Physical Properties: Identification of a Pure Liquid
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1 EXPERIMENT Physical Properties: Identification of a Pure Liquid 6 To identify an unknown liquid by comparin the experimental and theoretical boilin points and densities. OBJECTIVE A P P A R A T U S balance disposable lass pipette thermometer (-10 ºC to 150ºC) Bunsen burner rin stand rin clamp 1 mm cross section of rubber hose wire auze test tube (10 15 cm lon) boilin stone test tube clamp striker (lihter) Thermometer (or test tube) clamp 1000 ml beaker C H E M I C A L S Unknown liquid (~ 3.5 ml) Pure compounds can be obtained after a chemical reaction usin a purification process. This purified product can be evaluated by comparin its physical properties with those of the same substance in pure form. Physical properties are those characteristics of a substance that can be observed or measured without chemically chanin the substance. Taste, odor, and color are examples of physical properties that are more observable than measurable. Measurable physical properties include meltin point, boilin point, refractive index, density, solubility, and viscosity. Because impurities will alter a compound s physical properties, measurements close to the known values indicate that the substance is of hih purity. In addition, careful determination of only a few of these physical properties can discriminate between two possible compounds. Many scientists devoted their lives to collectin and tabulatin the physical properties of the elements and compounds. Two books have emered as references in this area: N. A. Lane s Handbook of Chemistry and The Chemical Rubber Company s Handbook of Chemistry Copyriht 2005 Chem21 LLC. No part of this work may be reproduced, transcribed, or used in any form by any means raphic, electronic, or mechanical, includin, but not limited to, photocopyin, recordin, tapin, Web distribution, or information storae 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.
2 and Physics. The handbook for this lab has been condensed to Table 1 eiht oranic liquids and their densities, meltin points and boilin points. With meticulous laboratory care, the collected data and this table will allow you to identify your particular unknown. Physical Properties: The boilin 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 boilin point, bubbles of vapor form within the liquid and rise unimpeded to the top of the liquid, breakin the surface tension and releasin the vapor into the atmosphere above. If the pressure of the atmosphere above the liquid is exactly 1 atmosphere, then the temperature at the boilin point is called the normal boilin point. Because boilin points are pressure dependent, certain corrections to the boilin point measurement must be made if the pressure is sinificantly different from 1 atmosphere. Fortunately for this lab, as lon as the atmospheric pressure is 760 mmh +/- 10 mm H, then the correction will be less than 0.3º C (well within the error rane of readin a thermometer). The meltin point of a substance is the temperature, approached from the solid phase, at which the solid and liquid are in equilibrium. Unlike boilin points, meltin points are not affected sinificantly by pressure chanes (pressure becomes important when ases are involved). The density of a substance relates two common measurements, mass and volume, as a ratio that is unique (thus meaninful) to the substance bein studied. Whether one has only a speck of a pure substance or a warehouse, the density will be the same. M D= V Equation 1 The mass of an object is determined with a laboratory balance. Balances have a TARE button which allows you to place a sheet of weihin paper (or beaker / watchlass) on the balance and then tare the mass to Once tared, the balance will report the mass of the sample that is placed on the weihin paper (or in the beaker / watchlass). It is IMPERATIVE that you use the SAME BALANCE when makin measurements durin the SAME LAB!! We are enerally interested in the differences in mass and this measurement is accurate only if the SAME INSTRUMENT is used for both measurements. Experiment 6 6-2
3 Typically, liquid volumes are determined usin calibrated lassware such as raduated cylinders, volumetric flasks, burettes, and pipettes. In today s lab, a reen chemistry approach to determinin the density and boilin point will be employed. Of the 12 principles of reen chemistry ( the first principle is it is better to prevent waste than to treat or clean up waste after it is formed. Each student will receive ~ 3.5 ml of an unknown liquid at the beinnin of the lab. After the density and boilin point of the liquid is determined, there will only be ~ 1 ml of chemical waste that must be placed in the labeled waste container. A. Thermometer Calibration PROCEDURE Useful measurements result from equipment that is precise and accurate. Precision enerally occurs when a reat deal of care has been used by a student to reproduce a measurement. However, even careful students will obtain bad results when their equipment is inaccurate. Calibration is a process where equipment inaccuracies are exposed and corrections are applied. Durin any calibration process, it is critical that students exercise the reatest amount of precision possible in order to obtain an accurate instrument. After the calibration process, careful students can obtain multiple measured values that are both accurate and precise. At the front of the class are two lare beakers of water one containin ice and water and the other containin boilin water. Each student will measure the temperature of water in the two beakers to calibrate their thermometer. 1. Place your thermometer in the beaker containin 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] there are manifyin lasses available to help read the thermometer. 3. Next, place the same thermometer in the beaker containin the boilin water. Make certain the water is boilin 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 boilin water when you read the temperature. 5. Durin the submission of your Online Lab Report, you will need to raph the temperature data collected above. A description of how to raph this data usin Experiment 6 6-3
