Chemistry Laboratory Techniques 35

Edmonton Catholic School District Locally Developed Complementary Course

Edmonton Catholic Resource Staff: Michel Landry Teacher; Ecole JH Picard Daryl Chichak Consultant; Secondary Science Cecilia Fenrich Consultant; Locally Developed Courses

Chemistry Laboratory Techniques 35

Edmonton Catholic School District Senior High Schools
Implementation Date: February 2006 Students who may be enrolled in the course:
Students in grades 11 or 12 may enrol in this course. Chemistry 30 is a pre or co requisite for Chemistry Laboratory Techniques 35. There will be a projected enrolment of approximately 30 students in a school, and 300 students in the district taking this course.

The credit value for these courses:

This course will be offered for 3 credits 75 hours.

Philosophy and Rationale:

Chemistry is an experimental sciencewe learn new things by making careful observations and then formulating possible explanations of these observations. The central role of experimentation as the basis of chemistry is best appreciated by personal experience in the laboratory. No description of a chemical principle, no explanation of a chemical theory, and no systematic ordering of chemical data can give one first-hand knowledge of the effort required to obtain reliable experimental results. An awareness of the complexity and difficulty in applying chemical principles to the solution of problems will develop as one actively acquires and interprets measurements in the laboratory sessions. The experiments in this course have been designed to provide a practical application of principles studied in high school chemistry courses and to provide an introduction to laboratory techniques that are used in all postsecondary chemistry laboratories. The equipment used by chemists may be more sophisticated; however, the basic principles of the equipment used in the laboratory are the same. Edmonton Catholic Schools, in keeping with the district vision of Christcentered learning, believes that all students must be given the opportunity to learn within a Catholic context so they can reach their full human potential. Chemistry Laboratory Techniques 35 adheres to the districts core values in its philosophy of broadening awareness and appreciation for the natural world and the creative genius

General Learner Expectations:

Students will: 1. develop a better understanding of conducting scientific experiments, in order to increase their proficiency in problem solving through the scientific inquiry process. Attitude: Students will be encouraged to: 1.1 acknowledge that all measurements possess inherent errors due to human or systematic errors occurring in the collection of data 1.2 develop improved self-confidence by familiarizing themselves with a variety of chemical reactions and the equations used to describe them Knowledge: Students will: 1.1 write balanced ionic and net ionic equations, including identification of spectator ions, for reactions taking place in aqueous solutions 1.2 use and interpret H notation for communicating energy changes in chemical reactions 1.3 predict the spontaneity of a redox reaction based on standard reduction potentials, and compare predictions to experimental results 1.4 sketch and qualitatively interpret titration curves, identifying regions of buffering and neutralization 1.5 identify types of organic compounds from the functional groups Skills: Students will: 1.1 analyze experimental data and apply mathematical and conceptual models to develop and draw conclusions from their own data 1.2 work as members of a team in addressing problems and apply the skills and conventions of science in communicating information and ideas 2. develop laboratory skills and techniques to be used in post-secondary or advanced laboratories. Attitude: Students will be encouraged to: 2.1 treat equipment with respect and carefully manipulate materials 2.2 use minimal quantities of chemicals when performing experiments Skills: Students will: 2.1 conduct investigations into relationships among observable variables and use a broad range of tools and techniques to collect and process data and information in traditional form or by calculator-integrated systems such as bunsen burners thermometers titration apparatus CBL probes

3. show concern for safety in planning, performing, and reviewing activities in the chemistry laboratory. Attitude: Students will: 3.1 include safety as a requirement in a chemistry lab activities 3.2 value the need for safe handling and storage of chemicals 3.3 clean up after an activity and dispose of used materials appropriately Skills: Students will: 3.1 describe procedures for safe handling, storing, and disposal of materials used in the laboratory

Special facilities or equipment necessary, or approved resources:

No specific facilities or equipment is necessary. The laboratory conditions and facilities already present for high school science classes provide the necessary materials for the requirements of Chemistry Laboratory Techniques 35. The Appendix contains five experiments using the Vernier probes and sensors with the Texas Instruments CBL2 and TI Graphing Calculators, which allow students to collect data electronically. These experiments illustrate the power of technology in the laboratory of today and give students an opportunity to analyze their data and results electronically. The final lab is a trip to NAIT where students will experience a practical application of techniques to real life applications. Acetyl salicylic acid will be synthesized and purified by recrystalization. The final product will then be weighed and its percent yield calculated. Its identity is confirmed by FTIR (Fourier Transform Infrared Spectroscopy) and its purity determined by HPLC (High Performance Liquid Chromotography) and by its melting point. Safety in the Science Classroom (Draft) http://www.education.gov.ab.ca/k_12/curriculum/bySubject/science/screpo rt.pdf The text/print resource for this course is in the Appendix.

Controversial or sensitive course components:

There are no sensitive or controversial issues in this course.

Significant overlap with provincially developed courses:

Although Chemistry classes in high school require time conducting experiments in the laboratory as part of their course content, Chemistry Laboratory Techniques 35 takes the basic requirements to a much more advanced level. The overlap of procedures with Chemistry 20 and 30 are in safety and basic management of laboratory materials and not with the content of the experiments themselves.

Assessment standards:
The breakdown for student assessment will be: experiments and their written components (50%); student performance in the laboratory (25%) Final Project (25%) See the Appendix for a detailed description of the experiments and their written components.

Course evaluation and monitoring by the school authority:

Edmonton Catholic Schools will monitor the delivery of the course.

Other school authorities offering the course:

No other authority offers Chemistry Laboratory Techniques 35; it has been locally developed in our district.

Appendix
Chemistry Laboratory Techniques 35

Chemistry Lab Techniques Manual and Workbook

Prepared and Edited by Michel Landry cole J.H. Picard School

Contents 1. 2. 3. 4. Decomposing copper oxide Hydrates Qualitative analysis of anions (double class) Analysis of stomach antacid tablets

5. Specific heats of metals 6. Molar heat of fusion of ice (CBL)* 7. Molar heat of solution of a salt 8. Molar heat of an acid/base reaction 9. Heats of reaction 10. Testing Hess Law 11. 12. 13. 14. 15. 16. 17. 18. 19. Spontaneity of redox reactions A cycle of copper reactions (double class) Establishing a table of reduction potentials (CBL)* Electrolysis of Copper(II) sulfate Corrosion of iron (double class) Iodine clock reaction (double class) Testing Le Chteliers principle Vapor pressure of liquids (CBL)* Determination of an equilibrium constant (double class)

20. Identifying an unknown acid (CBL)* 21. Buffers 22. 23. 24. 25. 26. 27. 28. 29. 30. Energy content of foods (CBL)* Vitamin C in juices Proteins (double class) Enzymes (double class) Organic chemical compounds Synthesis of esters Saponification Preparation of nylon Synthesis of acetylsalicylic acid (NAIT)

*CBL= Calculator-based Learning

Lab 1: Decomposing Copper Oxide

Many metals react with oxygen in the air to form metallic oxides. Many metals can form more than one type of cation. For example, the process of rusting involves the reaction of iron and oxygen. However, iron can form Fe2+ ions or Fe3+ ions in ionic compounds. In this lab, you will be given a copper oxide and will determine whether it is copper (I) oxide or copper (II) oxide by heating the powder in the absence of oxygen to form copper metal. From the masses of the original copper oxide and the copper metal you obtain, you will calculate the percent by mass of copper in the original compound. By comparing your result to the theoretical percent by mass of copper in copper (I) oxide and copper (II) oxide, you can decide which compound was the starting material.

Materials:
test tube 2 holed stopper fitted with glass tubing bunsen burner matches rubber tubing lab stand test tube clamp balance copper oxide powder

Procedure:
1. Accurately determine the mass of your empty test tube. 2. Accurately measure between 3.00 and 4.00 g of copper oxide powder and place it in a test tube. 3. Clamp the test tube to the lab stand so that the tube is slightly angled. Make sure there is a thin coating of copper oxide on the test tube and that the copper oxide is away from the mouth of the test tube. 4. Assemble the apparatus as shown in the illustration on the next page. The gas should flow through the test tube and into the Bunsen burner. 5. Light the Bunsen burner. Use the hottest part of the flame to heat the copper oxide in the test tube. Move the Bunsen burner back and forth over the length of the test tube. Make sure to keep the flame away from the rubber stopper. Continue heating until all the copper oxide has reacted. 6. Allow the test tube and contents to cool in the absence of oxygen by moving the Bunsen burner from under the test tube. 7. Accurately measure the mass of the test tube and copper. Determine the mass of copper formed.

Observations:
mass of empty test tube __________ mass of test tube + copper oxide (before heating) __________ mass of copper oxide (before heating) __________ mass of test tube + copper oxide (after heating)__________ mass of copper oxide (after heating) __________

Analysis:
1. How could you tell when the reaction was completed?

2. Why was the gas sent through the test tube? Could this lab be performed with a test tube open to the air? Explain your answer.

3. Calculate the mass percent of copper in copper (I) oxide and in copper (II) oxide.

4. Calculate the mass percent of copper in your copper oxide sample.

5. What is the formula of the copper oxide you reacted?

Lab 2: Hydrates
A hydrate is a compound that contains discrete water molecules as part of their

crystalline structure. The water molecules are a distinct part of the compound but are joined to the salt by bonds that are weaker than the bonds in the salt or the bonds in the water molecules. The water may be removed from the salt by heating the salt. The salt without the water is called an anhydrous salt. In the first part of this experiment, you will measure the mass of a hydrated cobalt (II) chloride sample, then remove the water from the crystals, and measure the mass of the anhydrous salt. The data gathered will allow you to determine the percent water in the hydrated salt and also the empirical formula for the hydrated salt. In the second part of this experiment, you will perform a simple test on a CuSO45 H2O(s) sample to study its properties.

Materials:
hydrate sample (unknown) lab stand + small ring clamp screen crucible + lid balance copper (II) sulfate pentahydrate Bunsen burner + matches test tube + test tube clamp 250 mL beaker lab scoop distilled water

Procedure:
Part I: 1. Clamp the small ring clamp onto the lab stand and place the screen on the clamp. 2. Wash your crucible, wipe it dry, and put it onto the screen. Gently heat the crucible (with the crucible cover slightly ajar) for about 2 minutes to dry it well. 3. Move the crucible cover so that it seals the crucible from the atmosphere and allow to cool for about 5 minutes. 4. Weigh the empty crucible with the lid. 5. Accurately weigh approximately 3.00 g of your unknown hydrate into the crucible. 6. Place the crucible back on the screen. Heat the uncovered crucible and contents, gently at first, until you observe whether the salt melts and dissolves in its own water of crystallization. It if does become a liquid, heat very gently around the edges at first to avoid splattering. Then, increase the heat moderately, but do not allow the crucible to become red hot. 7. Heat for about 10 to 12 minutes and cover the crucible. Allow the covered crucible and its contents to cool on the screen for about 10 minutes. While waiting for the crucible to cool, go to part II. 8. When cool, re-weigh the crucible, the cover and its contents carefully, but quickly, to avoid re-absorption of water from the air by the salt. 9. After obtaining this mass measurement, you must reheat the crucible and contents a second time, allow them to cool, and record the weight again to determine if a

constant mass has been reached (within 0.1 g). This time, do not heat as strongly or as long as before. 10. When you have finished this part of the experiment, put the solid in the solid waste container provided in the fumehood. Part II: 1. Obtain a few crystals of copper (II) sulfate pentahydrate in a clean, dry test tube. 2. Gently heat the crystals by holding the tube, with a test tube clamp, in an inclined position over a Bunsen burner flame. Do not point the open end of a test tube towards anyone. 3. Continue heating until no further change is observed. 4. Allow the test tube to cool, then add two or three drops of water to the residue. 5. Put the aqueous waste in the waste container provided on the table in the front.

Observations:
1. Observation regarding before/after heating ________________________________ ___________________________________________________________________ 2. Mass of crucible (dry) Mass of crucible + sample (before heating) (after first heating) (after second heating) Mass of sample (before heating) (after heating) Mass of water lost from heating __________ __________ __________ __________ __________ __________ __________

Analysis:
Part I: 1. Determine the mass percentage of water in the hydrated salt.

2. Determine the number of moles of water evaporated from your hydrate.

3. Determine the number of moles of anhydrous salt.

4. Calculate the empirical formula for your hydrated salt.

Part II: 1. What evidence is there that water is present in the CuSO4 5 H2O crystal?

2. Describe the difference in appearance and composition between the anhydrous residue and the hydrate.

3. What did you observe when water was added to the anhydrous salt?

Lab 3: Qualitative Analysis of Anions

The presence of an ion in solution is generally confirmed when a reaction takes place resulting in the formation of a precipitate or by a color change. In this experiment, identification of ions will be done using the techniques of qualitative analysis. The word qualitative refers to the fact that you are simply trying to ascertain whether a particular ionic species is present. You are not trying to find out how much is present. Testing will consist of adding solutions containing Fe2+ (with and without acid), Fe3+, and Ag+, to solutions containing each of ten anions. For each test, you must decide whether you see cloudiness, indicating the formation of an insoluble precipitate, a color change that is not simply the result of mixing or dilution, or no reaction at all. A word about color changes: If you add a colorless solution to one that is yellow, having the yellow color grow more pale is expected. If, on the other hand, the yellow solution turns to a green solution, that indicates a new species has been produced, so a reaction has occurred.

