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(d ) Procedure. Transfer 2.5 grams (accurately weighed to nearest 0.001 gram) of the polymer to the resin kettle. Add 1 liter of solvent and clamp top in position. Start water flowing through jacket of the reflux condenser and apply air pressure to the stirring motor to produce vigorous agitation. Turn on heating jacket with transformer set at a predetermined voltage to bring the temperature of the contents to 50 deg.C within 20-25 minutes. As the thermometer reading approaches 45 deg.C-47 deg.C, reduce the voltage to the predetermined setting that will just maintain the temperature at 50 deg.C. Do not overshoot the prescribed temperature. Should this occur discard the test and start afresh. Exactly 2 hours after the solvent temperature has reached 50 deg.C, disconnect the heater, remove the resin kettle from the heating jacket, and decant the solvent, while still warm, through a coarse filter paper placed on top of a fritted-glass funnel, collecting the filtrate in a tared, glass-stoppered Erlenmeyer flask of 1-liter capacity. Determine the weight of the filtrate recovered to the nearest gram. Recovery should be at least 90 percent of the original solvent. Losses due to evaporation during heating and filtering have been found not to exceed 10 percent. Transfer about half of the solvent filtrate to a 1-liter beaker placed on an opening in the steam bath and immediately cover with the special "gas" cover, the inlet tube of which has been attached with flexible tetrafluoroethylene tubing to a source of high-purity nitrogen in series with a stainless steel heating coil immersed directly in the body of the steam bath. Maintain a positive flow of warm nitrogen gas throughout the evaporation of the solvent, adding the remainder of the filtrate from the Erlenmeyer flask as the evaporation proceeds. When the volume of the solvent has been reduced to about 50 milliliters, transfer the concentrated liquid to a previously tared weighing dish of suitable size. Wash the beaker twice with 20-30 milliliter portions of warm solvent, adding the washings to the weighing dish while continuing to evaporate the remainder of the solvent under the gas cover with its flow of warm nitrogen directed toward the center of the dish. In the event that an insoluble residue that cannot be removed with warm solvent remains in the beaker, it may be necessary to heat with a small amount of a higher boiling solvent such as benzene or toluene, transferring these washings to the weighing dish before final evaporation to dryness. Transfer the weighing dish with its residue to a vacuum desiccator, and allow it to remain overnight (at least 12 hours), after which the net weight of the dry residue is determined to the nearest 0.0001 gram. Correct the result for any solvent blank equivalent to the nonvolatile matter determined to be contained in the amount of solvents used in the test.
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(c ) Procedure. Transfer 5 grams +/-0.001 gram of sample to the resin kettle, add 1,000 milliliters (840 grams) of xylene, and clamp top in position after inserting a piece of glass rod to prevent bumping during reflux. Start water flowing through the jacket of the reflux condenser and apply full voltage (115 volts) to the heating mantle. When the xylene starts to boil, reduce the voltage to a level just sufficient to maintain reflux. After refluxing for at least 2 hours, disconnect the power source to the mantle, remove the kettle, and allow to cool in air until the temperature of the contents drops to 50 deg.C, after which the kettle may be rapidly cooled to 25 deg.C-30 deg.C by immersing in a cold water bath. Transfer the kettle to a constant temperature bath set to maintain 25 deg.C +/-0.1 deg.C, and allow to equilibrate for a least 1 hour (may be left overnight if convenient). Break up any precipitated polymers that may have formed, and decant the xylene solution successively through a fast filter paper and then through a fritted-glass filter into a tared 1-liter Erlenmeyer flask, collecting only the first 450 milliliters - 500 milliliters of filtrate (any attempt to collect more of the xylene solution usually results in clogging the filter and risking losses). Reweigh the Erlenmeyer flask and calculate the weight of the filtrate obtained to the nearest 0.1 gram. Transfer the filtrate, quantitatively, from the Erlenmeyer flask to the 1-liter beaker, insert the beaker in its heating mantle, add a glass-coated magnetic stirring bar, and mount the gas cover in place, connecting the inlet tube to the nitrogen source and the outlet to the condenser of the receiving flask. Start a flow of nitrogen (2 to 3 liters per minute) into the gas cover and connect an aspirator to the receiver using a free-flow rate equivalent to 6-7 liters of air per minute. With the infrared lamp on, adjust the voltage to the heating mantle to give a distillation rate of 12-13 milliliters per minute when the magnetic stirrer is revolving just fast enough to promote good boiling. When the volume of solvent in the beaker has been reduced to 30-50 milliliters, transfer the concentrated extractive to a suitable weighing dish that has been previously tared (dry). Rinse the beaker twice with 10-20 milliliter portions of fresh xylene, adding the rinsings to the weighing dish. Evaporate the remainder of the xylene on an electric hotplate set at low heat under the gas cover with a stream of nitrogen directed toward the center of the dish. Avoid any charring of the residue. Transfer the weighing dish to a vacuum desiccator at room temperature and allow to remain under reduced pressure for at least 12 hours (overnight), after which determine the net weight of the residue to the nearest 0.0001 gram. Correct the result for nonvolatile solvent blank obtained by evaporating the equivalent amount of xylene under identical conditions. Calculate the weight of residue originally present in the total weight of solvent (840 grams), using the appropriate factor based on the weight of filtrate evaporated.