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KV 1.17 Elevation of the boiling point Materials Frame for complete experiments Rear cover for complete experiment panel Panel for complete experimental set-ups Shelf with hanging device Clamping holder, d = 18...25 mm Apparatus carrier with fixing magnets Apparatus holder, variable Spring plugs, 50 pieces G-clamp Round bottom flask, short-necked, DURAN, 250 ml, GL 25/12 Gaskets for GL 18, 8 mm hole, 10 pcs, 1 only Apparatus for boiling point elevation Silicone tubing, d = 7 mm Pinchcock, width 15 mm Temperature probe, immersion type, Teflon Pt100 Digital thermometer 4-2 45500.00 45501.00 45510.00 45505.00 45520.00 45525.00 45526.00 45530.00 02014.00 2 1 1 1 2 1 1 1 4 35812.15 1 41242.03 36820.00 39296.00 43631.15 1 1 1 1 11759.04 13617.93 1 1 Heating mantle in metal housing, 250 ml Support clamp for the housing of heating mantle Power regulator Beaker, DURAN, tall form, 250 ml Pellet press Spoon with spatula end, l = 150 mm, steel, micro Funnel, glass, d = 80 mm Laboratory balance with RS 232, 80/160/320 g Weighing dish, 80 x 50 x 14 mm Tweezers, l = 200 mm, straight, blunt, st. steel Wash bottle, 500 ml Boiling stones, 200 g Urea, 250 g Water, distilled, 5 l Vice 47550.93 1 47557.01 32247.93 36004.00 04403.04 1 1 1 1 33393.00 34459.00 1 1 48800.93 45019.05 1 1 40955.00 33931.00 36937.20 30086.25 31246.81 1 1 1 1 1 Fig. 1 Phywe series of publications • Complete Experiments Chemistry/Biotechnology • © PHYWE SYSTEME GmbH • D-37070 Goettingen 13102 73 KV 1.17 Elevation of the boiling point Safety measures Wear protective goggles. Observe the detailed information on safety measures in the appendix. (Should the experiment be carried out with other substances, ensure that the appropriate safety instructions are followed) Preparation Several separate determinations must be made to investigate the dependence of the elevation of the boiling point on the concentration. It is best to increase the concentration of the test solution by adding small portions of the substance to be dissolved (in this case, urea). These portions can be prepared prior to the experiment using a pellet press. The pellet press consists of a cylinder and a long and a short plunger. To prepare a pellet, fit the short plunger into the cylinder through the end without side slits. Fill a level spatula of substance into the press, then close it with the long plunger. Clamp the press in a vice to press the plungers against each other. The resulting pellet has a mass of between 0.200 g and 0.450 g. Weigh it to an accuracy of 1 mg! At least 4 pellets should be prepared prior to the experiment. Set-up Position the clamping holders on the panel for complete experiments as shown in Fig. 2. Subsequently assemble and fix the apparatus to the panel as shown in Fig. 1. When assembling the apparatus for boiling point elevation, ensure that the inlet opening in the wall of the vessel is below the sealing ring. In addition, ensure that the gasket of the 250 ml glass flask is replaced by a gasket with an 8 mm hole (see the list of materials). Fig. 2 74 13102 Phywe series of publications • Complete Experiments Chemistry/Biotechnology • © PHYWE SYSTEME GmbH • D-37070 Goettingen KV 1.17 Elevation of the boiling point Procedure First weigh the inner vessel without content, then pour about 40 ml of water into it and assemble the apparatus for the elevation of the boiling point (refer here to Fig. 3 and to the operating instructions supplied with this apparatus). Pour 150 to 200 ml of water into the 250 ml round bottom flask and add a few boiling stones. The hose clip on the lower silicone tube must be open. Neither of the tubings should reach to the bottom of the beaker! Heat the water in the round bottom flask with maximum power, at step 10 on the power regulator. As soon as the water boils, the power regulator setting can be reduced to step 8. After boiling for some minutes, close the lower silicone tube with the hose clip. Hot steam flows into the inner vessel and heats up the water there. The actual experiment begins when the water in the inner vessel has reached a constant temperature of around 100°C. This takes about half an hour! It is therefore recommended that the water be heated up prior to the start of the lesson, or that at least hot water be prepared. This can then be filled into the apparatus instead of cold water – important is the determination of the mass (not the volume) of the water filled into the inner vessel. The time to start of measurement is greatly shortened. As soon as a constant temperature has been attained in the inner vessel, switch the temperature measuring instrument to the operating mode for change in temperature (see the operating