Materials:
2 well plates 4 100 mL beakers 4 eyedroppers distilled water cotton swabs 10 anion test solutions: sodium bromide, NaBr(aq) sodium chloride, NaCl(aq) sodium iodide, NaI(aq) sodium phosphate, Na3PO4(aq) sodium oxalate, Na2C2O4(aq) sodium carbonate, Na2CO3(aq) sodium thiosulfate, Na2S2O3(aq) sodium nitrate, NaNO3(aq) sodium sulfate, Na2SO4(aq) sodium hydroxide, NaOH(aq) 4 test reagents: iron (II) sulfate, FeSO4 7 H2O(aq) iron (III) nitrate, Fe(NO3)3 9 H2O(aq) silver nitrate, AgNO3(aq) 8.0 M sulfuric acid, H2SO4(aq) 3 unknown samples

Procedure: Part I:

1. Label the four 100 mL beakers A, B, C, and D. In beaker A, obtain approximately 75 mL of iron (II) sulfate; in beaker B, 75 mL of iron (III) nitrate; in beaker C, 75 mL of silver nitrate; and in beaker D, 50 mL of sulfuric acid. 2. Into two separate wells of one of the test plates, place 10 drops of NaBr(aq). To one of the wells containing the NaBr(aq), add 5 drops of FeSO4(aq). Observe and record any changes that occur. NOTE: There are three types of changes that you must look for when adding strong acid: (1) evolution of a gas; (2) a color change that is not the result of mixing or dilution; (3) the formation of a precipitate. 3. If no changes are observed, add 3 drops of H2SO4(aq) to the solution in 2, and record your observations. 4. To the second well containing NaBr solution, add 5 drops of Fe(NO3)3(aq). As before, observe and record any changes that occur. If no changes are observed, add 3 drops of sulfuric acid, and observe and record any evidence of reaction. 5. Repeat steps 1 to 3 for the remaining anions. 6. Dispose of the solutions in the large waste beaker. Over a sink, rinse the well plate, use a cotton swab to remove all traces of precipitates from the wells, rinse with distilled water, and shake dry. Part II: In the second well plate, duplicate the tests done with the ten anion test solutions using silver nitrate. You need not add acid to these tests. Be sure to record your observations and dispose of the solutions in the waste beaker marked Ag waste. Over the waste beaker, use a wash bottle and cotton swabs to remove all traces of precipitate from the wells. Over the sink, rinse the well plate once more with distilled water and shake dry. Part III: You will be given three unknown solutions. The first contains one of the 3 halide solutions; the second contains one of the 7 polyatomic anion solutions; the third will contain either iron (II), iron (III), or silver ions. If iron ions were used to help identify the unknown, use the first well plate and dispose following the method at the end of part I; if silver ion was used, use the second well plate and dispose using the method described in part II.

Observations:
Anion BrClIPO43C2O42CO32S2O32NO3SO42OHUnknown #1 Unknown #2 Unknown #3 Result With Fe2+ Effect Of H2SO4 Result With Fe3+ Effect Of H2SO4 Result With Ag+

Analysis: 1. Identify the three unknown samples: solution #1: __________ solution #2: __________ solution #3: __________ solution #1: __________ solution #2: __________ solution #3: __________

2. What test confirmed their identities:

3. Suppose you are given three unlabeled solutions. You know that one contains copper (I) ions, another contains copper (II) ions, and the third has barium ions, but you dont know which is which. Devise a method by which you could identify each of the three cation solutions.

Lab 4: Analysis of Stomach Antacid Tablets

Antacid tablets consist of weakly basic substances that are capable of reacting with the hydrochloric acid found in the stomach, converting the stomach acid into neutral or nearly neutral salts. In this experiment, you will evaluate the effectiveness of various commercial antacids towards neutralizing hydrochloric acid (stomach acid) and you will compare these products to the effectiveness of simple baking soda (sodium hydrogen carbonate). The antacids will be dissolved in an excess of 1.0 mol/L hydrochloric acid, and then the remaining acid (i.e. the portion of the acid that did not react with the antacid) will be titrated with 2.0 mol/L sodium hydroxide solution. NOTE: It is not possible to titrate antacid tablets directly for several reasons. First, commercial antacid tablets frequently contain binders, fillers, flavorings, and coloring agents that may interfere with the titration. Second, the bases found in most antacids are weak and become buffered as they are titrated, often leading to an indistinct indicator endpoint.

Materials:
50 mL buret lab stand and buret clamp small funnel 100 mL graduated cylinder sodium hydrogen carbonate 1.0 mol/L hydrochloric acid 2.0 mol/L sodium hydroxide 2 brands of commercial antacid tablets 250 mL beaker 250 mL Erlenmeyer flask bromophenol blue or methyl orange indicator solution distilled water

Procedure:
1. Obtain approximately 100 mL of NaOH(aq) in the 250 mL beaker. 2. Rinse the buret with approximately 5 mL of distilled water. Use the small funnel to rinse the buret twice with approximately 5 mL of NaOH(aq). Fill the buret with the NaOH(aq). 3. Use the mortar and pestle to crush an antacid tablet. Weigh a clean, dry Erlenmeyer flask to the nearest 0.01 g. Transfer as much of the crushed antacid tablet as possible to the flask, and reweigh to the nearest 0.01 g. 4. Using the graduated cylinder, measure exactly 100 mL of hydrochloric acid and add it to the Erlenmeyer flask containing the crushed tablet. Swirl the flask to dissolve the tablet as much as possible. NOTE: As mentioned earlier, commercial antacid tablets contain various other ingredients, which may not completely dissolve. 5. Add 3-4 drops of indicator to the sample. 6. Record the initial reading of the buret. Titrate the acidified antacid sample with the

NaOH solution until the endpoint has been reached. Record the final reading of the buret at the color change. 7. Discard the solution in the sink. Rinse the Erlenmeyer with distilled water. Repeat steps 3 to 6 twice more using the same brand of antacid tablet. 8. Repeat the procedure (steps 3 to 7) with another brand of antacid tablet. 9. Repeat the procedure (steps 3 to 7) with 0.7 g (record the exact weight used) of sodium hydrogen carbonate. Add the hydrochloric acid to the sodium bicarbonate very slowly to prevent excessive frothing as carbon dioxide is liberated during the reaction.

Observations:
1. first tablet: brand: __________ mass: __________

Titration of __________ with 2.0 mol/L NaOH(aq) Trial Final buret reading (mL) Initial buret reading (mL) Volume of NaOH(aq) 1 2 3 4

2. second tablet:

brand: __________ mass: __________

Titration of __________ with 2.0 mol/L NaOH(aq) Trial Final buret reading (mL) Initial buret reading (mL) Volume of NaOH(aq) 1 2 3 4

3. sodium hydrogen carbonate mass:

__________

Titration of NaHCO3(aq) with 2.0 mol/L NaOH(aq) Trial 1 2 3 4

Final buret reading (mL) Initial buret reading (mL) Volume of NaOH(aq)

Analysis:
1. Calculate the millimoles of hydrochloric acid consumed by the antacid tablet/ sodium hydrogen carbonate in each titration.

2. Calculate the volume of dilute hydrochloric acid that corresponds to the number of millimoles consumed in each of the titrations.

3. Assuming that the density of HCl solution used was 1.00 g/mL, calculate the weight of the hydrochloric acid solution consumed by the tablet/ sodium hydrogen carbonate.

4. Calculate the mass of the HCl solution consumed per gram of antacid tablet. Divide the mass of HCl consumed by the mass of the tablet used.

5. List the antacids (including the NaHCO3) in order of effectiveness (most effective to least effective).

Lab 5: Specific Heat Capacity of Metals

The specific heat capacity, c, is the amount of energy required to change the temperature of one gram of a substance by one Celsius degree. Each substance has a unique specific heat capacity. Metallic substances generally have numerically small specific heat capacities. Metals are good conductors of heat energy and require very little input of heat energy to cause an increase in their temperature. Insulating substances, on the other hand, are very poor conductors of heat energy and have much larger specific heats. In this lab, you will determine the specific heat capacities of two unknown metallic substances using calorimetry. A known volume of cold water (at a known temperature) is placed in a calorimeter while a known mass of unknown metal is heated to approximately 100C. The hot metal is then transferred to the cold water in the calorimeter and the maximum temperature reached by the cold water as it absorbs heat from the metal is recorded. From the masses of cold water and metal used, and from the temperature changes for each substance, the specific heat of the metal may be calculated: mmetal cmetal Tmetal = -mwater cwater Twater One you have determined the specific heat of two unknown samples, you will compare these results with accepted values, and finally, identify the two unknown samples.

Materials:
lab stand and small ring clamp wire gauze matches bunsen burner stir rod tongs balance 100 mL graduated cylinder distilled water 250 mL beaker calorimeter apparatus unknown metal samples

Procedure:
1. Find the mass of one of the metal samples. 2. Set up the lab stand and ring clamp and place the 250 mL beaker on the wire gauze. Add about 100 mL of tap water to the beaker and place the metal in the water. 3. Heat the tap water until it begins to boil. Record the temperature of the boiling water. Allow the metal to remain in the boiling water for at least three minutes. 4. Measure 100 mL of cold distilled water in the graduated cylinder and place it in the calorimeter. 5. Record the initial temperature of the water (to 0.1C). 6. Using the tongs, quickly transfer the metal from the boiling water to the calorimeter. Gently stir the water in the calorimeter for several seconds. Cover the top of the calorimeter. 7. Record the highest temperature reached. 8. Repeat these steps with the other metal sample.

Observations:
sample 1 mass of unknown metal initial temperature of water in calorimeter final temperature of water in calorimeter temperature change of water in calorimeter temperature of boiling water final temperature of metal in calorimeter temperature change of metal _______ _______ _______ _______ _______ _______ _______ sample 2 _______ _______ _______ _______ _______ _______ _______

Analysis:
1. Calculate the specific heat capacity of each metal.

2. Compare your values to the data booklet and identify each metal.

3. Assuming the identities of your samples are correct, determine your percent error in the specific heat capacity of each metal.

Lab 6: Molar Heat of Fusion of Ice

Melting and freezing are among the characteristic properties that give a pure substance its unique identity. As energy is added, pure solid water (ice) at 0C changes

to liquid water at 0C. In this experiment, you will determine the energy required to melt one gram of ice. You will then determine the molar heat of fusion for ice. Excess ice will be added to warm water, at a known temperature, in a styrofoam cup. The warm water will be cooled down to a temperature near 0C by the ice. The energy required to melt the ice is removed from the warm water as it cools.

Materials:
CBL2 interface TI graphing calculator temperature probe 100 mL graduated cylinder 100 mL beaker 250 mL beaker tongs Styrofoam cup ring stand utility clamp ice cubes stirring rod warm water

Procedure:
1. Place a styrofoam cup into the 250 mL beaker. 2. Use the graduated cylinder to accurately transfer 100 mL of 60C water into the calorimeter. 3. Obtain 7 or 8 large ice cubes. 4. Turn on the calculator and start the Datamate program. Set up the calculator and interface for the Temperature Probe. Set up the data-collection mode to CHANGE TIME SETTINGS. Enter "5" as the time between samples in seconds. Enter "96" as the number of samples. The length of the data collection will be 8 minutes. 5. Lower the temperature probe into the warm water (to about 1 cm from the bottom). 6. Select START to begin to monitor temperature. The temperature reading, in C, is displayed on the upper-right corner of the graph. Wait until the temperature reaches a maximum (it will take a few seconds for the cold probe to reach the temperature of the warm water). This maximum will determine the initial temperature, t1, of the water. As soon as this maximum temperature is reached, fill the styrofoam cup with ice cubes. Shake excess water from the ice cubes before adding them. 7. Use a stirring rod to stir the mixture as the temperature approaches 0C. Important: As the ice melts, add more large ice cubes to keep the mixure full of ice. 8. When the temperature reaches about 4C, quickly remove the unmelted ice (using tongs). Continue stirring until the temperature reaches a minimum (and begins to rise). This minimum temperautre is the final temperature, t2, of the water. 9. Press the STO key to stop the data collection. Use the 100 mL graduated cylinder to measure the volume of water remaining in the styrofoam cup to the nearest 0.1 mL.

10. To confirm the t1 and t2 values you recorded earlier, examine the data points along the curve on the displayed graph. As you move the cursor right or left, the time (x) and temperature (y) values of each data point are displayed below the graph. Determine the maximum temperature, t1, and the minimum temperature, t2 (round to the nearest 0.1C).

Observations:
Initial temperature of water, t1 Final temperature of water, t2 Change in water temperature, t Final volume of water, V2 Initial volume of water, V1 Volume of melt C C C mL mL mL

Analysis:
1. Calculate the molar heat of fusion of ice. (-mc twater = nHice melting + mc tice water)

2. Find the % error of the experimental results, given that the accepted value is 6.01 kJ/mol. (% error = experimental value - theoretical value / theoretical value x 100 %)

3. List some possible sources of error.

Lab 7: Molar Heat of Solution of a Salt

When salts dissolve in water, the cations and anions in the salt interact with water molecules. Water molecules are very polar and arrange themselves in a layer around the ions of salt so as to maximize electrostatic attrative forces. Such a layer of water molecules surrounding an ion is called a hydration sphere. Formation of a hydration sphere around an ion necessarily involves an energy change. In this lab, you will determine the energy change for two examples of such a process.

