Page 1 of Lab Wet Lab: Molar Mass of a Volatile Liquid Note to Students To complete the Lab, you must work under the supervision of your onsite Laboratory Supervisor. See the Lab Materials and Safety Information in Course Resources for more information: (© Copyright 2006 Apex Lesming nc. Al nights rasrved. This mses nto fot [No potion othace materials may be reproduced or rediinbuted i any fm witout the srs ony. earning noPage 2016 Lab Wet Lab: Molar Mass of a Volatile Liquid Lab Overview Chemical and physical methods for determining atomic and molecular weights or molar masses have been important historically as a way of analyzing and categorizing new materials. The modern laboratory is generally equipped with instrumentation that makes many of these methods obsolete. However the principles upon which the older methods were based are important because they were the foundation for the preciction of physical and chemical properties and behaviors of substances, Jean Baptiste André Dumas (1800-1884) was a French chemist best known for his works on organic analysis and synthesis, as well as the determination of atomic weights by measuring vapor densities. ‘The Dumas method for determining the formula weight of a volatile liquid is one such historically important technique. Amadeus Avogadro proposed as early as the mid-1800's that equal volumes of gases measured under identical conditions would contain equal numbers of gas particles. With an established relative atomic mass scale it was possible to describe a constant volume which would contain one mole of a gaseous element or compound under fixed conditions. At STP this volume is 22.414 L for an ideal gas. In the Dumas method a volatile liquid is heated Simple equipment is to a known temperature (above its boiling needed for point). The vapor is allowed to escape from a determination of the container through a tiny opening (typically a molar mass of a pinhole). Once the liquid has vaporized, the volatile liquid: a container is cooled to room temperature. Bunsen burner, large | ‘Gradually the vapor that remained in the beaker, and container at the higher temperature condenses Erlenmeyer flask with | to a liquid. The difference in the weight of the an aluminum foil cap. A | container is the mass of the condensed vapor. ring stand with clamps If the volume of the container is known along and rings helps to with the high temperature, the room pressure support the equipment | can be used (because the system is open to over the Bunsen the atmosphere through the orifice) to burner. calculate moles. From there a molar mass can be determined The Dumas method for molar mass determination is based on a number of assumptions. One assumption is that while the liquid is volatile enough to vaporize at the elevated temperature, it is not so volatile that a significant amount will be lost to evaporation through the orifice as the container cools. The vapor is also assumed to behave ideally at the temperature and pressure at which it occupies the container. The amount of error implicit in this approximation varies from compound to compound and is tied to the variables which create deviations from ideal behavior: molecular volume and intermolecular forces. Generally speaking, the larger these are, the greater the error in the determination. The situation is further complicated by the interaction of these two factors. (© Copyright 2006 Apex Leaning nc. Al rights raerved. This mstartl is ntnded forthe excusive use of registered users ony No potion othace materials may be reproduce of reditnbutedn any form without th express wien permision of Apsr Leaning ncPage 3.016 Lab Wet Lab: Molar Mass of a Volatile Liquid There is another problem with the basic method which is more easily addressed. When the container is "empty", i.e., before the volatile liquid is added or the vapor forms, there is a fixed amount of air determinec by the volume, temperature and pressure in the container. This air has mass and contributes to the overall mass of the container assembly. But when the organic liquid is Present, some of it vaporizes (based on its its vapor pressure at room temperature). The presence of this vapor forces out some of the air through the orifice since the internal pressure is equalized with the room pressure and the number of gas particles remains constant if the temperature and pressure remain constant. Thus when the container is massed again there is air missing that should be considered in the final mass if the mass of the condensed liquid is to be determined by difference. This results in an apparent mass of liquid that is too small which in turn makes the molar mass calculation too small. The moles of air forced out by the vapor are equal to the moles of vapor that forms. This is determined by the vapor pressure of the liquid at room temperature. If this value is known, the moles of vapor that are present in the flask above the residual condensed liquid can be calculated as: oor # Vs Avogadro's Law tells us that these moles of vapor must equal the moles of air displaced since the conditions are the same for both. These "missing" moles of air can be converted to grams using the average molar mass of air (28.92 ¢/mol at 298 K) and added into the final mass of the assembly. The correction for the amount of air initially in the flask depencs on knowing the vapor pressure of the liquid, Pyapsr, at room temperature. A list of possible unknown volatile liquids and their vapor pressures at 298K is provided below. Volatile Liquid: | Chemical Formula Prapa298 K)E Boiling point: ‘Acetonitrile CHSCN 81 mmHg 816°C Ethanol CH3CH2OH 55 mmHg 78°C Ethyl acetate ‘CH,CO,CH,CH, 82 mm Hg 76.5°C Isopropyl acetate_[ CH,CO,CH(CHs)) ‘2 mm Hg 90°C 2-propanol ‘CH3CHOHCH3 41 mmHg 82.4°C Pre-Lab Questions 1. Derive an expression for the molar mass of a gas, starting from the Ideal Gas Law. 2. Based on the expression given in (1), what experimental data must be collected in order to determine the molar mass of a gas? 3. Why it is necessary to remove the Erlenmeyer flask from the hot water bath at the moment the volatile liquid disappears from the flask, rather than while there is still liquid in the flask, or several minutes after the liquid has completely evaporated? Materials + aluminum foil (~3" square) + barometer + rubber band + 600 mL beaker + small pin + Erlenmeyer flask, 125 mL + Bunsen burner + thermometer + matches or lighter + graduated cylinders, 10 mL and 100 mL + digital electronic balance (or larger) + ring stan¢, wire gauze, metal ring, and + 5-6 mL of an unknown volatile organic clamp liquid (© Copyright 2006 Apex Leaning nc. Al rights raerved. This mstartl is ntnded forthe excusive use of registered users ony No potion othace materials may be reproduce of reditnbutedn any form without th express wien permision of Apsr Leaning ncPage 4 of Lab Wet Lab: Molar Mass of a Volatile Liquid Procedure A. Preparation of Gas Production Apparatu: 1. Obtain a 1-hole rubber stopper that fits securely on the end of a large test tube. Insert a small length of glass or rigid plastic tubing into the hole. Attach the other end of the tube to a piece of rubber tubing that is long enough to extend from the gas production tube to the gas collection beaker (see below). 