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  • 1990-1994  (234)
  • 1980-1984  (412)
  • Gas chromatography
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Amino acids 6 (1994), S. 205-211 
    ISSN: 1438-2199
    Keywords: Amino acids ; Amino acid enantiomers ; Chiral analysis ; Chirasil-L-Val ; Gas chromatography ; Mass spectrometry ; Selected ion monitoring ; D-Serine ; D-Alanine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The relative amounts of free D-amino acids (D-AA) in the urine of seven healthy volunteers (age 27 to 49 years) were determined using chiral phase (Chirasil-L-Val) capillary gas chromatography in conjunction with selected ion monitoring mass spectrometry. The absolute amounts of free D-AA were determined by pre-column derivatization of the amino acids witho-phthaldialdehyde andN-isobutyryl-L-cysteine followed by high-performance liquid chromatographic separation and fluorescence detection of the isoindol derivatives formed. The following most abundant D-AA were found (highest and lowest absolute and relative amounts): D-Ser (379.8 — 30.1µMol/L; 56.5 — 19.0%), D-Ala (53.8 — 7.6µMol/L; 19.6 — 5.7%), D-Thr (5.8 — 0.25µMol/L; 3.4 — 1.0%), D-Val (3.7 — 0µMol/L; 4.2 — 0%), and D-Phe (3.5 — 0.35µMol/L; 4.8 — 1.4%).
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 265-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Triglycerides ; Packed vs. capillary columns ; Milk fat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Quantitative gas chromatography of triglycerides in conjunction with established triglyceride formulae can be used to determine various milk fat parameters. Since the evaluation of, for example, iodine number or content of non-milk fats (foreign fats) in milk fat requires only the separation of triglycerides by carbon number and since repeatabilities, especially of the highboiling triglycerides, have been less acceptable with capillary columns in the past, packed columns have been used exclusively. There is, however, an increasing demand for the use of capillary instead of packed columns and to that end the present investigation has been carried out. To achieve a suitable resolution, with this particularly exacting high-temperature application, a short 5 m capillary column of extreme temperature stability has been used. As well as modification of various analytical conditions different injection techniques have been investigated. On-column, PTV and split injection were compared with regard to repeatability. The cold-on-column injection technique was found to produce the best results, being comparable to the excellent precision of a packed column. Thus, a method is now available by means of which the determination of milk fat parameters by the triglyceride formulae, such as the amount of foreign fats in milk fat, can now be carried out with a standardized capillary column.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 294-298 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preconcentration ; Thermal modulator ; Cross-correlation ; Trace analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The inside wall of an uncoated polyethylene capillary traps organic substances from a water sample pumped through it by a nitrogen gas stream. Heating the capillary in a chromatographic oven slowly releases the trapped organic substances from the wall. Nitrogen carrier gas transports sample substances released through a thermal desorption modulator and onto a chromatographic column. Pulsing the temperature of the modulator modulates the concentrations of sample components as they enter the column. Computing the cross correlation of the detector output signal against the applied modulation signal generates the chromatogram. Detection limits below 1 ppb are possible using a flame ionization detector. No sample pretreatment or cold trap is required.
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  • 4
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Organonitrogen pesticides ; Organophosphorus pesticides ; Apples ; Solvent extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method employing a capillary column and a selective nitrogen/phosphorus detector (NPD) has been developed for the determination of organophosphorus (OP) and organonitrogen (NP) pesticides in horticultural samples (apples). The separation of sixteen pesticides and the internal standard was performed in thirteen minutes. The analytical characteristics of the method, including linear response ranges, detection limits, and reproducibility, have been studied using a 1∶1 mixture of ethyl acetate and xylene as extraction solvent. The possibility of mutual interference between pesticides has also been studied. A procedure for the quantitative extraction of the sixteen pesticides from apple samples has also been developed; for fifteen of the pesticides recoveries 〉85% were obtained after 90 minutes extraction. The effect of different solvents both on recovery and on the sensitivity of the subsequent chromatography were also investigated. It was found that the sensitivity required must be considered when the solvent for sample treatment is selected.
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Method validation ; Reggedness test ; Residual solvents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Ruggedness testing is performed on a gas chromatographic method for the quantitative determination of residual solvents in steroids. Eight experimental variables or factors which were expected to influence the quantitative results were selected. These factors were divided into two independent groups, i.e. four factors related to the injection process and four factors related to separation and detection. In order to determine interaction between factors and quadratic effects, a central composite design was selected for the set-up of the experiments. Because in the method an internal standard is used, relative peak area was used as response. A deviation of up to 2.5% per factor for the quantitative results was regarded as acceptable. Other responses studied are related to the system suitability. Observed main, quadratic and interaction effects were translated into rugged intervals of the experimental variables by graphical presentation. It was found that besides main effects significant interaction effects were present, for example between the temperature of the injector and the split-flow. Interaction effects can easily result in the reduction of the rugged intervals by a factor of 2. The calculated rugged intervals were compared with the precision of the instrument or factor settings in order to estimate the ruggedness of the factors. Eventually, the maximum effect of the variation in the instrument settings on the quantitative results regarding the precision of the factor settings was found to be only 2.2%. Overall, the method proved to be rugged for most factors, except for the split-flow of the injector for which the method was only rugged to a limited extent.
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 363-365 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Light hydrocarbons ; Stabilized crude oil ; Capillary guard column
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper reports a quick, and simple method for quantitative determination of C2 to C6 hydrocarbons in stabilized crude oil without using a back flush system. A mixture of crude oil and internal standard is injected into a GC equipped with a 6 meter length of fused silica capillary as a guard column. The light hydrocarbons are separated individually up to the last peak of the hexane group with the heavier components trapped in the guard column. The total analysis time for each sample is 15 minutes. The base line is table for up to 15 consecutive analyses. The guard column and the injector port are then reconditioned by simply heating them for one hour at 300 °C.
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 419-426 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chirasil-Val ; Amino acid enantiomers ; N-Isobutyryl-cysteine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Free D-amino acids (D-AA) were detected as native constituents in juices of vegetables (cultivars of cabbage, tomato, carrot, garlic) and fruits (organes, clementine, grapefruit, lemon, apples, pear, grapes) using gas chromatography (GC) or high-performance liquid chromatography (LC). For investigation by GC, AA enantiomers were converted into theirN(O)-pentafluoropropionyl 2-propyl esters and resolved on a Chirasil-L-Val capillary column. For determination by LC, precolumn derivatization of AA enantiomers usingo-phthaldialdehyde together with the chiral thiolsN-isobutyryl-L-cysteine orN-isobutyryl-D-cysteine and fluorescence detection of the diastereomeric isoindole derivatives, resolvable on an octadecylsilyl stationary phase, were used. D-Ala (0.6–3.8%) was detected in all freshly pressed plant juices usually in the highest relative amounts. Other D-AA detected were D-Asx (0.1–1.9%), D-Glx (0–1.3%), D-Ser (0–1.7%), D-Arg (0.4–1.2%, in grapes, orange, grapefruit, and clementine) and D-Leu and D-Val (1% in cabbage). Absolute amounts of native D-AA were totally 28–57 μmol L−1 in fruit juices, 14.5 μmol L−1 in a tomato juice and 8.5 μmol L−1 in a carrot juice.
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention/structure and retention/temperature ; relationships ; Experimental design ; Enthalpy-entropy compensation ; para-Hydroxy benzoic esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An experimental design has been used to study the effect of column temperature on the gas chromatographic retention of eightpara-hydroxy benzoic esters. A rapid procedure has been developed to reduce the number of experiments compared with traditional methods. Capacity factors were determined and the enthalpy and entropy of transfer from the mobile phase to the stationary phase, ΔHo and ΔSo, respectively, were calculated using the linear Van't Hoff equation (dependence of ln k′ on 1/T). A retention prediction system (RPS) for these compounds in GC was investigated. The molecular connectivity index was used to describe the quantitative structure relationships. Enthalpy — entropy compensation revealed that the mechanism was similar for all the compounds studied.
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 645-648 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Gonadotrophins ; Residual solvents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A headspace, gas chromatographic method for determining residual solvents in pharmaceutical products such as the gonadotrophin powders, has been developed. The method allows the determination of residual solvents by transferring the samples directly into a vial contianing 10 mL 2M sodium chloride; the analysis is carried out by sampling the headspace and separating by capillary gas chromatography using a programmedtemperature vaporizer (PTV) injector. The procedure described is simple, sensitive and reproducible. The lower limit of detection is 20 ppb for ethyl alcohol, 8 ppb for acetone and 0.5 ppb for diethyl ether.
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 224-227 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C1−C4 alkyl tert-butyl ethers ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of C1−C4 alkyl tert-butyl ethers with the general formula (CH3)3C−O−R (R-alkyl substituent) on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices were determined at two temperatures in order to understand their chromatographic behaviour. The respective standard deviations were 0.3 and 0.5 i.u.