Materials:
balance lab scoop distilled water graduated cylinder calorimeter apparatus 100 mL beaker sodium nitrate potassium hydroxide

Procedure:
1. Measure 100.0 mL of distilled water in the graduated cylinder and empty it in the calorimeter. 2. Record the initial temperature of the water (to 0.1C). 3. Obtain enough sodium nitrate to make a 1.00 mol/L solution, add to the water, stir with the thermometer, cover, and record the maximum temperature change obtained (to 0.1C). 4. Dispose of the contents in the proper waste container. 5. Place the second cup into the first and nest the cups into the 250 mL beaker. 6. Repeat the experiment with enough potassium hydroxide to make a 1.00 mol/L solution.

Observations:
initial temperature of water final temperature of water + NaNO3(s) temperature change of water mass of NaNO3(s) added __________ __________ __________ __________

initial temperature of water final temperature of water + KOH(s) temperature change of water mass of KOH(s) added

__________ __________ __________ __________

Analysis:
1. Show calculations for mass of NaNO3(s) added to 100.0 mL of water to make a 1.00 mol/L solution.

2. Determine the molar enthalpy of solution of NaNO3(s). (nHs = -vc twater)

3. Show calculation for mass of KOH(s) added to 100.0 mL of water to make a 1.00 mol/L solution.

4. Determine the molar enthalpy of solution of KOH(s).

5. Find the % error of the experimental results of the molar enthalpy of solution for sodium nitrate, given that the accepted value is +22.0 kJ/mol. (% error = experimental value - theoretical value / theoretical value x 100 %)

Lab 8: Molar Heat of an Acid/Base Reaction

Many chemical reactions are performed routinely with the reactant species dissolved in water. Heats of reaction between species dissolved in water are especially easy to measure because the measurement may be performed in a simple calorimeter. A measured volume of solution of one of the reagents is placed in the calorimeter cup, and its temperature is determined. The second reagent solution is prepared in a separate container. When the two solutions have come to the same temperature, they are combined in the calorimeter, and the temperature of the calorimeter contents is monitored. In this lab, you will measure the heat of reaction for four different reactions. Each of these reactions represents the neutralization of an acid by a base, and although the reactions formally appear to involve different substances, the net reaction occurring in each case is the same: H+(aq) (from the acid) + OH-(aq) (from the base) ---> H2O(l) The actual reaction that occurs in each situation is the combination of a proton with a hydroxide ion, producing a water molecule. For this reason, the heat flows should be the same for all of these reactions.

Materials:
calorimeter apparatus 100 mL graduated cylinder 100 mL beaker stir rod 2.0 mol/L hydrochloric acid 2.0 mol/L nitric acid 2.0 mol/L sodium hydroxide 2.0 mol/L potassium hydroxide

Procedure:
1. Obtain 75 mL of NaOH(aq) and place it in the calorimeter. Obtain 75 mL of HCl(aq) in a clean, dry 100 mL beaker. Measure and record the initial temperatures of the solutions to the nearest 0.1C (these should be the same ... if not, allow them to stand until their temperatures are 0.5C). Be sure to rinse off and dry the thermometer when transferring between the solutions to prevent premature mixing of the reagents. 2. Add the HCl(aq) from the beaker all at once to the calorimeter, stir for several seconds, and cover the calorimeter. Record the highest temperature reached by the mixture. 3. Repeat the procedure for the other combinations of acids and bases.

Observations:
NaOH/HCl initial temperature of base acid average temperature NaOH/HNO3 KOH/HCl ________ ________ KOH/HNO3 _________ _________

_________ __________ _________ __________

_________ __________ ________ _________ final termperature _________ __________ ________ _________ temperature change _________ __________ ________ _________

Analysis:
1. From the change in temperature undergone by the mixtures upon reaction and the total mass (volume) of the combined solutions, calculate the quantity of heat that flowed from the reactant species into the water of the solution. (q = mc T)

2. Calculate the number of moles of water produced when 75 mL of 2.0 mol/L HCl(aq) reacts with 75 mL of 2.0 mol/L NaOH(aq).

3. Calculate the H in terms of the number of kilojoules of heat energy transferred when 1.0 mol of water is formed in the neutralization of HCl(aq) with NaOH(aq).

4. Calculate the H for the neutralization of 1.0 mol of water for the other three reactions.

5. From your results, calculate a mean value and standard deviation for H for the net reaction occurring in the mixtures, i.e., H+(aq) + OH-(aq) ---> H2O(l)

Lab 9: Heats of Reaction

In this experiment, you will measure and compare the quantify of heat released in three chemical processes. Each reaction involves the preparation of a solution. Each preparation results in a change in temperature. After you measure the temperature change, you will calculate the energy change for these reactions. The processes to be compared are: 1. Solid sodium hydroxide dissolves in water to form an aqueous solution of ions ( H1): NaOH(s) ---> Na+(aq) + OH-(aq) 2. Solid sodium hydroxide reacts with an aqueous solution of hydrogen chloride to form water and an aqueous solution of sodium chloride ( H2): NaOH(s) + H+(aq) + Cl-(aq) ---> H2O(l) + Na+(aq) + Cl-(aq) 3. An aqueous solution of sodium hydroxide reacts with an aqueous solution of hydrogen chloride to form water and an aqueous solution of sodium chloride ( H3): Na+(aq) + OH-(aq) + H+(aq) + Cl-(aq) ---> H2O(l) + Na+(aq) + Cl-(aq) Three assumptions need to be made: -any small heat losses to the surroundings will be negligible -the aqueous solutions that are prepared have the same specific heat capacity as water -the solutions are so dilute that their densities are the same as that of pure water

Materials:
4 styrofoam cups 50 mL beaker 100 mL graduated cylinder thermometer stirring rod balance solid sodium hyroxide 2.0 mol/L sodium hydroxide solution 1.0 mol/L hydrochloric acid 2.0 mol/L hydrochloric acid

Procedure:
Part I: 1. Label the cups A, B, C, and D. 2. Measure 100 mL of distilled water with the graduated cylinder and place it into Cup A. Measure its temperature. 3. Obtain a sample of about 4.00 g of solid sodium hydroxide in the 50 mL beaker. Determine its mass to the nearest 0.01g. 4. Pour the solid NaOH into the water. Stir until it dissolves. Record the highest

temperature reached. Part II: 1. Measure 100 mL of 1.0 mol/L hydrochloric acid with the graduated cylinder and place it into cup B. Measure its temperature as precisely as possible. 2. Obtain another sample of about 4.00 g of solid sodium hydroxide in the 50 mL beaker. Determine its mass to the nearest 0.01 g. 3. Pour the solid NaOH into the HCl solution. Stir until it dissolves. Record the highest temperature reached. Part III: 1. Measure 50.0 mL of 2.0 mol/L hydrochloric acid into cup C. 2. Measure 50.0 mL of 2.0 mol/L sodium hydroxide solution into cup D. 3. Record the temperature of each solution. Both should be at, or slightly below, room temperature. Rinse and dry the thermometer before changing from one solution to the other. 4. Add the NaOH solution to the HCl solution in cup C. Stir quickly and record the highest temperature reached.

Observations:
Part I: mass of NaOH(s): initial temperature of water: final temperature of water: temperature change of water: mass of NaOH(s): initial temperature of HCl(aq): final temperature of HCl(aq): temperature change of HCl(aq): __________ __________ __________ __________ __________ __________ __________ __________

Part II:

Parti III:

initial temperature of NaOH(aq): __________ __________ initial temperature of HCl(aq): final temperature: __________ temperature change of NaOH(aq): __________ temperature change of HCl(aq): __________

Analysis:
1. Write the net ionic equations for each step. Now, using Hess Law, add the first and third equations together. Cancel any reaction species which appear on both sides of the equation. Compare the sum of those two equations to the second equation. Comment on how they are related.

2. Determine the total energy released per mole of NaOH consumed for each reaction.

3. Calculate the percent difference between H1 + H3 and H2 using (( H1 + H3 H2) / H2) 100%.

Lab 10: Testing Hess Law

In 1840, G. H. Hess recognized that the energy change that accompanies a reaction depends only on the reactants used and the products formed, not in the way in which reactants are converted to products. This came to be known as Hess Law. It will be your goal in this experiment to demonstrate for yourself that this statement is a valid one. To do that, you will measure the energy change for two different reactions, then combine them to predict the energy change for another reaction. Here are the three reactions: MgO(s) + 2 HCl(aq) ---> MgCl2(aq) + H2O(l) Mg(s) + 2 HCl(aq) ---> MgCl2(aq) + H2(g) Mg(s) + 1/2 O2(g) ---> MgO(s) You will measure the heats of reactions for the first two, then combine them to predict the heat of combustion for magnesium.

Materials:
15 cm strip of magnesium ribbon magnesium oxide(s) 1.00 mol/L hydrochloric acid 250 mL beaker calorimeter apparatus 100 mL graduated cylinder lab scoop balance steel wool

Procedure:
1. Measure precisely 1.04 g of magnesium oxide in a clean, dry calorimeter. 2. Obtain about 100 mL of HCl(aq) in the 250 mL beaker. Transfer 50.0 mL of the acid into the graduated cylinder. 3. Measure the temperature of the HCl(aq). 4. Add the acid to the magnesium oxide, stir, and cover. 5. Record the maximum temperature of the mixture. 6. Dispose of the contents in the proper waste container. 7. Place the second cup into the first and nest the cups into the 250 mL beaker. 8. Clean the magnesium ribbon with the steel wool. 9. Measure the mass of the clean magnesium ribbon. 10. Transfer 50.0 mL of HCl(aq) into the graduated cylinder. 11. Place the acid into the calorimeter and record the initial temperature. 12. Add the magnesium ribbon to the calorimeter, making sure all of the metal is in the acid. 13. Stir, cover, and record the maximum temperature.

Observations:
mass of magnesium oxide __________

initial temperature of HCl(aq) final temperature of HCl(aq) temperature change of HCl(aq) mass of magnesium ribbon initial temperature of HCl(aq) final temperature of HCl(aq) temperature change of HCl(aq)

__________ __________ __________ __________ __________ __________ __________

Analysis:
1. Calculate the molar enthalpy of reaction for magnesium oxide. (nHr = -vc twater)

2. Calculate the molar enthalpy of reaction of magnesium.

3. According to Hess Law, the three equations given below can be combined in such a way, that one may calculate the molar enthalpy of combusion for magnesium. Show how this can be done. H= MgO(s) + 2 HCl(aq) ---> MgCl2(aq) + H2O(l) H= Mg(s) + 2 HCl(aq) ---> MgCl2(aq) + H2(g) H = -285.8 kJ H2(g) + 1/2 O2(g) ---> H2O(l)

4. The standard molar enthalpy of combusion for magnesium is generally accepted at -601.6 kJ/mol. Reflect the accuracy of your results by showing the percent difference.

Lab 11: Spontaneity of Redox Reactions

Many reactions involve a transfer of electrons from one atom (or ion) to another. If an atom loses electrons, those electrons must be transferred to some other atom or ion; the atom or ion that takes the electrons is called the oxidizing agent. This name suggests that the receiver of the electrons caused the oxidation to occur. Similarly, the species that loses the electrons is called a reducing agent, because it provided the electrons that caused the other atom or ion to become reduced. In this lab, you will study a number of chemical reactions that involve the transfer of electrons from a reducing agent to an oxidizing agent.

Materials:
strips of copper, magnesium, silver, and zinc 0.10 mol/L solutions of copper (II) nitrate, magnesium nitrate, silver nitrate, and zinc nitrate test tube rack 16 test tubes 4 - 100 mL beakers steel wool tweezers masking tape distilled water

Procedure:
1. 2. 3. 4. 5. Obtain about 25 mL of each aqueous solution in four labelled beakers. Clean the four metal strips using steel wool. Label and rinse four test tubes with distilled water. Add 2-3 cm of Cu(NO3)2(aq) to each of the four test tubes. Drop a different metal strip into each test tube and observe for several minutes (there should be a color change). 6. Repeat steps 2 to 5 using Mg(NO3)2(aq), AgNO3(aq), and Zn(NO3)2(aq). 7. Dispose of the solutions into the labelled waste containers and clean the metal strips for reuse.

