Search results for "molar mass distribution"
showing 10 items of 115 documents
Characterization of Chemical Composition along the Molar Mass Distribution in Polyolefin Copolymers by GPC Using a Modern Filter-Based IR Detector
2013
Summary Gel permeation chromatography (GPC), also known as size exclusion chromatography (SEC), is the technique routinely used at high temperature to analyze the molar mass distribution in polyolefins. The distribution of comonomer along the molar mass distribution in a copolymer is a key microstructural feature that determines the macroscopic properties of the material, and thus, its range of possible applications and performance. The direct coupling of a modern filter-based infrared (IR) detector to a high temperature GPC instrument, by means of a heated flow-through cell, is here described. The analyses are carried out by recording the continuous IR absorbance chromatograms at selected …
High molecular arborescent polyoxyethylene with hydroxyl containing shell
2004
Abstract Arborescent polyoxyethylene of high molar mass (2×10 5 g/mol) and narrow molar mass distribution was synthesized in a three-stage process. In the first stage a triblock copolymer of ethylene oxide (central block, DP ca. 90) and 2,3-epoxypropanol-1 (short flanking blocks, DP ca. 5) was synthesized. The potassium alcoholate derived from this copolymer was used to initiate the polymerization of ethylene oxide and the subsequent addition of protected glycidol (1-etoxyethyl glycidyl ether). After deprotection the short polyglycidol blocks were used as branching units for the next generation. Repeated step by step process leads to the ‘pom-pom like’ branched polyoxyethylene macromolecul…
Über den absolutwert des fehlers bei der bestimmung von molekulargewichtsverteilungen mit der GPC-methode (messungen an polymethylmethacrylaten)
1970
Die Gelpermeationschromatographie (GPC) liefert unter konventionellen und definierten Bedingungen Molekulargewichtsverteilungen, die i. allg. um einen bestimmten Betrag zu breit sind. Um diesen Fehler quantitativ zu bestimmen, werden Fraktionen von Polymethylmethacrylat (PMMA) hergestellt, deren Uneinheitlichkeit (Mw/Mn - 1) durch osmotische und Lichtstreuungs- bzw. viskometrische Messungen bestimmt werden. Ferner werden unter definierten Bedingungen Polymerisate hergestellt, deren Uneinheitlichkeit durch die Kinetik und andere Kontrollen festgelegt ist. Unter Verwendung dieser Werte kann man Mw/Mn an PMMA auf wenige Prozent genau bestimmen und Molekulargewichtsverteilungen auf Grund korrig…
Synthesis of block copolymers with poly(methyl methacrylate): P(B-b-MMA), P(EB-b-MMA), P(S-b-B-b-MMA) and P(S-b-EB-b-MMA)
1993
Well-defined diblock copolymers poly(butadiene-b-methyl methacrylate) (=P(B-b-MMA)) and triblock copolymers poly(styrene-b-butadiene-b-methyl methacrylate) (=P(S-b-B-b-MMA)) have been prepared by sequential anionic polymerization in THF. The synthesis of P(B-b-MMA) and P(S-b-B-b-MMA) was most efficient in the presence of lithium alkoxides. By this method side reactions are suppressed and the polymerization can be performed at higher temperatures. The resulting triblock copolymers have narrow molecular weight distribution. The 1,2-PB midblock was quantitatively hydrogenated with tosylhydrazide to enhance thermal stability. Alternatively the hydrogenation can be performed at elevated pressure…
Testing of a kinetics equation of mechanical degradation
1987
A modification of the kinetics equation of mechanical degradation of Harrington and Zimm is proposed to fit experimental data taken on a molten polystyrene. This equation is applied to each molecular weight of the discretized molecular weight distribution curve, and the limiting molecular weight is determined for each molecular weight. With this modification the theoretical curves fit both Mw and Mn curves well.
Direct synthesis of fibrous high molecular weight polyethylene using vanadium catalysts supported on an SiO2ionic liquid system
2015
Polyethylene of fibrous morphology was obtained using Cp2VCl2 and VCl2(salenCl2) catalysts activated by AlEt2Cl and AlEtCl2 and heterogenized on a supported ionic liquid system prepared with SiO2 and 1-(3-triethoxysilyl)propyl-3-methylimidazolium chloroaluminate. The fibre length ranges from 15 to 60 µm, depending on the reaction conditions. The polyethylene is characterized by a high molecular weight ((1.1–2.4) × 106 g mol−1) and a narrow molecular weight distribution (1.4–2.5). It is a linear polymer, properly without branching. The DSC method reveals characteristic changes in melting temperature and crystallinity degree between the first and second scan heating cycles (141 °C and 136 °C,…
One-pot synthesis and characterization of aliphatic poly(oxytetramethylene) ionene
2002
Abstract One-pot synthesis of poly(oxytetramethylene) ionene (POI) composed of one dimethylammonium group in each repeating unit is described. POI was prepared by using the cationic polymerization of tetrahydrofuran, followed by the chain extension reaction of living poly(oxytetramethylene) (POTM) chain with N , N -dimethylaminotrimethylsilane. The weight average molecular weight of the ionene with bromide counter-anion (POI–Br) was 48,000 g/mol and the molecular weight of POTM between the ionic sites was ca. 2100. POI–Br showed polyelectrolyte behavior in polar solvent. The elastomeric film of POI–Br was prepared: its tensile strength at break and elongation at break were ca. 11 MPa and ca…
Size-Exclusion Chromatographic Determination of Polymer Molar Mass Averages Using a Fractal Calibration
2005
The characterization of polymers by size-exclusion chromatography basically consists of the determination of the weight-average molar mass (Mw), number-average molar mass (Mn), and polydispersity index (I). An accurate estimation of these magnitudes requires the use of a reliable and trusted calibration curve. Three procedures for building up a calibration curve are analyzed in this work. The first is the classical universal calibration (UC), based on the elution of tetrahydrofuran-polystyrene in a system as reference. The second is based on the proper calibration curve made with standards of the sample under study. However, two main drawbacks arise when using these methodologies: the nonfu…
Apparent Molar Mass of a Polyelectrolyte in an Organic Solvent in the Low Ionic Strength Limit As Revealed by Light Scattering
2013
The apparent molar mass of a partially quaternized poly-2-vinylpyridines (degree of quaternization 4.3% < Q < 35%) in 1-propanol is measured by light scattering at low ionic strength (10–6 M < cs < 10–3 M) as a function of polyion repeat unit concentration (7 × 10–5 monomol/L < cm,p < 4 × 10–2 monomol/L). No dialysis was applied prior to measurements. The apparent molar mass under “salt-free” conditions is smaller than the true molar mass by an order of magnitude, while approaching the true value at higher ionic strength. Concomitant data on the dependence of scattering intensity on scattering wave vector show that the dilute polyelectrolyte solutions are strongly correlated. A recent theor…
Characterization of lignin dissolved during alkaline pretreatment of softwood and hardwood
2015
Various alkaline pretreatments were applied to Scots pine (Pinus sylvestris) and silver/white birch (Betula pendula/pubescens) wood chips and the characterization of sulfur-free lignin dissolved was performed. The behavior of lignin during these pretreatments (alkali charge 1–8% NaOH, time 30–120 minutes, and temperature 130–150°C) was studied mainly in terms of lignin removal efficiency and molar mass distribution of dissolved lignin. The amount of lignin in pretreatment liquors increased along with an increase in the alkali charge of 0.8–4.4% and 0.6–3.4% of o.d. pine and birch wood, respectively. The most significant parameter affecting the molar mass of the dissolved lignin was shown to…