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  • 1990-1994  (21,430)
  • 1980-1984  (15,528)
  • Polymer and Materials Science  (36,309)
  • Physics  (2,658)
  • Gas chromatography
  • Nuclear reactions
Material
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Year
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  • 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%).
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 3
    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.
    Type of Medium: Electronic Resource
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  • 4
    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.
    Type of Medium: Electronic Resource
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  • 5
    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.
    Type of Medium: Electronic Resource
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  • 6
    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.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
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  • 9
    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.
    Type of Medium: Electronic Resource
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  • 10
    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.
    Type of Medium: Electronic Resource
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  • 11
    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.
    Type of Medium: Electronic Resource
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  • 12
    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.
    Type of Medium: Electronic Resource
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  • 13
    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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  • 14
    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.
    Type of Medium: Electronic Resource
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  • 15
    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
    Type of Medium: Electronic Resource
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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.
    Type of Medium: Electronic Resource
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  • 17
    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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  • 18
    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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  • 19
    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.
    Type of Medium: Electronic Resource
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  • 20
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 21
    Electronic Resource
    Electronic Resource
    Springer
    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.
    Type of Medium: Electronic Resource
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  • 22
    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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  • 23
    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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  • 24
    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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  • 25
    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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  • 26
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 113-120 
    ISSN: 0887-624X
    Keywords: polyurethane ; chromatography ; stoichiometry ; GPC ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The kinetics of formation of polyurethane prepolymers is studied by an analytical technique which involves reactive quenching of the isocyanate, separation of the oligomeric species by GPC, and measurement by UV absorbance of the quenched moieties. The precision of the kinetic parameters and the ratios of the oligomers are determined. The effect of changes in reactant stoichiometry on the ratio of oligomers is measured and compared to the value predicted by an equation from Flory. Toluene diisocyanate is shown to give fewer high oligomers than predicted, while methylene diphenylene diisocyanate gives nearly the predicted values. Tetramethylxylene diisocyanate gives more high oligomers than predicted, an unexpected but possibly important result. Catalyst is shown to increase the reaction rate of the last by more than 200 times. © 1994 John Wiley & Sons, Inc.
    Additional Material: 3 Ill.
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  • 27
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 159-165 
    ISSN: 0887-624X
    Keywords: 4-hydroxybenzoic acid ; 6-thioxantone-2-carboxylic acid ; copolyesters ; whiskers ; polycondensation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 6-Hydroxythioxanthone-2-carboxylic acid (HTCA) was prepared from commercial dimethylnitroterephthalate via 2-(4'-hydroxythiophenyl) terephthalic acid. HTCA was acetylated and polycondensed in an inert reaction medium at 350 or 400°C. An insoluble and infusible, highly crystalline polyester was obtained, which did not form whisker-like crystals. Furthermore, copolyesters with 4-hydroxybenzoic acid (4-HBA) were synthesized and whiskers were obtained at a molar ratio of 1 : 9 (in favor of 4-HBA). A meltable, nematic copolyester was prepared by cocondensation of silylated 6-acetoxythioxanthone-2-carboxylic acid and silylated 4-acetoxybenzoic acid in bulk. © 1994 John Wiley & Sons, Inc.
    Additional Material: 4 Ill.
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  • 28
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 167-174 
    ISSN: 0887-624X
    Keywords: polyimide molecular composite ; crosslinking ; internal acetylene ; laminate processing ; high modulus ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyimide/polyimide molecular composite (MC) films comprised of a rigid polyimide derived from biphenyltetracarboxylic dianhydride (BPDA) and p-phenylenediamine (PDA) and a flexible polyimide derived from BPDA and bis (3,3'-diaminodiphenyl) acetylene (intA) and/or oxydianiline (ODA) were prepared by blending the polyamic acid solutions in 7 : 3 weight ratio, and then imidizing the blend films. Acetylene content in the flexible polyimide backbone was controlled by the ratio of intA and ODA. Cold-drawing of the blend polyamic acid films, followed by imidization, gives high modulus polyimide/polyimide MC films. The modulus of the MC films increased almost linearly with the draw ratio, reaching 25.5 GPa for the 40% drawn film. Acetylene groups in the flexible polyimide can be thermally cured to crosslink. The onset of exotherm appeared at 340°C on DSC, reaching maximum at 398°C. After the thermal crosslinking, the MC films maintained the high modulus, though elongation became small. Taking advantage of the crosslinkable acetylene units, two MC films were laminated and processed at 400°C for 20 min under 100 kg/cm2 to give a good-quality laminate film. The interface of the two films was strongly bonded through the crosslinking of acetylene groups. Laminate films maintained the high modulus afforded by the cold-drawing. © 1994 John Wiley & Sons, Inc.
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  • 29
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 355-362 
    ISSN: 0887-624X
    Keywords: bisaryloxyencephthalic Acids ; polyaramides ; rigid-rod polymers ; molecular blends ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several 2,5-bisaryloxyterephthalic acids were prepared by a new method, namely arylation of diethyl-2,5-bistrimethylsiloxyterephthalate. Rigid-rod polyaramides were prepared by polycondensation of silylated diamines with a terephthaloylchloride with two diphenylsulfone side chains. Another polyamide was prepared from 2,5-bis(4′-cyanophenoxy) terephthalic acid and 1,4-diaminobenzene. None of these polyaramides is meltable and their solubilities differ largely. A copolymer of 1,4-diaminobenzene and 3,3′-dimethoxybenzidine is soluble in various organic solvents including polar vinyl monomers. © 1994 John Wiley & Sons, Inc.
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  • 30
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 149-158 
    ISSN: 0887-624X
    Keywords: metallocene ; stereoselective catalyst ; propylene polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new silolene-bridged compound, racemic (1,4-butanediyl) silylene-bis (1-η5-in-denyl) dichlorozirconium (1) was synthesized by reacting ZrCl4 with C4H8Si (IndLi)2 in THF. 1 was reacted with trialkylaluminum and then with triphenylcarbenium tetrakis (penta-fluorophenyl) borate (2) to produce in situ the zirconocenium ion (1+). This “constraint geometry” catalyst is exceedingly stereoselective for propylene polymerization at low temperature (Tp = -55°C), producing refluxing n-heptane insoluble isotactic poly(propylene) (i-PP) with a yield of 99.4%, Tm = 164.3°C, δHf = 20.22 cal/g and M̄w = 350 000. It has catalytic activities of 107-108 g PP/(mol Zr · [C3H6] · h) in propylene polymerization at the Tp ranging from -55°C to 70°C, and 108 polymer/(mol Zr · [monomer] · h) in ethylene polymerization. The stereospecificity of 1+ decreases gradually as Tp approaches 20°C. At higher temperatures the catalytic species rapidly loses stereochemical control. Under all experimental conditions 1+ is more stereospecific than the analogous cation derived from rac-dimethylsilylenebis (1-η5-indenyl)dichlorozirconium (4). The variations of polymerization activities in ethylene and in propylene for Tp from -55°C to +70°C indicates a Michaelis Mention kinetics. The zirconocenium-propylene π-complex has a larger insertion rate constant but lower thermal stability than the corresponding ethylene π-complex. This catalyst copolymerizes ethylene and propylene with reactivity ratios of comparable magnitude rE ˜ 4rp. Furthermore, rE.rp ˜ 0.5 indicating random copolymer formation. Both 1 and 4 activated with methylaluminoxane (MAO) exhibit much slower polymerization rates, and, under certain conditions, a lower stereo-selectivity than the corresponding 1+ or 4+ system. © 1994 John Wiley & Sons, Inc.
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  • 31
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 187-191 
    ISSN: 0887-624X
    Keywords: thermal degradation ; polysiloxane ; alternating copolymer ; thermal isomerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 32
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 219-227 
    ISSN: 0887-624X
    Keywords: Polyimidophosphonate ; dihydroxybismide ; phase transfer catalyst ; 31PNMR ; flame retardancy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of dihydroxybisimide monomers and their subsequent polycondensation with dichlorophenylphosphine oxide by use of a phase-transfer catalyst are reported. The monomers were characterized by melting point, elemental analysis, and IR spectroscopy. The polyimidophosphonates were characterized by viscosity measurement, molecular weight determination, elemental analysis, IR, ESCA, 1H-NMR, 31P-NMR, and X-ray diffraction. Thermal stability and glass transition temperature (Tg) of the polymers were evaluated by TGA, DTA, and TMA. These polymers are self-extinguishing and readily soluble in highly polar solvents like DMF, DMSO, DMAC, NMP, HMPA, etc. © 1994 John Wiley & Sons, Inc.
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  • 33
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 605-630 
    ISSN: 0887-624X
    Keywords: free radical ; exit ; emulsion ; polymerization ; model ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The exit or desorption of free radicals from latex particles is an important kinetic process in an emulsion polymerization. This article unites a successful theory of radical absorption (i.e., initiator efficiency), based on propagation in the aqueous phase being the rate determining step for entry of charged free radicals, with a detailed model of radical desorption. The result is a kinetic scheme applicable to true “zero-one” systems (i.e., where entry of a radical into a latex particle already containing a radical results in instantaneous termination), which is still, with a number of generally applicable assumptions, relatively simple. Indeed, in many physically reasonable limits, the kinetic representation reduces to a single rate equation. Specific experimental techniques of particular significance and methods of analysis of kinetic data are detailed and discussed. A methodology for both assessing the applicability of the model and its more probable limits, via use of known rate coefficients and theoretical predictions, is outlined and then applied to the representative monomers, styrene and methyl methacrylate. A detailed application of the theory and illustration of the methodology of model discrimination via experiment is contained in the second article of this series. © 1994 John Wiley & Sons, Inc.
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  • 34
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 675-681 
    ISSN: 0887-624X
    Keywords: nickel ; coupling polymerization ; aromatic dichloride ; tert-butyl-substituted poly (ether ketone) ; de-tert-butylation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: tert-Butyl substituted poly (aryl ether ketone)s with relatively high molecular weights were prepared by the Ni-catalyzed polymerization of tert-butyl substituted aromatic dichlorides containing ether ketone unit. These polymers were amorphous and soluble in common organic solvents, such as THF, dichloromethane, and chloroform. De-tert-butylation of the polymer by the treatment of trifluoromethanesulfonic acid in the presence of toluene proceeded smoothly and produced crystalline poly (aryl ether ketone). © 1994 John Wiley & Sons, Inc.