Observations:
Cu(s) Cu2+(aq) Mg2+(aq) Ag+(aq) Zn2+(aq) Mg(s) Ag(s) Zn(s)

Analysis:
1. List metals in order of reactivity (beginning with most reactive):

2. List metal ion solutions in order of reactivity:

3. What can be said of a metal reacting with a solution of its own ion?

Lab 12: A Cycle of Copper Reactions

In this lab, you will follow a sequence of reactions of copper that form a cycle. You will observe the color and physical property changes of those reactions. Because no copper is added or removed between the initial and final steps, and because each reaction essentially goes to completion, you should be able to recover all of the copper you started with, if you are careful and skillful. The following diagram shows an abbreviated form of the reactions: Cu(NO3)2(aq) Cu(OH)2(s) Cu(s) CuSO4(aq) CuO(s)

Materials:
copper powder zinc pellets 15.0 mol/L nitric acid 3.0 mol/L sodium hydroxide 6.0 mol/L sulfuric acid 6.0 mol/L hydrochloric acid methanol 250 mL beaker 50 mL beaker evaporating dish 10 mL graduated cylinder stir rod hot plate distilled water

Procedure:
CAUTION: Extremely concentrated solutions. Wear proper protection (including rubber gloves), especially when handling the acids and the sodium hydroxide. Teachers should consider all factors (students, lab safety etc.) before using such a concentrated solution. 1. Accurately weigh about 1.0 g of copper powder into a 250 mL beaker. 2. Have your teacher supervise as, in the fume hood, you add 5.0 mL of nitric acid to the copper powder. One of the products of this reaction is nitrogen monoxide, NO, which is a colorless gas. On exposure to air, however, this gas immediately reacts with oxygen to form the poisonous reddish-brown gas, nitrogen dioxide, NO2. As a consequence, you must carry out this reaction in the fume hood. Set the beaker on the fumehood surface for about 30 seconds until the vigorous bubbling has subsided. Carefully swirl the solution around in the beaker until all of the copper has

completely reacted. After the copper has reacted, add distilled water until the beaker is about half full. Steps 3 through 6 can be conducted at your lab table. 3. While stirring the solution with a glass rod, add 30 mL of sodium hydroxide. You should observe the formation of a precipitate. If no precipitate is formed, continue adding NaOH(aq) one drop at a time, while stirring. Let the reaction mixture stand for one minute. 4. Heat (but do not boil) the solution over a hot plate, stirring gently to prevent bumping (a phenomenon caused by the formation of a large steam bubble in a locally overheated area). If the solution bumps, you may lose some CuO, so dont neglect the stirring. 5. When the transformation is complete (it turns black), remove the heat source, continue stirring for a minute or so, then allow the CuO to settle overnight. Decant (pour off) the supernatant liquid, being careful not to lose any CuO. Add about 200 mL of hot distilled water, allow to settle again, and decant once more. 6. Add 15 mL of sulfuric acid, while stirring. 7. Add 2.0 g of zinc pellets to the solution in 6, stirring and heating until the supernatant liquid is colorless. When the evolution of gas has become very slow, decant the supernatant liquid. If you can see any silvery grains of unreacted zinc, add 10 mL of hydrochloric acid and warm gently, while stirring. When no hydrogen evolution can be detected by eye, decant the supernatant liquid, and transfer the copper to an evaporating dish. 8. Wash the product with about 5 mL of distilled water, allow it to settle, and decant the wash water. Repeat the washing and decantation at least two more times. Move to the fume hood, away from all heat sources. 9. Wash the copper with about 5.0 mL of methanol, allow to settle, and decant (in the proper waste receptacle). 10. Place the evaporating dish on the hot plate, and gently heat to dry the metallic copper. The product should be bright reddish-brown. Calculate the mass of the copper you recovered using a preweighed 50 mL beaker.

Observations:
initial mass of copper powder mass of empty 50 mL beaker mass of beaker plus copper mass of recovered copper __________ __________ __________ __________

Analysis:
1. For each step of the cycle, write the products of the reaction and balance the chemical equation: a. ___ Cu(s) + ___ HNO3(aq) + ___ O2(g) ---> b. ___ Cu(NO3)2(aq) + ___ NaOH(aq) ---> c. ___ Cu(OH)2(s) + heat ---> d. ___ CuO(s) + ___ H2SO4(aq) ---> e. ___ Zn(s) + ___ CuSO4(aq) ---> 2. Calculate your percentage recovery (mass of recovered copper divided by initial mass of copper powder)

Lab 13: Establishing a Table of Reduction Potentials

The main objective of this experiment is to establish the reduction potentials of four unknown metals relative to an arbitrarily chosen metal. This will be done by measuring the voltage, or potential difference, between various pairs of half-cells. A voltaic cell utilizes a spontaneous oxidation-reduction reaction to produce electrical energy. Half-cells are normally produced by placing a piece of metal into a solution containing a cation of the metal. The two half-cells are normally separated by a porous barrier or a salt bridge. In this micro-version of a voltaic cell, the half cell will be a small piece of metal placed into 3 drops of solution on a piece of filter paper. The solution contains the cation of the solid metal. The salt bridge will be several drops of aqueous NaNO3 placed on the filter paper between the two half cells. Using the graphing calculator and CBL2 as a voltmeter, the (+) lead makes contact with one metal and the (-) lead with another. If a positive voltage is recorded on the screen, you have connected the cell correctly. The metal attached to the (+) lead is the cathode (reduction) and thus has a higher, more positive reduction potential. The metal attached to the (-) lead is the anode (oxidation) and has the lower, more negative, reduction potential. If you get a negative voltage reading, then you must reverse the leads. By comparing the voltage values obtained for several pairs of half-cells, and by recording which metal made contact with the (+) and (-) leads, you can establish the reduction potential sequence for the four metals in this lab.

Materials:
CBL2 interface TI graphing calculator Voltage Probe U-tube 1.0 M solutions of the unknown metal cations 1 x 1 cm samples of the unknown metals 1.0 M solution of NaNO3 11.0 cm diameter filter paper steel wool 15 x 15 cm glass plate scissors

Procedure:
1. Turn on the calculator and start the DataMate program. Set up the calculator and the interface for the Voltage Probe. 2. Draw 4 small circles on the filter paper. Using a pair of scissors, cut wedges between the circles. Label the circles M1, M2, M3, and M4. Place the filter paper on top of the glass plate. 3. Clean the 4 unknown metals on both sides with the steel wool. Place each metal near the circle with the same number.

4. Place 3 drops of each solution on its circle. Place the corresponding metal on the wet spot with its respective cation. The top side of the metal should be kept dry. 5. Add several drops of NaNO3(aq) between each circle and the center of the filter paper. Be sure there is a continuous trail of NaNO3(aq) between each circle and the center. You may have to periodically dampen the filter paper with more NaNO(aq) during the experiment. 6. Use metal M1 (the one that is obviously copper) as the reference metal. Determine the potential of the other three cells by connectig M1 to M2, M1 to M3, and M1 to M4. This is done by bringing the (+) lead in contact with one metal and the (-) lead in contact with the other. If the voltage displayed on the main screen of the calculator is negative, then reverse the leads. Wait about 5 seconds to take a voltage reading, and record the (+) value appearing on the calculator screen in your observation table (round to the nearest 0.01 V). Record which metal is the (+) terminal and which is (-), when the voltage value is positive. 7. Use the same procedure and measure the potential of the other two cells, continuing to use M1 as the reference electrode. 8. Measure the potential of the three remaining half-cell combinations. If the NaNO3(aq) salt bridge has dried, you may have to re-moisten it. 9. When you are finished, select QUIT and exit the DataMate program. Rinse each piece of metal with tap water. Dry it and return it to the correct container. Remove and discard the filter paper. Rinse the glass plate with tap water.

Observations:
voltaic cell (metals used) M1 / M2 M1 / M3 M1 / M4 M2 / M3 M2 / M4 M3 / M4 measured potential (V) metal number of (+) lead metal number of (-) lead

Analysis:
1. Using copper as M1, identify the reduction potentials of the remaining metals.

2. Arrange the four metals (including M1) from the highest reduction potential at the top (most positive) to the lowest reduction potential at the bottom (most negative).

3. Using a reduction potential chart, identify the 3 remaining metals.

4. Complete the following table: voltaic cell (metals used) M1 / M2 M1 / M3 M1 / M4 M2 / M3 M2 / M4 M3 / M4 measured potential (V) predicted potential (V) percent difference (%)

Lab 14: Electrolysis of Copper(II) Sulfate

Electrolysis is the use of an electrical current to force a chemical reaction to occur that would ordinarily not proceed spontaneously. When an electrical current is passed through a molten or dissolved electrolyte between two physically separated electrodes, two chemical changes take place. At the positive electrode (anode), an oxidation half-reation takes place. At the negative electrode (cathode), a reduction halfreaction takes place. Exactly what half-reaction occurs at each electrode is determined by the relative ease of oxidation-reduction of all the species present in the electrolysis cell.

Materials:
low voltage power supply U-tube 2 - carbon electrodes lab stand utility clamp 2 - 250 mL beaker ethanol 0.50 mol/L copper (II) sulfate

Procedure:
1. Attach one of the U-tubes (inverted ... open ends up) to the lab stand by a utility clamp. 2. Using one of the 250 mL beaker, fill the U-tube with about 70 mL of CuSO4 solution. 3. Obtain about 150 mL of ethanol in a second 250 mL beaker. Clean the carbon electrodes with the ethanol. Place a carbon electrode in each end of the U-tube. 4. Connect the power supply and allow the electolysis to proceed for 5 to 10 minutes. 5. Disconnect the power supply, remove the carbon electrodes, and describe any changes which occurred during the electrolysis.

Observations:
CuSO4(aq) circuit condition of electrodes cathode _______ anode _______

Analysis:
1. Write out the net ionic reactions of the cell and determine the minimum voltage required.

2. What gas was evolved during electrolysis? At which electrode?

Lab 15: Corrosion of Iron

Corrosion is a general term applied to the process in which metals are converted to oxides or to other compounds. Iron (III) oxide is commonly called rust. The process of corrosion gradually deteriorates the metals involved. Although the detailed chemistry of the corrosion is often not completely understood, it clearly involves oxidation and reduction. Most metals are easily oxidized; that is, they lose electrons relatively easily. Conversely, the oxygen gas in the atmosphere is a good oxidizing agent because atoms of oxygen easily gain electrons (are reduced). In this lab, you wil study some of the factors involved in the corrosion of iron. You will observe the behavior of iron in the presence of a number of solutions as well as in the presence of other metals. This lab require two classes to complete.

Materials:
9 small iron finishing nails 6 small test tubes test tube rack 250 mL beaker pH paper test strips Petri dish tweezers pliers stir rod 1% phenolphthalein solution steel wool copper wire zinc strip prepared agar solution 0.1 mol/L potassium hexacyanoferrate solution, K3Fe(CN)6 solution sets: Group A Group B Group C NaOH KOH Na3PO4 Na2CO3 Na2C2O4 Na2Cr2O7 KSCN NaCl KNO3 H2SO4 HCl HNO3 distilled H2O distilled H2O distilled H2O

Procedure:
Part I: 1. Place a clean, bright nail into each of five test tubes. Use steel wool if necessary to clean the surface of the nails. Slide each nail carefully down the side of the test tube to avoid breaking the bottom of the test tube. 2. Label and partially fill each of the test tubes with one of the reagents in a solution set (assigned) so that the nail is just covered. 3. Dip pieces of pH paper into each solution to determine whether the solution is acidic, basic, or neutral. 4. Allow the nails to stand overnight in the solution and proceed to Part II. Part II: 1. Obtain about 100 mL of the prepared agar solution in a beaker. Add about 10 drops of K3Fe(CN)6(aq) and 10 drops of phenolphthalein indicator solution to the agar mixture. Stir thoroughly. 2. Place a clean, bright nail in a Petri dish. Bend another clean nail sharply with a pair of pliers and place it in the same dish. Make sure that the nails do not touch each other. 3. Twist a clean piece of bare copper wire around a third nail. Temporarily remove the nail from the coil and tighten the wire coil so that when the nail is forced back through, it makes tight contact with the wire coil. Place this nail in the lid of the Petri dish. 4. Twist a clean piece of zinc around a fourth nail. As in the previous step, be sure that the zinc makes tight contact with the nail. Place this nail in the lid of the Petri dish. Again, make sure that the nails do not touch each other. 5. Carefully pour the agar solution into the Petri dishes until the nails and attached metals are covered to a depth of about 5 mm. 6. Allow the dishes to sit overnight. Part III: 1. Make observations of the five test tubes containing the nails and reagent solutions. 2. To each of the five solutions, add 1-2 drops of K3Fe(CN)6(aq) (which contains K+(aq) and Fe(CN)6-(aq)). Observe and record any changes which occur. 3. In a separate test tube, add 1 drop of K3Fe(CN)6(aq) to about 1 mL of FeSO4 solution. Compare this result to that obtained when the K3Fe(CN)6(aq) was added to the test tubes in step 2. 4. Make observations of the reactions in the Petri dishes.

Observations:
Part I:

reagent

pH test

observations before adding K3Fe(CN)6

observations after adding K3Fe(CN)6

distilled water

2. Reaction of K3Fe(CN)6(aq) with FeSO4(aq):

Parts II and III: Fill in the following illustration. Be sure to indicate colors that you notice.

Analysis:
Part I: List the reagents in Part I for which there was indication of corrosion. What regularities caused the corrosion?

Part II: How do you explain the reactions at the head of the nail, at the pointed end, and at the sharp bend of the nail?

Part III: 1. Iron (II) ions are known to react with potassium hexacyanoferrate to form a colored precipitate. Write an equation for this reaction.

2. How does a coating of zinc on iron protect the iron from corrosion?

Lab 16: Iodine Clock Reaction

In this experiment, you will investigate the role of concentration and temperature on the rate of a chemical reaction. You will perform various experiments using an interesting reaction called a clock reaction. You will appreciate the significance of that name after you have completed your first determination. In order to determine the role of each factor independently, you will vary the concentration of one of the reactants in Part I of the experiment, and you will vary the temperature in Part II. In each case, you will keep other possible variables constant. The clock reaction is performed by mixing the two solutions described below: Solution A is a dilute solution of potassium iodate, KIO3. This is the source of the iodate ion, IO3-. Solution B contains starch and the other reacting species, the hydrogen sulfite ion, HSO3-. When the two solutions are thoroughly mixed, the ions of the resulting solution undergo the following reactions: IO3-(aq) + 3 HSO3-(aq) ---> I-(aq) + 3 SO42-(aq) + 3 H+(aq) 5 I-(aq) + 6 H+(aq) + IO3-(aq) ---> 3 I2(aq) + 3 H2O(l) I2(aq) + HSO3-(aq) + H2O(l) ---> 2 I-(aq) + SO42-(aq) + 3 H+(aq) I2(aq) + starch ---> a blue solution The reactions take place in sequence. Only when the hydrogen sulfite ion has been entirely consumed in the first three reactions will iodine molecules accululate in solution and react with the starch in the last reaction. The appearance of the blue color indicates that all of the hydrogen sulfite has been consumed and that the I2 formed remains in solution, available to react with the starch. This is a long lab which should be done over two classes: Part I in the first, Part II in the second. NOTE: Iodine can stain skin and clothing. Handle it with care.