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  • 11
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantiomer separation ; Permethylated cyclodextrin stationary phases ; Side-chain fluorinated alkylbenzenes ; Thermodynamic data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of racemic side-chain fluorinated alkylbenzenes and bromofluorinated analogues by capillary gas chromatography using permethylated α, β and γ-cyclodextrins dissolved in polysiloxanes of different polarity as stationary phases is described. The influence of the achiral polysiloxane matrices on the separation of enantiomers is discussed in the light of the results obtained with the different phases. For a part of the tested compounds thermodynamic data are determined which describe the interaction of enantiomers with the stationary phase. The mechanism of separation is discussed on this basis and by comparison with data for structurally similar compounds.
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 210-215 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Correlation chromatography ; Concentration methods ; Polymer dynamic head-space sampling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatography has been used to study the kinetics of evolution of volatiles from polypropylene samples (at 70°C). Correlation chromatography (CC) and the trapping of volatiles on Tenax sorbents and activated charcoal were employed to improve the detector signal. As a reference, the kinetics of gas evolution was studied by making a series of direct single injections of polymer head-space gas on a GC column. The results of trapping differed from those obtained by single injection. However, the data from single injections and CC were in good agreement. The CC method was found to offer far more operator convenience for dynamic head-space analysis than sample trapping, being less subject to operator errors.
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  • 13
    ISSN: 1612-1112
    Keywords: Gas chromatography ; MSD, ECD and NPD ; Non-steroidal anti-inflammatory drugs (NSAIDs) ; Plasma samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The aim of this work was to compare the performance of the MSD, ECD and NPD systems when used for drug assay in biological fluids. As a practical test, six non steroidal anti-inflammatory drugs added to plasma samples were detected and quantified. The analyses were carried out after solvent extraction from an acidic medium and subsequent methylation. The linearity of response was tested for all the detection systems in the range of 1 to 25 ng/ml. Precision and accuracy were determined at 1, 5 and 10 ng/ml. The minimum quantifiable level for the six drugs was about 1 ng/ml with each of the three detection systems.
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  • 14
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 706-712 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Short chain fatty acids ; Intestinal fluids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The quantification of short chain fatty acids in their free form, by gas chromatography, is the method of choice provided that the underivatized acids elute with good peak shape and reproducibility. In biological samples not only the highly polar acids themselves but also deposits of nonvolatile sample components may interact with the column or the packing material. As a result, the peak symmetry of the fatty acids and their reproducibility can become increasingly poor. Reduction of the nonvolatile matrix components by filtration of the sample has been examined in order to achieve direct analysis of the short chain fatty acids in intestinal samples by packed column GC. Membrane filter units (0.8 μm) allow a quick and simple filtration of the samples. This pretreatment reduces the peak tailing and the broadening of the peaks. The method, when applied to different intestinal samples, allowed the quantification of short chain fatty acids in hundreds of samples without derivatization. Good results are obtained at sample concentrations higher than 0.2 mmol l−1 for each acid.
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  • 15
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 38 (1994), S. 22-28 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral separation ; Capillary column ; 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin has been synthesized and used for enantiomer separation in capillary gas chromatography. Experimental results showed that the stationary phase has good enantiomer selectivity toward amino acids, amines, alcohols, diols, epoxides, and lactones,etc. 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin has good thermal stability: the highest recommended temperature isca 170°C.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 38 (1994), S. 93-97 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Adsorption effects ; Terpene alcohols ; Fused-silica capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention indices of 6 selected hydroxy compounds (aliphatic and bicyclic alcohols, phenols) were determined on 2 HP-5 fused-silica, capillary columns with different film thicknesses (0.11 μm and 0.33 μm) at 8 different oven temperatures between 80 and 150°C. For some substances the I-T plot was found to show a minimum which cannot be explained by the common retention-index temperature-dependence in gas-liquid chromatography. This result is discussed in terms of adsorption at the liquid-solid interface of the capillary column.
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  • 17
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid modified adsorption capillary columns ; Polar compound analysis ; Aqueous solution analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of graphite layer open tubular (GLOT) columns is described together with their application to the analysis of priority pollutants and polar compounds such as alcohols, free carboxylic acids, aliphatic amines and phenols at the sub-nanogram level. A specific application of GLOT columns is for the direct analysis of aqueous solutions avoiding solvent extraction procedures. Several chromatograms of critical separations are reported together with calibration curves. A study of the reproducibility of column preparation is reported in terms of the standard deviation of the capacity ratio and of the minimum HETP obtained.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Porous polymer stationary phase ; Selectivity studies
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The behaviour of GC columns packed with the copolymer of methacrylic ester of p,p'-dihydroxydiphenylpropane diglicydyl ether and divinylbenzene was studied. Selectivity studies were made for three polymer samples of different molar ratio of monomers. To determine the selectivities of these copolymers retention indices for seven test compounds in comparison to those obtained on Porapak Q are calculated. Additionally, the efficiency of porous polymer purification was studied by a SFE-GC-MS technique.
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  • 19
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Correlation chromatography ; Simulation model ; Adsorption effects ; Separation improvement
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Experiments and simulations prove that correlation chromatography can greatly reduce the disadvantage of a non-linear response of the chromatographic column. A factor that has been accepted as being an important source of error in correlation or multiplex chromatography, has been shown not to be. Separations affected, improve dramatically when correlation chromatography is used, and a substantial amount of correlation noise only arises when there is a large difference in separation between a conventional chromatogram and a correlogram. A model has been developed for simulating these nonlinearities. It is shown that, especially for correlation chromatography, the simulation results match the practical measurements very well.
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  • 20
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    Electronic Resource
    Springer
    Chromatographia 38 (1994), S. 304-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detector ; Theoretical model of ECD
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper reports a theoretical model of the ECD detector. The model presented here can be used to examine the influence of pulse parameters on the current and signal characteristics of the detector. On the basis of this model it was found that a space charge is created in the detector when it is supplied with pulse voltage. Due to the electric potential generated by the space charge, in the time between the pulses the electrons and negative ions move towards the detector electrodes. The ionization current of the detector is the sum of the electron current flowing to the anode under the influence of the supplied pulse voltage and the current flowing under the space charge potential in the time between the pulses. It was also found that the detector signal is the sum of the differences between those two currents caused by introducing the sample molecules to the detector. The model was tested for a detector with different electrode configurations which worked at temperature of 300 K or 573 K and which was supplied with nitrogen or Ar+10% CH4 as the carrier gas.
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  • 21
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Morpholine ; Hydrazine ; Boiler feed water and steam condensates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hydrazine, an oxygen scavenger in boiler water, was derivatised to the corresponding acetone azine and determined at the ng ml−1 level by gas chromatography. Morpholine, a corrosion inhibitor used in steam boilers, was estimated either directly (if 〉2.0 μg ml−1) or by quantitative preconcentration (0.1 ng – 2.0 μg ml−1). To obtain symmetrical peaks for these amines, the column packing was coated with KOH. Use of a nitrogen-specific detector improved accuracy of estimation of hydrazine and morpholine, giving a RSD of 1.9–3.6%. Chromatographic analysis of these amines in boiler feed water and steam condensate samples collected from boilers servicing a petroleum refinery is described. Environmental safety regulations calls for monitoring of hydrazine and the methods developed can easily be adapted for this purpose.
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  • 22
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    Springer
    Chromatographia 38 (1994), S. 475-478 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Phenolic acids ; Olive and elm tree tissues ; Soil phenolics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the separation of phenolic acids along with shikimic and quinic acids by means of capillary gas chromatography is described and discussed. The method involves the previous derivatization of the acids to trimethylsilyl derivatives and it has been applied to the separation of acids extracted from olive leaves and roots, elm leaves and a soil A horizon. Quite good results were achieved both from qualitative and quantitative points of view. Qualitative differences have been pointed out in the phenolic acid composition of two olive cultivars and between leaves and roots of the same cultivar; also two elm species can be discriminated on the basis of the phenolic acid content.
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  • 23
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid-liquid extraction ; Supercritical fluid extraction ; Pesticides ; Freeze-dried water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The stability of freeze-dried water samples spiked with eight agrochemicals (atrazine, simazine, linuron, carbaryl, propanil, fenitrothion, parathion and fenamiphos) were examined to evaluate their suitability as candidate reference materials for their determination in water samples. In addition, two different extraction procedures, liquid-liquid and supercritical fluid extraction, were compared for the isolation and trace enrichment of target analytes from freeze-dried water samples. Final analytical determinations were by gas chromatography-nitrogen phosphorus detection and electronic impact mass spectrometry, and by liquid chromatography-diode array detection. The whole methodology developed in this paper permitted the determination of pesticides spiked in water at levels varying from 0.03 to 6.9 μg L−1.