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  • 35
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 711-719 
    ISSN: 0887-624X
    Keywords: carbazolyl group ; liquid-crystalline polymer ; polyacrylate ; nematic phase ; smectic phase ; electron beam polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new acrylate monomers 4-(ω-acryloyloxyalkyloxy)-N-(9-methyl-2-carbazolylmethylene) anilines containing from 2 to 11 methylenic units in their alkyl group and a carbazolyl group in the mesogenic unit were synthesized and polymerized by azobisisobutyronitrile (AIBN) as radical initiator and by low-energy electron beam (EB) initiation. The thermal properties of the resulting polymers were examined using differential scanning calorimetry and thermal optical polarizing microscopy. The polymer prepared by AIBN with a hexamethylene spacer exhibited a nematic phase from 73 to 170°C and with an undecamethylene spacer exhibited a smectic phase from 55 to 202°C. The isotropization temperature of the polyacrylates increased with increasing the number of carbons of the methylenic spacer. The yield of the resulting polymer was changed by EB irradiation temperature from 4.5 to 41%. The highest yield was obtained when the monomer was polymerized in a liquid-crystalline phase. The same tendency was observed in the molecular weight of the resulting polymers. © 1994 John Wiley & Sons, Inc.
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  • 36
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 747-752 
    ISSN: 0887-624X
    Keywords: thermotropic copolyamides ; depression of transition temperatures ; p-aminobenzoic acid ; amide bond structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is proposed that depression of the transition temperatures, especially the melting point (Tm), can be achieved by the introduction of a different amide bond structure into the copolyamides of dicarboxylic acids and diamines by copolymerization of aminocarboxylic acids, such as p-aminobenzoic acid. The effect was examined by the amount and distribution of the structure in the copolylamindes. Copolycondensations of PEG3, p-aminobenzoic acid, and diamines with different chain lengths showed that the structural change of the amide bond in the copolymers, especially its distribution, was more important than its total amount in them. Several types of aminocarboxylic acids were briefly examined to study the effect. © 1994 John Wiley & Sons, Inc.
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  • 37
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 797-801 
    ISSN: 0887-624X
    Keywords: solid state photopolymerization ; exciton-phonon coupling ; homogeneous and heterogeneous reaction mechanism ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photopolymerization reaction in di n-propyl ester of dicyano p-phenylene diacrylic acid crystal is shown to be mediated by exciton-phonon coupling. Raman phonon spectra suggest that at the initial stage of reaction progress, the reactant and the product form a solid solution. In the later stage, the reactant segregates out and forms its own lattice. The polymer lattice is shown to maintain a good degree of order. Infrared and Raman spectra confirm that the polymerization occurs by cyclobutane ring formation. © 1994 John Wiley & Sons, Inc.
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  • 38
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 829-840 
    ISSN: 0887-624X
    Keywords: chemical modification ; poly (epichlorohydrin) ; nadimide ; polyethers ; DSC ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chemical modification of poly(epichlorohydrin) (PECH) with nadimide derivatives using 1,8-diazabicyclo (5.4.0)-7 undecene to catalyze the substitution of the chlorine atom by acid compounds (DBU method) was accomplished. The linear polyethers obtained showed a degree of substitution from 5-80%, depending on time and temperature reaction. The Tg of modified polymers and Ea, calculated in the cure reactions, increases with substitution degree. Residual enthalpies were observed in all cases, which suggests that the curing reaction is incomplete. TGA measurements showed that the degradation has a greater dependence on the modification degree than on the introduced pendant group. © 1994 John Wiley & Sons, Inc.
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  • 39
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 869-877 
    ISSN: 0887-624X
    Keywords: polymer modification ; block copolymer ; hydroxylation of polyisoprene ; trifluoroacetylation of polyisoprene ; polymer monolayer ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyisoprene (PIP) was found to react with trifluoroacetic acid (TFA) to give an adduct. Saponification of the ester gave a new alternating copolymer of ethylene and α-methyl vinyl alcohol. TFA did not react with polybutadiene (PBD) under these conditions, thus providing a way to produce amphiphilic block copolymers from PBD-b-PIP. TFA addition to the PIP block took place cleanly at an ambient temperature with 2 equiv of the acid in toluene to give block copolymer of PBD and trifluoroacetated PIP. This polymer is very soluble in toluene regardless of molecular weight. Methanolysis with NaOMe cleaved the ester to give PDB-b-(ethylene-alt-α-methyl vinyl alcohol) (PIPOH) in a MeOH/toluene mixture. Low molecular weight hydroxylated diblock copolymer is a viscous liquid when the ratio of PIP/PBD is 0.1 ( \documentclass{article}\pagestyle{empty}\begin{document}$\overline {M_n }$\end{document} = 4100, D = 1.3), but a solid with the ratio 0.5 (\documentclass{article}\pagestyle{empty}\begin{document}$\overline {M_n }$\end{document} = 7170, D = 1.6). High molecular weight polymer (\documentclass{article}\pagestyle{empty}\begin{document}$\overline {M_n }$\end{document} = 114,000, D = 1.4) with PIP/PBD ratio 0.1 is a hazy rubbery material. Block copolymers of PIPOH and poly(methacrylic acid) was also obtained from copolymers of PIP and poly(t-butyl methacrylate). The hydroxylated copolymers showed surface activity by monolayer formation on a Langmuir-Blodgett trough. The transfer of the monolayer on a silicon wafer gave z-type deposition, with the average ellipsometer thickness of the layer being about 40 Å thick per monolayer for \documentclass{article}\pagestyle{empty}\begin{document}$\overline {M_n }$\end{document} = 4100 copolymer. © 1994 John Wiley & Sons, Inc.
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  • 40
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 909-915 
    ISSN: 0887-624X
    Keywords: high-temperature polyarylates ; dihydroxytetraphenylethylene ; solubility behavior ; thermal behavior ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New polyarylates and aromatic polyethers were synthesized from 1,2-bis(4-hydroxyphenyl)-1,2-diphenylethylene, and aromatic dicarboxylic acid chlorides and aromatic dihalides, respectively. The polyarylates having inherent viscosities of 0.28-1.05 dL/g were synthesized by either the two-phase method or the high-temperature solution method. All the polymers were easily soluble in N-methyl-2-pyrrolidone, N,N-dimethylformamide, pyridine, m-cresol, 1,4-dioxane, and 1,1,2,2-tetrachloroethane. They have glass transition temperatures in the range of 217-250°C and showed no weight loss below 315°C in both air and nitrogen atmospheres. Aromatic polyethers with inherent viscosities of 0.85-1.21 dL/g were obtained by the polycondensation of 1,2-bis(4-hydroxyphenyl)-1,2-diphenylethylene and aromatic difluorides in the presence of potassium carbonate. These polymers having glass transion temperatures of 193-220°C were also soluble in the aforementioned solvents and stable up to around 350deg;C in both atmospheres. © 1994 John Wiley & Sons, Inc.
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  • 41
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 929-935 
    ISSN: 0887-624X
    Keywords: reduced titanium dioxide ; supported titanium tetrachloride ; ethylene polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Titanium tetrachloride heterogenized on reduced TiO2 has been studied as a catalyst for ethylene polymerization. The catalyst has good storage stability and exhibits good activity for ethylene polymerization. The polymer chains grow linearly during ca. 1 h, giving an average molecular weight of up to 2.5 × 106 which indicates that practically no β-elimination occurs. The activity of the catalyst at 50°C, based on Ti(III), is 7.6 × 106 PE/mol Ti h bar and based on the quantity of polyethylene formed it is 1.25 × 106 g PE/mol Ti h bar. The molecular weight of the polymer can be controlled with the addition of hydrogen, under 0.5 bar hydrogen, polyethylene with a molecular weight of 411,000 and a relatively low polydispersity index of 2.2 is obtained. The catalyst shows good thermal stability; the Arrhenius activation energy is 31.8 kJ/mol for the polymerization. The catalyst is also active for propylene polymerization, giving 3 × 106 g PP/mol Ti h bar with the high isotacticity of 93%. © 1994 John Wiley & Sons, Inc.
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  • 42
    ISSN: 0887-624X
    Keywords: ε-caprolactone ; ring-opening polymerization ; rare earth coordination catalyst ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ring-opening polymerization of ε-caprolactone has been carried out by using rare earth coordination catalysts for the first time. The rare earth compounds, RE(acac)3.3H2O, Nd(P204)3, Nd(P507)3, Nd(naph)3, Nd(BA)3.2H2O, etc. (where RE = La, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Lu, Y; acac = acetylacetone; BA = benzoylacetone), combined with trialkyl aluminum, greatly increased the degree of conversion and the molecular weight of poly(ε-caprolactone) (PCL). The influence of reaction conditions on the polymerization of ε-caprolactone catalyzed by the Nd (acac)3.3H2O-AlEt3 system has been examined in detail. The kinetics indicates that the polymerization rate has the first-order in monomer and a half-order in catalyst. The overall activation energy of the ring-opening polymerization amounts to 59.4 kJ/mol. By IR and UV-Vis spectra, 1H- and 13C-NMR data, it is assumed that the ring-opening polymerization of ε-caprolactone catalyzed by the Nd(acac)3.3H2O-AlEt3 system proceeds via complexation of monomer to catalyst, acyl-oxygen cleavage insertion propagation mechanism. © 1994 John Wiley & Sons, Inc.
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  • 43
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 683-697 
    ISSN: 0887-624X
    Keywords: hydrosilation ; epoxy monomers ; epoxy functional oligomers ; cationic photopolymerization ; regioselective hydrosilation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several series of multifunctional silicon-containing epoxide monomers and oligomers have been prepared using rhodium catalyzed hydrosilation reactions. Dialkyl and diarylsilanes can be condensed with vinyl epoxides to give high yields of the desired diepoxides while the hydrosilation of alkyl and aryl silanes yields a mixture of di and tri epoxy substituted products. The condensation of αω,—Si—H difunctional compounds with vinyl epoxides can be carried out regioselectively to give α-hydrogen-ω-epoxy intermediates, which can be further reacted with di and tri olefins bearing terminal double bonds to give a series of well characterized epoxy functional oligomers. An investigation of the photoinitiated cationic polymerization of the monomers and oligomers, which were prepared during the course of these studies, was carried out. © 1994 John Wiley & Sons, Inc.
