Chemistry 2B Laboratory Manual

Department of Chemistry University of California - Davis Davis, CA 95616

Student Name _____________________

Locker Number____________

Laboratory Information Teaching Assistant's Name Laboratory Section Number Laboratory Room Number Dispensary Room Number _______________________ _______________________ _______________________ 1060 Sciences Lab Building

Location of Safety Equipment Nearest to Your Laboratory Safety Shower Eye Wash Fountain Fire Extinguisher Fire Alarm Safety Chemicals _______________________ _______________________ _______________________ _______________________ _______________________

TABLE OF CONTENTS PREFACE ........................................................................................................................iii ACKNOWLEDGMENTS ...............................................................................................iv INTRODUCTION ...........................................................................................................v A) Time Allocation and Grading of the Experiments.........................................v B) Safety Policy ..................................................................................................vi EXPERIMENTS: THERMOCHEMISTRY..................................................................................................1 COLLIGATIVE PROPERTIES ......................................................................................13 CHEMICAL EQUILIBRIUM .........................................................................................19 STRONG ACID - STRONG BASE TITRATION..........................................................27 ACID DISSOCIATION CONSTANTS AND THE TITRATION OF A WEAK ACID.........................................................................................................37 POLYPROTIC SYSTEMS..............................................................................................47 ACID-BASE BUFFERS..................................................................................................55 SOLUBILITY PRODUCTS ............................................................................................65 APPENDIX: A) General Experimental Guidelines..................................................................A-1 1. Pre-Laboratory Preparation.................................................................A-1 2. Data Collection ...................................................................................A-1 3. Unknowns ...........................................................................................A-1 4. Writing A Laboratory Report..............................................................A-1 5. Statistical Treatment of Data ..............................................................A-3 B) On-line Pre- & Post-Laboratory Procedures..................................................A-5 1. Accessing the Website .........................................................................A-5 2. Viewing the Pre-laboratory Presentations. ..........................................A-10 3. Taking the Pre-laboratory Quiz ...........................................................A-11 4. Completing the Post-Laboratory Exercises. ........................................A-12 Scoring Scheme ...........................................................................A-14 Due Date/ Late Submission of Post-lab Exercise. .......................A-15 C) Late Reports & Make-Up Policy ...................................................................A-15 1. Late Reports ........................................................................................A-15 2. Laboratory Make-Up Policy ...............................................................A-16 3. Laboratory Make-up Procedure ..........................................................A-16 4. Plagiarism and Unauthorized Collaboration........................................A-16 D) Common Laboratory Procedures...................................................................A-17 1. Using the Balance ...............................................................................A-17 2. Handling Solids...................................................................................A-18 3. Handling Liquids ................................................................................A-19 4. Capping a Flask...................................................................................A-19 5. Measuring Liquid Volumes ................................................................A-20 6. Filtration..............................................................................................A-22

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.....A-234 E) Maps...7........................................................................... Heating.............................................A-23 8......A-27 1............................................................................................................................................................................... Barometric Readings and Unit Conversions..............................................A-22 8....... Locker Inventory..A-25 F) Dispensary Procedures ........ Dispensing Policies...............A-31 ii .................................................................A-27 2..................................A-29 3.......................................................................................................... pH Meter Operating Instructions ......... Waste Labels.....................................

This commitment to the environment has presented an enormous challenge. We encourage you to discuss ideas for improvements or suggestions for new experiments with your TA. you are encouraged to complete the report as soon after laboratory as possible. Thus. It is important that you try to answer each question as it appears in the manual. Finally. In conclusion. While there is no "best" way. This was not only done to protect students but also to lessen the impact of this program upon the environment. Questions are presented throughout each experiment. In this way you can maximize the laboratory experience. The laboratory can also aid the student in the study of the science by clearly illustrating the principles and concepts involved. we view this manual as one of continual modification and improvement. Some experiments are completely environmentally safe and in these the products can be disposed of by placing solids in the wastebasket and solutions down the drain. Some instructors strongly feel that the lecture should lead the laboratory while other instructors just as strongly believe that the laboratory experiments should lead the lecture. Finally. instructors will sometimes vary the order of material covered in lecture and thus certain experiments may come before the concepts illustrated are covered in lecture or after the material has been covered. A unique aspect of this laboratory program is that a concerted effort has been made to use environmentally less toxic or non-toxic materials in these experiments. The faculty of the Chemistry Department at UC Davis clearly understands the importance of laboratory work in the study of chemistry. In addition. The sequence of experiments in this Laboratory Manual is designed to follow the lecture curriculum. However. and still a third group feel that they should be done concurrently. we hope you find this laboratory manual helpful in your study of chemistry. iii . The Department is committed to the further development of environmentally safe experiments which still clearly illustrate the important principles and techniques.PREFACE Chemistry is an experimental science. The Department is committed to this component of your education and hopes that you will take full advantage of this opportunity to explore the science of chemistry. as this is much more efficient than waiting until the night before it is due. it is important that students of chemistry do experiments in the laboratory to more fully understand that the theories they study in lecture and in their textbook are developed from the critical evaluation of experimental data. it is important that you carefully prepare for each experiment by reading the related text material before coming to the laboratory. as it will help you understand the experiment as you do it. Others contain a very limited amount of hazardous waste and in these cases the waste must be collected in the proper container for treatment and disposal. Over the past few years many improvements have come from student comments and criticisms. laboratory experimentation allows students the opportunity to develop techniques and other manipulative skills that students of science must master. as many traditional experiments could not be used due to the negative impact of the chemicals involved.

