 (1988), S. 1087-1088 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Log plot ; Homologous series
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The slope of the log plot of the adjusted retention time of a homologous series usually varies from that of the n-alkane series by no more than 2%, though with unusual interactions between the functional group and the stationary phase the difference may be as high as 7%.
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  • 99
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale separations ; Plate model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two close-boiling materials, diethyl ether (DEE) and dichloromethane (DCM), were separated to investigate the effects of the pure components and the mixture on elution in preparative gas-liquid chromatography. Nitrogen was used as the carrier gas, and the chromatographic column (1 cm I.D. and 0.75m length) was packed with Chromosorb A with different quantities of dinonyl phthalate stationary phase and particle sizes. Below ca. 7% (by wt.) of feed concentration, the experimental elution curves of pure DEE and DCM were almost the same as those of the mixture, and the theoretical plate model can be used successfully to predict the elution curves.
    Type of Medium: Electronic Resource
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  • 100
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Macrolide antibiotic azithromycin ; Intermediates of azithromycin ; Optimization of separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary HPLC is the most convenient method for the assay of the azithromycin (10-dihydro-10-deoxo-11-methyl-11-azaerythromycin A), a semisynthetic macrolide antibiotic and its reaction intermediates. Data concerning the effects of pH, temperature and column type are presented. The analytical procedures enabling the reliable assay of azithromycin and its intermediates, as well as other impurities are defined. Use of a reversed-phase octadecyl column, a pH of 9.3–9.5, and isocratic mode at ambient temperature are the best conditions of analysis.
    Type of Medium: Electronic Resource
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