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  • 44
    ISSN: 0887-624X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syndioselective propylene polymerization has been promoted by rac-2,2-dimethylpropylidene (1-η5-cyclopentadienyl) (1-η5-fluorenyl) dichlorozirconium (1). The active catalytic species were generated using either triphenylcarbenium tetrakis (pentafluorophenyl) borate (2) (Zr+ method) or methylaluminoxane (MAO method). The former exhibited much higher activity than the latter, especially at low polymerization temperatures (Tp). Syndiotactic poly (propylene) (s-PP) obtained at Tp = -20°C has Tm approaching 160°C, [rrrr] pentad fraction of 0.92 to 0.95, and 45% crystallinity (Xc). It crystallized in two antichiral unit cells B and C. The C structure is favored by low temperature of polymerization, slow crystallization from melt, and annealing. The s-PP has M̄w/M̄n ranging from 3.6 to 4.4, which can be separated into stereoregular fractions soluble in heptane and hexane and stereoirregular fractions soluble in pentane, ether, and acetone. Therefore, this system cannot be considered to be a single-site catalyst. A parallel study was made on the isopropylidene (1-η5-cyclopentadienyl) (1-η5-fluorenyl) dichlorozirconium (3)/MAO catalyst. Molecular mechanics calculations were performed for all combinations of the configuration of asymmetric centers. The steric energy favors syndiotactic enchainment for both catalysts 1 and 3, with 1 forming the more syndioselective catalyst. © 1994 John Wiley & Sons, Inc.
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  • 45
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 767-777 
    ISSN: 0887-624X
    Keywords: emulsion polymerization ; ion-free ; polybutadiene ; poly (vinyl pyrrolidone) ; polymer electrolyte ; latex ; core-shell ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of polybutadiene (PB) by emulsion polymerization with use of poly (vinyl pyrrolidone) (PVP) stabilizer was investigated. The goal was to prepare flexible latex films that clearly retain particle morphology in the solid state after heat treatment and contain no ionic, hydroxyl, or (primary, secondary) amino groups. The latex particle core composed of PB was nonpolar and rubbery, while the particle shell composed of PVP was polar and glassy. Average particle diameter was measured by the dynamic light scattering technique, and particles were imaged by scanning and transmission electron microscopic analyses. Dialysis of the latices resulted in successful exchange of the dispersion medium without precipitation. © 1994 John Wiley & Sons, Inc.
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  • 46
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 789-795 
    ISSN: 0887-624X
    Keywords: polycondensation ; serine ; aspartic acid ; inhibitors ; crystallization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Biocompatable, degradable polymers that are powerful inhibitors of mineral formation were synthesized by automated solid phase and thermal polycondensation techniques. These polymers are analogues of natural proteins isolated from CaCO3 biomineral and consist primarily of polyaspartic acid and serine or modified serine residues. Phosphorylation of the serine residues greatly enhanced the inhibitory activity of the polymers. Synthesis in the presence of orthophosphoric acid resulted in the decomposition and modification of serine. These modified residues when incorporated into the polyaspartic acid also enhanced inhibitory activity of the polymers. © 1994 John Wiley & Sons, Inc.
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  • 47
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 841-847 
    ISSN: 0887-624X
    Keywords: ethylene-carbon monoxide copolymer ; propylene-carbon monoxide copolymer ; polythiophene ; polyfuran ; polyalcohol ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the alternating ethylene-carbon monoxide copolymer with Lawesson's reagent resulted in the conversion of 75% of the carbonyl groups to thiophene units. A few thioketone groups were also present in the derived polymer. A polymer with furan units in the backbone was formed upon treatment of the alternating propylene-carbon monoxide copolymer with P2O5. Depending on the reaction conditions, up to 90% of the carbonyl groups were converted. Finally, 1,4-polyalcohols were prepared from the alternating propylene-carbon monoxide copolymer by reduction. Hydrogenation using Raney nickel as catalyst resulted in the reduction of 60% of the carbonyl groups, whereas reaction with LiAlH4 at room temperature caused the reduction of 85% of the carbonyl groups. The glass transition temperature was found to increase monotonically with increasing concentration of hydroxyl groups in the polymer backbone. © 1994 John Wiley & Sons, Inc.
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  • 48
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 879-887 
    ISSN: 0887-624X
    Keywords: living cationic polymerization ; isobutyl vinyl ether ; added Lewis base ; EtAlCl2 ; Et1.5AlCl1.5 ; polymerization mechanism ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the living cationic polymerization of isobutyl vinyl ether (IBVE) by the CH3CH (OiBu) OCOCH3 (1)/EtAlCl2 initiating system in the presence of the added base in hexane at +40°C, the stability of the initiating system 1/EtAlCl2, which form initiating species CH3CH⊕ (OiBu) derived from 1, was investigated. In the presence of the Lewis base such as ethyl acetate or 1,4-dioxane, the active species was stable for 300 min even at +40°C in the absence of IBVE, and the living polymers were quantitatively obtained by adding IBVE. However, the active species was partly consumed by side reactions during the standing time for 60 min in the presence of a less basic additive such as ethyl benzoate, and about 50% of the active species was deactivated in the presence of methyl chloroacetate. Consequently, in the case of a less basic additive such as methyl chloroacetate (which was effective for the fast living polymerization), it can be seen that the careful selection of polymerization conditions was required. The living polymerization rate was dependent on the second order of EtAlCl2 concentration. EtAlCl2 induced the cleavage of 1 into CH3CH⊕ (OiBu) and EtAl⊖Cl2(OCOCH3), and the reactivity of CH3CH⊕ (OiBu) and propagating carbocation may be controlled by EtAl⊖Cl2(OCOCH3) with the aid of other EtAlCl2. Et1.5AlCl1.5 exists as a bimetallic complex of EtAlCl2 and Et2AlCl, and it is expected that the polymers having a bimodal molecular weight distribution will be obtained due to two kinds of counteranions coming from EtAlCl2 and Et2AlCl. However, in the cationic polymerization of IBVE by 1/Et1.5AlCl1.5 in the presence of ethyl acetate, the living polymer exhibiting a unimodal and very narrow molecular weight distribution was obtained. Thereby, it was suggested that the counteranions, EtAl⊖Cl2(OCOCH3) and Et2Al⊖Cl(OCOCH3), exchange rapidly with each other. © 1994 John Wiley & Sons, Inc.
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  • 49
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 917-928 
    ISSN: 0887-624X
    Keywords: radical polymerization ; stable phenoxyl radical ; intramolecular hydrogen transfer ; termination ; hindered phenol ; copolymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Radical polymerizations of methyl methacrylate (MMA), styrene (St), and vinyl acetate (VAc) were carried out in the presence of a novel phenyl acrylate derivative bearing a hindered phenol moiety (HPA). It has been clarified that HPA acts as a retarder and inhibitor for the polymerizations of MMA and VAc, respectively, and that in the polymerization of St it behaves as a monomer to give a copolymer. These additive effects were interpreted in terms of intramolecular transfer of the phenolic hydrogen in competition with propagation of the HPA radical to monomers. © 1994 John Wiley & Sons, Inc.
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  • 50
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 961-969 
    ISSN: 0887-624X
    Keywords: ethylene ; copolymerization ; hindered piperidine ; UV stabilizer ; chemically bound antioxidant ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monomers having a norbornene as polymerizable group and a 2,2,6,6-tetramethyl piperidine as stabilizing moiety were prepared. This monomer was successfully copolymerized with ethylene using VAc3/AlEt2Cl as the catalytic system. Copolymers exhibited better stability under accelerated aging than polyethylene stabilized by classical blending with commercial hindered amines. Any attempt made to obtain copolymers using a high activity TiCl4/MgCl2 catalyst was unsuccessful. © 1994 John Wiley & Sons, Inc.
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  • 51
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 987-991 
    ISSN: 0887-624X
    Keywords: palladium-catalyzed polycondensation ; soluble ethynylene-containing polyamides ; ethynyl-containing amide monomers ; thermal behavior ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 52
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 993-995 
    ISSN: 0887-624X
    Keywords: metathesis ; regioselective polymerization ; 7-alkylnorbornenes ; ab initio MO Calculations ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 53
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 343-354 
    ISSN: 0887-624X
    Keywords: thermotropic polyester ; nematic ; X-ray diffraction ; synthesis ; characterization ; 3,4′-dihydroxybenzophenone ; 4,4′-bibenzoic acid ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of fully aromatic, thermotropic polyesters, derived from 3,4′-dihydroxybenzophenone and various aromatic dicarboxylic acids, was prepared by the high-temperature solution polycondensation method and examined for thermotropic behavior by a variety of experimental techniques. The aromatic dicarboxylic acids used in this study were 2,6-naphthalenedicarboxylic acid, 4,4′-bibenzoic acid, and terephthalic acid.The two homopolymers of 3,4′-DHB with either 2,6-NDA or 4,4′-BBA formed nematic LC phases at 285°C and 255°C and also exhibited isotropization transitions (Ti) at 317°C and 339°C, respectively. The copolymer of 3,4′-DHB with 50% TA and 50% 2,6-NDA also formed a nematic LC phase and had a broader range of LC phase than that of its respective homopolymers. Two other copolymers of 3,4′-DHB, both containing 50% 4,4′-BBA, also formed nematic LC phases at low Tf values. All of the thermotropic polyesters had high thermal stabilities. © 1994 John Wiley & Sons, Inc.
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  • 54
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 369-382 
    ISSN: 0887-624X
    Keywords: N-phenyl-3,3-bis[4-(p-aminophenoxy)phenyl] phthalimidine ; N-phenyl-3,3-bis (4-hydroxyphenyl) phthalimidine ; polyamides ; polyimides ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: N-Phenyl-3,3-Bis[4-(p-aminophenoxy)phenyl] phthalimidine (II) was used as a monomer with various aromatic dicarboxylic acids and tetracarboxylic dianhydrides to synthesize polyamides and polyimides, respectively. The diamine II was derived by a nucleophilic substitution of N-phenyl-3,3-bis(4-hydroxyphenyl) phthalimidine with p-chloronitrobenzene in the presence of K2CO3 and then hydro-reduced. Polyamides IVa-g having inherent viscosities of 0.55-1.64 dL/g were prepared by the direct polycondensation of the diamine II with various aromatic diacids using triphenyl phosphite and pyridine as condensing agents. All the aromatic polyamides were amorphous and readily soluble in various polar solvents such as N,N-dimethylacetamide (DMAc), N,N-dimethylformamide, dimethylsulfoxide, and N-methyl-2-pyrrolidone (NMP). Transparent and flexible films of these polymers could be cast from the DMAc solutions. These aromatic polyamides had glass transition temperatures in the range of 293-319°C and 10% weight loss occurred up to 480°C. The polyimides were synthesized from diamine II and various aromatic dianhydrides via the two-stage procedure that included ring-opening polyaddition in DMAc to give poly(amic acid)s, followed by thermal or chemical conversion to polyimides. Most of the aromatic polyimides obtained by chemical cyclization were found to be soluble in NMP, m-cresol, and o-chlorophenol. These polyimides showed almost no weight loss up to 500°C in air or nitrogen atmosphere. © 1994 John Wiley & Sons, Inc.