ACKNOWLEDGMENTS This manual is the culmination of the efforts of many individuals. have had a role in helping to develop these experiments and. In addition. many undergraduates have been involved in the development of experiments as part of undergraduate research projects. Many faculty members have provided ideas for the creation of these laboratories and have made numerous suggestions regarding their implementation. helping to ensure that the experiments are tailored to our laboratories here at UC Davis. in particular. iv . Stockroom Dispensary Supervisors. both past and present.

Students who fail these quizzes are considered unprepared and unsafe to work in the laboratory and will not be allowed to begin the laboratory procedure until the TA is convinced the student is prepared. If the quiz is failed on the first attempt. Because the questions are chosen randomly.Pre-lab (eight) *On Line Pre-laboratory Quizzes: Each 2 point pre-lab quiz must be completed at least 1 hour prior to attending the student’s scheduled lab class. The TA will allow entry into the laboratory only if the student answers the questions correctly and the pre-laboratory write-up is complete.INTRODUCTION A) Time Allocation and Grading of the Experiments Below is an indication of the time allocation and point value of each experiment. This policy will be strictly enforced. the student’s TA will sum the scores and give this to the instructor. The TA will check the pre-laboratory write-up and quiz the student. who will modify it as described in the course syllabus. the student may take the quiz a second time. v . different questions may be generated on the second attempt. At the end of the quarter. All three quiz questions must be answered correctly before the student will be allowed to perform the laboratory experiment. . Lab Periods Allocated 2 1 1 1 1 1 1 1 2 2 Title of Experiment Thermochemistry Colligative Properties Chemical Equilibrium Strong Acid-Strong Base Titration Acid Dissociation Constants and the Titration of a Weak Acid Polyprotic Systems Acid/Base Buffers Solubility Product On-Line Pre-lab Quizzes (seven) Lab Notebooks .

beverage. fire extinguisher. Strict adherence to these policies is mandatory and greatly reduces an individual’s risk of exposure to hazardous materials. 2. Close-toed shoes must be worn at all times. A number of policies have been developed in order to make sure that the laboratory is safe and that it runs smoothly. and fire alarm box. chewing gum. First aid for acid or base in the eyes is to wash with copious amounts of water using the eyewash fountain for 15 minutes. except as instructed. Goggles must be worn by EVERY student in the lab until EVERYONE has finished with the experimental procedure and has put away ALL glassware.B) Safety Policy It is critical that you prepare for each experiment by reading it carefully before entering the laboratory. consumption and use of food. Use the emergency shower if appropriate. or Dispensary Supervisor. tobacco. It is strongly recommended that you wear clothing that completely covers your arms. and the application of contact lenses or cosmetics in laboratories where chemical. Learn the location and how to operate the nearest eyewash fountain. course instructor. Not only will this ensure that you get the maximum benefit of the experience. but it also makes for a safer environment in the laboratory. Absolutely NO food or drinks are allowed in the laboratory. biological or radioactive materials are used or stored. No laboratory work will be done without supervision. Five campus policies address the prohibition pertaining to the storage. Then immediately go to the Student Health Center for further treatment. This is important not only for your own safety but also for those around you. and only in the manner instructed: Do not alter experimental procedures. medicine. First aid for acid or base on skin or clothing is to wash thoroughly with water for 15 minutes. Avoid wearing expensive clothing to lab as it may get damaged. 4. safety shower. are not followed. 1. Violations of these rules are grounds for expulsion from the laboratory. The Laboratory Instructor (TA) has complete authority for enforcement of these rules and any other procedures to ensure safe practices in carrying out the laboratory work. Perform only authorized experiments. 3. Safety goggles may not be modified in any manner. No one is allowed in the laboratory without the supervision of a laboratory instructor. vi . Accidents commonly occur when the following rules. 5. Approved safety goggles must be worn at all times. In each experiment specific hazards are indicated by bold type and procedures are described that must be adhered to. Inadequate protection often leads to injury. as approved by the Chemistry Department Safety Committee. At NO time are safety glasses of any kind acceptable in the laboratory. legs. and feet while working in the laboratory. Safety Rules for Laboratory Work The following rules are designed for your safety in the laboratory.