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  • 24
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Adsorption and partition columns in series ; Molecular sieves ; Isomers of benzene homologs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibility of using short gas chromatographic columns packed with different molecular sieves (silicalite and aluminophosphates), showing definite selectivity to para-isomeric compounds, in series with columns containing a liquid stationary phase was investigated. The molecular sieves were of different origin, while 1,2,3-tris (2-cyanoethoxy)propane (TCEP) and polyethylene glycol adipate (PEGA) were used as the liquid stationary phase. Ortho-, meta- and para-isomers of xylene, chlorotoluene and dichlorobenzene were chromatographed on these columns. It is shown that the best separation is obtained on a combined column with silicalite containing pure silica gel as the molecular sieve, and 10% PEGA as the liquid phase. Molecular sieves of aluminophosphate origin show only weak selectivity toward the para isomers.
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  • 25
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    Chromatographia 38 (1994), S. 624-628 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ion-trap detection ; Nitriles ; Cerelas ; Perfluoroacylation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Bromoxynil and ioxynil have been determined inplants and soil by gas chromatography. These herbicides are extracted from soil samples with methylene chloride at acidic pH. Plant samples are extracted with a basic acqueous solution and extracts purified by solvent partitioning. Herbicide residues are submitted to perfluoroacylation prior to GC separation. These compoiunds are determined by ion-trap detection with single ion monitoring; N-(3-chloro-4 methyl-phenyl_ perfluoropropyl amide is used as internal standard. The detection limit of the method is near 0.001 μg g−1 for the samples studied. The proposed methods are sensitive and reproducible enough to allow determination of these herbicides at residue levels in plants and soil.
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  • 26
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitrogen phosphorus detection ; Atrazine and simazine ; Freeze-dried water analysis ; ELISA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The determination of atrazine in freeze-dried water samples containing simazine, 0.6% glycine as stabilizer and other pesticides has been compared using three different techniques: (i) direct rapid-magnetic particlebased ELISA, (ii) dichloromethane liquid-liquid extraction (LLE) and Florisil column clean-up prior to ELISA determination and (iii) LLE, Florisil column clean-up and gas chroamtography with nitrogen phosphorus detection (GC-NPD). The methodology developed in this paper has shown the advantages of the introduction of a clean-up step prior to ELISA determination and its correlation with GC-NPD determinations. Atrazine could be determined at levels between 0.1 to 5 μg l−1 in water smaples using the different methods described in this paper. The crossreactivity problems found in the ELISA test associated with the presence of simazine are also discussed.
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  • 27
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    Chromatographia 39 (1994), S. 11-14 
    ISSN: 1612-1112
    Keywords: Supercritical fluid extraction (SFE) ; Gas chromatography ; Pesticide residues ; Oxadixyl
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This work describes the study of a degradation curve of Oxadixyl in field-treated potato and tomato samples. The residues were extracted using classical and supercritical fluid (SFE) extraction methods and analyzed by HRGC/ECD. The extraction techniques were compared and the results indicate the advantages of using SFE as an alternative method for pesticide analyses in these samples.
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  • 28
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    Chromatographia 39 (1994), S. 71-73 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Spectinomycin ; Silylation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic assay for spectinomycin hydrochloride is described. The method is based on that prescribed by the United States Pharmacopeia (USP XXII). The method involves silylation of spectinomycin hydrochloride; phenazone is used as an internal standard. Spectinomycin and phenazone have adequate stability under the prescribed conditions. The stationary phase is 3% OV-17 on Gaschrom Q 100–120 mesh. The selectivity of the proposed method is better than that of the GLC method described in the USP XXII.
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  • 29
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Priority pollutants ; EPA methods ; Unleaded gasoline ; Volatile organochlorine compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The complete separation of the sixty volatile organochlorine (VOC) priority pollutants has been achieved by coupling two different liquid-modified adsorption chromatography columns. Two temperature programs were used to obtain the complete separation in a relatively short analysis time. Detection was by FID alone
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  • 30
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pentachlorophenol residues ; Off-flavours ; Wines and corks ; Electrolytic conductivity detector/mass spectrometry ; detectors
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic methodology with selective detection is presented for the analysis in wines and corks of pentachlorophenol residues, which are suspected to be the most likely precursors of some off-flavours described in several wine samples. After derivatisation, pentachlorophenol acetate residues were monitored by electrolytic conductivity detection and/or mass spectrometric detection in the selective ion mode at m/z 264 and 266. Recoveries varied from 80 to 96% for wine samples fortified with 5 to 100 μg l−1 and from 83 to 91% for corks (fortified at 25 to 100 μg kg−1). The proposed methodology allowed for a determination limit of μg l−1 for wine and 10 μg kg−1 for corks.
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  • 31
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    Chromatographia 38 (1994), S. 151-157 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C5−C12 hydrocarbons in air ; Cryogenic focussing ; Thermal desorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A homemade cryogenic system derived from readily available material is described, illustrating its usage as an accessory for adsorption/thermal desorption chromatography. A small Chromsorb-W-HP packing (1 cm) was introduced into a deactivated precolumn as a cryofocussing, preconcentrating unit. This was able to retain the analyte which had been thermally desorpted from a Tenax TA sampling tube at a relatively higher temperature (−80°C∼−90°C), with the analyte also reinjected on the analytical column in a relatively narrow band. Average overall recoveries for 24 hydrocarbons tested were 97.5%. Cryofocussing enhanced sensitivity and improved resolution. Field studies at a petroleum industry site were carried out and the accessory proved to be useful for complex C5−C12 hydrocarbon analysis in ambient air.
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  • 32
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral phases ; Phenylalanine tetraamides ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A wide series of L-phenylalanine tetraamide selectors (Phe-n-O-TA) have been synthesized and used as stationary phases for chiral resolution of D,L-amino acids by capillary gas chromatography. The influence of length and polarity of the oxaalkanoyl bridge spacing the diamide chains of the selectors and the effects of steric hindrance on separating power were investigated. The characteristics of the chiral columns and the separation factors of D,L-n-butyl-N-trifluoroacetyl amino esters are reported.
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  • 33
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Reversed-flow technique ; Absorption rate ; Air pollutants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple chromatographic method is developed to determine the rate constant for expulsion of an air pollutant from water or its diffusion parameter in the liquid, the rate constant for chemical reaction of the pollutant with water, its mass transfer coefficient in the liquid, and the partition coefficient between liquid water and air. From these physicochemical parameters, the absorption rate by sea water and, therefore, the depletion rate of a polluting substance from the air can be calculated, together with the equilibrium state of this absorption. The method has been applied to nitrogen dioxide being absorbed by triple-distilled water and by sea water, at various temperatures. From the temperature variation of the reaction rate constant and of the partition coefficient, the activation energy for the reaction and the differential heat of solution were determined.
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  • 34
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase characterization ; Principal component analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this study, several new stationary phases were characterized by principal component analysis. Fourteen new stationary phases, including substituted phenyl and oligoethyleneoxide functionalities on polysiloxane polymers, were tested and compared to three well known stationary phases. The main features of these phases were studied using a series of test solutes of varying chemical characteristics representing the data set for principal component analysis. Two principal compounds were found to account for 99.20% of the variance (the first accounted for 94.96% and the second for 4.24%). The data were represented as a two-dimensional map for visual representation of the characteristics of these stationary phases. The first principal component represented a selectivity based on polarity (r2=0.998), while the second showed Lewis acid-base characteristics of the phases. Polarizable and amphoteric characteristics of these phases also became evident using this evaluation method.
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  • 35
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    Chromatographia 38 (1994), S. 595-598 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral / enantiomeric separation ; Amphetamine ; Methamphetamine ; Cyclodextrin-derivatized phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Enantiomeric separation of amphetamine and methamphetamine as achiral derivatives on 2,6-di-O-pentyl-3-O-trifluoroacetyl-β-cyclodextrin, 2,6-di-O-pentyl-3-O-trifluoroacetyl-γ-cyclodextrin and 2,6-di-O-pentyl-3-O-propionyl-γ-cyclodextrin stationary phase in capillary gas chromatography is described. Trifluoroacetic anhydride and acetic anhydride were used as derivatizing reagents. Excellent precision was obtained for concentrations down to 0.1% / e.e. On 2,6-di-O-pentyl-3-O-propionyl-γ-cyclodextrin the elution order of R,S-amphetamine was reversed when the derivatizing reagent was changed but could not be reversed on any of the other phase types.
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  • 36
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    Chromatographia 38 (1994), S. 679-688 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phases ; Phase constants ; Explanatory coefficients
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Explanatory phase coefficients according to Abraham et al. are calculated from McReynolds index differences and the phase constant B. The retention expression (log Vg)−A=BI/100 connects specific retention volumes and retention indices. McReynolds phase constants and Abrahams explanatory coefficients can be used with similar accuracy for the prediction of relative retention data and for the characterization of stationary phases in gas chromatography. The application of polarity constants for the characterization of stationary phases is discussed.