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  • 55
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1389-1392 
    ISSN: 0887-624X
    Keywords: methyl-(trifluoromethyl) acrylate ; propagation rate constant ; termination rate constant ; rotating sector method ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [no Abstrat]
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  • 56
    ISSN: 0887-624X
    Keywords: thermoplastic elastomers ; poly (-methylstyrene-b-isobutylene-b--methylstyrene) ; triblock copolymer ; living carbocationic polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparatory to triblock synthesis experiments, the cationic polymerization of α-methylstyrene (αMeSt) was investigated using the 2-chloro-2,4,4-trimethylpentane (TMPCI)/TiCl4 initiating system in the presence of triethylamine (Et3N) as electron donor (ED) and CH3Cl/n-hexane mixed solvent in the -80 to -40°C range. Conversions are influenced by temperature, [TiCl4], [Et3N], and [αMeSt]. The polymerization of αMeSt is living at -80°C: Both termination and chain transfer to monomer are frozen out, however, initiation is slow relative to propagation. Highly syndiotactic (〉94%) Pα Mest was obtained. At-60deg;C initiator efficiency is ca. 100%, but termination becomes evident. Et3N may act both as Ed and as proton scavenger. Novel poly(α-methystyrene-b-isobutylene-b-α-methylstyrene) (PαMeSt-PIB-PαMeSt) triblocks have been synthesized by adding αMeSt to biliving polyisobutylene carbocations (⊕PIB⊕) in the -80 to -40°C range. The effects of temperature, solvent polarity, and [Et3N] on the block copolymerization have been investigated. At -80°C, the rate of crossover from ⊕PIB⊕ to αMeSt is lower than that of propagation of PαMeSt⊕, so that the triblock is contaminated by PIB and PIB-b-PαMeSt. At -60°C, crossover occurs preferentially. The rate of propagation relative to that of crossover is also reduced by lowering the solvent polarity and increasing the [Et3N]. High crossover efficiency and blocking efficiency can be obtained under optimum blocking conditions. The triblocks are novel thermoplastic elastomers (TPEs). © 1994 John Wiley & Sons, Inc.
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  • 57
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 451-456 
    ISSN: 0887-624X
    Keywords: hexamethylenediammonium adipate ; solid-state polycondensation (polyamidation) ; acid catalysts ; solid-melt transition ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Loss of diamine and distinct transition phenomena from the solid to the melt state restrain solid-state polymerization (SSP) of nylon salts from industrial application. To depress these phenomena temperatures well below the melting point of the starting material are employed, resulting however in low reaction rates. The need to use catalysts arises and accordingly in this study hexamethylenediammonium adipate (HMA) particles were polymerized containing a strictly controlled amount of uniformly distributed catalyst. The catalysts included boric, sulphuric, and phosphoric acids with boric acid being the most effective in accelerating the reaction while eliminating the tendency to agglomeration. In general, catalyst concentration up to a critical value plays a considerable role in the overall behavior. Furthermore, in agreement with non catalytic processes, the reaction temperature remains an influential parameter. © 1994 John Wiley & Sons, Inc.
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  • 58
    ISSN: 0887-624X
    Keywords: polyaddition ; phosphorus-containing polymer ; saturated polymer ; phenylphosphine ; 1,4-divinylbenzene ; 1,4-diisopropenylbenzene ; flame resistance ; thermal stability ; DSC ; TG ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A polyaddition of phenylphosphine (PH) to 1,4-divinylbenzene (DVB) or 1,4-diisopropenylbenzene (DIPB) was carried out by radical initiations or UV irradiation at 60-80°C in toluene under a nitrogen atmosphere. The soluble polymer with higher molecular weight ($\[ \bar M_w = 2 \times 10^4 \]$) was obtained in a high yield with AIBN initiator for 95 h in the presence of 5% excess of PH to DVB (monomer feed ratio [DVB]0/[PH]0 = 1/1.05). On the other hand, a polyaddition of PH to DIPB proceeded much slower than the case of DVB, but the high polymer was obtained in a high yield by choosing polyaddition conditions such as polyaddition temperature and initiator concentration. From 1H-NMR, IR analyses, and phosphorus content of the polymers, it was characterized that both polymers have the alternating structure consisting of PH and DVB or DIPB units in 1 : 1 ratio. The glass transition and decomposition temperatures of both polymers under a nitrogen atmosphere were almost similar: 15-30°C and 380-385°C, respectively; but, the polymers were oxidized by heating under an atmosphere of air. The polymers had a self-extinguishing property and the polymer blend of the flammable polymers such as polystyrene and polyethylene with the phosphorus-containing polymers exhibited an excellent flame resistance. © 1994 John Wiley & Sons, Inc.
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  • 59
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1295-1304 
    ISSN: 0887-624X
    Keywords: poly (ethylene naphthalate) ; transesterification kinetics ; reaction order ; activation energy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The transesterification of dimethyl naphthalate (DMN) with ethylene glycol (EG) was kinetically investigated in the presence of various catalysts at 185°C. The transesterification was assumed to obey first-order kinetics with respect to DMN and EG, and a rate equation was derived. The rate constant of transesterification which was calculated from the quantity of methanol which distilled from the reaction vessel was used to evaluate the activity of each metal compound. The first-order dependence on the catalyst concentration is valid below a critical concentration which was found to be dependent on the catalyst type. The order of decreasing catalytic activity of various metal ions was found to be: Pb ≥ Zn 〉 Co 〉 Mg 〉 Ni ≥ Sb, but in the case of highly basic metal salts, the rate constants were found to be extremely large at the initial stage of the reaction, and then rapidly decreased with the progress of the reaction. Effects of reaction temperature were also discussed. The activation energies for zinc acetate and lead acetate were 97.84 and 108.8 kJ/mol, respectively, which were calculated from the Arrhenius equation. © 1994 John Wiley & Sons, Inc.
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  • 60
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1341-1350 
    ISSN: 0887-624X
    Keywords: addition polyimides ; biphenyldiamine ; benzidine ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new series of high flow PMR-type addition curing polyimides was developed, which employed the substitution of 2,2′-bis(trifluoromethyl)-4,4′-diaminobiphenyl (BTDB) for p-phenylenediamine (p-PDA) in a PMR-II formulation. These thermoset polyimides, designated as 12F resins, were prepared from BTDB and the dimethyl ester of 4,4′-(hexafluoroisopropylidene)-diphthalic acid (HFDE) with either nadic ester (NE) or p-aminostyrene (PAS) as the endcaps for addition curing. The 12F prepolymers displayed lower melting temperatures in DSC analysis, and higher melt flow in rheological studies than the corresponding PMR-II polyimides. Long-term isothermal aging studies showed that BTDB-based 12F resins exhibited comparable thermo-oxidative stability to p-PDA based PMR-II polyimides. The noncoplanar 2- and 2′-disubstituted biphenyldiamine (BTDB) not only lowered the melt viscosities of 12F prepolymers, but also retained reasonable thermal stability of the cured resins. The 12F polyimide resin with p-aminostyrene endcaps showed the best promise for long-term, high-temperature application at 343°C (650°F). © 1994 John Wiley & Sons, Inc.
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  • 61
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1377-1384 
    ISSN: 0887-624X
    Keywords: ozonization ; grafting ; kinetics ; radical polymerization ; EVAg-styrene ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polymers can be ozonized with an ozone/oxygen mixture to create peroxides and hydroperoxides on the polymer chain. These heat-sensitive functional groups can be used to initiate radical polymerization of vinyl monomers and give graft copolymers. The properties of these copolymers are well described in literature; however, we notice that available data concerning decomposition rate constants are inconsistent. Decomposition rate measurements, time of assay of free radicals and stability of the ozonized polymers do not give the same results. In this work, we studied the kinetics of the styrene polymerization initiated by an ozonized ethylene vinyl acetate copolymer. Consequently, the f·kd product can be calculated (f is the efficiency and kd the decomposition rate constant). The ozonized copolymer is not similar to usual radical initiators. The initial viscosity of the solution has an important effect on the calculation of the kinetic values. Activation energy and Arrhenius coefficient are different than the one obtained for the usual initiators. © 1994 John Wiley & Sons, Inc.
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  • 62
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 699-709 
    ISSN: 0887-624X
    Keywords: contact angle goniometry ; chemical derivatization ; plasma treatment ; polyethylene ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Plasma-oxidized polyethylene (O-PE) was derivatized with various chemicals and the advancing and receding contact angles with water, formamide, and tricresylphosphate were measured. The contact angles were used to evaluate the surface free energy (SFE) components in terms of the Lifshitz-van der Waals-acid base (LW-AB) model. The derivatization was directed to couple alkyl chains to carbonyl, hydroxyl, and carboxyl groups generated on the surface of O-PE. Carbonyl groups were treated with hydrazine and then reacted with dodecanoyl chloride. Hydroxyl groups were first reacted with reactive dicarboxylic acid dichlorides or cyanuric chloride, respectively, and then with alkylamines because the direct bonding of long-chain alkyl carboxylic acid chlorides proceeds slowly and is, therefore, completed by surface restructuring. Carboxyl groups were chlorinated and in a second step reacted with alkylamines. The bonding of C12-alkyl chains can be sensitively detected by the LW part of the SFE. Concerning the receding contact angles, it is pointed out that the carbonyl groups are present on the surface in a higher concentration than hydroxyl and carboxyl groups. The combination of contact angle goniometry (CAG) and chemical derivatization reactions supplies semiquantitative information about functional groups in the uppermost surface layer. In this way, a major shortcoming of CAG can be overcome. © 1994 John Wiley & Sons, Inc.
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  • 63
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 741-746 
    ISSN: 0887-624X
    Keywords: polymerization mechanism ; polymerization kinetics ; carbonate macrocyclization ; polycarbonate ; stopped-flow spectroscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The kinetics of phenylchloroformate (PCF) reactions have been used to model some of the key chemical events in carbonate macrocyclization. Three reactions have been studied using stopped-flow FT-IR spectroscopy: formation of acyl ammonium salt from PCF and three different trialkylamines, the conversion of acyl ammonium salt to urethane, and the condensation reaction between acyl ammonium salt and 4-isopropylphenol. The rate dependence was studied for triethylamine (TEA), diethylmethylamine (DEMA) and tri-n-butylamine (TBA) at 0°C in anhydrous CH2Cl2. The reactivity order for acyl ammonium salt formation for TBA: TEA: DEMA is 1 : 2.7 : 〉444. By contrast, condensation and urethane formation are not sensitive to the structure of the amine. The rate of condensation is comparable to the rate of acyl ammonium salt formation for TEA and TBA, while the rate of urethane formation is the slowest process for all three amines. These results are consistent with the view that the yield of macrocyclic polycarbonates is related to the concentration of the acyl ammonium salt. The optimum amine concentration for obtaining high yields of cyclics varies with the amine structure and parallels the difference in the rates of acyl ammonium salt formation. © 1994 John & Sons, Inc.