Mouth suction must never be used to fill pipets. Specific permission from your laboratory instructor is required before you may work in a laboratory other than the one to which you have been assigned. Hair can catch on fire while using open flames. 10. course instructor. 11. The student must have one UNGLOVED hand when outside the laboratory. rollerblades and other personal equipment not necessary to the course will be stored on the shelves of the wooden cabinet near the front door. The student should always be accompanied to the Student Health Center by someone. Only use the ungloved hand to open doors. except to the dispensary for refill. please ask your laboratory instructor before starting any laboratory work in this course. or any other objects. injuries. Horseplay and carelessness are not permitted. 7. 16. All containers must be CAPPED before you take them into the hallway and to the dispensary: never take uncapped glassware containing chemicals into the hallways or other public areas. Any spilled reagents must also be wiped up immediately. Do NOT hold the door open with chairs. 14. 13. explosions. Exercise the appropriate care to protect yourself from skin contact with the substance. Equipment too large (or otherwise unable) to fit on the shelves of the cabinet WILL NOT be allowed inside the laboratory. Only laboratory rooms where the same laboratory course is currently operating may be used for this purpose.6. students are also encouraged to seek medical attention if they deem it necessary. Maintain your working area in a reasonable state of neatness. The doors to the laboratory must remain closed except when individuals are actively entering or exiting the lab. Gloves are presumed to be contaminated and must not come into contact with anything outside the laboratory except containers of chemicals. 17. Always use a bulb to fill pipets. You are responsible for everyone’s safety. 18. Skateboards. Confine long hair while in the laboratory. If you spill water or a reagent. If you have questions about these rules and procedures. 12. or fires must be reported at once to the laboratory instructor. 15. stools. 8. the student must visit these facilities if requested to do so. 9. All accidents. In cases of serious injury. Containers of chemicals may not be taken out of the laboratory. replacement. call 911 for an ambulance. vii . All operations in which noxious or poisonous gases are used or produced must be carried out in the fume hood. or Laboratory Manager decides that the extent of an injury is serious enough to warrant inspection and treatment by the Student Health Service. or break a piece of glassware. or the exchanging of full waste jugs for empty ones. Put all toxic or flammable waste into the appropriate waste container(s) provided in your laboratory. Clean off your lab work bench before leaving the laboratory. clean it up immediately. In cases where the laboratory instructor. You must sign the Safety Acknowledgement sheet before you may work in the lab.

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EXPERIMENTS .

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In the first part of this experiment you will construct a simple "coffee-cup" calorimeter. 1 . Carefully follow the procedure outlined. thermodynamics. visit the stockroom (Room 1060). of water. After completing this experiment. During this first laboratory period you will go over the laboratory safety rules. They will give you the glassware that you are missing. Please look in the Introduction of this manual for a locker list and drawings of common laboratory equipment. ∆Hfus. Please replace all missing equipment the first day of laboratory since the stockroom is only prepared to replace glassware during the first week. You will be exploring the factors that cause a reaction to occur. Place extra glassware in the box at the back of the room. become acquainted with the layout and equipment in the laboratory. you will determine the enthalpies. When used properly. If you still cannot find the missing equipment. you have probably noticed that a wooden spoon does not heat as fast as metal one. first check the box of extra glassware that is located at the back of the laboratory. In an exothermic reaction.Thermochemistry INTRODUCTION Welcome to the Chemistry 2B Laboratory. In the fifth part of the experiment. Remember to always follow the safety instructions when performing all experiments! Wear your goggles! Locker Check-in Make sure your locker contains all of the proper equipment in the correct quantities. For example. ∆Hrxn. this calorimeter can give very good results. you will better understand the reasons behind these and other thermal phenomena. sign the back of the safety sheet and return it to your TA. which involves one of the most important areas of science. of endothermic and exothermic reactions. In the next part of the experiment you will measure the specific heat of an unknown solid. you will design your own procedure to determine the heat of fusion. Thermochemistry Experiment This experiment is an introduction to the basic principles of thermochemistry and involves the exchange of energy as heat. If you are missing any items. In order to make sense of your observations for the third and fourth parts of the experiment you will need to consider an additional concept. In the third and fourth parts of the experiment. Safety: After reviewing the safety rules with your TA. Then you will begin the first experiment of the quarter. and check-out the equipment in your locker. on a hot summer day the hood of a car can get hotter than the sidewalk cement and when cooking. The ideas and concepts involved in thermodynamics are illustrated in your everyday experiences.

Entropy can be thought of as a measure of the disorder or randomness in a system. 2 . A reaction that results in an increase in the total moles of particles (nf .ni > 0) is said to have an increase in entropy (∆S > 0). in an endothermic reaction heat is absorbed. Please note that you must come to the laboratory with an outline of the procedure you plan to use. indicating that the products are higher in energy (∆Hrxn is positive). Entropy is high. but a brief introduction is provided here. implying that the products are of lower energy than the reactants (∆Hrxn is negative). The more freedom particles have to move around. dissolving a salt in water will increase the entropy because the particles go from a very organized crystal to a less organized solution of free-moving ions. the more entropy they will have. Increasing the entropy of a system has the same effect as minimizing the enthalpy of the system --. Changing a specific sample of a solid to a liquid does not increase the number of moles of the sample.it drives the reaction forward. Entropy will be fully discussed later in the course. attention is focused on the number and motion of particles in a system. all quietly facing the same direction with their attention focused in pretty much the same place. What provides the driving force for an endothermic reaction? The answer to this question is entropy. Nature tends to minimize enthalpy (∆H) and maximize entropy (∆S). For instance. However. but the energy and motion of the molecules does increase. Finally. that one of the reactions is enthalpy-favored (-∆H) but not entropy-favored (-∆S). Endothermic reactions occur because entropy increases. Entropy is low. You will see.the reaction releases heat. You will look at reactions that vary in their enthalpic and entropic properties in the third and fourth parts of this experiment. symbolized "S". The gain from increasing entropy (+∆S) in these reactions is enough to counterbalance the unfavorable enthalpic conditions (+∆H). As preparation for this experiment you should read the section on thermochemistry in your textbook. in the last part of this experiment you will design your own procedure to determine the heat of fusion for ice. the greater the disorder the higher the entropy. Similarly. At the beginning of the lecture everyone is coming into the room and milling around. Changing the liquid to a gas dramatically increases the entropy of the system. and one is favored by both enthalpy (-∆H) and entropy (+∆S). Entropy also depends in part upon particle distribution in space and in part on the distribution of energy (and motion) among the particles. the entropy of the sample has increased. When entropy is discussed in chemistry. one is entropy-favored (+∆S) but not enthalpy-favored (+∆H). In the middle of the lecture everyone is seated in rows of chairs. ∆Hfus. compare your lecture at the beginning of the hour and in the middle of the hour. finding seats and getting settled. Therefore. Entropy can therefore be a driving force for a reaction since greater entropy is a preferred condition.