Materials:
10 mL graduated cylinder 2 large test tubes test tube rack stop watch distilled water thermometer hot plate 2 400 mL beakers (for water baths) ice solution A solution B

Procedure:
Part I: 1. Measure 10.0 mL of solution A into the graduated cylinder. Pour the solution into a

clean test tube. Rinse the graduated cylinder with distilled water. 2. Place 10.0 mL of solution B into the graduated cylinder. Pour the solution into the second test tube. Rinse the graduated cylinder with distilled water. 3. Start the stopwatch just as you pour solution A into solution B. As the solutions are poured together, the mixer should pour them back and forth quickly three times to obtain uniform mixing. Time should be recorded from the instant both solutions are in contact. Watch the solution and record the time at the first sign of a reaction. Rinse both test tubes. 4. Measure 9.0 mL of solution A into the clean graduated cylinder. Add distilled water until the volume in the cylinder is exactly 10.0 mL. Pour this solution into a test tube. 5. Place 10.0 mL of solution B into the second test tube. 6. Mix and time once again as you did in step 3. 7. Continue diluting solution A as indicated in the observation table. Repeat the timing procedure, adding the diluted solution of A to 10.0 mL of solution B. Part II: 1. Prepare an ice bath by placing a mixture of ice and tap water into a 400 mL beaker. 2. Prepare a hot water bath by warming about 250 mL of tap water to about 60C in the other 400 mL beaker. 3. Measure 10.0 mL of solution A into a clean test tube. Rinse the graduated cylinder. 4. Measure 10.0 mL of solution B into the other test tube. These solutions must be at room temperature before they are mixed. Rinse and dry the thermometer before placing it into the second test tube to avoid contamination. If the solutions are not already at the same temperature, you may put both test tubes into another 400 mL beaker about two-thirds full of water at room temperature. Let them stand for several minutes before proceeding. 5. Start the stopwatch just as you pour solution A into solution B. As the solutions are poured together, the mixer should pour them back and forth quickly three times to obtain uniform mixing. Time should be recorded from the instant both solutions are in contact. Watch the solution and record the time at the first sign of a reaction. Rinse both test tubes. 6. Repeat the experiment, using 10.0 mL of solution A and 10.0 mL of solution B for each of the temperature ranges described in the observation table. In each case, put the two test tubes in either the ice bath or the hot water bath for several minutes until their temperatures fall into the appropriate temperature range. Record the exact temperature. 7. Once again, start the stopwatch as solution A is poured into solution B. Place the test tube back in the water bath and observe it carefully. Record the time at the first sign of a reaction.

Observations:
Part I: mL solution A 10.0 9.0 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 mL solution B 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 10.0 mL distilled water 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 time

Part II: temperature range 0C - 5C 10C - 15C 20C - 25C 30C - 35C 40C - 45C 50C - 55C exact temperature time

Analysis:
Part I: 1. The concentration of solution A is 0.02 mol/L. Calculate the concentration of KIO3 in moles per liter for each of the solutions after all the components have been mixed. mL solution A 10.0 9.0 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 moles KIO3(aq) / mL mL water 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 moles KIO3(aq) / L

2. Plot a graph of the concentration-time data by plotting concentration of KIO3(aq) vs time. How is the time of a reaction related to the rate of that reaction?

Part II: Using your data, plot a graph of the temperature vs. time. What general relationship can you derive from the graph?

Lab 17: Testing Le Chteliers Principle

Le Chteliers Principle describes the effect of applying various types of stress on the position of a system that is initially at equilibrium ... that is, whether it will shift to increase or decrease the concentration(s) of products in the equilibrium system. The principle tells us that when a system at equilibrium is subjected to a stress, it will shift in such a way so as to relieve the effects of the imposed stress. Stresses include variations in the concentrations of reactants or products, the temperature of the system, and (for reactions involving gases) the pressure. Of these, only a change in temperature actually changes the value of the equilibrium constant.

Materials:
cobalt (II) chloride equilibrium mixture in ethanol sodium chloride silver nitrate distilled water crushed ice hot water 100 mL beaker 2 - 400 mL beakers 4 - test tubes, 2 with stoppers

Procedure:
1. Obtain about 50 mL of the cobalt (II) ion equilibrium mixture in a 100 mL beaker. 2. Place some hot water in one of the 400 mL beakers, place some ice and water in the other 400 mL beaker. 3. Fill two of the test tubes about half full with the cobalt (II) mixture. 4. Hold one of the test tubes of the mixture in the hot water for one minute. Record any change in the color of the mixture. 5. Hold the other test tube of the mixture in the ice water for two minutes. Record any color change of the mixture. 6. To determine if the color changes are reversible, place the second test tube of the mixture in the hot water for one or two minutes. Record any color change of the mixture. 7. Fill the last two test tubes with the colbalt (II) equilibrium mixture. 8. Add a few grains of solid sodium chloride to one of the test tubes, and then stopper and shake the test tube. Record any observations. 9. Add a few grains of solid silver nitrate in the other test tube. Stopper and shake the test tube, and record any changes in color. 10. Dispose of the waste solutions in the appropriate containers.

Observations:
color change of the mixture when placed in hot water ____________________ color change of mixture when placed in cold water ____________________

is the color change reversible?

____________________

color change of the mixture when NaCl(s) is added ____________________ color change of the mixture when AgNO3(s) is added ____________________

Analysis:
The purpose of this investigation was to test Le Chteliers Principle by studying the equilibrium between two complex ions containing the cobalt (II) ion dissolved in ethyl alcohol (al): CoCl42-(al) + 6 H2O(al) ---> Co(H2O)62+(al) + 4 Cl-(al) 1. Use your experimental observations to explain how the equilibrium described by the above equation is shifted as: a) the temperature decreases.

b) the temperature increases.

c) NaCl(s) is added.

d) AgNO3(s) is added.

2. Is the reaction endothermic or exothermic? Explain, using your answers to the above question.

Lab 18: Vapor Pressure of Liquids

In this experiment, you will investigate the relationship between the vapor pressure of a liquid and its temperature. When a liquid is added to the Erlenmeyer flask shown in Figure 1, it will evaporate into the air above it in the flask. Eventually, equilibrium is reached between the rate of evaporation and the rate of condensation. At this point, the vapor pressure of the liquid is equal to the partial pressure of its vapor in the flask. Pressure and temperature data will be collected using a Gas Pressure Sensor and a Temperature Probe. The flask will be placed in water baths of different temperatures to determine the effect of temperature on vapor pressure. You will also compare the vapor pressure of two different liquids, ethanol and methanol, at the same temperature.

Materials:
CBL2 interface TI graphing calculator gas pressure sensor temperature probe 4 - 1 L beakers 20 mL syringe rubber stopper assembly plastic tubing 2 125 mL Erlenmeyer flasks methanol ethanol ice

Procedure:
1. Use 1 L beakers to prepare four water baths, one in each of the following temperature ranges: 0C to 5C, 10C to 15C, 20C to 25C, and 30C to 35C. For each water bath, mix varying amounts of warm water, cool water, and ice to obtain a volume of 800 mL in a 1 L beaker. To save time and beakers, several lab groups can use the same set of water baths. 2. Attach the gas pressure sensor to the rubber stopper. Leave the two-way valve on the rubber stopper open. Twist the stopper into the neck of one of the Erlenmeyer flasks to ensure a tight fit. 3. Turn on the calculator and start the DataMate program. Set up the calculator and interface for a Temperature Probe in CH 1 and a Gas Pressure Sensor in Ch 2. Press ENTER to select CH 1. Select TEMPERATURE. Press enter to select CH 2. Select PRESSURE. Select the calibration listing for units of kPa. Set the data

collection mode to SELECTED EVENTS. 4. The temperature and pressure readings should now be displayed on the calculator screen. Record the value for atmospheric pressure in your data table (round to the nearest 0.1 kPa). 5. Place the temperature probe into a room-temperature water bath. Hold the flask in the water bath, with the entire flask covered, as shown in Figure 1. After 30 seconds, close the two-way valve above the rubber stopper. 6. Draw 3 mL of methanol up into the syringe. With the two-way valve still closed, screw the syring onto the two-way valve. 7. Introduce the methanol into the Erlenmeyer flask by opening the two-way valve above the rubber stopper, squirting the methanol into the flask, and quickly returning the plunger of the syringe back to the 3-mL mark. Close the two-way valve. Remove the syringe. 8. Select START to begin data collection. The flask should still be submerged in the water bath. When the temperature and pressure readings displayed on the calculator screen have both stabilized, equilibrium between methanol liquid and vapor has been established. Select ENTER on the calculator to store the first temperature-pressure data pair. 9. Place the Erlenmeyer flask assembly and the temperature probe into the 30C-35C water bath. Make sure the entire flask is covered. When the temperature and pressure readings displayed on the calculator screen have both stabilized, select ENTER on the calculator to store the second data pair. 10. Repeat step 9, using the 10C-15C and 0C-5C water baths. After you have collected the last data pair, press STO to stop data collection. Remove the flask and the temperature probe from the last water bath. 11. Open the side valve of the gas pressure sensor so the Erlenmeyer flask is open to the atmosphere. Remove the stopper assembly from the flask and dispose of the methanol in the organic waste container. 12. Scroll down twice, then press ENTER to chose CH2 VS. CH1. Examine the data points along the displayed graph of pressure vs. temperature. As you move the cursor right or left, the temperature (x) and pressure (y) values of each data point are displayed below the graph. Record the data pairs in your data table. Round pressure to the nearest 0.1 kPa and temperature to the nearest 0.1C. 13. Obtain another clean, dry 125 mL Erlenmeyer flask. Draw air in and out of the syringe enough times that you are certain that all of the methanol has evaporated from it. 14. Press ENTER, then return to the main screen. Repeat steps 5 to 8 to do one trial only for ethanol in the room temperature water bath. When the pressure reading in Channel 2 stabilizes, record its value in the data table. 15. Open the side valve of the gas pressure sensor. Remove the stopper assembly from the flask and dispose of the ethanol in the organic waste container.

Observations:
Atmospheric pressure: _______ kPa substance 1 temperature temperature measured pressure C K kPa 2 C K kPa methanol 3 C K kPa 4 C K kPa C K kPa ethanol

Analysis:
1. Convert each of the Celsius temperatures in the data table to Kelvin. 2. To obtain the vapor pressure of methanol and ethanol, the air pressure must be subtracted from each of the measured pressure values. However, for trials 2 4, you must convert the atmospheric pressure at the temperature of the first water bath to a corrected air pressure at the temperature of the water bath in trials 2 4. To do this, use the gas law equation of P1/T1 = P2/T2. Solve for P2, and record this value as the corrected air pressure for trials 2 4. air pressure no correction corrected kPa kPa corrected kPa corrected kPa no correction kPa

3. Calculate the vapor pressure by subtracting the corrected air pressure from the measured pressure in trials 2 4. Subtract the uncorrected air pressure in trial 1 of the methanol and in the ethanol from the measured pressure. vapor pressure kPa kPa kPa kPa kPa

4. Plot a graph of vapor pressure vs. temperature for the four data pairs you collected for methanol. Temperature is the independent variable and vapor pressure the dependent variable.

5. How would you describe the relationship between vapor pressure and temperature, as represented in the graph? Explain this relationship using the concept of kinetic energy of molecules.

6. Which liquid, methanol or ethanol, had the larger vapor pressure value at room temperature? Explain your answer, taking into account various intermolecular forces in these two liquids.

Lab 19: Determination of an Equilibrium Constant

Many chemical reactions, especially those of organic substances, do not go to completion. Rather, they come to a point of chemical equilibrium before the reactants are fully converted to products. At the point of equilibrium, the concentrations of all reactants remain constant with time. The position of this equilibrium is described by a function called the equilibrium constant, Keq, which is a ratio of the amount of product present to the amount of reactant remaining once the point of equilibrium has been reached. In this lab, you will determine the equilibrium constant for the esterification reaction between 1-propanol and acetic acid. CH3COOH(l) + CH3CH2CH2OH(l) ---> CH3COOCH2CH2CH3(l) + H2O(l) You will set up the reaction in such a way that the initial concentrations are known. The reaction will then be allowed to stand for one week to come to equilibrium. As the acetic acid reacts with the 1-propanol, the acidity of the mixture will decrease, reaching a minimum once the system reaches equilibrium. The quantity of acid present in the system will be determined by titration with standard sodium hydroxide solution. Esterification reactions are typically catalyzed by the addition of a strong mineral acid. In this experiment, a small amount of sulfuric acid will be added as a catalyst. The amount of catalyst added will have to be determined, because this amount of catalyst will also be present in the equilibrium mixture and will contribute to the total acid content of the mixture. By analyzing the amounts of each reagent used this week in setting up the reaction, and by determining the amount of acetic acid that will be present next week once the system has reached equilibrium, you will be able to calculate the concentration of all species present in the equilibrium mixture. From this, the value of the equilibrium constant can be determined.