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  • 64
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1471-1480 
    ISSN: 0887-624X
    Keywords: methyl methacrylate ; redox polymerization ; kinetics ; mechanism ; additives ; iron saccharinate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The role of N,N-dimethyl-p-toluidine (DMPT) and saccharin as accelerators in the polymerization of methyl methacrylate initiated by the redox decomposition of cumene hydroperoxide (CHP) in the presence of iron saccharinate has been kinetically investigated. DMPT reduces ferric ions to ferrous ions, so that an equilibrium is established between the two oxidation states. With the assumption of a steady-state concentration of propagating radicals, the rate of initiation was deduced from the rate of polymerization and the kinetic orders with respect to each compound involved in the initiation step have been determined. The reaction is first-order in CHP, iron saccharinate, and saccharine and second-order in DMPT. In a proposed scheme, Fe2+ ions, complexed by two DMPT molecules, are much more reactive than uncomplexed Fe2+ and saccharin activates the decomposition of CHP by protonation of the O—O bond. This mechanism, similar to that proposed in the case of copper saccharinate, explains the synergistic effect of both accelerators. © 1994 John Wiley & Sons, Inc.
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  • 65
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1523-1530 
    ISSN: 0887-624X
    Keywords: amphiphilic polymers ; graft copolymers ; poly(oxyethylene) ; activated esters ; emulsifying properties ; thermal properties ; crystallinity ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Amphiphilic graft copolymers were synthesized via activated ester substitution of derivatives of fumaric acid with amino-functionalized methoxypoly (oxyethylene)s (MPEO-NH2) of different molecular weights. The monomeric activated esters, isopropyl pentachlorophenyl fumarate (PCPFA) and isopropyl succinimido fumarate (SIFA), were copolymerized with styrene (St) or N-vinyl pyrrolidone (VP) at equimolar ratio. The polymeric-activated esters proved to be good precursors for grafting of definite amounts of MPEO-NH2. The aminolysis of the succinimide esters and VP-containing copolymers proceeded with gel formation due to extensive hydrogen bonding. The hydrodynamic behavior, the emulsifying ability, the thermal properties, and crystallinity of the graft copolymers were studied as a function of their molecular characteristics. The length of the PEO grafts and the degree of grafting are the factors which affect the melting parameters and the crystallinity of the side chains. © 1994 John Wiley & Sons, Inc.
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  • 66
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1551-1555 
    ISSN: 0887-624X
    Keywords: poly(vinyl pyrrolidone) ; cationic polymerization ; electropolymerization ; thin films ; surface modification ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electroinitiated polymerization of N-vinyl-2-pyrrolidone has been investigated. After electrolysis at controlled potential, a thin, covering, and homogeneous film of poly(N-vinyl-2-pyrrolidone) appears on the electrode. The insolubility of the polymer in its classical solvents implies the existence of a true chemical grafting of macromolecules on the platinum surface. Chain propagation occurs by a cationic mechanism initiated by a direct electron transfer leading to grafted cations on the surface, followed by the nucleophilic attack of neutral molecules. The molecular weight of the polymer was estimated by gel permeation chromatography after having mechanically removed the film from the electrode. A molecular weight distribution curve showing an average value of 16,000 was observed. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1569-1579 
    ISSN: 0887-624X
    Keywords: functional group gradients ; corona discharge ; graft copolymerization ; water contact angles ; FTIR-ATR ; ESCA ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Functional group gradient surfaces where the density of functional groups changes gradually along the sample length were prepared. The functional group (— COOH, — CONH2, and — OH group) gradient surfaces were produced by the treatment of low-density PE sheets using a corona with gradually increasing power, followed by the graft copolymerization of acrylic acid and subsequent substitution reaction of carboxylic acid groups to amide or hydroxyl groups. The prepared gradient surfaces were characterized by the measurement of water contact angle, FTIR-ATR, and ESCA. The gradient surfaces prepared can be used to systematically investigate the interactions of biological or other species in terms of the surface functional groups and their density of polymeric materials. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1609-1617 
    ISSN: 0887-624X
    Keywords: selenium-containing polymer ; radical addition polymerization ; 1,4-benzene-diselenol ; 1,4-divinylbenzene ; 2,2′-azobisisobutyronitrile ; dimethyl 2,2′-azobisisobutyrate ; 1,1′-azobis(1-acetoxy-1-phenylethane) ; model addition reaction ; side reaction ; properties of polymer ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel addition polymerization of 1,4-benzenediselenol (BDSe) to 1,4-divinylbenzene (DVB) was carried out with various azo radical initiators [dimethyl 2,2′-azobisisobutyrate (DAIB), 1,1′-azobis(1-acetoxy-1-phenylethane) (AAPE), and AIBN] in toluene at 65 and 75°C under a nitrogen atmosphere. The polymerization proceded without an induction period, and pale-yellowish powder polymers were obtained in 89% yields for 75 h (DAIB), 89% yields for 24 h (AAPE), and 60% yields for 8 h (AIBN). The molecular weight (Mw) of the insoluble polymers in toluene was about 4000 (IBN) to 14,000 (DAIB or AAPE) by GPC. The polymer had an alternating structure of BDSe to DVB units by 1H-NMR, IR analyses, and selenium contents, but the polymer contained the diselenide linkage by Raman spectroscopy. By AIBN initiator, the yield of the polymers did not increase over 60% and higher molecular weight polymer was hardly obtained. According to the model addition reaction of benzeneselenol to styrene by AIBN, it was found that AIBN was consumed by the side reaction between dimethyl-N-(2-cyano-2-propyl)ketenimine derivedAppl 11 from AIBN and benzeneselenol to give the adduct C, MH+ 295 by DCI MS. On the other hand, DAIB and AAPE initiators, which do not form a ketenimine intermediate, gave the polymers of higher molecular weight in a higher yield. The polymer film exhibited high refractive index (n25D = 1.81) and a reversible phase transition between a transparency and an opaque by thermal mode. © 1994 John Wiley & Sons, Inc.
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  • 69
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1657-1664 
    ISSN: 0887-624X
    Keywords: photofunctionalization ; photocrosslinking ; synthetic membranes ; permselectivity ; pervaporation ; surface properties ; tetrazole ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new type of membrane polymer, containing a photosensitive moiety, was synthesized. The photochemically induced functionalization and crosslinking of poly [acrylonitrile-co-butadiene-co-styrene-co-2-(4-ethenyl) phenyl-5-phenyl-2H-tetrazole], ABSV, has been studied. A variety of dipolarophiles and phenolic compounds were applied to alter the polarity of the membrane surface. The functionalization and crosslinking were initiated by photoirradiation. DSC and contact angle measurements were used to characterize the modified polymer. Pervaporation experiments with a cyclohexane/benzene mixture (5 wt% benzene) were carried out, with the results showing, that the photochemical treatment significantly effects both permselectivity and flux. Solubility parameters were found to be useful to interpret the pervaporation data. In general, the selectivity towards benzene increases with the polarity of the membrane surface, i.e., with increasing polarity of the modifier. A mechanism to explain the influence of both functionalization and crosslinking on the membrane performance, is proposed. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1691-1702 
    ISSN: 0887-624X
    Keywords: grafting ; basic functionalization ; free radical polymerization ; methacrylate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The grafting of 2-(dimethylamino)ethyl methacrylate (DMAEMA) onto two model hydrocarbons, squalane and n-eicosane, and to linear low density polyethylene (LLDPE) has been investigated. The results of the study indicate that a high reaction temperature, 160°C, and a low concentration of monomer, less than 0.3 M, are optimum conditions for the grafting reaction. Reaction products, which consisted of grafted hydrocarbons and poly(DMAEMA), were separated by solvent extraction and vacuum distillation; samples were then analyzed by NMR and FTIR spectroscopy and size exclusion chromatography. 1H-NMR spectroscopy indicates that grafted squalane contained approximately 6 DMAEMA units per squalane residue. 1H- and 13C-NMR and molecular weight studies strongly suggest that the grafts onto the model hydrocarbons consist of single DMAEMA units. Results of the melt grafting of DMAEMA onto LLDPE show that the grafting efficiency and degree of grafting are substantially lower than were expected from the model system. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1977-1982 
    ISSN: 0887-624X
    Keywords: poly(arylamino-quinone)s ; p-benzoquinone ; aromatic diamine ; tetrahydrofuran ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several poly(arylamino-quinone)s (PAAQs) were prepared by the conventional solution polymerization of p-benzoquinone with various aromatic diamines in tetrahydrofuran. Polymers prepared by this method were found to be more soluble in many organic solvents compared to the PAAQs prepared by other reported methods. The poly(arylamino-quinone)s were obtained in 82.3-94.5% yield and had inherent viscosities in the range of 0.073-0.251 dL/g. Among the PAAQs, the polymer prepared from p-benzoquinone and 1,3-bis(3-aminophenoxy)benzene (APB) had demonstrated exceptionally good solubility and thermal stability. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2003-2010 
    ISSN: 0887-624X
    Keywords: kinetics of polyesterification ; effect of diol chain length ; unsaturated polyesters ; energy of activation ; rate of reaction ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Kinetics of polyesterification of maleic anhydride with polyethylene glycol (PEG) of varying molecular weights have been evaluated. The investigations have been carried out by employing heating cycles comparable to those employed in industrial processes and under nonisothermal conditions. The rate of reaction was found to decrease with increase in the chain length of the polyether. The energy of activation was estimated as 26.91, 40.25, and 47.30 Kcal/mol for PEG of molecular weights 200, 300, and 400, respectively. © 1994 John Wiley & Sons, Inc.