the amount of heat lost from the hotter substance equals the heat gained by the colder one. Before you can use this calorimeter to determine thermodymanic quantities you must determine the heat capacity of the calorimeter itself. energy in the form of heat is exchanged between them until they reach a common temperature. the specific heat of the substance. and Molar Heat Capacity All parts of this experiment require the use of a calorimeter. The amount of energy required to change the temperature of an object or a sample of a substance by one degree Celsius or Kelvin is called that object's J heat capacity.   The specific heat of a substance is the heat required to raise the temperature of one gram of the substance one degree. When two substances having different temperatures come into contact. If they are insulated from their surroundings. The heat lost or gained is related to the mass.   There are two variations on heat capacity that you also need to be familiar with:  J  specific heat. you will construct an inexpensive but effective coffee-cup calorimeter. You will do this by adding a weighed sample of hot water to a known amount of cold water in the calorimeter and measuring the temperature change. All substances have characteristic specific heats and molar heat capacities. you will determine the heat capacity of your calorimeter. and ∆T is the change in temperature. This can be done since the mass of the calorimeter does not change. symbolized cp °C . When dealing with the calorimeter itself. and molar heat capacity is substituted for specific heat. In this experiment. Specific Heat. In the first part of this experiment. Csp g °C   and  J  molar heat capacity. q = cp(calorimeter) * ∆Τ 3 . and the temperature change. Cp mol °C . the calorimeter's heat capacity. This equation can also be used if moles are substituted for mass. This relationship is expressed as q = m * Csp * ∆T where q is the heat. Heat Capacity. m is the mass. you will combine the mass and specific heat of the calorimeter into a single term. and the molar heat capacity is the amount of energy required to raise one mole of the substance by one degree. Csp is the heat capacity of that substance.Background: Heat.

PROCEDURE Work individually on this experiment. Insert a thermometer through the hole.Safety: To avoid burns. 2. Never pick up a heated metal with your bare hands. gently clamp the thermometer and lower it into the cup so that the whole bulb is covered with water but is not touching the bottom of the cup. We will refer to this mass as the “mass of the cool water”. Place the cup back into the calorimeter set-up. Take a 4"x 4" piece of cardboard. and calibrate the balance to zero mass. Put two Styrofoam coffee cups in a 250 mL or a 400 mL beaker. masscool water. Allow the flask of water to sit in the boiling water for 15 minutes in order for the temperature of water in the flask to equilibrate to the temperature of the boiling water in the beaker. Wear gloves and use caution when handling acids and bases. Take the top Styrofoam cup from the calorimeter. (You may share a waterbath only. If the hole is too big. Wear your goggles. Place one of the labeled flasks in the beaker of boiling water using a utility clamp to hold it in place. Part I. 3.) You may need to refresh your water supply periodically to prevent the water from boiling away completely. 4 . use crucible tongs to pick up hot metal. Determining the Heat Capacity of the Calorimeter 1. Set up a hot plate and heat 500 mL of deionized water to boiling in an 800 mL beaker. Weigh out about 70 grams of room temperature deionized water into the calorimeter and record the mass of the water to the nearest thousandth of a gram. 5. Make sure that the water level in the flask is below the water level in the 800 mL beaker. All waste from this experiment can be poured down the drain. and place it on top of the coffee cups. We will refer to this mass as the “mass of hot water. Place your 50 mL Erlenmeyer flask in a 150 mL beaker and tare this assembly. place it on the balance. Using the buret holder. This is called "taring" the container. Put 30 ml of room temperature deionized water in the 50 mL Erlenmeyer flask and record the mass of the water to the nearest thousandth of a gram in your notebook along with the corresponding flask label. with the hole in the center. 4. cover it with two pieces of masking tape and punch a hole with your pen or pencil big enough so the thermometer can fit. 6. Avoid positioning the calorimeter too close to a Bunsen burner or hot plate so that the water inside the calorimeter remains cool.” Repeat this step with two more 50 mL Erlenmeyer flasks.