2. Attach a utility clamp to a 125 mL Erlenmeyer flask. Immerse the flask as deeply as possible into a 600 mL beaker. Pour water into the beaker around the outside of the flask until the beaker is almost full, while still allowing room for vigorous boiling. 3. Add a few boiling chips to the beaker and heat the water to boiling over a Bunsen burner. 4. While the water is heating, raise the clamp, remove the flask from the clamp, and dry the outside of the flask thoroughly with a paper towel. 5. Place a small square of aluminum foil over the mouth of the flask. Loosely fold the foil down around the flask’s neck. Secure the foil in place with a rubber band, Make a small hole in the center of the foil with a straight pin. Be certain that the hole is open and not partially blocked by displaced aluminum foil. 6. Weigh the flask, foil cap, and rubber banc to the nearest milligram and record the mass in the data table. B. Vaporization and Condensation of the Volatile Liauid 1. Obtain a small sample of an unknown liquid. Record its number in the data table. 2. Remove the foil cap from the Erlenmeyer flask and add about 2 mL of unknown liquid to the flask. Replace the foil and rubber band. 3. Clamp the flask to the ring stand and immerse the flask as deeply as possible in the boiling water. Measure the temperature of the boiling water and record the value in the data table. 4. Read the barometer in the room and record the air pressure. 5. Watch the liquid in the flask. As it begins to boil, follow the vapor up through the flask with your eye. Soon vapor will start to escape through the pin hole, When all of the liquid has vaporized, including any droplets that may have formed on the neck, no more vapor is seen escaping through the pin hole (this should take no more than 1 to 2 minutes). 6. When the vapor stops escaping, very quickly remove the flask and set it on a folded paper towel. Remove the clamp from the neck of the flask. Dry the outside of the flask carefully with a paper towel. Be sure to dry under and around the folds of aluminum foil. Allow the flask to come to room temperature. As the flask cools, you will see a small amount of liquid condense in the bottom of the flask. 7. When the flask has returned to room temperature, weigh the flask and contents and record the mass in the data table. 8. Repeat steps 2-8 two additional times by first adding 1 to 2 mL of your unknown liquid. Replace the cap and heat the flask as described above. After heating and cooling the flask, reweigh and record the mass of the flask and contents. 9. After the final weighing, remove the foil and rinse out the flask with water. Completely fill the flask, level full, with water. Measure the volume of the flask by measuring the volume of water that it can hold. Pour the water in the flask into a graduated cylinder. You may have to fill the cylinder several times to accommodate the volume of water in the flask. Record the total volume of the flask in the data table. (© Copyright 2006 Apex Lesming nc. Al nights rasrved. This mses nto fot [No potion othace materials may be reproduced or rediinbuted i any fm witout the srs ony. earning noPage Sof 6 Lab Wet Lab: Molar Mass of a Volatile Liquid Name: Username: Date: Pre-Lab Questions (3 points) 1. Derive an expression for the molar mass of a gas, starting from the Ideal Gas Law. 2. Based on the expression (1), what experimental data must be collected order to determine the molar mass of a gas? 3. Why it is necessary to remove the Erlenmeyer flask from the hot water bath at the moment the volatile liquid disappears from the flask, rather than while there is still liquid in the flask, or several minutes after the liquid has completely evaporated? Results (7 points) Unknown liquid number: Trial 1 Trial 2 Trial 3 Mass of empty flask + foil cap and rubber band Mass of flask, cap, rubber band, and condensed vapor Temperature of water Barometric pressure of room Volume of flask No ponte" tese materials may be reproduced of reaibuted nan form wehaut he express witen permission of Apex Leaming nePage 60f 6 Lab Wet Lab: Molar Mass of a Volatile Liquid Name: Username: Date: Data Analysis and Interpretation (30 points) Attach sheets containing the answers to these questions. Be sure to include your name, username, and submission date on each page you submit. Show a complete sample calculation for one trial in each question involving a computation. Show the final answers for the remaining trials and present all of your results in tabular format. 1, What is the apparent mass of condensed vapor at the boiling point of water? (1 point) 2. How many moles of vapor were produced at the boiling point of water? (3 points) 3. What is the approximate molar mass of the gas and what is its tentative identity? (3 points) 4. How many moles of air were displaced by the vapor? (3 points) 5. What mass of air was displaced by the vapor? (3 points) 6. What is the true mass of vapor that filled the flask at the temperature of boiling water? (3 points) 7. What is the corrected molar mass of the vapor? (3 points) 8. What is the actual identity of the volatile liquid? (2 points) 9. What is the percent error between your experimental molar mass and the compound's actual molar mass? (3 points) 10.What are some of the sources of error in this experiment (other than human error)? (3 points) 11. Consider the table of possible unknown volatile liquids used in this experiment. What physical characteristics do these substances share that make it possible to cetermine their molar mass using the Dumas procedure? (3 points) pyight 2008 Apex Leaming in. Allighs reeerved. This mara intended forthe excuive use of registered users ety No ponte" tese materials may be reproduced of reaibuted nan form wehaut he express witen permission of Apex Leaming ne