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  • 73
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2029-2038 
    ISSN: 0887-624X
    Keywords: 1,2-bis(p-vinylphenyl)ethane ; divinylbenzene ; crosslinker ; network structure ; size exclusion chromatography resins ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New size exclusion chromatography (SEC) resins based on a crosslinker having independent vinyl groups have been produced and compared with SEC resins based on divinylbenzene-55 (DVB). 1,2-Bis(p-vinylphenyl)ethane (p,p-BVPE) and its meta-isomers were suspension-copolymerized with p-methylstyrene in the presence of different porogens to give particles of about 5 μm average diameter. The porous particles were slurry-packed into stainless steel columns for SEC evaluation. Calibration curves were obtained using narrow disperse polystyrene standards with molecular weights ranging from 580 to 3,040,000. The calibration curves for the new BVPE resins covered wider useful molecular weight ranges than those for comparable divinylbenzene resins. Particle size, surface morphology and the properties of pores were studied using a Coulter Multisizer II, scanning electron microscopy, nitrogen adsorption, and mercury porosimetry. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2065-2071 
    ISSN: 0887-624X
    Keywords: poly(ether-ketone-amide) ; palladium-catalyzed polycondensation ; aromatic dibromide ; carbon monoxide ; thermal behavior ; tensile properties ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Aromatic poly(ether-ketone-amide)s were prepared by the palladium-catalyzed polycondensation of aromatic dibromides containing ether ketone units, aromatic diamines, and carbon monoxide. Polymerizations were carried out in N,N-dimethylacetamide (DMAc) in the presence of palladium catalyst, triphenylphosphine, and 1,8-diazabicyclo [5,4,0]-7-undecene (DBU), and resulted in poly(ether-ketone-amide)s with inherent viscosities up to 0.82 dL/g under mild conditions. The polymers were quite soluble in strong acid, dipolar aprotic solvents, and pyridine. Thermogravimetry of the polymers showed excellent thermal stability, indicating that 10% weight losses of the polymers were observed in the range above 400°C in nitrogen atmosphere. The glass transition temperatures of the polymers were about 200°C, which are higher than those of poly(ether-ketone) analogues. These polymers also showed good tensile strength and tensile modulus. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1393-1397 
    ISSN: 0887-624X
    Keywords: cyclic carbonate ; epoxide ; cationic copolymerization ; spiro orthocarbonate ; ring-opening polymerization ; poly (ether-carbonate) ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [no Abstrat]
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1423-1430 
    ISSN: 0887-624X
    Keywords: block copolymers ; free radical polymerization ; polydimethylsiloxane ; chain transfer ; rate constants for the transfer reactions ; thiuram disulfide ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chain transfer constants (Ctr) for thiuram disulfide (TD) groups, included in the backbone of polydimethylsiloxane (PDMS) of different chain lengths, in methyl methacrylate (MMA) and styrene (St) were determined from measurements of the degree of polymerization. Two methods were used. The first consisted of using the initiation and transfer properties of the thiuram disulfides groups, and the second, of using a more efficient free radical initiator than TD groups, in which case the former behaves only as a transfer agent. In both the methods, the Ctr of TD was evaluated in bulk polymerization of MMA at 60, 70, 80, and 90°C. Using the first method, the Ctr of TD was measured also in solution polymerization of MMA in toluene at 100°C and, with the second one, in bulk polymerization of styrene at 60, 80, and 90°C. PDMS-based macrothiuram disulfide (macroiniferter) behaves as an “azeotropic” transfer agent for MMA and styrene at 125°C and 110°C, respectively. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2147-2153 
    ISSN: 0887-624X
    Keywords: polyaniline ; derivatives ; doping ; processing ; films ; gel ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High molecular weight poly(o-methoxyaniline) was synthesized using a novel method in which the polymerization occurs in the presence of a neutral salt. The molecular weight of the polymer was greatly affected by the quenching procedure employed to conclude the polymerization. Conventional doping of the base form of poly(o-methoxyaniline) produced a yellow coloration of the doping solution and polymer degradation. It was found that the molecular weight of the polymer decreased significantly after washing or doping with certain aqueous acid media. The gelation conditions of N-methyl pyrrolidinone (NMP) solutions and film preparation were also investigated for polymers of various molecular weights. The gelation time in NMP decreased drastically with the increase in the polymer molecular weight (the same for solution concentration and temperature), until a critical point was reached after which its decrease was very slow. Flexible, free-standing, and stretchable films were readily obtained from the higher molecular weight polymers. Good quality doped gel films with conductivity of up to 1 S/cm were obtained under optimized doping conditions. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2177-2185 
    ISSN: 0887-624X
    Keywords: photo-initiated base-formation ; polymer matrix ; O-acyloxime ; photolysis ; yield of amine ; acyloxyimino group ; thermal crosslinking ; recombination ; cage effect ; 6-membered cyclic intermediate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It was found that amines were formed efficiently by the photolysis of O-acyloximes followed by hydrolysis in polystyrene films and the relationship between structures of O-acyloximes and yields of amines were investigated. O-phenylacetyl acetophenone oxime (PaApO), O-pivaloyl acetophenone oxime (PApO), and O-benzoyl acetophenone oxime (BApO) as monofunctional O-acyloximes and O,O′-succinyl diacetophenone oxime (SDApO) and O,O′-glutaryl diacetophenone oxime (GDApO) as bifunctional O-acyloximes were examined. The yields of amines for PaApO and SDApO under N2 were ca. 70%, which was the highest among O-acyloximes examined in this experiment. On the other hand, the yields for PApO, BApO, and GDApO were less than 15% and it was verified that the hydrogen abstraction by imino radicals via 6-membered cyclic intermediates resulted in the lowering of yields. Although the effect of oxygen under photolysis on the yields of amine for PaApO was negligible under 50% conversion of PaApO, the yield decreased with further increase in the conversion and was 50% at 90% conversion. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2229-2234 
    ISSN: 0887-624X
    Keywords: tetrafluoroethylene ; propylene ; emulsion redox copolymerization ; fluoroelastomers ; reaction conditions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Emulsion polymerization of tetrafluoroethylene and propylene with ammonium perfluorooctanoate, initiated by a redox system containing tert-butylperbenzoate (TBPB) was carried out. The effect of the components of the redox system Is (TBPB, FeSO4.7H2O, ethylenediamine tetraacetic acid (EDTA), and CH2(OH)SO2Na.2H2O) on the polymerization rate (R) and molecular weight ($\[ \bar M_n \] $) was studied. Among redox system components, Fe2+ concentration exerts the most significant effect (by power of 0.54) on the polymerization rate. It was found that R ∝ [Is]0.2-0.54 and Mn ∝ [Is]0.0-0.1 and polymerization reaction scheme was suggested for the action of the initiating system. The influence of the copolymerization conditions (pressure, temperature, stirring speed, and pH) is also discussed. The apparent activation energy of the reaction was found to be 46.0 kJ/mol. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2203-2221 
    ISSN: 0887-624X
    Keywords: cyanate ; epoxy ; mixed resins ; curing ; cross reaction ; 13C-, 15N-, and 1H-NMR ; oxazolidinone ; carbamate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possible cross reactions indicated by solid-state NMR between cyanate functionalized resin and epoxy functionalized resin have been investigated by using both natural abundance and labeled monofunctional model compounds. These soluble products were isolated and purified by silica gel adsorption chromatography and gel permeation chromatography. They were fully characterized by high resolution 1H-, 13C-, 15N-NMR spectroscopy and by mass spectrometry. The major cross-reaction product is a racemic mixture of enantiomers, which contain an oxazolidinone ring formed by one cyanate molecule and two epoxy molecules. However, epoxy consumption lags cyanate consumption in the overall reaction as triazine formation from the cyanate is much faster than the two competing reactions, the cross reaction between cyanate and epoxy, and the self-polymerization of epoxy, under the conditions investigated. The cross reaction between cyanate and epoxy is limited. Approximately 12% of cross reaction between cyanate and epoxy was found in the overall reaction. In addition to the cross reactions of epoxy and cyanate, the reactions of epoxy and the carbamate, which is the major side product for the curing reaction of cyanate resin in solution, have also been investigated, and the mechanism of these reactions discussed. From the reactions of epoxy and carbamate, several products related to cross reaction between epoxy and cyanate have been isolated and identified. It is suggested that the reaction of epoxy and carbamate is one of the pathways in the overall cross reaction between epoxy and cranate resins. Finally, the mechanism of the overall cross-curing reaction between the diepoxy and dicyanate mixed resins is discussed. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2241-2249 
    ISSN: 0887-624X
    Keywords: iniferter ; living radical polymerization ; photopolymerization ; spin trapping ; dithiocarbamate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The photodissociation of several N,N-diethyldithiocarbamate derivatives (RDC), i.e., benzyl, 1-phenylethyl, 2-phenylethyl, n-butyl, sec-, and tert-butyl N,N-diethyldithiocarbamates, was investigated by the spin trapping technique to elucidate the polymerization mechanism of styrene (St) with RDC as iniferters. The scission of RDC occured at two different C—S bonds depending on the structure of the alkyl groups of RDC and the cleavage manner was dominated by both resonance and steric effects. It has been confirmed that RDC generating an N,N-diethyldithiocarbamyl radical acts as an effective iniferter and induces the living radical polymerization of St in homogeneous system. The polymerizations of St with tetraethylthiuram disulfide and p-xylylene bis(N,N-diethyldithiocarbamate) were also discussed on the basis of the results of the spin trapping for RDC as the model compounds of the poly(St) chain ends. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1481-1496 
    ISSN: 0887-624X
    Keywords: aliphatic-aromatic poly(amide-imide) ; trimellitic anhydride ; ω-amino acids ; triphenyl phosphite ; direct polycondensation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Seven imidodicarboxylic acids II-1 to 5, II-10, and II-11 were prepared from trimellitic anhydride and ω-amino acids, such as glycine, β-alanine, 4-aminobutyric acid, 5-aminopentanoic acid, 6-aminohexanoic acid, 11-aminoundecanoic acid, and 12-aminododecanoic acid. Several aliphatic-aromatic poly(amide-imide)s were prepared by triphenyl phosphite promoted polycondensation reaction from the combination of 3-(4-carboxyphthalimido)propionic acid (II-2) or 6-(4-carboxyphtalimido)hexanoic acid (II-5) with various aromatic diamines and of all the imidodiacids with p-phenylenediamine or 4,4′-oxydianiline. All poly(amide-imide)s were characterized by inherent viscosity, gel permeation chromatography (GPC) measurements, solubility, tensile test, wide-angle X-ray scatting patterns, differential scanning calorimetry (DSC) measurements, and thermogravimetric (TGA) analyses. Effects of structural changes such as polymethylene length and diamine moieties on the properties of poly(amide-imide)s were studied. © 1994 John Wiley & Sons, Inc.