We will refer to this temperature as the initial temperature of the cool water. Replace the thermometer and cardboard top on the calorimeter. Next. We will refer to this temperature as the final temperature. This is the equilibrium temperature. you may need to refresh your water supply to prevent the water from boiling away completely. repeat steps 2. Determining the Specific Heat of a Metal Using the same calorimeter for which you determined the heat capacity. Continue to heat 500 mL of deionized water to boiling in an 800 mL beaker either using a hotplate. Once the water in the flask has equilibrated complete steps 7. measure the temperature of the boiling water in the beaker with your second thermometer and record to the nearest 0.2 °C. Monitor the temperature and record the highest temperature attained to the nearest 0. Take the top Styrofoam cup from the calorimeter. and rise again due to the initial uneven distribution of heat within the calorimeter. you will analyze an unknown metal sample to find its characteristic specific heat capacity and identify the sample as lead. 1.2 °C. 9. Tihot water. 10. Stirring the water in the calorimeter distributes the heat throughout the calorimeter. Ti cool water. aluminum or copper.2 oC.7. Place the next 50 mL Erlenmeyer flask in the boiling water and allow it to equilibrate to 100°C for 15 minutes. Again. . Gently stir the water in the calorimeter until the highest temperature is reached. While you are waiting. Just before transferring the hot water in the flask to the calorimeter. Set up your calorimeter by placing the two Styrofoam cups in a 250 mL or a 400 mL beaker as before. place it on the balance and tare it. measure the temperature of the water in the calorimeter and record to the nearest 0. 9. Watch the thermometer closely as it rises. 8. Be careful that no hot water on the outside of the flask drips into the calorimeter. 11. Adjust the thermometer's height so that it is not touching the bottom or sides of the calorimeter yet the water is covering the thermometer bulb. and 10. Repeat the same procedure using your final 50 mL Erlenmeyer flask of water. Dry the calorimeter and thermometer between trials. 8. remove the thermometer and cardboard top from the calorimeter. 3 and 4. 12. We will refer to this temperature as the initial temperature of the hot water. Part II. Tf. Sometimes it will rise. Using your clamp. fall. After the 15 minutes. grasp the flask containing the 30 ml of hot water near the top and quickly but carefully pour the hot water into the calorimeter. Weigh out about 70 grams of room temperature deionized 5 2.

Make sure the beaker does not tip over. Take your 4"x 4" piece of cardboard. The sample should be a piece of metal strung with nylon string. Tiwater. 3. gently clamp the thermometer and lower it into the cup so that the whole bulb is covered with water but is not touching the bottom of the cup.water into the calorimeter and record the mass of the water to the nearest thousandth of a gram. 8. Obtain a sample of the unknown metal from the box at the front of the room. Place the cup back into the calorimeter set-up. Using the buret holder. Adjust the thermometer's height so that it is not touching the metal or the Styrofoam cup. Next. 7. Record the mass of the metal to the nearest thousandth of a gram. Adjust the height of the utility clamp so that the metal is completely submerged in the boiling water. Quickly but carefully drop the metal into the calorimeter and cover with the cardboard. This will be the initial temperature of the metal. Just before transferring the metal to the calorimeter. This is the initial temperature of the water. This will insure the temperature of the metal to be approximately 100 oC. lift and shake the suspended metal vertically so that a maximum amount of hot water will drip off the metal surface and back into the beaker.2 °C. Weigh the unknown metal sample using a weigh boat to protect it from contamination. measure the temperature of the boiling water in the beaker with your second thermometer and record to the nearest 0. 5. Make sure that the metal sample is completely covered with water.2 °C. and calorimeter. 6 . Identify the metal based on density and color and write down the type of metal you obtained in your laboratory manual. and place it on top of the coffee cups. 4. Allow the metal to sit in the boiling water for 3-4 minutes. measure the temperature of the water in the calorimeter and record to the nearest 0. Tare the weigh boat. 10. Insert a thermometer through the hole. Suspension of the sample insures that the metal will have the same equilibrium temperature as the boiling water by preventing direct heating by the flame or hot plate (which would result if the metal were allowed to rest on the bottom of the beaker). 9. Add more water to the beaker if necessary and return to a boil. Replace the thermometer through the hole in the cardboard top on the calorimeter. Do not remove the nylon string. Ticalorimeter. with the hole in the center. 6. After the 3-4 minutes. Timetal. yet the water is covering the thermometer bulb. Suspend the string of metal disks from a utility clamp that is attached to the superstructure at the laboratory bench above the 800 mL beaker of boiling water.