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  • 37
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    Chromatographia 38 (1994), S. 689-693 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantioselectivity ; GC-MS ; GC-GC-MS ; Pinus peuce ; Monoterpenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Needles of the Macedonian Pine,Pinus peuce Griseb., a conifer growing in the Balkan mountains, were extracted by a Likens-Nickerson simultaneous distillation-solvent extraction device. The components of this essential oil were identified by the retention times obtained on two columns differing in polarity and by GC-MS. Because of the complex nature of such plant extracts, a multidimensional GC method for enantiomer analysis, using a non-chiral pre-column and a chiral main column has been developed. The enantiomeric ratios of five monoterpene hydrocarbons were estimated by GC-GC and GC-GC-MS.
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  • 38
    ISSN: 1612-1112
    Keywords: Gas chromatography ; PTV injection system ; Aqueous samples ; Pesticides ; Breakthrough volumes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A GC method is described for the determination of pollutants in aqueous samples by direct enrichment out of large sample volumes in a PTV injector. The vaporized water is eliminated through the split vent and the analytes are concentrated on an adsorbent inside the insert of the PTV. For the selection of suitable adsorbents, breakthrough volumes of selected pesticides and nitroaromatics on Tenax TA, Tenax GR, Chemipack C18 and graphitized carbon blacks have been determined by experiment. The determination of the breakthrough volumes was carried out directly in the PTV insert. Tenax TA proved to be the best sorbent with regard to the breakthrough volumes and its inertness to the analytes to be determined. As the result of the investigations, 500 μl of aqueous standard solutions of pesticides and nitroaromatics (concn.=0.02 ... 2 μg/l) were analyzed with an average relative standard deviation of 10%. The procedure was successfully applied for the analysis of real samples.
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  • 39
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary Phase and solute polarity ; Molecular structural coefficients ; Retention index ; Takács equation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Molecular structural coefficients, Sc, for one hundred solutes have been calculated by means of the Takács equation using retention data obtained with over fifty stationary phases, SP. Employing data of seven SP's (characterized in our laboratories) it was found that the variation of Sc with column temperature was linear for most solutes. With data of n-decane and the ten McReynolds probes on up to fifty SP's of polarity less than RP=72, at 120°C, it was found that the Sc of n-decane and cis-hydrindane decreased slightly with increasing SP polarity, while the Sc of non-alkanes remained constant or increased very little as the SP polarity increased. The points for n-decane fit well to a second order polynomial. Again using a temperature of 120°C, the increments of Sc for solutes belonging to an homologous series were correlated with the polarity of SP's. Reasonably straight lines were obtained for all the chemical functions studied, Sc increasing with increasing SP polarity.
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Particle beam MS detection ; Polycyclic aromatic metabolites ; Biodegradation in water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two liquid chromatography-particle beam mass spectrometry (LC-PBMS) systems have been used for analysis of polycyclic aromatic hydrocarbon metabolites in water samples from a biological decomposition model experiment. The results were compared with those obtained by classical gas chromatography-mass spectrometry. Evaluation of spectral data indicated the presence of six main metabolites; 1H,3H-naphtho [1,8-cd]pyran-1,3-dione, 1-(hydroxymethyl)naphthalene, and 1,2-acenaphthenedione were identified by use of standard substances and spiking experiments. Enrichment of the investigated water samples with online pre-column (C18) concentration, freeze-drying, and solvent extraction led to similar results with only slight differences. The application of microbore separation columns proved to be a promising tool in particle beam LC-MS measurements.
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  • 41
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Curie-point pyrolysis ; Multivariate analysis ; Sodium dodecylbenzene sulfonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Multivariate analysis was used to develop a viable method for determination of sodium dodecylbenzene sulfonate (DBS) by Curie-point pyrolysis gas chromatography. The pyrograms obtained were normalized against a maximum peak area and peak height. Normalized values were used for Quantification IV, which is one of the multivariate analysis methods, to select useful values initially. Then cluster analysis was carried out using both the selected values and their deviations. This method corresponds to qualitative analysis and indicates which data-base is similar to the sample. On the basis of this data-base, calibration data-bases are chosen. Principal component analysis (PCA) was performed using the calibration data-base and a set of sample data simultaneously. The principal component scores and contribution coefficients obtained were used to construct a calibration curve from which the DBS content of the sample was calculated. The results are in fair agreement with theoretical values.
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  • 42
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 411-414 
    ISSN: 0935-6304
    Keywords: Size exclusion chromatography ; Gas chromatography ; Coupled LC-GC ; Cleanup and analysis ; Automation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A fully automated on-line sample cleanup system based on the coupling of size exclusion chromatography to high resolution gas chromatography is described. The transfer technique employed is based on fully concurrent solvent evaporation using a loop-type interface, early vapor exit and co-solvent trapping. Optimization of the LC-GC transfer was done visually via an all-glass oven door. To circumvent the problem of mixing within the injection loop, an adaptation was made to the standard loop-type interface. The determination of a series of additives in a polymer matrix is presented as one example of the vast range of applications opened up by this technique.
    Additional Material: 6 Ill.
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  • 43
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 457-462 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Flame photometric detector ; Pyrolyzer ; Sulfur boiling point distribution ; Light cycle oils ; Exponential dilution flask ; Low sulfur diesel ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed to determine the boiling point distribution of sulfur compounds in light cycle oils (LCO'S). The method chosen for this analysis was GC with a flame photometric detector (FPD) and pyrolyzer. Tests were carried out to evaluate the recovery efficiency, repeatability, and accuracy of the method. Repeatabilities within 2% were obtained. The recovery of benzothiophenes and dibenzothiophenes was close to 100%; this was important because these are the major sulfur components in LCO's. No hydrocarbon or solvent interferences were observed with the use of the pyrolyzer, even for a 95% solvent level. Comparison with results from other techniques showed that the method accurately determined the levels of sulfur compounds in the LCO boiling point range.
    Additional Material: 10 Ill.
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  • 44
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection (AED) ; Programmed temperature vaporization (PTV) ; Nitro musks ; Human adipose tissue ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Atomic emission detection (AED) has been successfully applied to the determination of nitro musks in the fat of human adipose tissue by gas chromatography at trace concentration levels. Element specific detection with the AED combined with a clean-up procedure for nonpolar substances makes target screening analysis for lipophilic nitro aromatic compounds possible for the first time. The lack of sensitivity, especially in the AED nitrogen and oxygen trace, was compensated by higher concentration of the extracts and injection of larger sample volumes performed by cold programmed temperature vaporization (PTV) in the solvent split mode. The combination of the superior quantification properties of the atomic emission detector with large sample volume introduction makes the quantification of nitro musks down to the ppb level possible. All five nitro musks investigated exhibit linear dynamic ranges going down close to instrumental limits of detection. Moreover, organochlorine compounds could be sensitively detected in the same sample extract by the AED chlorine trace without any interferences from coeluting matrix compounds.
    Additional Material: 7 Ill.
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  • 45
    ISSN: 1432-0738
    Keywords: Pigment Yellow 17 ; 3,3′-Dichlorobenzidine ; Biotransformation ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Rats were exposed by inhalation to the technically highest administrable concentration of 230 mg Pigment Yellow 17/m3 air for 4 h. Inhalability of the dust was guaranteed by a mass-median aerodynamic diameter of 1.0–1.1 μm. For 14 days after exposure, urine and serum samples were analysed for 3,3′-dichlorobenzidine, the parent carcinogenic amine of the test compound. No 3,3′-dichlorobenzidine could be detected either in urine or blood, the detection limit being 5 ng/ml for both media. Based on the results of this study there is no evidence for metabolic cleavage of Pigment Yellow 17 to 3,3′-dichlorobenzidine in the rat.
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  • 46
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    International archives of occupational and environmental health 64 (1993), S. 503-507 
    ISSN: 1432-1246
    Keywords: Biological monitoring ; Carbon disulphide ; Dithiocarbamate ; Gas chromatography ; Mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Blood carbon disulphide (CS2), both free and total, was determined by gas chromatography-mass spectrometry in 112 “normal” subjects and in 20 subjects employed in a dithiocarbamate factory, comprising ten blue-collar workers involved in dithiocarbamate production and ten white-collar office staff. The ten production workers were examined over two workshifts, the first at the beginning of the week (Monday) and the second after an intervening period of at least 1 day. Three blood samples were taken for each shift studied, one prior to starting work, one at the end of the shift and the third 16 h after the end of the shift (on the following morning). The mean CS2 blood levels measured in the 112 normal subjects was 663 ng/l for the free fraction and 3178 ng/l for the total. In 16 blood samples taken from the ten dithiocarbamate factory office workers, the mean free and total CS2 blood levels were 846 and 4140 ng/l, respectively, i.e. not significantly different from those observed in the normal subjects. At the end of the first 8-h shift, the ten dithiocarbamate factory production workers had free and total CS2 values of 1070 and 8471 ng/l, respectively, which were significantly higher than those observed prior to starting work (240 and 4738 ng/l). All the total CS2 levels measured in the shop-floor workers, with the sole exception of the values recorded prior to the start of the Monday shift (4738 ng/l), ranged from 7047 to 8471 ng/l and were significantly higher than those measured in the white-collar staff (4140 ng/l).
