EXPERIMENT Physical Properties: Identification of a Pure Liquid 7 Prepared by Edward L. Brown, Lee University and Verrill M. Norwood, Cleveland State Community College OBJECTIVE To identify an unknown liquid by comparing the experimental and theoretical boiling points and densities. A P P A R A T U S balance Bunsen burner disposable glass pipette ring stand thermometer (-10ºC to 150ºC) ring clamp 1 mm cross section of rubber hose wire gauze test tube (10 – 15 cm long) striker (lighter) boiling stone Thermometer (or test tube) clamp test tube clamp 1000 mL beaker C APPARATUS AND CHEMICALS H E M I C A L S Unknown liquid (~ 3.5 mL) Physical properties are those characteristics of a substance that can be observed or measured without chemically changing the substance. Taste, odor, and color are examples of physical properties that are more observable than measurable. Measurable physical properties include melting point, boiling point, refractive index, density, solubility, and viscosity. Many scientists devoted their lives to collecting and tabulating the physical properties of the elements and compounds. Two books have emerged as references in this area: N. A. Lange’s Handbook of Chemistry and The Chemical Rubber Company’s Handbook of Chemistry and Physics. The “handbook” for this lab has been condensed to Table 1 – eight organic liquids and their densities, melting points and boiling points. With meticulous laboratory care, your collected data and this table will allow you to identify your particular unknown. Copyright 2005 Chem21 LLC. No part of this work may be reproduced, transcribed, or used in any form by any means – graphic, electronic, or mechanical, including, but not limited to, photocopying, recording, taping, Web distribution, or information storage or retrieval systems – without the prior written permission of the publisher. For permission to use material from this work, contact us at info@Chem21Labs.com. Printed in United States of America. Physical Properties: Identification of a Pure Liquid The boiling point of a liquid is the temperature at which the vapor pressure of the liquid equals the pressure of the atmosphere above the liquid. At the boiling point, bubbles of vapor form within the liquid and rise unimpeded to the top of the liquid, breaking the surface tension and releasing the vapor into the atmosphere above. If the pressure of the atmosphere above the liquid is exactly 1 atmosphere, then the temperature at the boiling point is called the normal boiling point. Because boiling points are pressure dependent, certain corrections to the boiling point measurement must be made if the pressure is significantly different from 1 atmosphere. Fortunately for this lab, as long as the atmospheric pressure is 760 mmHg +/- 10 mm Hg, then the correction will be less than 0.3º C (well within the error range of reading a thermometer). The density of a substance relates two common measurements, mass and volume, as a ratio that is unique (thus meaningful) to the substance being studied. Whether one has only a speck of a pure substance or a warehouse, the density will be the same. D= M V Equation 1 In this lab, mass will be determined using a balance. It is IMPERATIVE that you use the SAME BALANCE when making measurements during the SAME LAB!! We are generally interested in the differences in mass and this measurement is accurate only if the SAME INSTRUMENT is used for both measurements. Typically, liquid volumes are determined using calibrated glassware such as graduated cylinders, volumetric flasks, burettes, and pipettes. In today’s lab, a “green chemistry” approach to determining the density and boiling point will be employed. In this green chemistry approach, the total volume of liquid unknown you will be given is ~ 3.5 mL. After the density and boiling point of the liquid is determined, there will be ~ 1 mL of chemical waste that must be placed in the labeled waste container. A. Thermometer Calibration PROCEDURE Useful measurements result only from using equipment that is precise and accurate. Calibration is a process where equipment inaccuracies are exposed and corrections are determined. During any calibration process, it is critical that students exercise the greatest amount of precision possible in order to obtain an accurate instrument. At the front of the class are two large beakers of water – one containing ice and water and the CHEM 1001 - Experiment 7 7-2 Physical Properties: Identification of a Pure Liquid other containing boiling water. You and your lab partner will measure the temperature of water in the two beakers to calibrate your thermometer. 1. Place your thermometer in the beaker containing ice and water. Make sure the beaker has plenty of ice (at least ½ ice) and carefully stir the contents with your thermometer to make sure the entire solution is at the same temperature. 