Using the buret holder. Part III. Gently swirl the calorimeter cup until an equilibrium temperature (highest temperature) is reached. This is the final temperature. add the ammonium nitrate to the calorimeter and cover with the cardboard. 3. in J/mol. Sometimes it will rise. Tf. Tiwater. ∆Hrxn. 12. 2. Ticalorimeter. Swirling the water in the calorimeter distributes the heat uniformly. measure the temperature of the water in the calorimeter and record to the nearest 0. Place the cup back into the calorimeter set-up. place it on the balance and tare it. Insert a thermometer through the hole. 7 . You will be simulating this reaction in your calorimeter in order to calculate the enthalpy of reaction. Replace the thermometer through the hole in the cardboard on top of the calorimeter. Repeat this procedure two more times using the same metal sample. Record the mass of the ammonium nitrate to the nearest thousandth of a gram. Take your 4"x 4" piece of cardboard. and rise again due to the uneven distribution of heat within the calorimeter. Watch the thermometer closely as it rises. the inner bag is broken and an endothermic reaction occurs as the ammonium nitrate dissolves in the water.11. Monitor the temperature and record the highest temperature attained to the nearest 0. and place it on top of the coffee cups. Make sure that none of the ammonium nitrate or water spills out of the calorimeter. When the cold pack is bent. Just before transferring the ammonium nitrate to the calorimeter. As a result the pack gets colder. Next. Take the top Styrofoam cup from the calorimeter. and calorimeter. fall. Weigh out about 25 grams of room temperature deionized water into the calorimeter and record the mass of the water to the nearest thousandth of a gram. remove the thermometer and cardboard top from the calorimeter. Dry the calorimeter and thermometer between trials. This is the initial temperature of the water. Tare a clean weigh boat and weigh out about 5 g of ammonium nitrate. Carefully.2 oC. 6. 1. gently clamp the thermometer and lower it into the cup so that the whole bulb is covered with water but is not touching the bottom of the cup. Set up your calorimeter by placing the two Styrofoam cups in a 250 mL or a 400 mL beaker as before. Calculating the Enthalpy of an Endothermic Reaction The cold packs in some first-aid kits are made of ammonium nitrate pellets encased in a plastic bag surrounded by water. 5.2 °C. 4. Adjust the thermometer's height so that it is not touching the bottom or sides of the calorimeter yet the water is covering the thermometer bulb. with the hole in the center.

Make sure that none of the sodium hydroxide or hydrochloric acid spills out of the calorimeter. strictly speaking. Repeat this procedure two more times.0 M NaOH(aq) already contain water and we are using this water as the calorimeter water. Take your 4"x 4" piece of cardboard. This is the final temperature. Adjust the thermometer's height. measure out about 15 mL of 6. Lift the cardboard top from the calorimeter keeping the thermometer in place. Record the volume to the nearest 0. 7. add the sodium hydroxide to the calorimeter and cover with the cardboard.2 mL. the enthalpy of reaction of hydrochloric acid and sodium hydroxide. 8 . Clean and dry the calorimeter and 8. Clean and dry your Styrofoam cups and set up your calorimeter by placing the two Styrofoam cups in a 250 mL or a 400 mL beaker as usual. and calorimeter. gently clamp the thermometer and lower it into the cup so that the bulb is near but not touching the bottom of the cup. so that it is not 2. Gently stir the water in the calorimeter until the ammonium nitrate is dissolved and the lowest temperature is reached. Tiwater. Stirring the solution in the calorimeter achieves a uniform temperature throughout the calorimeter. thermometer between trials. Carefully. Monitor the temperature and record the lowest temperature attained to the nearest 0. measure out about 15 mL of 6. Carefully. transfer the hydrochloric acid from the graduated cylinder to the calorimeter. Calculating the Enthalpy of Exothermic Reactions Neutralization reactions are exothermic reactions. Just before transferring the sodium hydroxide to the calorimeter. Ticalorimeter. Part IV. carefully. Tf.0 M HCl(aq) and 6. 6. Make sure that none of the hydrochloric acid splashes out of the calorimeter. Using the buret holder. Do not add any water to the calorimeter. In a clean and dry graduated cylinder. 4. 5. The heat released by diluting the acid and the base is also included in that number. with the hole in the center. The number you will calculate is not.2 mL.0 M sodium hydroxide. 3. Record the volume to the nearest 0. and place it on top of the coffee cups.0 M hydrochloric acid in a clean and dry graduated cylinder.7.2 oC. The solutions 6. Do not add water to your calorimeter. Carefully. This is the initial temperature of the water. if needed. 1. Watch the thermometer closely. Insert a thermometer through the hole.2°C. measure the temperature of the hydrochloric acid in the calorimeter and record to the nearest 0. You will be measuring quantities to estimate the enthalpy change for the neutralization of hydrochloric acid with sodium hydroxide.

touching the bottom or sides of the calorimeter yet the solution is covering the thermometer bulb. 8. Gently stir the water in the calorimeter until the solutions are well mixed and the highest temperature is reached. Watch the thermometer closely as it rises. Stirring the solution in the calorimeter distributes the heat throughout the calorimeter. Monitor the temperature and record the highest temperature attained to the nearest 0.2 oC. This is the final temperature, Tf. Repeat this procedure two more times. Clean and dry the calorimeter, thermometer, and graduated cylinder between trials.

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Part V. Calculating the Heat of Fusion of Water In this part of the experiment you will design an experiment to determine the heat of fusion of ice. You will need your calorimeter, ice, water, and a balance. You may use any of the equipment in your locker. Be sure your method is repeatable. See how close you can come to the known result. 1. 2. Design an experiment to determine the heat of fusion of ice. You should come to the laboratory with an outline of the procedure you plan to use. Do the experiment performing three separate trials. Write-up the detailed procedure you used.

Clean-Up: All solutions may be disposed of by washing down the sink with copious amounts of water. Be sure to rinse out the calorimeter before returning it to the box at the front of the room.

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DATA ANALYSIS Part I 1. In step 8, why do you not want any of the water on the outside of the 50 mL Erlenmeyer flask to drip off into the calorimeter? 2. For each trial, calculate the heat lost by the hot water, qhot water. Is this quantity positive or negative? The specific heat of water is 4.184 J/g.C. 3. For each trial, calculate the heat gained by the cool water, qcool quantity positive or negative?
water.