Materials:
50 mL buret lab stand and buret clamp small funnel pipet and bulb 250 mL beaker graduated cylinder 2 125 mL Erlenmeyer flasks, one with rubber stopper plastic wrap 1.0 mol/L NaOH(aq) 1-propanol glacial acetic acid 6.0 mol/L sulfuric acid phenolphthalein indicator solution distilled water

Prodecure:
First Week:

CAUTION: Extremely concentrated solutions. Wear proper protection (including rubber gloves), especially when handling the acids. Teachers should consider all factors (students, lab safety etc.) before using such concentrated solution. 1. Obtain approximately 100 mL of sodium hydroxide solution in a 250 mL beaker. 2. Rinse the buret with approximately 5 mL of distilled water. Using the small funnel, rinse the buret twice with approximately 5 mL of the sodium hydroxide solution. Fill the buret with the sodium hydroxide solution. 3. Cover with plastic wrap a rubber stopper that securely fits an Erlenmeyer flask (this will prevent the stopper from being attacked by the vapors of the reaction mixture). 4. Using the graduated cylinder, obtain 14 mL of glacial acetic acid (0.25 mol) and transfer the acid to a clean, dry Erlenmeyer flask. 5. Rinse the graduated cylinder with distilled water. Obtain 19 mL of 1-propanol (0.25 mol) and add it to the acetic acid in the Erlenmeyer flask. Stopper the flask and swirl it for several minutes to mix the reagents. 6. Place approximately 25 mL of distilled water in the second Erlenmeyer flask. Rinse the pipet with approximately 1.0 mL of the reaction mixture. Transfer 10 mL of the reaction mixture to the second Erlenmeyer flask. Restopper the first flask to prevent evaporation. 7. Add 3-4 drops of phenolphthalein indicator to the sample to be titrated. 8. Record the initial level of the NaOH solution in the buret. Titrate the reagent mixture with the NaOH solution. The endpoint of the titration is the appearance of a faint, permanent pink color. Record the level of NaOH(aq) in the buret. 9. Rinse out the Erlenmeyer flask with distilled water and repeat the titration until three trials are within 0.1 mL of each other. 10. Clean out the Erlenmeyer flask with distilled water. Place approximately 25 mL of distilled water into it. 11. To the first Erlenmeyer flask, add 10 drops of 6.0 mol/L sulfuric acid, cover, and swirl. Immediately pipet a 10 mL sample into the second Erlenmeyer flask. Do not delay in pipeting, or the concentration of the acetic acid will begin to change as the reaction occurs. 12. Recording the initial and final NaOH(aq) levels in the buret, titrate the calatyzed reaction mixture, using 3-4 drops of phelphthalein indicator to signal the endpoint. 13. Make sure that the first Erlenmeyer flask (containing the catalyzed reaction mixture) is stoppered. Label this flask with your name. Clean and return all materials. Second Week: Titrate three10 mL samples of the catalyzed reaction mixture with the NaOH(aq).

Observations: First Week:

Titration of original mixture with 1.0 mol/L NaOH(aq) 1 final buret reading (mL) initial buret reading (mL) volume of NaOH(aq) used 2 3 4

Titration of catalyzed mixture with 1.0 mol/L NaOH(aq) 1 final buret reading (mL) initial buret reading (mL) volume of NaOH(aq) used 2 3 4

Second Week: Titration of catalyzed mixture with 1.0 mol/L NaOH(aq) 1 final buret reading (mL) initial buret reading (mL) volume of NaOH(aq) used 2 3 4

Analysis:
First Week: 1. Calculate the concentration of the acetic acid in the original mixture. Because the reaction was started using equal molar amounts of acetic acid and 1-propanol, the concentration of this calculated acetic acid also represents the concentration of the 1-propanol in the original mixture.

2. Subtract the average volume of NaOH(aq) used in the first part (original mixture) from the average volume of NaOH(aq) used in the second part (catalyzed mixture). Since the samples of catalyzed reaction mixture contain the same quantity of acetic acid as the samples of the uncatalyzed mixture, the increase in volume of NaOH(aq) required to titrate the second set of 10 mL samples represents a measure of the amount of sulfuric acid present. This volume represents a correction that must be applied to the volume of NaOH(aq) that will be required to titrate the samples the second week.

Second Week: 3. Calculate the concentration of the acetic acid in reaching equilibrium. Do not forget to correct the volume of NaOH(aq).

4. Using an ICE table, calculate the equilibrium constant for the reaction.

Lab 20: Identifying an Unknown Acid

The primary purpose of this experiment is to identify an unknown diprotic acid by finding its molecular mass. A diprotic acid is titrated with NaOH solution of known concentration. Weighing the original sample of acid will give you its mass in grams. Moles can be determined from the volume of NaOH titrant needed to reach the first equivalence point. The volume and the concentration of NaOH titrant are used to calculate moles of NaOH. Moles of unknown acid equal moles of NaOH at the first equivalence point. Once grams and moles of the diprotic acid are known, molecular mass can be calculated, in g/mol. Molecular mass determination is a common way of identifying an unknown susbstance in chemistry. You may use either the first or second equivalence point to calculate molecular mass. The first is somewhat easier, because moles of NaOH are equal to moles of the unknown. If the second equivalence point is more clearly defined on the titration curve, however, simply divide its NaOH volume by 2 to confirm the first equivalence point.

Materials:
CBL 2 interface TI graphing calculator pH sensor unknown diprotic acid centrigrade balance 0.1 M NaOH solution 50 mL buret ring stand with buret clamp utility clamp 100 mL beaker 250 mL beaker funnel stirring rod distilled water

Procedure:
1. Use the funnel with the 100 mL beaker to rinse and fill the buret with NaOH(aq). Record the initial buret reading to the nearest 0.1 mL. 2. Weigh out about 0.12 g of the unknown diprotic acid in the 250 mL beaker. Dissolve the acid in about 100 mL of distilled water. 3. Use the utility clamp to suspend the pH sensor on the ring stand. Position the pH electrode in the diprotic acid solution and adjust its position toward the outside of the beaker so that it is not struck by the stirring rod. 4. Turn on the calculator and start the DataMate program. Set up the calculator and interface for the pH sensor. Set up the data collection mode to EVENTS WITH ENTRY. 5. Select Start to begin data collection. a. Before you have added any NaOH solution, press ENTER and type in the

initial reading of the buret. Press ENTER to save the first data pair for this experiment. b. Add the next encrement of NaOH titrant (enough to raise the pH about 0.20 units). When the pH stabilizes, press ENTER and enter the current buret reading. You have now saved the second data pair for the experiment. c. Continue adding NaOH solution in increments that raise the pH by about 0.20 units and enter the buret reading after each increment. Proceed in this manner until the pH is 3.5. d. When pH 3.5 is reached, change to 2-drop increments. Enter the buret reading after each increment. e. After pH 4.5 is reached, again add larger increments that raise the pH by about 0.20 units and enter the buret reading after each addition. Continue in this manner until a pH of 7.5 is reached. f. When pH 7.5 is reached, change to 2-drop increments. Enter the buret reeading after each increment. g. When H 10 is reached, again add lareger increments that raise the pH by 0.20 units. Enter the buret reading after each increment. Continue in this manner until you reach a pH of 11 or use 25 mL of NaOH, whichever comes first. 6. Press STO when you have finished collecting data. 7. Examine the data on the displayed graph to find the equivalence pointthat is the largest increase in pH upon the addition of 1 drop of NaOH solution. As you move the cursor right or left on the displayed graph, the volume (x) and the pH (y) values of each data point are displayed below the graph.

***One of the two equivalence points is usually more clearly defined than the other; the
two-drop increments near the equivalence point frequently result in larger increases in pH (a steeper slope) at one equivalence point than the other. Determine the the volume of NaOH titrant used for the equivalence point you selected. To do so, examine the data to find the largest increase in pH values during the 2-drop additions of NaOH. Find the NaOH volume just before this jump. Then find the NaOH volume after the largest pH jump. Add the two, and divide by two.

Observations:
mass of diprotic acid NaOH(aq) volume added before and after the largest pH increase NaOH(aq) volume added at the equivalence point _______ g _______ mL _______ mL _______ mL

Analysis:
1. Calculate the number of moles of NaOH used at the equivalence point you selected.

2. Determine the number of moles of the diprotic acid.

3. Using the mass of the diprotic acid you measured, calculate the molecular mass of the diprotic acid, in g/mol.

4. From the following list of five diprotic acids, identify you unknown diprotic acid. Diprotic acid Oxalic acid Malonic acid Maleic acid Malic acid Tartaric acid Formula H2C2O4 H2C3H2O4 H2C4H2O4 H2C4H4O5 H2C4H4O6 Molecular mass 90 104 116 134 150

5. Determine the percent error for your molecular mass value.

Lab 21: Buffers

Buffered solutions are remarkably resistant to pH changes caused by the

addition of an acid or base from an outside source. In general, a buffered solution is a mixture of a weak acid and a weak base. The most common sort of buffered solution consists of a mixture of a conjugate acid-base pair.

Materials:
K2HPO42 H2O(s) NaH2PO42 H2O(s) 1.0 mol/L hydrochloric acid 1.0 mol/L sodium hydroxide distilled water 2 medicine droppers pH meter lab scoop balance 5 - 100 mL beakers 100 mL volumetric flask stirring rod masking tape

Procedure:
1. Measure exactly 1.56 g of NaH2PO42 H2O(s) and 2.14 g of K2HPO42 H2O(s) into a clean, dry 100 mL beaker. 2. Dissolve the solid mixture to make a 100 mL solution in the volumetric flask. 3. Using a 50 mL graduated cylinder, measure 40 mL of the buffer solution into each of two clean, dry, labelled (A and B) 100 mL beakers. 4. Measure 40 mL of distilled water into a clean, dry 100 mL beaker. 5. Obtain about 10 mL of 1.0 mol/L HCl(aq) in a clean, dry 100 mL beaker. 6. Measure and record the initial pH of the buffer (A) solution. 7. Add two drops of HCl(aq) to the solution, stir, and measure the pH. 8. Continue adding HCl(aq), two drops at a time, until 14 drops have been added, measuring the pH after each addition. 9. Repeat steps 6 to 8 using distilled water in place of the buffer. 10. Repeat steps 4 to 9 using 1.0 mol/L NaOH(aq) in place of the HCl(aq). Use the solution B and a fresh supply of distilled water in the cleaned 100 mL beaker.

Observations:
volume of HCl(aq) (drops) pH of buffer solution ___ pH of distilled water volume of NaOH(aq) (drops) pH of buffer solution ___ pH of distilled water 0 ___ ___ 0 ___ ___ 2 ___ ___ 2 ___ ___ 4 ___ ___ 4 ___ ___ 6 ___ ___ 6 ___ ___ 8 ___ ___ 8 ___ ___ 10 ___ ___ 10 ___ ___ 12 ___ ___ 12 ___ ___ 14 ___ 14 ___

Analysis:
1. Identify the buffer system used in this experiment.

2. Use the dissociation equilibrium equations and Le Chteliers Principle to explain the effects of adding the HCl(aq) and the NaOH(aq) to the buffer.

Lab 22: Energy Content of Foods

All human activity requires "burning" food for energy. In this experiment, you will determine the energy released (in kJ/g) as various foods burn. You will look for patterns in the amounts of energy released during burning of the different foods.

Materials:
CBL2 interface TI graphing calculator temperature probe cashews peanuts marshmallows popcorn food holder wooden splint ring stand with 10 cm ring clamp utility clamp stirring rod 100 mL graduated cylinder small can cold water matches centigrade balance screen

Procedure:
1. Turn on the calculator and start the DataMate program. Set up the calculator and interface for the Temperature Probe. Set up the data collection mode to CHANGE TIME SETTINGS. Enter "6" as the time between samples in seconds. Enter "100" as the number of samples. 2. Obtain a piece of one of the foods assigned to you and a food holder. Measure and record the initial mass of the food sample. 3. Measure and record the mass of an empty can. Add 50 mL of cold water to the can. Measure and record the mass of the can and water. 4. Set up a ring and screen. Place the can about 2.5 cm from the food sample. Use a utility clamp to suspend the temperature probe in the water. The probe should not touch the bottom of the can. Allow the temperature probe to sit in the water for at least 30 seconds before you go on. 5. Select START to begin collecting data. Record the initial temperature of the water, t1, in your data table. You can monitor temperature in the upper right corner of the real-time graph on the calculator screen. Remove the food sample from under the can and use a wooden splint to light it. Quickly place the burning food sample directly under the center of the can. Allow the water to be heated until the food sample stops burning. 6. Continue stirring the water until the temperature stops rising. Record this maximum temperature, t2. Data collection will stop after 10 minutes. Press STO to stop the data collection. 7. Measure and record the final mass of the food sample and holder. 8. To confirm the initial (t1) and final (t2) values you recorded earlier, examine the data points along the curve on the displayed graph. As you move the cursor right or left, the time (x) and temperature (y) values of each dat point are displayed below the graph. 9. Press ENTER to return to the main screen. Select START to repeat the data

collection for the second food sample. Use a new 50 mL portion of cold water. Repeat steps 2-8.

Observations:
food sample #1 mass of empty can mass of can + water mass of water initial mass of food sample final mass of food sample change in mass of food sample initial temperature of water final temperature of water temperature change of water food sample #2

Analysis:
1. Calculate the energy content (in kJ/g) of each food sample using q = -mct.

2. Which food group had the highest energy content?

3. Food energy is often expressed in calories. There are 4.18 kJ in one calorie. Calculate the number of calories in a 50 g package of your two food samples.

4. Two of the foods in the experiment have a high fat content (peanuts and cashews) and two have a high carbohydrate content (marshmallows and popcorn). From your results, what genralization can you make about the relative energy content of fats and carbohydrates?

