Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 TEC Related concepts Differential molar mixing enthalpy, real and ideal behaviour, integral molar mixing enthalpy, fundamental principles of thermodynamics, calorimetry. Principle When two miscible liquids are mixed, a positive or negative heat effect occurs, which is caused by the interactions between the molecules. This heat effect is dependent on the mixing ratio. The integral mixing enthalpy and the differential molar mixing enthalpy can be determined by calorimetric measurements of the heat of reaction. Equipment 2 1 1 1 1 1 1 1 1 3 3 1 1 1 4 1 1 1 Cobra4 USB Link Cobra4 Sensor Unit Temperature Cobra4 Sensor Unit Energy Software measure Cobra4 Precision Balance, Sartorius QUINTIX5102-1S, 5100 g / 0.01 g Magnetic stirrer MR Hei-Standard Magnetic stirrer bar, l = 30 mm, oval Separator for magnetic bars Support rod, l = 500 mm, M10 thread Right angle clamp Universal clamp Power supply universal Calorimeter, transparent Heating coil with sockets Connection cable, l = 500 mm, black External circulation set for thermostat Alpha A Immersion thermostat Alpha A Bath for thermostat, 6 l, Makrolon 12610-00 12640-00 12656-00 14550-61 49285-99 35751-93 35680-04 35680-03 02022-20 37697-00 37715-00 13500-93 04402-00 04450-00 07361-05 08493-02 08493-93 08487-02 1 1 3 4 1 2 5 1 1 6 1 1 Pasteur pipettes Rubber bulbs Rubber tubing, di = 6 mm Hose clips, d = 8…16 mm Retort stand, h = 500 mm Erlenmeyer flask, 250 ml, narrow neck, PN 29 Erlenmeyer flask, 100 ml, narrow neck, PN 19 Funnel, do = 80 mm Powder funnel, do = 65 mm Acetone, chem. pure, 250 ml Wash bottle, 500 ml Water distilled, 5 l 36590-00 39275-03 39282-00 40996-02 37692-00 36424-00 36418-00 34459-00 34472-00 30004-25 33931-00 31246-81 Additional equipment 1 PC with USB interface, Windows XP or higher Fig. 1: Experimental set-up. www.phywe.com P3020661 PHYWE Systeme GmbH & Co. KG © All rights reserved 1 TEC Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 Safety instructions When handling chemicals, you should wear suitable protective gloves, safety goggles, and suitable clothing. Please refer to the appendix for detailed safety instructions. Tasks 1. Measure the integral mixing enthalpy of 7 different water acetone mixtures. 2. Plot the molar integral mixing enthalpy versus the quantity of substance (mole fraction) and determine the molar mixing enthalpy. 3. Discuss the results on the basis of the interactions in the mixture. Set-up and procedure Weigh out the individual components of these mixtures with an accuracy of 0.1 g in accordance with the values given in Table 1. Table 1: Preparation of the seven test mixtures. - - Substance quantity Calorimeter Erlenmeyer flask Mixture number X = 0.1 475 g Water 169 g Acetone 1 X = 0.2 Mixture 1 213 g Acetone 2 X = 0.9 557 g Acetone 19 g Water 7 X = 0.8 Mixture 7 24 g Water 6 X = 0.6 Mixture 6 72 g Water 5 X = 0.5 Mixture 5 59 g Water 4 X = 0.4 Mixture 4 86 g Water 3 Set up the experiment as shown in Fig. 1. Combine the Cobra4 Sensor Unit Energy and the Cobra4 Sensor Unit Temperature with the Cobra4 USB Links. Connect the power supply and the heating coil with the Cobra4 Sensor Unit Energy as shown in Fig. 2. Fig. 2: Connection between the Cobra4 Sensor Unit Energy and the power supply (“in”) and the heating coil (“out”). - - - 2 Start the PC and connect the Cobra4 USB Links with the computer via USB cables. Call up the “Measure” programme and boot the experiment “Determination of the mixing enthalpy of binary fluid mixtures with Cobra4” (experiment > open experiment). The measurement parameters for this experiment are loaded now. Now the sensors are automatically recognized and some ID numbers (01 and 02) are allocated to them, which is indicated in the display of the Cobra4 USB Links. For the first measurement, fill 475 g water into the calorimeter. PHYWE Systeme GmbH & Co. KG © All rights reserved P3020661 Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 - - - - - - TEC Insert the oval magnetic stirrer bar in the calorimeter and switch the magnetic stirrer on (Caution: Do not switch on the heating unit by mistake!). Insert the heating coil and the temperature probe into the lid of the calorimeter and fix them in position. Weigh 169 g of acetone in a 250 ml Erlenmeyer flask. Wait until temperature equilibrium has been established. Cut a rubber stopper with hole lengthwise, put the temperature probe through the hole and close the Erlenmeyer flask before hanging it into the temperature-controlled bath. Adjust the immersion thermostat to the temperature of the water in the calorimeter and wait until the temperature difference between the acetone in the bath and the calorimeter does not exceed 0.02 K. Insert the temperature probe back into the lid of the calorimeter. Start the measurement with . Wait a few minutes, then pour the acetone into the water in the calorimeter. After a new temperature equilibrium has been reached, perform electrical calibration for the determination of the total heat capacity of the calorimeter. Do this by supplying 10 V AC to the