instructions for the measuring instru- ment). This has a resolution of one hundredth of a degree. Open the upper closure of the inner vessel, which holds the temperature probe and, as quickly as possible, drop in one of the urea pellets and close the vessel. After a short time, read off the difference in temperature between the now elevated boiling point and the boiling point of the plain water. Repeat this procedure with as many urea pellets as intended. At least four are recommended for a graphical plot. On completion of the measurements, first open the hose clip on the lower silicone tube. This avoids a sucking over of liquid from the inner vessel into the round bottom flask that would otherwise result from the volume contraction when the apparatus cools. Should this happen, it would prevent an accurate determination of the contents of the inner vessel. Only after having opened the hose clip, lower the heating mantle and switch it off! Now disassemble the boiling point apparatus(Caution! Still hot!) and re-weigh the inner vessel. The difference in mass of the full and the empty vessel gives the mass of solution. The mass of water is given from the mass of the solution less the mass of the ureas pellets used. Observations After each addition of a compressed portion of urea, the boiling temperature drops briefly and then increases by a few hundredths of a degree. The new boiling point remains constant. Fig. 3 Phywe series of publications • Complete Experiments Chemistry/Biotechnology • © PHYWE SYSTEME GmbH • D-37070 Goettingen 13102 75 KV 1.17 Elevation of the boiling point Results The following results were obtained from an actual experiment: There was 50.94 g of water in the inner vessel and during the experiment seven portions of urea of between 0.237 g and 0.442 g were added (see Table 1). A straight line is obtained on plotting the values of the elevations of the boiling points above that of water against the total concentration of urea (see Fig. 4). Explanation On adding urea to water, this first dissolves. Subsequent to this, a new boiling point equilibrium, at a temperature that is changed by some hundredths of a degree, is attained. It is clear from the graph that this elevation of the boiling point is proportional to the concentration of the solution. Solutions of solid substances in water have a higher boiling point than pure water. The boiling point is higher, the higher the concentration of the solution. The elevation of the boiling point is only dependent on the concentration of the solution. One mole of dissolved particles increases the boiling point temperature by 0.515 K (the ebullioscopic constant for water = 0.515 g·K/mole). This enables the molar mass of the added substance to be calculated from the elevation of the boiling point and the mass of added substance (ebullioscopy). For more on the theory of boiling point elevation and freezing point depression, or on ebullioscopy, please refer to the technical literature. set-up or procedure. For details on this, refer to the technical literature and the operating instructions for the “Apparatus for boiling point elevation”. From the results of the measurement example, seven values are given, between 55.32 g/mole and 64.70 g/mole. The average of these gives a molar mass of 60,66 g/mole for the substance used (literature value: 60.05 g/mole). A Beckmann thermometer can be used for temperature measurement instead of the digital measuring instrument. In this case, refer to the operating instructions for the “Apparatus for boiling point elevation” for details on the procedure. The graphical evaluation of the measured values can be simplified by use of “measure” software. This software is license-free for the purpose of evaluating and graphically representing measured values (freeware). It is available as download-file under URL “www.phywe.de”, or can be installed from the demo-CD supplied with the digital thermometer 4-2. Figure 4 was created with this software. Fig. 4 Notes Hydroquinone or common salt can be used as alternatives. When using the latter, take the correction factor for the ionic activity into consideration! The same apparatus can also be used to determine molar masses from the elevation of the boiling point. As long as no other chemicals are used, no change is required in the Table 1 76 Mass of urea in g Conzentration of urea in mole/1000 g water Boiling point elevation in K Total boiling point elevation in K 0.442 0.144 0.07 0.07 0.383 0.270 0.07 0.14 0.300 0.368 0.05 0.19 0.418 0.504 0.07 0.26 0.237 0.582 0.04 0.30 0.256 0.666 0.04 0.34 0.237 0.743 0.04 0.38 13102 Phywe series of publications • Complete Experiments Chemistry/Biotechnology • © PHYWE SYSTEME GmbH • D-37070 Goettingen