Lab 23: Vitamin C in Juices

Fruits and juices are a primary source of vitamin C in the diet. But are all fruits equal? In this lab, you will test a number of juices and fruit drinks with the intent of determining their value as a source of vitamin C. Recognize that you are taking a very narrow measure of the juices, and that a low vitamin C content does not mean that the juice has no other food value, nor does a high vitamin C content necessarily make one juice overall superior to the others. As you may remember from lab 17, starch is used to test for the presence of iodine and vice-versa. When an iodine solution, which has a red color, is added to a solution or other material that contains starch, the red color is changed to a dark blue. Vitamin C (ascorbic acid) will also react with iodine solution, but it does so in such a way that the red color of the iodine is lost. If an iodine solution is added to a solution containing both vitamin C and starch, the iodine will react with the vitamin C first, and the iodine color will disappear; then, when the vitamin C has all been consumed, any additional iodine that is added will react with the starch to produce the dark blue color. This will be the basis for your analysis. You will place a little starch in each of several beverages, then you will add iodine solution, one drop at a time, until the solution turns blue, indicating that all of the vitamin C has been consumed. If you always use the same amount of beverage, you can compare the vitamin C contents of the different products. And, if you carry out the same procedure on a solution whose vitamin C content is accurately known, you can actually determine the amount of vitamin C in a serving of that beverage.

Materials:
6 small test tubes test tube rack 50 mL beaker 100 mL beaker 2 eye droppers standard vitamin C solution (1 mg/mL) iodine solution starch indicator solution 5 beverages to be tested

Procedure:
1. In the 100 mL beaker, obtain approximately 50 mL of the iodine solution. In the 50 mL beaker, obtain approximately 20 mL of the starch indicator solution. 2. Place exactly 25 drops of vitamin C standard solution in a small test tube. Add 2 drops of starch solution. 3. Add iodine solution, one drop at a time, agitating the test tube gently after each drop to help with mixing. Continue until the mixture turns blue (the color will be somewhat faint). Record the number of drops of iodine needed. 4. Carry out the same procedure using 25 drops of each of the five beverages.

NOTE: Some of the beverages have colors of their own, so you will need to use some judgement in deciding when you have reached the endpoints of the analyses.

Observations:
1. Calculate the relative concentration of vitamin C in each juice: divide the number of drops of iodine needed for 25 drops of juice by the number of drops needed for 25 drops of standard. Express the ratio as a decimal with two significant figures. Enter you results in column (b) of the Summary Table (next page). 2. Enter the concentration of the vitamin C standard in column (c) of the Summary Table. This value is the same for all trials. 3. Find the concentration of vitamin C in each juice by multiplying the ratios you calculated in 1 by the concentration of vitamin C in the standard. Enter the results in column (d) of the table. 4. We will assume that a standard serving of beverage is about 180 mL. Multiply the concentration of each beverage, in mg/mL, by this volume to determine the number of milligrams of vitamin C in one serving. Enter the results in column (e) of the table.

Summary Table
juice drops of iodine conc. of ratio to standard conc. Of standard (mg/mL) (c) mg vitamin C in juice (mg/mL) (d) mg vitamin C in 180 mL of juice (e)

(a)

(b)

Analysis:
The average high school student, male or female, needs about 60 mg of vitamin C per day. This is called the minimum recommended daily allowance (MRDA). For each of the juices that do not deliver adequate vitamin C in one serving, calculate the volume in mL that you would have to drink in order to achieve the 60 mg MDRA.

Lab 24: Proteins

Proteins are long-chain polymers of the a-amino acids and make up about 15% of our bodies. Proteins have many functions in the body. Some form the major structural feature of muscles, hair, fingernails, and cartilage. Other proteins help to transport molecules through the body, fight infection, or act as catalysts (enzymes) for biochemical reactions in the cells of the body. When the physical or chemical environment of a protein is modified, and the protein responds by changing its structure, the protein is said to have been denatured. Denaturation of a protein may be reversible or irreversible. Changes in environment that may affect a proteins structure include changes in temperature, changes in the pH of the proteins environment, changes in the solvent in which the protein is suspended, and the presence of any other ions or molecules that may chemically interact with the protein (such as ion of the heavy metals). In the first part of this lab, you will do three tests on four common proteinaceous materials. The biuret test detects the presence of proteins and polypeptides, but does not detect free amino acids. The CuSO4 solution will turn purple in those samples that contain proteinaceous material. The xanthoproteic test results in the formation of a yellow color in two of the common amino acids found in proteins, tryptophan and tyrosine. In strongly basic solutions, the amino acid crysteine found in proteins will react with lead acetate solution to produce a black precipitate of lead sulfide, PbS. The strongly basic conditions are necessary to break up polypeptide chains into individual amino acids. In the second part of this lab, you will study the effects of denaturation of proteins.

Materials:
1% albumin solution (from egg whites) 250 mL beaker 1% alanine solution hot plate nonfat milk (containing the protein casein) 7 test tubes gelatin cubes test tube rack 10% NaOH solution stir rod distilled water 3% CuSO4 solution 6.0 mol/L nitric acid ethyl alcohol 6.0 mol/L NaOH solution 5% Pb(CH3COO)2 solution 3.0 mol/L hydrochloric acid 3.0 mol/L NaOH solution saturated (5.4 mol/L) NaCl solution CAUTION: Extremely concentrated solutions. Wear proper protection (including rubber gloves), especially when handling the acids and the sodium hydroxide. Teachers should consider all factors (students, lab safety etc.) before using such concentrated solutions.

Procedure:
Part I: 1. Set up a 250 mL beaker containing approximately 100 mL of tap water on a hot

plate and heat to boiling. Place about 10 drops of albumin solution, alanine solution, nonfat milk, and a small cube of gelatin in separate clean test tubes. 2. Add 10 drops of 10% sodium hydroxide solution to each test tube, followed by 3-4 drops of 3% copper (II) sulfate. 3. Carefully mix the contents of each test tube with a clean stir rod, being sure to clean the rod when switching between solutions. Be sure to break up the gelatin sample as much as possible when mixing. Record your observations. Dispose of test tube contents into the waste beaker, and rinse out the test tubes. 4. Place about 10 drops of the albumin solution, alanine solution, nonfat milk, and a small cube of gelatin in separate clean test tubes. 5. Add 8-10 drops of nitric acid to each test tube. 6. Carefully mix the contents of each test tube with a clean stir rod. Again, be sure to break up the gelatin sample as much as possible when mixing. 7. Transfer the test tubes to the boiling water bath and heat for 3-4 minutes. Record your observations. Dispose of test tube contents into the waste beaker, and rinse out the test tubes. 8. Place about 10 drops of albumin solution, alanine solution, nonfat milk, and a small cube of gelatin in separate clean test tubes. If you are willing to make the sacrifice, you may also test small samples of your hair (roll up 2 or 3 strands into a ball that will fit in a test tube) or some fingernail clippings. 9. Add 15-20 drops of 6.0 mol/L sodium hydroxide to each sample. 10. Carefully mix the contents of each test tube with a clean stir rod. Again, be sure to break up the gelatin sample as much as possible when mixing. 11. Transfer the test tubes to the boiling water bath and heat the sample for 10-12 minutes. If the volume of the test tubes begins to decrease during tyhe heating period, add 5-10 drops of distilled water to replace the volume. 12. After the heating period, allow the samples to cool for 5-6 minutes. Add 5 drops of 5% lead acetate solution to each test tube. Record your observations. Dispose of test tube contents into the waste beaker, and rinse out the test tubes. Part II: 1. Place 10 drops of 1% albumin solution in each of seven clean test tubes. 2. Heat one sample in a boiling water bath for 5 minutes and describe any changes in the appearance of the solution after heating. 3. To the remaining albumin samples, add 3-4 drops of the following reagents (each to a separate albumin sample): hydrochloric acid, 3.0 mol/L sodium hydroxide, saturated sodium chloride solution, ethyl alcohol, 5% lead acetate solution. Record any changes in the appearance of each albumin sample. Dispose of test tube contents into the waste beaker, and rinse out the test tubes. 4. Repeat the tests above, using 10-drop samples of nonfat milk in place of the albumin solution.

Observations:
Part I: biuret test xanthoproteic test lead acetate test

albumin alanine nonfat milk gelatin

Part II: albumin Heat hydrochloric acid sodium hydroxide sodium chloride ethyl alcohol lead acetate nonfat milk

Analysis:
1. Why did the 1% alanine solution give a negative result in the biuret test? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 2. Explain what happens to cause the denaturation in part II. _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 3. Draw the basic structure of the a-amino acid.

Lab 25: Enzymes

Enzymes are proteinaceous materials that function in the body as catalysts to control the speed of biochemical processes. Without enzymes, life would be impossible because important reaction in our bodies would occur far too slowly. Enzymes are said to be specific because a given enzyme typically acts on only a single type of molecule (or functional group). Like other proteins, enzymes can be denatured by changes in their environment. In this lab, you will examine the catalytic properties of several common enzymes: The digestion of carbohydrates begins in the mouth, where the enzyme ptyalin is present in saliva. Ptyalin is a type of enzyme called an amylase. Enzymes called proteases break down proteins into free amino acids. Since gelatin is a network of protein molecules, you will use it to experiment on the functioning of the proteases. Meat tenderizers and several contact lens cleaners contain the enzyme papain, which breaks down the proteins contained in muscle fibers of meat (making it more tender) and dissolves the deposits that may cloud contact lenses. Again, this lab will be spread over two periods: the first to set up the reactions, the second to observe the results.

Materials:
250 mL beaker hot plate 50 mL beaker soda cracker 4 small test tubes test tube rack distilled water 5% lead acetate solution 0.1 mol/L iodine/potassium iodide solution 6 plastic cups of gelatin toothpicks microwave oven fresh pineapple canned pineapple meat tenderizer contact lens cleaner

Procedure:
First Class: 1. Heat approximately 100 mL of water in a 250 mL beaker to a gentle boil. 2. Using the 50 mL beaker, collect approximately 3 mL of saliva by letting the saliva flow freely from your mouth (do not spit). 3. Obtain a soda cracker and crush it finely on a sheet of paper using the bottom of the 50 mL beaker. 4. Label four test tubes with your name and as 1, 2, 3, and 4. Transfer a small amount (about the size of a matchhead) of the crushed cracker into each test tube. 5. To the first test tube, add 2 mL of distilled water (as a control). To the second test tube, add 1 mL of your saliva and 1 mL of distilled water. To the third test tube, add 1 mL of your saliva, followed by 1 mL of the lead acetate solution (as a heavy metal, lead (II) ion should denature the protein of the salivary enzyme). To the final test tube, add 1 mL of your saliva, then place the test tube in the boiling water bath for 510 minutes (heating the saliva sample should denature the protein of the salivary enzyme). Carefully remove the test tube from the boiling water bath and allow it to cool to room temperature. 6. Place the test tubes in the refrigerator. 7. Obtain and label 6 plastic cups of gelatin (although the gelatin is similar to the type used as a dessert, it has been made up double-strenth to make it drier and easier to handle). 8. Place a piece of fresh pineapple in a microwave oven and cook on the highest setting for one minute. Allow the pineapple to return to room temperature. 9. To one gelatin sample, add a small piece of fresh pineapple. To the second sample, add of piece of canned pineapple. To the third, the piece of pineapple that was microwaved. To the fourth, a spoonful of meat tenderizer. To the fifth, a teaspoon of contact lens cleaner. The final sample will act as a control. Place all samples in the refrigerator. Second Class: 1.To each of the test tubes, add 1 drop of iodine/potassium iodide solution. Remember that the iodine is a standard laboratory test for the presence of starch: if the starch is present even in trace quantities in a sample, the iodine will cause a deep blueblack color to appear. 2. Examine each of the gelatin samples for any evidence of breakdown.

Observations:
1. Action of ptyalin: control: saliva: saliva/lead: saliva/heat: _____________________________________________ _____________________________________________ _____________________________________________ _____________________________________________

2. Action of proteases: control: fresh pineapple: canned pineapple: microwaved pineapple: meat tenderizer: contact lens cleaner:

__________________________________ __________________________________ __________________________________ __________________________________ __________________________________ __________________________________

Analysis:
1. List five ways in which an enzyme can be denatured. _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 2. Is canned pineapple more like fresh or microwaved? What does this tell you about the canning process? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 3. From your results, would you say that meat tenderizers and/or contact lens cleaners contain proteases? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________

Lab 26: Organic Chemical Compounds

The simplest types of carbon compounds are known as hydrocarbons. Such

molecules contain only carbon and hydrogen atoms. There are various sorts of molecules among the hydrocarbons, differing in the arrangement of the carbon atoms in the molecule (chainlike or closed-ring) or in the bonding between the carbon atoms. Single bonded hydrocarbons will react slowly with the halogen elements, whereas molecules with double and triple bonds are much more reactive. When another atom or group of atoms is added to a hydrocarbon framework, the new atom frequently imparts its own very strong characteristic properties to the resulting molecule. Such an atom or group of atoms is called a functional group. With millions of carbon compounds known, it has been helpful to chemists to divide these compounds into families, on the basis of what functional group they contain. Generally, it is found that all the members of a family containing a particular functional group will have many similar physical properties and will undergo similar chemical reactions. In this lab, we will examine three such families. Simple hydrocarbon chains or rings that contain a hydroxyl group (-OH) bonded to a carbon atom are called alcohols. Many alcohols can be oxidized by reagents such as permanganate ion and dichromate ion, with the product depending on the structure of the alcohol. Alcohols are very important in biochemistry, since many biological molecules contain the hydroxyl group. For example, carbohydrates (sugars) are alcohols, with each particular carbohydrate molecule generally containing several hydroxyl groups. An oxygen atom that is double-bonded to a carbon atom of a hydrocarbon chain is referred to as a carbonyl group. Two families of organic compounds contain the carbonyl function, and the difference between the families has to do with where along the chain of carbon atoms the oxygen atom is attached. Molecules having the oxygen atom attached to the first (terminal) carbon atom of the chain are called aldehydes, whereas molecules having the oxygen atom attached to an interior carbon atom are called ketones. Aldehydes and ketones are important biologically, because all carbohydrates are also either aldehydes or ketones, as well as being alcohols. Molecules such as glucose and fructose, which contain both the carbonyl and the hydroxyl function, are easily oxidized by Benedicts reagent. Benedicts reagent is a specially prepared solution of copper (II) ion that is reduced when added to certain sugars, producting a precipitate of red copper (I) oxide. Benedicts reagent is the basis for the common test for sugars in the urine of diabetics.