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  • 47
    ISSN: 1432-1246
    Keywords: Acrylonitrile ; Adducts ; Biological monitoring ; Gas chromatography ; Hemoglobin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A new, simple and fast procedure of measuring acrylonitrile (ACN) in ACN derived mercapturic acids such as S-(2-cyanoethyl)-L-cysteine(CyEC), and in hemoglobin (Hb) and plasma protein adducts and urinary metabolites in rats and humans exposed to ACN was developed. ACN in mercapturic acids or proteins was analyzed by capillary gas chromatography (GC) by liberating ACN at a high-temperature in the injector port of GC with or without oxidizing sulfur atoms of the ACN-bound cysteines into sulfoxide form by hydrogen peroxide in vitro. At 350 °C, more than 90% of ACN in authentic CyEC was recovered by this method. Increasing a single ip dose of ACN from 5 to 50 mg/kg produced proportional increases in ACN bound to Hb 24 hr after the treatment. The alkylation of plasma protein with ACN was about 1/10 as low as that of Hb. After repeated daily ip doses of 1–10 mg/kg, ACN in Hb decreased with a half-life of about 9 days. ACN was also detected in the blood of workers exposed to ACN for 1 to 10 years at a Siberian synthetic rubber factory.
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  • 48
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    Chromatographia 35 (1993), S. 33-37 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crown ether polysiloxane phases ; Selectivity mechanisms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The phase recognition mechanism of nine groups of position isomers on four crown ether polysiloxanes, OV-1701 and PEG 20M has been investigsated by measuring various thermodynamic parameters. The high selectivity of crown ether polysiloxane phases is due to hydrogen bonding and the extent of fitting between the analytes and the crown ethe cavity. The effects on selectivity of cavity size, heteroatoms and substituent groups on the crown ether are discussed.
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  • 49
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    Chromatographia 35 (1993), S. 109-110 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention index ; Correlation of data ; Hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic unified retention indices for 43 hydrocarbons (alkanes and cycloalkanes) are given for squalane and OV-101. Comparison of these values and unified retention index increments are presented as linear regression equations with high correlation coefficients and acceptable standard deviations.
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  • 50
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    Chromatographia 35 (1993), S. 237-240 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantioselectivity ; Polysaccharide chiral stationary phase ; Amylose tris(n-butylcarbamate) ; Grob test
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Seven aromatic and alkyl amylose and cellulose carbamates have been tested as chiral stationary phases in gas chromatography. One of them, amylose tris(n-butylcarbamate) can be used for enantiomer separation.
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  • 51
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Retention behavior ; LC silica packing materials ; Silanol groups
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention of cyclohexane and benzene on microcolumns packed with silica-based materials for liquid chromatography has been investigated to elucidate the relationship with the surface properties of the packing materials. Differences in capacity factors (Δk′) for these two hydrocarbons were related to the surface area of the packing materials. For untreated silica gels, the Δk′ value increased with increasing total surface area of the column employed and measurement of Δk′ for chemically-bonded stationary phases allowed estimation of accessible residual silanol groups.
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  • 52
    ISSN: 1432-2285
    Keywords: Abies alba ; Abscisic acid ; Damage ; Gas chromatography ; Needles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary The amount of abscisic acid (ABA) in needles of silver fir from a natural location was investigated with regard to position in the crown, damage, seasonal variation, and needle age. Because of problems of quantification of ABA in coniferous needles, which contain numerous secondary plant products, a method for reliable determination of both isomers cis-trans-ABA (c-ABA) and transtrans-ABA (t-ABA) was developed. By means of gas chromatography (GC) using an electron capture detector (BCD) and a programmed temperature vaporizer (PTV) injector complete separation of both compounds was achieved. Two different pairs of fir were investigated — in each case a damaged and a healthy tree. Needles from both trees from the first and the second pair collected in September contained 500–1100 ng c-ABA/g fresh weight (FW), and the concentrations of t-ABA varied from 400 to 700 ng/g FW. Investigations from the second pair show highest amounts of 2900 ng/g Fw c-ABA and 1800 ng/g FW of t-ABA in May and June. For the first pair a higher c-ABA content was found in needles from the top of the crown than in those from the middle and the base. This difference could not be confirmed in the analysis of the second pair. Because of the strong natural deviation no statistically significant difference between the healthy and the damaged tree was found. The first pair of firs examined showed a higher t-ABA concentration than the second one. In this case the highest amount was found in the top of the crown. Methodical mistakes during the clean-up procedure and in quantification by gas chromatography could be excluded. The presence of c- and t-ABA in the purified extract was corroborated by mass spectrometry. With regard to the seasonal variation both isomers of ABA show an unequivocal trend. The maximum concentration is achieved in May to June, whereas the content is minimal in August/September. In any case the level of t-ABA is lower than that of c-ABA. No correlation between the amount of ABA and the needle age could be established.
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  • 53
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    Chromatographia 35 (1993), S. 503-505 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silanol terminated Chirasil-Val ; Cross-linking with polyfunctional silanes ; Enantiomer separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the immobilization of Chirasil-Val has been studied based on the cross-linking which takes place between terminal silanols of Chirasil-Val and polyfunctional silanes. A leached, dehydrated and tetramethoxysilane-treated glass capillary coated with silanol terminated Chirasil-Val containing 5% tetraacetoxysilane as a cross-linking agent showed a maximum extractability of 15% without any loss of chirality.
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  • 54
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    Chromatographia 36 (1993), S. 187-190 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid-phase extraction disks ; Pesticides ; Soil analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A systematic study comparing the methodology and analytical results obtained in an investigation of seven pesticide residues (Molinate, Atrazine, Carbofuran, Pirimicarb, Prometryn, Malathion and Tetrachlorvinphos) in soil samples is reported. Solid-phase extraction (SPE) using glass columns and 47 mm disks of octyl and octadecyl-bonded silica was used in the pesticide analysis. The best extraction efficiency and clearest extracts are obtained with C8 disks. The analyses were carried out by capillary gas chromatography with nitrogen and phosphorus detection. Recovery experiments were performed at ppb levels in spiked soil samples. The average recoveries of the compounds were 53–77%. Detection limits are between 5 and 30 ng g−1 based on 5 g moist soil sample. The method was validated by comparing it with conventional liquid-liquid extraction.
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  • 55
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; PTV-System ; Ethephon in drinking water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An indirect GC method is described for the determination of Ethephon in drinking water on the basis of the headspace analysis of the ethylene formed from Ethephon. In order to reach the necessary detection limit, the entire volume of the static headspace distribution is transferred into a cold injection system (CIS). There, the ethylene is adsorbed on Carbosieve SIII at 10°C and, subsequently, desorbed at 300 °C. The water vapour included in the headspace is completely eliminated through the splitting system. By means of this technique, a detection limit of 0.05 μg/l water was reached.
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  • 56
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crown ether polysiloxane phases ; Capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two crown ethers, di(tert-butylbenzo)-propyl-15-crown-5 polysiloxane (PSO-DTB-15C5) and dibenzo-propyl-15-crown-5 polysiloxane (PSO-DB-15C5) have been synthesized and coated onto fused-silica capillary columns. The chromatographic characteristics, including column efficiency, polarity, phase transition temperature, operating temperature range and selectivity, were studied. Excellent selectivity was obtained for the separation of polar position isomers, especially phenol and dinitrotoluene isomers. The separation mechanism is discussed.
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  • 57
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    Chromatographia 37 (1993), S. 399-401 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Viscosity ; Carrier gases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Equations are derived for viscosities of H2, He, N2 and Ar for use at chromatographic temperatures which are accurate to within 0.3% for H2, and 0.1% for the other gases. The effect of pressure is usually negligible but may increase the viscosity of N2 or Ar by as much as 0.5% at 25°C or lower and 5 atm or higher.
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  • 58
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Inverse gas chromatography ; Poly(ethylene glycol) 20M ; Retention mechanisms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of poly(ethylene glycol) 20M (PEG 20M) coated on the hydroxylated surface of Chromaton N AW were investigated by inverse gas chromatography. It was found that the solid form of PEG 20M exhibits partition as the retention mechanism even below its melting range. The contribution of adsorption to the specific retention volume was also determined. It was demonstrated that inverse gas chromatography establishes the existence of a polymer surface layer but precise determination of its thickness is difficult. The limitation of the applicability of inverse gas chromatography results from the structure of the investigated surface layer which is thin and not coherent so that solute molecules can penetrate it.
