Laboratory melts

Figure 3.18 Laboratory melt polymerization setup (a) 250 mL (b) 50-mL reactor in either oil bath or heating block.

The use of mechanical stirrers (forced convection) is a special case of intensive homogenization. In practice, the method has been used for many years in the manufacture of optical glasses and has more recently also been introduced into tank furnaces for other glasses. Quantitative evaluation of the mixing effect has so far only been carried out on models and in laboratory melting (e.g. Cable and Hakim, 1972). 

Flow Rate Ratio. The FR ratio is used as a rough estimate of the MWD of a resin. Molecular weight distribution can be measured directly by gel permeation chromatography, but this is a time-consuming, technically challenging measurement that is not commonly found in quality control laboratories. Melt-flow ratio measurements are easily done, since the MFR of a resin is the flow index of the sample divided by the melt index of the sample. 

This is one of the most familiar types of structure in inorganic chemistry. The crystals can usually be melted in the laboratory... 

The sodium fusion and extraction, if performed strictly in accordance with the above directions, should be safe operations. In crowded laboratories, however, additional safety may be obtained by employing the follow ing modification. Suspend the hard-glass test-tube by the rim through a hole in a piece of stout copper sheet (Fig. 69). Place 1 -2 pellets of sodium in the tube, and heat gently until the sodium melts. Then drop the organic compound, in small quantities at a time, down — =. the tube, allowing the reaction to subside after each addition before the next is made. (If the compound is liquid, allow two or three small drops to fall at intervals from a fine dropping-tube directly on to the molten sodium.) Then heat the complete mixture as before until no further reaction occurs. 

The term distillation is applied to vaporisation and subsequent condensation according to (i) it should also be applied to (ii) since it is really the liquid which is converted into vapour and is first formed by condensation. Strictly speaking, the term sublimation should be applied to changes according to (iii). However, in practice, a substance when heated may first melt and then boil, but on cooling it may pass directly from the vapour to the solid the process is then also called sublimation. Indeed the mode of vaporisation, whether directly from solid to vapour or through the intermediate formation of a liquid, is of secondary importance it is the direct conversion of vapour to solid which is really the outstanding feature of sublimation in the laboratory. 

The comparatively inexpensive long-scale thermometer, widely used by students, is usually calibrated for complete immersion of the mercury column in the vapour or liquid. As generally employed for boiling point or melting point determinations, the entire column is neither surrounded by the vapour nor completely immersed in the liquid. The part of the mercury column exposed to the cooler air of the laboratory is obviously not expanded as much as the bulk of the mercury and hence the reading will be lower than the true temperature. The error thus introduced is not appreciable up to about 100°, but it may amount to 3-5° at 200° and 6-10° at 250°. The error due to the column of mercury exposed above the heating bath can be corrected by adding a stem correction, calculated by the formula ... 

PRELIMINARY LABORATORY OPERATIONS III.l. DETERMINATION OF MELTING POINTS... 

National Institute of Standards and Technology (NIST). The NIST is the source of many of the standards used in chemical and physical analyses in the United States and throughout the world. The standards prepared and distributed by the NIST are used to caUbrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. At present, over 1200 Standard Reference Materials (SRMs) are available and are described by the NIST (15). Included are many steels, nonferrous alloys, high purity metals, primary standards for use in volumetric analysis, microchemical standards, clinical laboratory standards, biological material certified for trace elements, environmental standards, trace element standards, ion-activity standards (for pH and ion-selective electrodes), freezing and melting point standards, colorimetry standards, optical standards, radioactivity standards, particle-size standards, and density standards. Certificates are issued with the standard reference materials showing values for the parameters that have been determined. 

Hot tack strength is the abiUty of a heat-seal layer to hold together while molten, before the seal cools and sets up. This is a technically important property which is difficult to measure reproducibly in the laboratory. Owing to the reinforcing effect of ionic bonding on melt strength, ionomer sealing layers provide superior performance in a wide spectmm of appHcations. 

Dense Symmetrical Membranes. These membranes are used on a large scale ia packagiag appHcations (see Eilms and sheeting Packaging materials). They are also used widely ia the laboratory to characterize membrane separation properties. However, it is difficult to make mechanically strong and defect-free symmetrical membranes thinner than 20 p.m, so the flux is low, and these membranes are rarely used in separation processes. Eor laboratory work, the membranes are prepared by solution casting or by melt pressing. 

Many polymers, including polyethylene, polypropylene, and nylons, do not dissolve in suitable casting solvents. In the laboratory, membranes can be made from such polymers by melt pressing, in which the polymer is sandwiched at high pressure between two heated plates. A pressure of 13.8—34.5 MPa (2000—5000 psi) is appHed for 0.5 to 5 minutes, at a plate temperature just above the melting point of the polymer. Melt forming is commonly used to make dense films for packaging appHcations, either by extmsion as a sheet from a die or as blown film. 

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