TURLA, NYGEN KEITH LOUISE D. (18-05544) BS Chemical Engineering PHYSICAL CHEMISTRY FOR ENGINEERS 2 ACTIVITY 1 LABORATORY EXPERIMENTAL PROCEDURE FOR A TERNARY LIQUID SYSTEM MISCIBILITY GAP IN A TERNARY SYSTEM Overview Short description Principle A number of completely miscible two component mixtures are prepared to investigate the three component acetic acid / chloroform / water system. These mixtures are titrated with the third component until a two phase system is formed which causes turbidity. The phase diagram for the three component system is plotted in a triangular diagram. 1 TASKS 1. Titrate nine different acetic acid / chloroform mixtures with water until a two phase system is formed in each case. 2. Titrate six acetic acid / water mixtures with chloroform until phase separation is observed. 3. Plot the results of the titrations, expressed as molar fractions, in a trianglular diagram. PROCEDURE 1. Set up the experiment as shown in Fig. 1. 2. Prepare the chloroform / acetic acid mixtures listed in Table 1 by weighing the specified quantities of chloroform and pure acetic acid into 100 ml flat-bottomed flasks. Table 1: Quantities and mixing proportions of chloroform / acetic acid mixtures MIXTURE mchloroform (in g) nchloroform macetic acid (in g) nacetic acid A 119.5 1.0 0.0 0.0 B 107.6 0.9 6.0 0.1 C 95.6 0.8 12.0 0.2 D 83.7 0.7 18.0 0.3 E 71.7 0.6 24.0 0.4 F 59.8 0.5 30.0 0.5 G 47.8 0.4 36.0 0.6 H 35.9 0.3 42.0 0.7 I 0.0 0.0 60.0 1.0 3. Shake the samples well and transfer 10 g of each mixture to suitably labelled test tubes. 4. Temperature equilibrate the test tubes to 25 °C in a temperature controlled water bath. 5. Titrate the samples with distilled water from a microburette until the liquid becomes turbid as a result of separation. 6. Shake the test tubes from time to time to ensure good mixing of the samples (insert rubber stoppers before shaking). 7. Record the quantity of water added (in ml) as approximation for the mass of water (in g). 8. Repeat the procedure for samples K to P listed in Table 2. Table 2: Mixing proportions of water/acetic acid MIXTURE mwater (in g) nwater K 1.00 9.00 L 2.00 8.00 M 3.00 7.00 N 4.00 6.00 O 5.00 5.00 P 6.00 4.00 macetic acid (in g) 10 20 30 40 50 60 nacetic acid 0.021 0.046 0.076 0.113 0.161 0.22 9. Again transfer 10 g of each sample to a separate test tube and temperature equilibrate them to 25 °C in the temperature controlled bath. 10. Titrate with chloroform until turbidity occurs and record the quantity added. 11. Calculate the mass of chloroform from the density ( ρchloroform= 1.489 g / ml) and the consumption (in ml). 12. Calculate the molar fractions for all mixtures and plot the results in a phase diagram using triangular co-ordinates (see Fig. 2) 2 Source: https://repository.curriculab.net/files/versuchsanleitungen/p3030601/p3030601e.pdf 3 ACTIVITY 2 EXAMPLES OF THE TYPES OF PARTIALLY MISCIBLE THREE-LIQUID SYSTEMS TYPE 1 FORMATION OF ONE PARTIALLY MISCIBLE PAIR Mixture 1 Acetone-Water-Methyl isobutyl ketone MISCIBLE Acetone-water Acetone-methyl isobutyl ketone Mixture 2 Methanol-water-chloroform MISCIBLE Methanol-water Methanol-chloroform Mixture 3 water-benzene-alcohol MISCIBLE Water-alcohol Benzene-alcohol Mixture 4 Acetic acid-chloroform-water MISCIBLE Acetic acid-chloroform Acetic acid-water Mixture 5 Acetone-water-phenol MISCIBLE Acetone-water acetone-phenol PARTIALLY MISCIBLE Water-methyl isobutyl ketone PARTIALLY MISCIBLE Water-chloroform PARTIALLY MISCIBLE Water-benzene PARTIALLY MISCIBLE chloroform-water PARTIALLY MISCIBLE water-phenol TYPE 2 FLORMATION OF TWO PARTIALLY MISCIBLE PAIRS Mixture 1 Aniline-n heptane- methylcyclohexane MISCIBLE n heptane-methylcyclohexane Mixture 2 Nitrile-water-ethanol MISCIBLE water-ethanol Mixture 3 Water-phenol-aniline MISCIBLE phenol-aniline Mixture 4 Water-ethyl acetate-n butyl alcohol MISCIBLE ethyl acetate-n butyl alcohol PARTIALLY MISCIBLE Aniline-n heptane Aniline-methylcyclohexane PARTIALLY MISCIBLE Nitrile-water Nitrile- ethanol PARTIALLY MISCIBLE Water-phenol Water-aniline PARTIALLY MISCIBLE Water-ethyl acetate Water-n butyl alcohol 4 Mixture 5 Methanol-water-heptane MISCIBLE Methanol-water PARTIALLY MISCIBLE Water-heptane Methanol-heptane TYPE 3 FORMATION OF THREE PARTIALLY MISCIBLE PAIRS Mixture 1 Succinic nitrile-water-ether MISCIBLE PARTIALLY MISCIBLE Succinic nitrile-water Succinic nitrile-ether water-ether 5