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  • 59
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Equilibrium headspace sampling ; Partition coefficient determination ; Theory of chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The new phase ratio variation method is described which represents a convenient way for the determination of gas-liquid partition coefficients for practical purposes, utilizing equilibrium headspace-gas chromatography (EHS-GC). This method is based on the relationship between reciprocal peak area and the phase ratio in the vial containing the sample solution; it involves regression analysis of the EHS-GC measurements of a number of sample vials containing the same sample solution but with a wide variation of phase ratios. Examples are given for both aqueous systems and systems consisting of a stationary (liquid) phase used as the solvent; comparison of the measured values with results obtained by other methods shows satisfactory agreement. A critical discussion of the conditions influencing the accuracy of the analytical results is given.
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  • 60
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    Chromatographia 35 (1993), S. 290-294 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase extraction ; Organochloride pesticides ; Water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatography of chlorinated pesticides in water is carried out after adsorption of a 50 mL sample using a cartridge containing 100 mg CN-bonded porous silica and extraction with 500 μL pentane. The average recovery for eight organochloride pesticides at 1 ppb was 〉95%. The procedure described is simple, selective and reproducible.
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  • 61
    ISSN: 1612-1112
    Keywords: Supercritical fluid chromatography ; Gas chromatography ; High speed analysis ; Thermal desorption ; Two dimensional analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A two-dimensional supercritical fluid-gas chromatography system was constructed and evaluated. A 50-μm i.d. capillary column coated with a 50 % cyanopropyl polysilixane stationary phase was used as the firstdimensional column. Group-type separations of polycyclic aromatic hydrocarbons, based on the number of aromatic rings, were achieved using this column under SFC conditions. A 25-μm i.d. liquid crystal column was used as the second-dimensional column under GC conditions. The effluent from the first column (SFC) was received continuously by the second column (GC) through a thermal desorption modulator. The thermal desorption modulator (prepared at the head of the second column) generated a series of concentration pulses from the first column effluent. These concentration pulses served as injections to the second column, and were developed into a corresponding series of high-speed chromatograms. Grouptype sample bands from the first column were separated into individual components on the second column. All sample substances passed through both columns to generate two sets of retention data, which could be used for more accurate compound identification.
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  • 62
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Mass spectrometry ; β-agonists
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Different chromatography — mass spectrometry techniques for the analysis of β-agonists have been compared. Gas chromatography — mass spectrometry (electron impact) has been used, as also has liquid chromatography coupled to the mass spectrometer by either thermospray or electrospray interfaces. The results obtained by the three method were compared in terms of sensitivity, selectivity, and richness of information provided by the analysis. It was found that using electrospray ionization, very powerful analysis could be achieved with high sensitivity, thus providing significant potential for the analysis of β-agonists.
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  • 63
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused silica open tubular columns ; Serial coupled columns ; Phase ratio optimization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary There are a number of parameters which have to be chosen depending on the analysis being done in gas chromatography. While the choice of stationary phase material is based on the solutes to be separated, the thickness is dependent on the concentration and the volatility of the components to be analyzed. This study undertakes a coupled column phase ratio optimization by connecting a short piece of a particular column prior to a normal length of an analytical column. Various columns of different dimensions (phase ratio), but of the same stationary phase material (methyl silicone), are coupled together by a deactivated glass press-fit connector, and the efficiency and capacity are measured. The coupling of fused silica open tubular columns is optimized in efficiency by matching or decreasing the phase ratio of successive columns. Capacity optimization is accomplished by increasing the phase ratio of consecutive columns. Capacity and efficiency optimization are opposing each other; therefore, if some efficiency can be sacrificed a substantial increase in capacity is possible.
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  • 64
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    Chromatographia 37 (1993), S. 105-106 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Occupational hygiene analysis ; Epichlorohydrin in air ; Trace analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method has been developed for the determination of trace amounts of epichlorohydrin in workplace atmospheres. Collection is peroormed in two bubblers in series both containing dichloromethane. Optimum conditions for sampling and analysis have been established. The lower limit of determination is 0.05 μg/mL with an RSD of ±5%.
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  • 65
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    Chromatographia 37 (1993), S. 250-258 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention data ; Stationary phases ; Phase constants ; Linear free energy relationships
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes and retention indices for selected compounds can be predicted from different sets of stationary phase constants by multiple regression. Errors in the corresponding calculated retention times are between 5 and 15%. Intercept (A) and slope (B) values are given for 72 McReynolds stationary phases. The A value can be predicted from the retention index of benzene with a standard deviation of 9%.
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  • 66
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pesticides in groundwater ; Solvent extraction ; Multiresidue analysis ; Selective detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple multi-residue procedure has been developed and applied to the analysis of pesticides in groundwater samples from the Comunidad Valenciana, a predominantly agricultural area on the Mediterranean coast of Spain. The procedure includes a liquid-liquid extraction, after addition of NaCl on the samples, and a subsequent analysis by capillary gas chromatography using a dual detection system with electron capture and nitrogen-phosphorous detectors. This allows the determination of more than 30 compounds (organophosphorous, organochlorine and pyrethroid pesticides) at the low ppb (μg l−1) levels. Detection limits obtained varied between 0.01 μg l−1 (lindane, fonofos) and 0.5 μg l−1 (cypermethrin). An additional injection of the sample extracts into a gas chromatograph equipped with a column of different polarity and electron capture detector is used for the confirmation of chromatographic peaks. The recommended procedure has been applied to 66 ground water samples. Pesticides, including organophosphorus and organochlorine compounds were detected in 31 of them, in levels ranging from 0.02 to 0.7 μg l−1.
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  • 67
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; Adsorption effects ; n-Tetradecenes ; n-Tetradecynes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The correction of the reproducibility of retention indices on polar capillary columns with different film thickness, using more polar reference standards instead ofn-alkanes, was investigated. It was found that the replacement ofn-alkanes by 1-alkenes, 3-alkynes and n-alkylbenzenes as standards significantly improves the reproducibility of retention indices and diminishes their temperature increments forn-alkanes,n-alkynes and arenes on PEG 20M columns.
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  • 68
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    Chromatographia 37 (1993), S. 546-548 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Methyl methacrylate monomer ; Contact lens
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified gas chromatographic method is described for the determination of free monomer in contact lenses, irrespective of the method of production. It thus becomes possible to assess very quickly the conformity of such lenses with hygiene regulations. This method allows direct supervision of production or determination of the quality of a product of unknown origin in only 15 min. Production tests of new polymerization initiators, reactors for polymerization, etc. can also be carried out.
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  • 69
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    Chromatographia 35 (1993), S. 160-166 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Neural networks ; Classification ; Pattern recognition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Artificial Neural Networks are proposed for the classification of vegetable oils submitted to gas chromatography analysis through their FAME profiles. Three important neural networks are evaluated here: the Hopfield model as a content-addressable memory (CAM), the Hamming model and the multi-layer perceptron. A brief description of these nets is first presented and further implemented for the classification of known vegetable oils. After the learning step, unknown samples are presented to the nets and the identification step performed. The performances of these nets are compared for the recognition of popular vegetable oils, including several edible oils.
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  • 70
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass spectrometry ; Atomic emission spectroscopy ; Pulp mill effluents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Three chlorinated dimethyl sulfones and five chlorinated thiophenes have been identified in the alkaline extraction liquor from a bleach plant by gas chromatography with atomic emission detection (GC-AED) and with mass spectrometry (GC-MS). The information on elemental content obtained by GC-AED enabled a rapid screening of the sulfur compounds and provided important structural information complementary to the mass spectral data. Quantitation was accomplished by GC-AED based on universal calibration.
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  • 71
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    Chromatographia 35 (1993), S. 209-215 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas chromatography-mass spectrometry ; Tagetes ; Plant volatiles ; Extractions ; Natural insecticides ; Mosquitos
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Volatiles from three species of the genustagetes, commonly called marigold have been isolated and characterized. Simultaneous steam distillation extractions (SSDE) produced consistently extracts of higher insecticidal activity than Soxhlet extractions. Methylene chloride was the best solvent. Volatiles isolated from theminutae species showed higher activity than those frompatula anderecta. Comparison of extracts from the flower, foliage and roots of the plant showed that most of the activity is located in the flower. The volatiles are highly effective toward both larvae and adult mosquitoes.
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  • 72
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    Chromatographia 35 (1993), S. 649-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Triglycerides in cheese ; Programme temperature (PTV) injection ; Silica capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid gas chromatographic method for the analysis of triglycerides in cheese on a capillary column with a programmed temperature vaporizer has been developed. Fat were extracted with hexane to dryness. The reproducibility of the method was assessed and the coefficient of variation for the total triglycerides was 2.50%. Recovery of individual triglycerides ranged between 87 to 105%.
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  • 73
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Curie-point pyrolysis ; Multivariate analysis ; Sodium dodecylbenzene sulfonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Multivariate analysis can be applied to quantitative analysis of sodium dodecylbenzene sulfonate (DBS) by pyrolysis gas chromatography. The pyrograms obtained from mixtures of DBS and polyoxyethylene lauryl ether (PEG) were normalized for the peak heights and areas of several internal standards which appeared in every pyrogram, against the characteristics peaks for DBS and PEG. This normalization method gave smaller experimental errors than when using one internal standard. The normalization values were used for cluster analysis unchanged. The values were calculated correlation coefficients and principal component analysis was performed using 11 data base and a set of sample data simultaneously. One calibration curve was calculated from the principal component scores. The DBS content of a sample was obtained from the calibration curve. Calculated values were in fair agreement with theoretical values.