heating coil. The system is now continuously heated and the supplied quantity of energy is measured. When the temperature increase in the calorimeter induced by the electrical heater is approximately equal in size to the temperature change resulting from mixing the two liquids, switch off the heating and read the exact quantity of electrical energy supplied. Continue to measure for another three minutes, then stop the measurement by pressing . Send all data to “measure” and save the measurement (File > Save meausrement as…). Fig. 3 shows the graph as it is now presented by the programme. Fig. 3: Temperature-time diagram of the mixing of two miscible fluids and determining the heat capacity of the system. - - - Use for determining the temperature difference for the mixing process (see Fig. 3) In a second experiment, add an additional portion of acetone (213 g) to the mixture in the calorimeter (see Table 1). Perform the experiment completely analogously to the first measurement and pay attention that the temperature of the mixture in the calorimeter and of the acetone is the same. In a further series of experiments, successively add the 5 portions of water listed in Table 1 to the 557 g of acetone in the calorimeter. www.phywe.com P3020661 PHYWE Systeme GmbH & Co. KG © All rights reserved 3 TEC - - Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 Carry out this series in the same manner as in the first set of measurements, after carefully cleaning and drying the calorimeter. It is important that the calorimeter is recalibrated after each addition, as the heat capacity of the system is different after each temperature change. Theory and evaluation The change in enthalpy observed when two liquids are mixed is the sum of the changes in enthalpy which occur during the mixing process. The mixing enthalpy ΔM 𝐻 is influenced by the interactions of the molecules involved, which in turn are a function of the mixing ratio. The mixing enthalpy is zero if there are no interactions between the molecules (so-called ideal mixtures). The interactions between two liquids can cause endothermic effects (decreasing supramolecular assemblies) or exothermic effects (formation of supramolecular assemblies of different molecules). The quantity of heat exchanged by mixing 𝑛A moles of the component A with 𝑛B moles of component B is termed the integral mixing enthalpy ΔM 𝐻I . If a substance is successively added to another one until a certain mixing ratio is reached, the integral mixing enthalpy is obtained by adding the individual enthalpy values: ∆M ℎI = ∑ ∆M ℎ𝐽I (1) 𝐽 with ∆M ℎ𝐽I = 𝑄exp = 𝑄cal ∆𝑇exp ∆𝑇exp = 𝑊el ∆𝑇cal ∆𝑇cal (2) The molar integral mixing enthalpy (referred to 1 mol of the mixture) is calculated as follows: ∆M 𝐻 I = ∆M ℎ I 𝑛A + 𝑛B (3) The mixing ratio is normally characterised by the molecular abundance (mole fraction). 𝑛A 𝑥A = 𝑛A + 𝑛B (4.1) 𝑛B 𝑛A + 𝑛B (4.2) 𝑥A + 𝑥B = 1 (4.3) 𝑥B = for binary mixtures. The dependence of the integral mixing enthalpy on the number of moles of the two components at constant pressure and constant temperature is defined by: d(∆M ℎI ) = ( 𝛿∆M ℎI 𝛿∆M ℎI ) d𝑛A + ( ) d𝑛B 𝛿𝑛A 𝑛 𝛿𝑛B 𝑛 B (5) A or d(∆M ℎI ) = ∆M 𝐻A d𝑛A + ∆M 𝐻B d𝑛B (6) with ∆𝑀 𝐻𝑗 = ( ΔM 𝐻𝑗 4 𝛿∆M ℎI ) 𝛿𝑛𝑗 𝑇,𝑝,𝑛 (7) Differential molar mixing enthalpy of the component 𝑗 PHYWE Systeme GmbH & Co. KG © All rights reserved P3020661 Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 TEC Integration at constant composition results in: ∆M ℎI = ∆M 𝐻A 𝑛A + ∆M 𝐻B 𝑛B (8) Division of (5) by (𝑛A + 𝑛B ) results in: ∆M 𝐻I = ∆M 𝐻A 𝑥A + ∆M 𝐻B 𝑥B (9) Fig. 4 shows the graph of ΔM 𝐻I versus the mixing ratio expressed as the molecular abundance of acetone 𝑥acetone . Fig. 4: Temperature-time curve of the mixing enthalpy of mixture 1. Using the equations (10) and (11), 𝛿∆M 𝐻I ) 𝑥B + ∆M 𝐻I 𝛿𝑥A (10) 𝛿∆M 𝐻I ) 𝑥A + ∆M 𝐻I 𝛿𝑥B (11) ∆M 𝐻A = ( ∆M 𝐻B = ( the differential molar mixing enthalpy of water and acetone for the different compositions of the solutions can be calculated. You can enter the results each for water and acetone into a data table (measurement > enter data manually) and put them together in one diagram as shown in Fig. 5. Fig. 5: Differential molar mixing enthalpies of water and acetone as a function of the composition. www.phywe.com P3020661 PHYWE Systeme GmbH & Co. KG © All rights reserved 5 TEC Determination of the mixing enthalpy of binary fluid mixtures with Cobra4 Disposal The organic substances have to be collected in a correspondingly labelled container and passed to safe waste disposal. Appendix Hazard symbol, signal word Hazard statements Precautionary statements H225: Highly flammable liquid and vapour H319: Causes serious eye irritation H336: May cause drowsiness or dizziness EUH 066: Repeated exposure may cause skin dryness or cracking P210: Keep away from heat/sparks/open flames/hot surfaces – No smoking P233: Keep container tightly closed P305+351+338: IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses if present and easy to do – continue rinsing Acetone Danger 6 PHYWE Systeme GmbH & Co. KG © All rights reserved P3020661