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  • 83
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1539-1542 
    ISSN: 0887-624X
    Keywords: polymerization ; ethylene ; polyethylene ; catalyst ; zeolites ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ethylene polymerization has been studied in the presence of catalyst based on vanadium or vanadium-chromium supported on a zeolite HY. The effect of vanadium over chromium has been investigated as a function of the sequence of exchange of metals on the support and metal contents. Both effects were investigated in relation to the characteristics of the polyethylene (PE) obtained. Low activity has been found for the V (II) zeolite HY catalyst. Moreover, vanadium acts either as an inhibitor or as a promoter for the polymerizing activity of the Cr (III)/zeolite catalyst, depending on the preparation method. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2223-2227 
    ISSN: 0887-624X
    Keywords: bulk ; copolymerization ; reactivity ratios ; methyl acrylate ; vinyl esters ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The course of composition drift in copolymerization reactions is determined by reactivity ratios of the contributing monomers. Since polymer properties are directly correlated with the resulting chemical composition distribution, reactivity ratios are of paramount importance. Furthermore, obtaining correct reactivity ratios is a prerequisite for good model predictions. For vinyl acetate (VAc), vinyl 2,2-dimethyl-propanoate also known as vinyl pivalate (VPV), and vinyl 2-ethylhexanoate (V2EH), the reactivity ratios with methyl acrylate (MA) have been determined by means of low conversion bulk polymerization. The mol fraction of MA in the resulting copolymer was determined by 1H-NMR. Nonlinear optimization on the thus-obtained monomer feed-copolymer composition data resulted in the following sets of reactivity ratios: rMA = 6.9 ± 1.4 and rVAc = 0.013 ± 0.02; rMA = 5.5 ± 1.2 and rVPV = 0.017 ± 0.035; rMA = 6.9 ± 2.7 and rV2EH = 0.093 ± 0.23. As a result of the similar and overlapping reactivity data of the three methyl acrylate-vinyl ester monomer systems, for practical puposes these data can be described with one set of reactivity data. Nonlinear optimization of all monomer feed-copolymer composition data together resulted in rMA = 6.1 ± 0.6 and rVEst = 0.0087 ± 0.023. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2235-2239 
    ISSN: 0887-624X
    Keywords: tetrafluoroethylene ; propylene ; emulsion redox copolymerization ; fluoroelastomers ; polymerization mechanism ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Emulsion copolymerization of tetrafluoroethylene (TFE) and propylene (P) initiated by trilon-rongalite catalytic system containing tert-C4H9OH, initial monomer mixture, emulsifier (C7F15COONH4) concentration, and monomer mixture/water ratio on the polymerization rate (R) and molecular weight (M̄n) was investigated. Both R and M̄n increased considerably with TFE content in monomer mixture up to 75 mol %. Alternating rubber-like copolymers in a wide range of initial monomer mixture (from 55-85 mol %) were obtained. The reactivity ratio was found to be rTFE = 0.005 ± 0.04 and rp = 0.17 ± 0.07. Above the critical miscelle concentration, the effects of the initiating system Is and emulsifier Cs on R and M̄n were found to obey the following relations: \documentclass{article}\pagestyle{empty}\begin{document}$$ {R \propto [Is]^{0.54} \times [Cs]^{0.42} }\quad {{\rm and}}\quad {\bar M}_n \propto [Is]^{ - 0.1} \times [Cs]^{0.1} ,$$\end{document} according to which emulsion copolymerization proceeds by the I case of Smith-Ewart theory. Polymerization mechanism of the reaction studied was suggested. The copolymerization is mainly terminated by degradative chain transfer of the propagating radicals to propylene. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2251-2255 
    ISSN: 0887-624X
    Keywords: grafting ; spectroscopy ; N-vinyl carbazole ; cellulose-acetate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: N-vinyl carbazole (VCZ) was grafted on cellulose acetate film using simultaneous cobalt-60-γ ray irradiation grafting technique. Absorption, excitation, and emission spectral studies on the grafted film were carried out to ascertain the grafting of VCZ on the polymer matrix. Laser-flash photolysis studies with the solution of grafted film indicate the opening of the double bond of VCZ, which leads to the grafting. On the basis of the observed results, the mechanism of grafting in the system was proposed. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1877-1883 
    ISSN: 0887-624X
    Keywords: insoluble chelating polymers ; thiol ligand ; poly(ethylene glycols) chains ; functional polymers ; heavy metal ion recovery ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of chelating resins, derived from a macroreticular styrene-divinylbenzene (2%) copolymer beads grafted with various poly(ethylene glycols) HO—(—CH2—CH2—O—)n—H(n = 0, 4, 9, 13) and containing thiol groups as chelating functions, have been synthesized in a three-step reaction sequence. The structure of the functionalized resins was confirmed by IR spectrophotometry, elemental analysis, and differential scanning calorimetry. The complexation behavior of these thiol resins was investigated towards Hg(II), Cu(II), and Pb(II) ions in aqueous solution by a batch equilibration technique. The influence of pH on adsorption capacity was also examined. The adsorption values for metal ions' intake followed the order Hg(II) 〉 Cu(II) 〉 Pb(II). The affinity of these polymers towards Hg(II) ions was so high that the total mercury level in the liquid decreased from 20 ppm to below 10 ppb after 2 h of treatment. Polymers can be regenerated by washing with a solution of hydrochloric acid (6N) and 10% by weight of an aqueous solution of thiourea. © 1994 John Wiley & Sons, Inc.
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    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2543-2549 
    ISSN: 0887-624X
    Keywords: oxetane ; 19F-NKR ; triflic ; ring opening ; cationic polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The nature of ring-opening polymerization of oxetane derivatives initiated by triflic acid and triflic anhydride was investigated via 19F-NMR spectroscopy. Two types of propagating species, which were directly observed from the 19F-NMR spectra, were found to be oxonium macroions and triflic macroesters. These two propagating species established and equilibrium relationship during the polymerization process. The forming of oxonium macroion active species was highly dependent upon the substituents of the oxetane ring, and were enhanced when a more polar solvent was employed. The initiator effect, which occurred primarily in the initiating stage of the polymerization, is also discussed. © 1994 John Wiley & Sons, Inc.
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  • 89
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2565-2576 
    ISSN: 0887-624X
    Keywords: acrylate monomers ; polymerization kinetics ; stereostructure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of new unsaturated monomers containing functional groups has been theoretically analyzed by considering a simple kinetic scheme. In the reactions between acetyl and acryloyl chloride with neopentylglycol, it was shown that the comparison between theoretical and experimental results, does not allow us to conclude that the two rate constants controlling the reactions are equivalent. Kinetic experiments of the polymerization of 3-hydroxyneopentyl acrylate were carried out in benzene and 1,4-dioxane solution at different temperatures. Dilatometric techniques and nonlinear least-squares methods were used to obtain kinetic data and to determine the kinetic constants, respectively. The values of \documentclass{article}\pagestyle{empty}\begin{document}$k_p /k_t^{1/2}$\end{document} for this monomer were found higher in dioxane than in benzene due, probably, to the fact that in the last solvent the polymerization is heterogeneous. The activation energy, determined by using different values of \documentclass{article}\pagestyle{empty}\begin{document}$k_p /k_t^{1/2}$\end{document} was found 7.6 kcal/mol. The stereostructure of the polymers derived from 3-hydroxyneopentyl acrylate and 3-acetoxyneopentyl acrylate was determined by 13C-NMR spectroscopy from the analysis of the resonance signals belonging to the carbonyl groups, obtaining values for the fraction of isotactic dyads in the range 0.36 ± 0.03 for both polymers. Finally, the glass transition temperatures of both polymers, determined calorimetrically, were found 281 and 255 K, respectively. © 1994 John Wiley & Sons, Inc.
    Additional Material: 15 Ill.
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  • 90
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1899-1902 
    ISSN: 0887-624X
    Keywords: poly(p-phenylenebenzobisoxazole) ; poly(terephthalic acid anhydride) ; 1,3-diamino-4,6-dihydroxybenzene ; polyphosphoric acid ; intrinsic viscosity ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High molecular weight poly(p-phenylenebenzobisoxazole) (PBO) was prepared from poly(terephthalic acid anhydride) (PTAA) and 1,3-diamino-4,6-dihydroxybenzene dihydrogenchloride in polyphosphoric acid (PPA). PTAA may react directly with the o-aminophenol groups to form benzoxazoles or react with PPA to generate terephthalic acid (TA) of very small particle size, which dissolves readily in PPA. PTAA provides the advantages of bypassing the requirement of small particle size TA, reducing the amount of water liberated by half, and possibly providing faster kinetics in PBO synthesis. © 1994 John Wiley & Sons, Inc.
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  • 91
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1923-1929 
    ISSN: 0887-624X
    Keywords: thermotropic copolyamides ; p-aminobenzoic acid ; p-phenylenediamine ; monomer sequence ; triethyleneglycol bis(4-carboxyphenyl)ether ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Copolycondensations of triethyleneglycol bis(4-carboxyphenyl)ether (PEG3), p-amino-benzoic acid (PABA), and p-phenylenediamine (PPD) were studied in order to examine the effect of monomer sequences in the copolyamides upon the transition temperatures of the resulting copolymers. Random copolymerization of these monomers resulted in the copolymers exhibiting a nematic mesophase in a wide range of PABA content. On the other hand, the sequential copolymers composed of PABA/PPD = 1/1 and 2/1, which were prepared from 4,4′-diaminobenzanilide (DABA) and N,N′-bis(4-aminobenzoyl)-p-phenylenediamine (BAB-PPD), respectively, did not show a mesophase. The copolymers of a diamine combination of DABA and PPD exhibited a nematic mesophase, despite the lack of a mesophase for each homopolymer. The combinations of DABA and other diamines were also examined. © 1994 John Wiley & Sons, Inc.
    Additional Material: 4 Ill.
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  • 92
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 1957-1968 
    ISSN: 0887-624X
    Keywords: radical polymerization ; alkyl crotonate ; 1,2-disubstituted ethylene ; propagation rate constant ; termination rate constant ; substituted polymethylene ; thermal property ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Radical polymerization of several alkyl crotonates (RCr) was carried out in bulk or in benzene in the presence of radical initiators. Homopolymerization of RCr bearing bulky ester alkyl groups, e.g. tert-butyl (tBCr), 1-adamantyl (AdCr), and 3,5-dimethyl-1-adamantyl crotonate (DMAdCr) proceeded to give a polymer with molecular weight of several thousands despite of the steric hindrance and chain transfer by the presence of the β-methyl group, while the methyl and ethyl esters gave no polymer. The kinetics of the polymerization was examined in detail and absolute rate constants were evaluated by means of electron spin resonance spectroscopy. The propagation rate constants of RCr were 0.41-1.0 L/mol s, being much smaller than those of the corresponding methacrylates (530-570 L/mol s). The termination rate constants were also determined from the analyses of steady state and non-steady state polymerizations. Radical copolymerizations of AdCr (M2) with several vinyl monomers (M1) were carried out in bulk at 60°C and the rate constants for cross propagations were calculated to examine reactivities of the monomer and its polymer radical. The structure and thermal properties of the resulting poly (AdCr) were also investigated. Onset temperature of decomposition and glass transition temperature of poly(AdCr) were revealed to be much high as 302 and 234°C, respectively. © 1994 John Wiley & Sons, Inc.