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  • 74
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary column sampling ; Additivity of variance in GC ; Aqueous samples ; PAHs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibility of using capillary columns for both sampling and gas chromatographic analysis of aqueous micropollutants has been studied. Factors influencing gas chromatographic band dispersion of the solute were investigated and a mathematical relationship developed correlating the properties (ID, df) of the capillary columns to the degree of dispersion of adsorbed substances has been derived. The experimental results obtained with aqueous samples are in good agreement with the theoretically forecast data. The method developed allows gas chromatographic dosing of traces of organic substances, reducing inconvenience deriving from excessive sample handling to a minimum. Non-refocusing of the analyte does not, in any significant way, compromise column efficiency for substances that are not very soluble in water.
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  • 75
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Steam distillation ; Phenols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-temperature headspace analysis performed under static conditions above 100°C increases the sensitivity of gas chromatographic determination of volatile phenols in aqueous solutions 20–100 fold and reduces the detection threshold, to 10 μg×1−1. To improve the sensitivity and reduce the threshold still further, preliminary concentration by high-temperature microdistillation at elevated pressure is proposed. A theoretical model of this process has been developed. The possibility of concentrating volatiles by high-temperature microdistillation has been experimentally confirmed.
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  • 76
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fatty acid methyl esters ; Diesel fuel substitute ; Glycerol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A GC method for the determination of free glycerol in vegetable oil methyl esters used as diesel fuel is described. The sample preparation includes dissolving in dimethylformamide, silylation with bistrimethylsilyltrifluoroacetamide (BSTFA) and separation on a methyl silicone capillary column using either FID or MS detection. The recovery was tested using standard samples containing known amounts of glycerol. The results of the analysis of different samples were compared with those obtained by enzymatic determination. The method described offers a far more sensitive and quick determination of free glycerol compared to other methods.
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  • 77
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    Chromatographia 37 (1993), S. 215-217 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention indices ; Dimethylsiloxane stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic, unified retention-indices of 56 alkylbenzenes up to C15 on dimethylsiloxane OV-101 and SE-30 stationary phases are given. These values agree well with the corresponding experimental values used in the statistical treatment of the experimental data.
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  • 78
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    Chromatographia 37 (1993), S. 211-214 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Organic solvents ; Routine analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method for the analysis of organic solvents in chemical products is described. The analysis is performed by the use of a polar column, Supelcowax 10, and a non-polar column CP-Sil-5CB. Samples containing a non-volatile matrix or water were analysed by headspace analysis. The identification of the solvents in a sample, based on GC retention times on one column, is confirmed by GC of the sample on the second column. The method has been found to be suitable for the routine analysis of solvent mixtures.
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  • 79
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    Chromatographia 37 (1993), S. 277-280 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Hydrogenation of 1,5,9-cyclododecatriene ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of the products obtained by the hydrogenation of 1,5,9-cyclododecatriene stereoisomers on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices of cyclododecatrienes, cyclododecadienes, cyclododecenes and cyclododecane were determined at three temperatures. The respective standard deviations were 0.3 and 0.6 i.u. The influence of the polarity of the stationary phases on the chromatographic retention of these cyclic hydrocarbones is discussed.
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  • 80
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    Chromatographia 37 (1993), S. 264-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Temperature programmed ; Peak widths ; Polynomial interpolation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Isothermal chromatographic measurements lead directly to ΔH v o and A (entropy term) of solutes, and three constants of an empirical relationship between peak width and column temperature. From the thermodynamic parameters ΔH v o and A retention temperatures have been computed by means of a theoretical model including temperature dependence of carrier gas viscosity, and subsequently retention times; programmed retention indices have been determined by linear and polynomial interpolations. By substituting the value of the calculated retention temperature in the above-mentioned relationship, peak width at half-height for a linear temperature may be estimated. Predicted retentions correlate with observed data, with a P-value ≤0.01; simulation accuracy is generally 6–10% for peak widths. Retention indices of some organochlorine species, separated on an OV-101 capillary column, may differ by as much as 26 units depending on the method of calculation. Polynomial-calculated indices are more consistent with the retention index scheme, and have smaller standard deviations and better constancy at different heating rates.
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  • 81
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    Chromatographia 35 (1993), S. 339-343 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preconcentration techniques ; Trace gas analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The blanks in preconcentration methods for determining trace amounts of impurities in ultra-pure gases, which include the preconcentration volume of sample gases, carrier gas impurities and atmospheric contamination are discussed and three concentration methods for eliminating blank errors are proposed. These are, the differential volume method by concentrating at the same flow-rate but different times (DVMSF), the differential time method by concentrating the same volumes at different flow-rates (DTMSV) and the differential volume method by concentrating for the same times but different flow-rates (DVMST). DVMST is proposed as the best method for its ability to eliminate all blank errors described. The methods are used to determine trace amounts of Ar+O2 and N2 in ultra-pure hydrogen. Calculations demonstrate that the methods can effectively improve analytical accuracy.
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  • 82
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    Chromatographia 35 (1993), S. 539-542 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystals ; Diffusion coefficients ; Xylenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The molecular diffusion coefficients of xylene isomers have been determined at different temperatures in the three phases (smectic, nematic and isotropic) of 4,4′-bis(heptyloxy)azoxybenzene (BHOAB) by gas chromatography. The results obtained are discussed in terms of molar volume, polarity and length-to-breadth ratio of several isomers. The activation energy of diffusion processes of solutes in the three phases of the liquid crystal has been calculated.
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  • 83
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    Chromatographia 36 (1993), S. 215-217 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polar columns ; Vegetable oils ; Sterols ; Unsaponifiable matter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The analysis of both the total unsaponifiable matter and the sterol fractions in vegetable oils has been performed with a new polar column (TAP, Chrompack). The use of a polar column, which is characterized by high thermal stability, has led to the identification of a greater number of constituents than the use of a nonpolar column (i.e. SE 52, SE 54). The polar column enhances the separation of the main classes of unsaponifiable matter (sterols, 4-methyl sterols and 4,4′-dimethyl sterols). When used for the unsaponifiable and sterol fraction analyses, it offers a powerful tool for characterizing the lipid source.
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  • 84
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    Chromatographia 36 (1993), S. 225-233 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective ionization detectors ; Organic fuelled flames ; Lead, tin, phosphorus, halogens
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The selectivities of two flame-based ionization detectors identified as a Remote FID (RFID) and a Flame Thermionic Ionization Detector (FTID) have been improved by introducing methane as a fuel for the flame. Both the RFID and FTID feature a detector struture in which the ionization polarizer and collector are located several centimeters downstream of an oxygen-rich flame, rather than immediately adjacent to the flame as in a flame ionization detector. The RFID detects long-lived negative ions produced in the flame by the combustion of lead, tin, phosphorus, or silicon compounds. The FTID re-ionizes and detects neutral electronegative products generated by combustion of nitrogen, halogen, or phosphorus compounds. An organic-fuelled RFID can detect 1 pg Pb (Sn, P)/sec with a selectivity of the order of 106 versus hydrocarbons. An organic fuelled FTID is applicable to detection of compounds at nanogram and higher levels. FTID selectivity for PCB compounds in a transformer oil matrix is of the order of 105∶1. The improved selectivity achieved by using an organic-fuelled flame is also applicable to the detection of phospholipid and other non-volatile N, P, or Cl compounds using an FID/FTID detector accessory for a TLC/FID analyser.
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  • 85
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    Chromatographia 37 (1993), S. 51-56 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Halogenated hydrocarbons ; Headspace sampling ; ECD detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Simple sampling and preconcentration technique for the analysis of volatile halogenated hydrocarbons in water is described. For the separation a selective capillary column is used in combination with an ECD. Quantitative data are given.
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  • 86
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detection ; Trichothecenes ; Cereal grain
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various analytical methods developed for trichothecene determination, including TLC, HPLC, GC, supercritical fluid chromatography (SFC) and enzyme immuno assay (EIA) are reviewed. In addition a new method is described for the simultaneous determination of the trichothecene mycotoxins deoxynivalenol (DON), nivalenol (NIV), 3-acetyldeoxynivalenol (3-ADON), diacetoxyscirpenol (DAS), T-2 toxin (T-2), HT-2 toxin (HT-2) and T-2 triol (TRIOL), in Austrian wheat and corn samples by GC-ECD. A clean-up procedure has been developed using a combination of liquid-liquid and liquid-solid extraction. Trichothecenes were detected as their heptafluorobuturyl esters or alternatively as trimethylsilyl ethers (only sensitive for deoxynivalenol and nivalenol) using nandrolone or chloramphenicol as internal standard. Four derivatization techniques using HFBI, HFBA+DMAP on polystyrene, TMSI and TMSI+BSA+TMCS have been studied and the advantages and disadvantages of each are discussed. Quantification of trichothecenes from 10 to 1000 ppb in cereals could be accomplished routinely.