Materials:
hexane 1-hexene cyclohexane cyclohexene toluene methanol ethanol 2-butanol 2-methyl-2-propanol 24 test tubes 5 test tube stoppers hot plate 400 mL beaker droppers bromine water 0.063 mol/L potassium permanganate 0.20 mol/L acidified potassium dichromate acetone 10% glucose solution 10% fructose solution

Procedure:
Part I: hydrocarbons 1. Obtain 10 drop portions of hexane, 1-hexene, cyclohexane, cyclohexene, and toluene in separate test tubes. 2. Take the test tubes to the exhaust hood and add a few drops of bromine water to each. Those samples containing double bonds will decolorize the bromine immediately. 3. Expose those test tubes that did not immediately decolorize the bromine to a highintensity incandescent lamp. The reaction is sensitive to wavelengths of ultraviolet light. 4. Obtain additional 10 drop samples of the hexane, 1-hexene, cyclohexane, cyclohexene, and toluene in separate clean test tubes. 5. Add a few drops of the potassium permanganate solution to each test tube, stopper, and shake. Those samples containing double bonds will cause a change in the purple color of the permanganate. Part II: alcohols 1. Obtain 10 drop samples of methanol, ethanol, 2-butanol, and 2-methyl-2-propanol in separate clean test tubes. 2. Add 10 drops of acidified potassium dichromate to each sample, transfer to a hotwater bath, and heat until a reaction is evident. Dichromate ion oxidizes primary and secondary alcohols.

Part III: ketones 1. Obtain 10 drop samples of acetone, glucose, and fructose in separate clean test

tubes. 2. . To each test tube, add 1 mL of Benedicts reagent and transfer the test tubes to a hot water bath. Molecules containing a hydroxyl group next to a carbonyl group on a carbon atom chain will cause a color change in Benedicts reagent.

Observations:
Part I: hydrocarbons 1. Which compounds decolorized the bromine immediately? ___________________________________________________________________ 2. Which compounds decolorized bromine on exposure to light? ___________________________________________________________________ 3. Which compounds caused a color change in the potassium permanganate? ___________________________________________________________________ Part II: alcohols 1. Identify the tertiary alcohol in the group. ___________________________________________________________________ Part III: ketones 1. Which samples caused a color change in the Benedicts reagent? ___________________________________________________________________

Analysis:
Complete the following table: single bonded hydrocarbons double bonded hydrocarbons primary/secondary alcohols tertiary alcohols ketones

Lab 27: Synthesis of Esters

One of the most important types of organic syntheses involves the reaction of an organic acid with an alcohol to produce an ester (the reaction usually requires an acid catalyst). Unlike many organic chemical compounds, esters often have sweet, pleasant odors. Many of the odors and flavorings of fruits and flowers are due to the presence of esters in the essential oils of these materials. However, a fruit or flower generally contains only a few drops of ester, giving a very subtle odor. When prepared in the laboratory in relatively large amounts, the ester may seem to have a pronounced chemical odor, and it may be difficult to recognize the fruit or flower that has this aroma. In this lab, you will synthesize two esters. Since you are only interested in the nature of the product, and have no concern for the stoichiometry or percentage yield, precise measurements of reactant quantities is not necessary.

Materials:
salicylic acid methanol 18 mol sulfuric acid 2 test tubes 250 mL beaker 2-50 mL beakers scoop balance 10 mL graduated cylinder thermometer hot plate lab stand with test tube clamp List B: acetic acid / methanol acetic acid / ethanol acetic acid / pentanol acetic acid / 1-propanol acetic acid / 1-octanol methanoic acid / isobutyl alcohol propanoic acid / isobutyl alcohol butanoic acid / methanol butanoic acid / ethanol benzoic acid / ethanol

Procedure:
CAUTION: Extremely concentrated solutions. Wear proper protection (including rubber gloves), especially when handling the acids and the sodium hydroxide. Teachers should consider all factors (students, lab safety etc.) before using such concentrated solutions. 1. Add 3.0 g of salicylic acid to one of the test tubes. Using the graduated cylinder, add about 6 mL of methanol to the same test tube. Swirl to dissolve. 2. Have your teacher supervise as you add 8 to 10 drops of sulfuric acid to the mixture. 3. Set up a hot water bath using the 250 mL beaker. The temperature of the water should be maintained throughout the experiment at between 60 and 70 C. 4. Clamp the test tube so that it is immersed in hot water to the depth of the mixture. 5. As a safety precaution to block any eruption of the volatile mixture, invert a 50 mL beaker above the end of the test tube. Let the mixture heat up for about 10 minutes. 6. After heating the mixture, rinse the 50 mL beaker with cold tap water and add about 30 mL of cold tap water to the beaker.

7. Cool the test tube with cold tap water and pour its contents into the cold water in the beaker. Using proper technique, carefully smell the mixture. 8. Rinse out the graduated cylinder. Repeat steps 1 to 7 using a different combination of equal volumes (about 5 mL) of an organic acid and an alcohol from list B.

Observations:
Odors: Ester 1: ____________________ Ester 2: ____________________

Analysis:
1, Which esters did you prepare? Ester 1: _________________________ Ester 2: _________________________

2. Draw the structures of the resulting esters.

Lab 28: Saponification

Soap is produced when a fat (or oil) is mixed and heated with sodium hydroxide, commonly known as lye, in a chemical process called saponification. Solid soap is the sodium salt of a fatty acid. Soft soap is a mixture of soap and glycerol. Liquid soap is the potassium salt of a fatty acid. In this experiment, you will synthesize soap during the first session and analyze its properties through several different chemical tests in the second.

Materials:
250 mL beaker spatula 10 mL graduated cylinder hot plate stirring rod 3 small tests tubes and stoppers balance vegetable shortening vegetable oil ethanol NaOH pellets phenolphthalein commercial soap commercial detergent 0.5 mol/L calcium choride

Procedure:
Part I: CAUTION: Extremely concentrated solutions. Wear proper protection (including rubber gloves), especially when handling the sodium hydroxide pellets. Teachers should consider all factors (students, lab safety etc.) before using such concentrated solutions. 1. Weigh out 15-20 g of shortening in the 250 mL beaker. 2. Add 7-8 g of NaOH(s) and 25 mL of water to the beaker. 3. Measure 10 mL of ethyl alcohol using the graduated cylinder. Add this to the 250 mL beaker. 4. Carefully heat the mixture on the hot plate, stirring constantly for at least 20 minutes. The solution should be hot, but not boiling. As you heat, carefully drip in 10 additional mL of ethyl alcohol. 5. At the end of the 20 minutes, add 25 mL of tap water and continue heating and stirring for an additional 10 minutes. Allow the mixture to cool. 6. Remove the coagulated soap mass with a spatula. Place it on several layers of paper towel and pat it dry. Using the towel, shape it into a bar or ball. Observe and

record its appearance and smell. 7. Allow the soap to air dry until the next lab session. Part II: 1. Place 5 mL of tap water in each of the three test tubes. Add a small portion of your soap to the first test tube. Stopper and tube and shake vigorously to test the foaming action of your soap. Repeat this process using commerical soap in the second test tube and commercial detergent in the third test tube. Clean out the test tubes. 2. Place 5 mL of tap water in each of the three test tubes. Add 8-10 drops of vegetable oil to each tube. Note that the oil forms a separate layer on top of the water. Stopper and shake the first tube. Allow the tube to stand for a few minutes and observe again. Add a small portion of your soap to the first test tube. Stopper the tube and shake. Allow the tube to stand a few minutes. Repeat this process using commercial soap in the second test tube and commercial detergent in the third test tube. Clean out the test tubes. 3. Place 5 mL of water in each of the three test tubes. Add a small portion of your soap to the first test tube. Stopper the tube and shake to dissolve the soap. Add 10-15 drops of CaCl2 solution to the soap solution. Shake and record the results. Repeat this process using commercial soap in the second test tube and commercial detergent in the third test tube. Clean out the test tubes. 4. Place 5 mL of water in each of the three test tubes. Add a small portion of your soap to the first test tube. Stopper the tube and shake to dissolve the soap. Add 2-3 drops of phenolphthalein indicator solution. Shake and record your observations. Repeat this process using commercial soap in the second test tube and commercial detergent in the third test tube. Clean out the test tubes.

Observations:
Part I: appearance and smell of your soap ________________________________________________________ ________________________________________________________ ________________________________________________________

Part II: your soap alone vegetable oil CaCl2 phenolphthalein commercial soap commercial detergent

Analysis:
1. Compare the sudsing actions of soaps and detergents. _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 2. How do the breakup capabilities of the soaps and detergent compare? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 3. Calcium chloride releases calcium ions into the water. This makes the water hard. How do the results of the soaps and detergent compare in hard water? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 4. How do the pH values of the commercial soap and detergent compare with your soap? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ _____________________________________________________________

Lab 29: Preparation of Nylon

In general, a polymeric substance contains long-chain molecules, in which a

particular unit (monomer) is found repeating over and over again along the entire length of the polymers chain. Condensation polymers are formed when two substances that ordinarily would not polymerize on their own are reacted, and the product of the condensation is a monomer that is now capable of polymerizing. A small molecule is also spit out during the condensation. Nylon is a synthetic polyamide resulting from the polymerization of an amine and an acid or an acid chloride. As the condensation reaction occurs, it is possible to pull the nylon being produced into thin fibers (threads). Because of hydrogen bonding between the polymeric molecules, the resulting nylon is very strong and stable.

Materials:
0.50 mol/L hexamethylenediamine (1,6-hexanediamine) in 0.50 mol/L sodium hydroxide 0.20 mol/L sebacyl chloride in hexane 250 mL beaker watchglass forceps

Procedure:
CAUTION: Hydrogen chloride gas is evolved during the reaction. Confine work with the reagents to the exhaust hood! 1. Have ready a 250 mL beaker of cold tap water for washing the nylon after it is produced. 2. Place about 5 mL of the hexamethylenediamine solution on a watchglass. 3. Gently add 10-12 drops of the sebacyl chloride solution as a second layer on top of the diamine solution. Try to float the chloride solution on top of the aqueous layer. Avoid bulk mixing of the two solutions; otherwise, the nylon will congeal into a blob rather than remaining threadlike. 3. On standing a few seconds, nylon will begin to form at the interface between the aqueous and nonaqueous solution. With forceps, grasp the polymer film that has formed at the liquid junction. Pull the filament of nylon slowly and evenly from the center of the glass until you a have thread of nylon about 5 cm long. 4. Transfer the nylon filament to the beaker of rinsing water, and allow it to stand for several minutes. 5. Take the beaker with the nylon filament to your bench, rinse the nylon with several additional portions of tap water, and examine its color, hardness, and strength when pulled.

Observations:
Comment on the color, hardness, and strength of the nylon filament. _____________________________________________________________ _____________________________________________________________ _____________________________________________________________

Analysis:
1. Why did the sebacyl chloride solution float on the surface of the 1,6-hexanediamine solution? _____________________________________________________________ _____________________________________________________________ _____________________________________________________________ 2. Write a chemical equation showing the formation of a unit of nylon from the sebacyl chloride and the 1,6-hexanediamine.

Bibliography
Hall, James A. Experimental Chemistry. Boston: Houghton Mifflin Company, 2003. Grant MacEwan Community College. Introductory University Chemistry Laboratory Manual (Chem 101, 103). Edmonton: 1998. Homquist, Dan D., et al. Chemistry with Calculators. Beaverton, Oregon: Vernier Software & Technology, 2000. Jenkins, Frank, et al. Chemistry. Scarborough, Ontario: Nelson Canada, 1993. Mustoe. Frank, et al. Chemistry. McGraw-Hill Ryerson Limited, 2004. Postma, James M., et al. Chemistry in the Laboratory. New York: W. H. Freeman and Company, 2000. Williamson, Kenneth L., et al. Microscale Experiments for General Chemistry. Boston: Houghton Mifflin Company, 1997. Zumdahl, Steven S., et al. Laboratory Experiments for World of Chemistry. Boston: Houghton Mifflin Company, 2002.

Edmonton Catholic School District Board Motion on Locally Developed Courses December 12, 2005
Chemistry Lab Techniques 35 Trustee Buddle moved that the Board of Trustees of Edmonton Catholic Separate School District #7 approves the new locally developed course, Chemistry Laboratory Techniques 35, for implementation in February 2006. CARRIED