2. After 1 minute, record the temperature (make sure the thermometer is still in the ice water when you read the temperature – don’t lift it out) to the nearest 0.2 °C [Data Sheet]. 3. Next, place the same thermometer in the beaker containing the boiling water. Make certain the water is boiling and do not allow the thermometer to touch the sides of the beaker. 4. After 1 minute record the temperature to the nearest 0.2 °C [Data Sheet] - make sure the thermometer is still in the boiling water when you read the temperature. B. Density of a Liquid Unknown 5. Obtain a numbered vial containing a liquid unknown – Do Not Share This Unknown With Anyone Except Your Lab Partner! 6. Record the four digit number of your unknown liquid [Data Sheet]. 7. Obtain a micropycnometer and a glass pipette from the Instructor’s Desk. 8. Place a small beaker on the balance and TARE its mass to 0.000 g. Then, place the micropycnometer into the beaker and record its mass [Data Sheet]. 9. Place a rubber pipette bulb on the pipette. Use this pipette to transfer your unknown liquid into the micropycnometer. Avoid air bubbles Make sure the micropycnometer is completely filled with liquid Don’t break the glass tip of your pipette inside the micropycnometer 10. Place a small beaker on the balance and TARE its mass to 0.000 g. Place the micropycnometer filled with unknown liquid in this beaker and record its mass [Data Sheet]. 11. Remove the unknown liquid with the same delivery pipette – Place This Liquid In A Clean, Dry Test Tube (this will be used in Step 15)!! CHEM 1001 - Experiment 7 7-3 Physical Properties: Identification of a Pure Liquid 12. Return the vial containing any “extra” unknown liquid to the Instructor’s Desk. 13. Fill the micropycnometer to the top with distilled water using the pipette you constructed. Avoid air bubbles Make sure the micropycnometer is completely filled with water Don’t break the glass tip of your pipette inside the micropycnometer 14. Place a small beaker on the balance first and TARE its mass to 0.000 g. Place the micropycnometer filled with water in this beaker and record its mass [Data Sheet]. C. Boiling Point of a Liquid Unknown 15. Add a boiling stone to the Unknown liquid already in the Pyrex test tube from Step 11 [see Figure 2]. 16. Secure the test tube with a three-fingered clamp and lower it into a beaker filled with tap water. 17. Heat the water rapidly with a Bunsen burner until the unknown liquid begins to boil. 18. Clamp (or hold) your thermometer approximately 1 cm above the boiling unknown liquid for about 20 seconds before recording the temperature to the nearest 0.2 °C [Data Sheet] – the liquid should be dripping off the end of your thermometer when you read the temperature. Lift the test tube out of the hot water as soon as possible (without burning yourself) after recording the boiling point to prevent the vaporization of your unknown into the lab’s atmosphere. D. Boiling Stones Figure 2 Unknown Identification 19. Compare your unknown’s density and boiling point to those recorded in Table 1 to identify your unknown. You will report the identity of your unknown in the online report sheet for this lab. CHEM 1001 - Experiment 7 7-4 Physical Properties: Identification of a Pure Liquid Substance Chemical Formula Density Melting Boiling (g/mL) Point (°C) Point (°C) Acetone (1) C3H6O 0.79 -95.4 56.2 2,3-Butanedione (2) C4H6O2 0.98 -2.4 88 Cyclohexanol (3) C6H12O 0.96 24.0 161 Chloroform (4) CHCl3 1.48 -63.5 61.7 Bromoform (5) CHBr3 2.90 7.5 150 Hexane (6) C6H14 0.66 -94.0 69 Isopropyl alcohol (7) C3H8O 0.79 -89.5 82.4 Methyl alcohol (8) CH4O 0.79 -98.0 64.7 Table 1 Waste Disposal: Place any liquid remaining from the boiling point determination in the waste beaker in the hood. You should have returned the unknown vial (along with any unused liquid unknown) to the Instructor’s desk in Step 12. Lab Report: Once you have turned in your Instructor Data Sheet, lab attendance will be entered and you will be permitted to access the online data / calculation submission part of the lab report (click on Lab 7 – Identification of an Unknown Liquid). Enter your data accurately to avoid penalty. CHEM 1001 - Experiment 7 7-5 CHEM 1001 - Lab 7 Student Data Sheet Actual Freezing Point of Water 0 ºC Actual Boiling Point of Water 100 ºC Freezing Point of Water recorded on Your Thermometer ºC Boiling Point of Water recorded on Your Thermometer ºC Unknown Number (liquid) Mass of micropycnometer g Mass of micropycnometer + unknown liquid g Mass of micropycnometer + water g Boiling Point of the unknown liquid ºC Name: CHEM 1001 - Lab 7 Instructor Data Sheet Actual Freezing Point of Water 0 ºC Actual Boiling Point of Water 100 ºC Freezing Point of Water recorded on Your Thermometer ºC Boiling Point of Water recorded on Your Thermometer ºC Unknown Number (liquid) Mass of micropycnometer g Mass of micropycnometer + unknown liquid g Mass of micropycnometer + water g Boiling Point of the unknown liquid ºC CHEM 1001 - Experiment 7 7-6