Is this

4. For each trial, calculate the heat gained by the calorimeter, qcalorimeter, This can be done by using the equation: - qhot water = ( qcool water + qcalorimeter ). Is qcalorimeter a positive or negative quantity? Hint: Be careful with your negative values here. Remember that (- qhot water) has the opposite algebraic sign value of (qhot water). 5. For each trial, calculate the heat capacity of your calorimeter. Hint: Write an expression for the heat capacity of the calorimeter in terms of qcalorimeter and the temperature change of the calorimeter. Note that the temperature change of the calorimeter is assumed to be the same as the temperature change of the “cool water” in the calorimeter. 6. Calculate the average heat capacity for the calorimeter. 7. Calculate a standard deviation for the average heat capacity. 8. Calculate a 90% confidence limit for this data. Part II 9. Why do we want the water to drip off the metal before it is placed in the calorimeter? 10. Calculate the specific heat for your metal for each trial. Remember that the heat lost by the metal is equal to the heat gained by the water in the calorimeter and by the calorimeter itself. This can be expressed as –qmetal = (qwater + qcalorimeter). The specific heat capacities are positive numbers. 11. Calculate the average specific heat capacity for your metal sample. 12. Calculate the standard deviation of your average specific heat capacity. 13. Using the physical properties of your metal, i.e. density & color, identify your metal. 10

14. Calculate the percent error of your average specific heat as compared to the accepted value. Csp(Pb) = 0.128 J/g·°C; Csp(Al) = 0.900 J/g·°C; Csp(Cu) = 0.387 J/g·°C Part III 15. Write a chemical equation that describes the dissolution of ammonium nitrate in water. 16. For each trial, calculate the number moles of ammonium nitrate dissolved. 17. For each trial, calculate the heat gained by the chemical system of ammonium nitrate, qrxn. This can be done by using the equation: qrxn = - (qwater + qcalorimeter). The calorimeter and the water are losing heat. Therefore, qwater and qcalorimeter are negative values. 18. The heat transfer in the calorimeter is taking place at constant pressure. Therefore, we can equate the heat gained by the chemical system of ammonium nitrate, qrxn, to its enthalpy of reaction, ∆Hrxn. For each trial, calculate the enthalpy of the reaction per mole of ammonium nitrate in units of Joules per mole. 19. Calculate the average enthalpy of reaction for the dissolution of ammonium nitrate in J/mol. 20. Calculate the standard deviation of the enthalpy of reaction. 21. Is the dissolution reaction of ammonium nitrate enthalpy-favored? Explain your answer. Part IV 22. Write the chemical equation for the neutralization reaction of hydrochloric acid and sodium hydroxide. 23. Calculate the number moles of hydrochloric acid used in the reaction for each trial. 24. In order to calculate the heat gained by water, qwater, the mass of calorimeter must be determined. Calculate the mass of water using the combined volume of 6.0 M hydrochloric acid with 6.0 M sodium hydroxide and the density of water, 1.00g/mL. 25. For each trial, calculate the heat lost by the chemical system, qrxn. This can be done by using the equation: qrxn = - (qwater + qcalorimeter). 11

The heat gained by the ice resulted in the ice melting. calculate the enthalpy of the neutralization reaction per mole of hydrochloric acid in units of Joules per mole. The heat transfer in the calorimeter is taking place at constant pressure. qcalorimeter. we can equate the heat lost by the chemical system. Note that this value is reported here only to 2 significant figures. Discuss the reasons for your measured value of the specific heat of the metal being too high or too low. For each trial. 33. Calculate your percent error. Calculate the average enthalpy of reaction for the neutralization in J/mol. ∆Hrxn. qice. 35. qwater. Part V 30. calculate the heat of fusion per gram of ice. Calculate the standard deviation for the average. Is the neutralization reaction enthalpy favored? Explain your answer. 34. For each trial. 27. 32. 12 . 29. Calculate the average heat of fusion per gram of ice. Calculate the standard deviation of the enthalpy of reaction. For each trial. 31. 28. according to the textbook is 330 J/g. calculate the heat lost by the calorimeter. Compose a paragraph summary of this experiment. and raised the temperature of the melted ice from 0°C to the final temperature of the water in the calorimeter. calculate the heat lost by the water in the calorimeter. qice-water. to its enthalpy of reaction. For each trial. Conclusion. qrxn. Include some comments about the sources of error in the experiment that may be responsible for the difference between the values you have obtained and the accepted literature values for the properties you studied in this experiment. The accepted value for the Heat of Fusion of ice.26. Therefore.