4 True y = mx + b T = m T + b read from Thermometer Equation 2 Excel is provided on that webpae. On the raph produced in Excel will be the equation of a line in the standard form of a line where the true temperature will equal the slope (m) times the experimental temperature plus the y-intercept (b). This type of raph is called a Calibration Curve even thouh it is a straiht line. This equation will be used later durin the online lab submission to accurately report the boilin point (Part C) of your unknown. B. Density of a Liquid Unknown 6. Obtain a numbered vial containin a liquid unknown Do Not Share This Unknown Vial With Anyone Else In The Class! 7. Record the four diit number of your unknown liquid [Data Sheet]. 8. Construct a micropycnometer accordin to the directions below and those iven by your Instructor. Obtain a clean dry Pasteur pipette you will construct a micropycnometer accordin to Fiure 1. Grasp the pipette at its ends with both hands and place it in an oxidizin (blue inner cone) flame 1 cm away from the tapered end. Rotate the pipette at the tip of the inner blue cone to evenly distribute the heat. After a minute, the lass will bein to soften. When it has softened to the point that it is difficult to rotate the pipette without twistin the lass (Do Not Twist The Glass), remove the pipette from the flame and immediately (within 0.5 seconds) pull the two ends apart (~ 25 cm or about 10 inches). Hold this position 3-5 seconds to allow the lass to cool and the capillary to become riid Pull Apart 3. Micropycnometer Fiure 1 9. At ~ 0.5 cm from the bottom of what will become the micropycnometer, heat the capillary stronly to cut the lass into two pieces. Experiment 6 6-4
5 10. Continue heatin the bottom of the micropycnometer to form a rounded end. 11. Allow the micropycnometer to cool before weihin it. Place a small beaker / flask on the balance first and TARE its mass to Then, place the micropycnometer in the beaker /flask and record its mass [Data Sheet]. 12. Place a rubber pipette bulb on the pipette you constructed when you made the micropycnometer and use this pipette to transfer the unknown liquid into the micropycnometer. Place your unknown vial in a small beaker so it won t overturn. Clamp the micropycnometer with a small three-finered clamp and position it above the unknown vial / beaker so that any spilled liquid oes into the beaker holdin the micropycnometer. Transfer the unknown liquid into the micropycnometer until it is completely filled with liquid there are no air bubbles. Do Not break the lass tip of your pipette inside the micropycnometer. 13. TARE a beaker (or small flask) at the balance and place the micropycnometer filled with unknown liquid in this beaker and record its mass [Data Sheet]. 14. Determine the mass of the unknown liquid [On-line Report Sheet]. 15. Remove the unknown liquid with the same lass delivery pipette. Place This Liquid In A Clean, Dry Test Tube (this will be used in Step 22)!! 16. Return the vial containin any extra unknown liquid to the Instructor s Desk. 17. Fill the micropycnometer to the top with distilled water usin the pipette you constructed. Clamp the micropycnometer with a small three-finered clamp. Make sure the micropycnometer is completely filled with water / no air bubbles. Don t break the lass tip of your pipette inside the micropycnometer. 18. TARE a beaker (or small flask) at the balance and place the micropycnometer filled with water in this beaker and record its mass [Data Sheet]. 19. Determine the mass of the water [On-line Report Sheet]. Experiment 6 6-5
6 20. Usin 1.00 /ml as the density of water, determine the volume of the micropycnometer [On-line Report Sheet]. 21. Determine the density of the unknown liquid [On-line Report Sheet]. C. Boilin Point of a Liquid Unknown 22. Secure the test tube with a three-finered clamp and lower it into a beaker filled with tap water. 23. Place the thermometer in the test tube and let it rest on the bottom of the test tube. 24. Heat the water rapidly with a Bunsen burner until the unknown liquid inside the test tube beins to boil bubbles are formin around the thermometer. The unknown will boil before the water boils - if the water beins to boil before you see the unknown boil, turn off the as and proceed with the next step if you still have liquid in the test tube (if no liquid remains, contact your lab instructor). 25. Hold your thermometer approximately 1 cm above the boilin unknown liquid for about 20 seconds before recordin the temperature to the nearest 0.2 C [Data Sheet] the liquid should be drippin off the end of your thermometer when you read the temperature. 26. Turn the as off and lift the test tube out of the hot water immediately after recordin the boilin point to prevent further vaporization of your unknown into the lab s atmosphere. Experiment 6 6-6
7 27. Use the information from the Excel-enerated Thermometer Calibration Curve to correct the observed temperature usin Equation 2. Record the true boilin point of the unknown liquid [On-line Report Sheet]. D. Unknown Identification 28. Compare your unknown s density and boilin point to those recorded in Table 1 to identify your unknown [On-line Report Sheet]. Substance Chemical Formula Density (/ml) Meltin Point ( C) Boilin Point ( C) Acetone (1) C 3 H 6 O ,3-Butanedione (2) C 4 H 6 O Cyclohexanol (3) C 6 H 12 O Chloroform (4) CHCl Bromoform (5) CHBr Hexane (6) C 6 H Isopropyl alcohol (7) C 3 H 8 O Methyl alcohol (8) CH 4 O Table 1 Waste Disposal: Place any liquid remainin from the boilin point determination in the waste beaker in the hood. You should have returned the unknown vial (alon with any unused liquid unknown) to the Instructor s desk in Step 16. Lab Report: Once you have turned in your Instructor Data Sheet, lab attendance will be entered and lab attendees will be permitted to access the online data / calculation submission part of the lab report (click on Lab 06 Physical Properties). After your data has been accepted, the lab proram will uide you throuh the submission process. Experiment 6 6-7
8 Laboratory 6 Student Data Sheet Actual Freezin Point of Water 0 ºC Actual Boilin Point of Water 100 ºC Freezin Point of Water recorded on Your Thermometer ºC Boilin Point of Water recorded on Your Thermometer ºC Unknown Number (liquid) Mass of micropycnometer Mass of micropycnometer + unknown liquid Mass of micropycnometer + water Boilin Point of the Liquid Unknown ºC Laboratory 6 Instructor Data Sheet Name: Lab Section: Actual Freezin Point of Water 0 ºC Actual Boilin Point of Water 100 ºC Freezin Point of Water recorded on Your Thermometer ºC Boilin Point of Water recorded on Your Thermometer ºC Unknown Number (liquid) Mass of micropycnometer Mass of micropycnometer + unknown liquid Mass of micropycnometer + water Boilin Point of the Liquid Unknown ºC Experiment 6 6-8
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