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  • 87
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    Chromatographia 37 (1993), S. 259-263 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Quantitative analysis ; Ethylene oligomer by-products ; n-Alkanes, n-alkenes and 2-alkyl-1-alkenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method using temperature-programmed poly-dimethylsiloxane OV-101 and poly(pheny ether) (5 rings) capillary columns was developed to separate and quantify the reaction by-products in ethylene oligomers. It was found that the content of 2-alkyl-1-alkenes, 2-alkenes and n-alkanes in the C8−C18 α-olefin fractions amounts to 29, 10 and 2.6% respectively.
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  • 88
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    Journal of High Resolution Chromatography 16 (1993), S. 437-440 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Open tubular column ; n-Pentane ; Human breath analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new procedure, requiring expired sample volumes of approximately 2L, has been developed for the quantitative determination of n-pentane in human breath. The methodology capitalizes on the superior resolving power and separating efficiency of the open tubular capillary column and incorporates an effective prechromatographic cryofocusing technique. Molecular sieve is used to simultaneously remove moisture and carbon dioxide from breath samples which are “spiked” with an internal standard to optimize the validity of analysis. Reproducible data for both internal standard spiking (CV = 5.8%) and sample n-pentane level (CV = 3.2%) have been obtained, together with a mean recovery of 104%. Preliminary data show n-pentane levels in normal female subjects (n = 10) to range from 0.62 to 3.16 nmole/L (mean 1.76 nmole/L) and in males (n = 10) from 3.20 to 8.76 nmole/L (mean 5.66 nmole/L).
    Additional Material: 2 Ill.
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  • 89
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    Journal of High Resolution Chromatography 16 (1993), S. 501-503 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Vaporizing injectors ; Matrix effects ; Organophosphorus pesticide residues ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
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  • 90
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    Journal of High Resolution Chromatography 16 (1993), S. 495-500 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Retention index standards ; Benzodiazepines ; Drug screening ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An homologous series of benzodiazepine retention index standards (the R-series) has been synthesized and the gas chromatographic behavior of the series investigated on NB-54 and NB-1701 capillary columns. The compounds were stable, exhibited symmetrical peak shapes, and fairly linear retention behavior was observed on both columns. The series can be coinjected with every sample to enable the high precision analysis of toxicological samples; screening for 20 benzodiazepine drugs was possible in 23 minutes (including cooling). The R-series method was compared with a retention index method based on a series of benzodiazepine drugs as standards and with a method employing relative retention times. The precision of the R-series method was found to be generally better than that of the two other methods in both long- and short-term studies.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 91
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 530-535 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Resolution of enantiomers ; Stereoselectivity ; Chiral stationary phase ; Derivatized cyclodextrin ; Trifluoroacetylated cyclodextrin ; Thermodynamic properties ; Derivatization ; Alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two acyl and three fluoroacyl derivatives of 32 chiral alcohols have been chromatographed on a GC column coated with octakis(2,6-di-O-n-pentyl-3-O-trifluoroacetyl)- γ-cyclodextrin. Significant differences were observed between the stereoselectivity obtained for the derivatives and that for the underivatized alcohols. Of the derivatives, only the fluoroacylated compounds were separated into enantiomers. Derivatization with fluoroacyl groups reversed the elution order for at least some of the analytes. Stereoselectivity towards simple 2- and 3-hydroxy alkanes and their fluoroacyl derivatives was highest for those alcohols with a four-carbon chain attached to the stereogenic center. For longer-chain fluoroacyl derivative groups stereoselectivity was higher for the 2- and 3-hydroxy alkanes. Differences in stereoselectivity towards alcohols with a methyl-branched alkane chain and their fluoroacyl derivatives was related to the distance between the methyl group and the hydroxyl or fluoroacyl groups. Different degrees of saturation in the carbon chain resulted in differences in stereoselectivity. Thermodynamic data calculated for a number of analytes suggest that the alcohols and trifluoroacetate derivatives are interacting with the stationary phase by similar mechanisms. The stereospecific interaction appears to have a hydrogen bonding or dipole-dipole contribution and some form of steric component, depending upon the shape and/or size of the solute.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 92
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 561-564 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Trace analysis ; Solvent effect inlet technique ; Solvent purification ; Solvent storage ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 93
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 539-548 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection ; Pesticide residue analysis ; Multi-residue methods ; Complex foodstuff matrices ; Maximum residue tolerance levels ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The high selectivity of element-specific atomic emission detection has proven suitable for screening analysis of plant foodstuffs for pesticide residues by capillary gas chromatography, especially for those foodstuffs which contain high levels of matrix compounds. The elemental composition of a peak can, furthermore, be examined by looking at the partial emission spectra recorded during a GC run. This instrumental feature prevents false positive signal interpretation as a result of high concentration levels of eluting matrix compounds.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
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  • 94
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 53-55 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Plant extract ; Photochemical degradation ; Insecticides ; Volatile compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 95
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 59-61 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary micropacked columns ; SPE sorbents ; Aliphatic hydrocarbons ; Aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 96
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 188-191 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Thermostable WCOT columns ; PLOT columns ; Stainless steel ; Silicon layer for deactivation ; Simulated distillation ; PNA analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A layer of elemental silicon has been deposited on the surface of stainless steel tubing by means of chemical vapor deposition (CVD). Two kinds of capillary column were prepared from the deactivated tubing: cross-linked, silanol-terminated polydime-thylsiloxane wall coated open tubular (WCOT) columns and molecular sieve 13X porous layer open tubular (PLOT) columns. Unlike fused silica capillary columns, stainless steel WCOT and PLOT columns can be operated at temperatures in excess of 400°C. High temperature simulated distillation has been performed successfully with a macro bore WCOT column and rapid PNA (paraffin, naphthene, and aromatic) analysis with a multidimensional gas solid chromatographic (GSC) system using PLOT columns.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 97
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 379-380 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Natural gas ; Tetrahydrothiophene (THT) ; Odorant ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 98
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    Springer
    Archives of toxicology 66 (1992), S. 298-299 
    ISSN: 1432-0738
    Keywords: 2,4-Dichlorophenol ; Accident ; Fatality ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A case involving an accidental fatality resulting from skin absorption of 2,4-dichlorophenol in a factory is presented. The compound was quantified using gas chromatography after separation on a SP-1240 DA column and detection with flame ionization. Confirmation was obtained with mass spectrometry. Blood concentration was 24.3 mg/l. Other drugs, including ethanol, were not detected.
    Type of Medium: Electronic Resource
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  • 99
    ISSN: 1432-1246
    Keywords: Stereometabolism ; Ethylbenzene exposure ; R- and S-mandelic acid ; Gas chromatography ; Enantiomer separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Ethylbenzene is an important industrial solvent and a key substance in styrene production. Ethylbenzene metabolism leads to the formation of mandelic acid, which occurs in two enantiomeric forms, and phenyl-glyoxylic acid. To decide which enantiomer is preferably formed, 70 urine samples of exposed workers were taken at the end of shifts and — after 3-pentyl ester derivatisation — gas chromatographically analysed. The R/S ratio of mandelic acid enantiomers in urine amounts to 19:1, which means that R-mandelic acid is a major metabolite and S-mandelic acid is one of the minor urinary metabolites of ethylbenzene in man. The R/S ratio is independent of ambient air concentration of ethylbenzene within the investigated range. Compared to an ethylbenzene monoexposure the height of total mandelic acid excretion is decreased in the case of coexposure to other aromatic solvents.
    Type of Medium: Electronic Resource
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  • 100
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 34 (1992), S. 398-410 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Reversed-flow technique ; Catalysis ; Hydrodenitrogenation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Many important parameters of surface catalysed reactions can be determined simultaneously, under nonsteady state conditions using Reversed-Flow Gas Chromatography. A simple, slightly modified gas chromatograph is required. The distorted diffusion bands, obtained experimentally for reactant and product(s), can be analysed mathematically, using simple PC programs, to give the pre-exponential factors and the exponential coefficients of a function consisting of the sum of two-four exponential functions of time. From these, and some geometrical and diffusional characteristics of the reaction cell, the values of adsorption, desorption and reaction rate constants, the overall mass transfer coefficients in the gas and in the solid catalyst, and the adsorption equilibrium constant, for both reactant and product(s) can be calculated. The above parameters were determined at various temperatures and over three catalysts for the hydrodenitrogenation of piperidine ton-pentane, an industrially important hydrotreating process. The results obtained can help to understand the mechanism of reactions on solid surfaces and to confirm experimentally theoretical calculations on adsorption and surface reactions.
    Type of Medium: Electronic Resource
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