    Additional Material: 14 Ill.
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  • 93
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2093-2098 
    ISSN: 0887-624X
    Keywords: high-performance aromatic polyethers ; aromatic nucleophilic substitution polymerization ; aromatic polyethers containing triazine ; thermal behavior ; high-temperature polymers ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of new poly(arylene ether phenyl-s-triazine)s was prepared by the nucleophilic aromatic substitution polymerization of the potassium salt of bisphenols with 2,4-bis (halophenyl)-6-phenyl-s-triazine in N-methyl-2-pyrrolidone at elevated temperature. The polymers with inherent viscosities exceeding 0.5 were obtained after polymerization for 1 h using 2,4-bis(fluorophenyl)-6-phenyl-s-triazine as a monomer. The glass transition temperatures of the resulting polymers ranged from 200 to 260°C depending on the bisphenol used in the polymer synthesis. The poly(arylene ether phenyl-s-triazine)s demonstrated excellent thermal stabilities in excess of 490°C (5% weight loss in air). The isothermal TGA measurements (400°C under air or nitrogen atmosphere) revealed that the 4,4'-biphenol- and hydroquinone-based poly(arylene ether phenyl-s-triazine)s belong to the most superior class of heat resistant polymers, such as polyimide Kapton™. The mechanical properties of these polymers are also described. © 1994 John Wiley & Sons, Inc.
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  • 94
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2119-2126 
    ISSN: 0887-624X
    Keywords: poly(phosphate ester)s ; liquid crystalline polymer ; smectic phase ; thermal stability ; biodegradation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Poly(phosphate ester)s, PPE 1a-d, were synthesized from polycondensation of methyl phosphorodichloridate (MPDC) with various bisphenols such as 4,4′-biphenol 1a, 4,4′-dihydroxyphenylether 1b, bis(4-hydroxyphenyl)methane 1c, and 3,3′-dimethyl-4,4′-dihy-droxybiphenyl 1d. PPE 2a-d with hexamethylene spacers were also obtained from poly-condensation of MPDC with 4,4′-bis(6-hydroxyhexyloxy)biphenyl 2a, 4,4′-di(6-hydroxyhexyloxy)phenyl ether 2b, bis[4-(6-hydroxyhexyloxy)phenyl]methane 2c, and 3,3′-dimethyl 4,4′-di(6-hydroxyhexyloxy)biphenyl 2d. The degree of crystallinity of PPE 1a-1d without hexamethylene spacer was 3.3-17.6%, whereas PPE 2a and PPE 2b which exhibit mesomorphic behavior were 20.1 and 18.6%, respectively. PPE 2a and PPE 2b show the mesophase at 139.6-195.5°C and 42.4-66.3°C, respectively. PPE 2c and PPE 2d were obtained as rubbery. From pyrolysis of PPE in air the temperature corresponding to 5% weight loss was found to be 322-408°C and 284-291°C for PPE 1 and PPE 2, respectively. It was also found that PPE 2a was enzymatically degraded by phospholipase C. © 1994 John Wiley & Sons, Inc.
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  • 95
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2161-2168 
    ISSN: 0887-624X
    Keywords: emulsion copolymerization ; composition drift ; modelling ; sensitivity analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Recently a model has been developed capable of predicting absolute monomer concentrations and their ratios in the polymer, aqueous, and monomer droplet phases as a function of conversion in batch emulsion copolymerizations without using any adjustable parameters. In this article the sensitivity of model predictions of composition drift toward deviations of 10% in all model parameters (maximum swellabilities of monomer in the polymer phase, water solubilities, reactivity ratios, and monomer and polymer densities) was estimated using the monomer combination methyl methacrylate-styrene as an example. From the sensitivity analysis it can be concluded that the reactivity ratios are the most important parameters affecting composition drift. The effects of deviations in maximum swellabilities and monomer and polymer densities on composition drift can be neglected, while the water solubility is important only in those cases where the amount of monomer in the aqueous phase cannot be neglected as compared with the total monomer amount. © 1994 John Wiley & Sons, Inc.
    Additional Material: 6 Ill.
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  • 96
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2099-2110 
    ISSN: 0887-624X
    Keywords: polylactide ; macromonomer ; ring-opening polymerization ; graft copolymers ; amphiphilic gel ; biocompatible ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The functional aluminum alkoxide, Et2Al—O—(CH2)2—O-C(O)—C(CH3)=CH2, is a very effective initiator for the (D,L)-lactide (LA) polymerization in toluene at 707deg;C. The coordination-insertion type of polymerization is living and exclusively yields linear P (D,L)-lactide macromonomers of a predictable molecular weight and a narrow molecular weight distribution. IR and 1H-NMR studies show that the methacryloyl group of the initiator is selectively and quantitatively attached to one chain end, whereas the second extremity is systematically a hydroxyl function resulting from the hydrolysis of the living growing site. α,ω-Dimethacryloyl-P(D,L)-lactides, i.e., α,ω-macromonomers, have also been successfully synthesized by the additional control of the termination step, i.e., by reaction of Al alkoxide end groups with methacryloyl chloride. α-Macromonomer and α,ω-macromonomer P(D,L)-lactides are easily free-radical copolymerized with 2-hydroxyethyl methacrylate (HEMA), resulting in a hydrophilic poly (HEMA) backbone grafted with hydrophobic P(D,L)-lactide subchains and a biodegradable amphiphilic network, respectively. © 1994 John Wiley & Sons, Inc.
    Additional Material: 10 Ill.
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  • 97
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2629-2639 
    ISSN: 0887-624X
    Keywords: molecular composite ; liquid-crystalline polymer ; lyotropic polyamide ; polyimide ; semi-interpenetrating polymer network ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2,2'-Dimethyl-4,4'-diamino-biphenyl was used to prepare a lyotropic amine-terminated polyamide (PBTA) prepolymer with terephthaloyl dichloride, and an amide oligomer with reactive endcaps of maleimide, respectively. The former was employed in an attempt to increase the solubility of PA/PI block copolymers, and the latter to produce a three-dimensional (isotropic) reinforced molecular composite through the technology of a semiinterpenetrating polymer network (semi-IPN). PBTA prepolymer was copolymerized with an amine-terminated polyimide via a coupling reaction using terephthaloyl dichloride. The resultant block copolymers were characterized by IR, NMR, ηinh and GPC to confirm that the copolymerization reaction was precisely accomplished, as well as to determine their composition and molecular weight. Thermal analysis and lyotropic behavior were also studied for these copolymers. Rigid-rod amide oligomer was crosslinked in the presence of another flexible polyimide. Five sets of semi-IPN films were prepared under varying compositions. The curing conditions were investigated by DSC; in addition, the cured semi-IPNs exhibited a single phase (1 Tg) according to examination by an instrument for thermally stimulated current (TSC). No large-scale phase separation was observed in SEM images of the fractured surfaces. © 1994 John Wiley & Sons, Inc.
    Additional Material: 8 Ill.
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  • 98
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2677-2686 
    ISSN: 0887-624X
    Keywords: polystyrene-based ionomers ; cationic ionomers ; nucleophilicity ; phasetransfer catalysts ; quaternary salts ; triphase catalysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polystyrene-based crosslinked cationic ionomers containing ammonium or phosphonium chlorides (AxRCI and PxBuCI) were reacted with decyl methanesulfonate. The kinetic data were correlated with the swelling behavior of the ionomers and the solution viscosity of the corresponding linear ionomers. The reactivity of the ionomers was independent of the particle size of the ionomer beads, indicating no diffusion control of the reaction. The solvent and the ion content of the ionomers greatly affect the reactivity. In nonpolar solvents with a low acceptor number, AN, such as toluene, the aggregation of ionic groups with an increasing ion content reduces the reactivity. A solvent with a high value of AN, such as chloroform, led a very low reactivity independent of the ion content. Aprotic polar solvent, such as acetonitrila, promoted the dissociation of the ionic groups and furnished a relatively high reactivity independent of the ion content. Several catalytic substitution reactions were carried out under liquid-solid-solid triphase conditions. The kinetic results were accounted for in terms of slow nucleophile transport and fast chemical reaction within the ionomer particles. © 1994 John Wiley & Sons, Inc.
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  • 99
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2727-2737 
    ISSN: 0887-624X
    Keywords: fullerenes ; carbazole ; acid catalyzed alkylation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new homogeneous fullerenated carbazole polymer has been synthesized, revealing a new substitution pattern for carbazole and a new photodecomposition-resistant substitution pattern for fullerenes. The synthetic method may be accomplished in one pot via acid catalyzed alkylation. The new polymer has several unusual photovoltaic, charge storage, and photoconductivity capabilities. © 1994 John Wiley & Sons, Inc.
    Additional Material: 13 Ill.
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  • 100
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    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 32 (1994), S. 2755-2763 
    ISSN: 0887-624X
    Keywords: photopolymerization ; propenyl ethers ; cationic polymerization ; diaryliodonium salt ; triarylsulfonium salt ; free radicals ; inhibition ; 1,2,3-tris (1-propenoxy) propane ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of 1,2,3-tris (1-propenoxy) propane (GTPE) was carried out by the rearrangement of 1,2,3-tris(2-propenoxy) propane (glycerol triallyl ether, GTAE) and the Z: E isomer composition of the GTPE was determined using gas chromatography and 1HNMR. The photoinitiated cationic polymerization of the GTPE was studied using realtime infrared spectroscopy (RTIR). Employing the data from these studies, rates of polymerization for the respective E and Z propenyl ether double bonds were calculated. The rate of incorporation of Z-double bonds of GTPE into the crosslinked polymer matrix is 1.6 times that of E-double bonds. The effects of oxygen and several other free radical polymerization inhibitors were investigated. An increase in the photogel time and decrease of the gel-content in the presence of these inhibitors implicates the involvement of free radicals in the process of the generation of propagating cationic centers when diaryliodonium salt cationic photoinitiators are used. © 1994 John Wiley & Sons, Inc.
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