A solution of NaCl has an i factor of 2. This will be below room temperature and thus will require the use of an ice bath. the freezing point depression is large for even dilute solutions of this solvent.Colligative Properties INTRODUCTION Colligative properties are those properties of a solution that depend on the amount of a chemical species in solution. In the next part of the experiment you will measure the freezing point of a solution of cyclohexane with para-dichlorobenzene as a solute to determine the freezing point depression constant for cyclohexane. This will require the use of a colder salt-ice water bath. it is convenient to use because it freezes at a temperature just above the freezing point of water. Kf is the freezing point constant of the solvent. Examples of these properties are boiling point elevation. As pre-laboratory preparation you should read the section on colligative properties in your textbook. has an i factor of 3 and a solution of a non-dissociating substance like sugar would have an i factor of 1. and osmotic pressure. In this experiment. Cyclohexane is chosen as the solvent in this experiment for two reasons. i is known as the van't Hoff i factor. Thus. you will study the second of these common examples using the solvent cyclohexane. is the difference between the freezing point of the pure solvent and the freezing point of the solution. you will use the Kf that you have determined in Part II to find the molecular mass of an unknown. freezing point depression. 13 . Finally. and second because it has a large Kf value. First. a solution of MgCl2. and m is the molality of the solution. The freezing point depression. You may recall from your textbook that freezing point depression is described by the equation: ∆Tf = i x Kf x m where ∆Tf is the freezing point depression. ∆Tf. During this experiment you will first measure the normal freezing point of cyclohexane in your experimental apparatus. and not on the identity of the species in solution. C6H12.

Measure the temperature of the ice-water bath for later comparison in Part II. the bulb of the thermometer must be well covered by the cyclohexane. by cooling the cyclohexane slowly to below room temperature using an ice-water bath. You will need to adjust your thermometer so that you can read the temperature scale between 0 and 10oC without the tape on the test tube interfering.7726 g/mL @ 25oC).2oC. Assemble the inner test tube of the apparatus with the cork. Absolutely NO flames of any kind can be used while this experiment is in progress. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs. Obtain a freezing point apparatus found on the main supply shelf. A good technique is for one student to 14 2. adding equal portions of ice and water. and stirrer. Record the temperature to the nearest 0. . Set up the apparatus as shown in Figure 1. Place the freezing point apparatus in the ice-water bath so that the cyclohexane is well below the surface of the water.00 mL of cyclohexane from the dispenser on the cyclohexane bottle in the fumehood. In addition. calculate the mass of cyclohexane measured. Dispense 10. Place the assembled inner test tube carefully into the larger test tube. Colligative Properties Experiment Part I. Mount your 800 mL beaker containing the ice-water bath onto a wire gauze and an iron ring. The tape around the outer test tube forms a seal between the two. Make sure that you avoid unauthorized collaboration and plagiarism. 3. The actual data analyses and the written reports must be done entirely independently of your lab partner or other students. Ice may be found in a large bucket near the laboratory door. Determining the Freezing Point of Pure Cyclohexane 1. Wear your goggles. 5. Each student must collect data and submit a separate report. Cyclohexane is extremely flammable.Safety: Wear your goggles throughout the entire experiment. Make an ice-water bath in an 800 mL beaker. as demonstrated by your TA. Clamp the freezing point apparatus in place. Measure the freezing point. Note the listed volume on the dispenser so that the mass of cyclohexane is known for the molality calculation in Part II. PROCEDURE Work in pairs on this experiment. 4. Using the known density of cyclohexane (0. thermometer. Use the fume hood as much as possible to reduce odors.

Save the pure cyclohexane to use in Part II.) Freeze and melt the same sample for all trials. A thermometer and a metal stirring rod are inserted into the cork. say every 15 seconds. 6. or plateaus. Three or more trials need to be performed to obtain good precision in your measurements. The correct freezing point is when the temperature stops decreasing. warm the sample in the palm of your hand to just above the melting point after each trial. Figure 1: The Measurement of a Freezing Point The freezing point apparatus is constructed of a 20x150mm test tube which is stoppered with a cork. The 20x150mm test tube is inserted into a larger test tube (25x150mm). The outside surfaces of the test tube and beaker will have to be wiped with a paper towel periodically in order to accurately read the thermometer and see the sample. To save time. Be sure to raise and lower the metal stirrer carefully to mix the sample thoroughly thereby maintaining a uniform temperature while it cools. 15 .5 oC of each other. (The melting points should be within 0.carefully stir and read the thermometer while the other student records the temperature at regular intervals. Insufficient stirring will cause non-uniform cooling. and stirring too vigorously will cause the solution to splash and freeze on the side of the test tube.

As the solid begins to form. 2. This may take a few minutes. To measure the freezing point of the mixture. Weigh out 0. work with your partner to record the decreasing temperature at regular intervals.6 g of p-dichlorobenzene. The temperature of the salt-ice-water bath needs to be -10°C or lower. Rinse out the smaller test tube. Caution: To avoid breakage. a plateau will occur.5 – 0. When you thaw the solution. As you approach the freezing point. Do not become impatient here. Clamp the freezing point apparatus into the salt-ice-water bath as in Part I.001g). only allow it to warm about 5°C ABOVE its freezing point. do not stir the salt-ice-water bath with a thermometer. Allow the cyclohexane from Part I to warm to room temperature. Record the mass to the nearest thousandth of a gram (0. You will need to view the temperature scale through the walls of the test tubes. the thermometer needs to be adjusted so that it is well submerged in the solution while allowing you to read the temperature scale between -8°C and 0°C without interference from the tape on the test tube. Use a stir rod. Place the cyclohexane rinse in the waste bottle as well. 3. The salt-ice-water bath must be mixed well to achieve the sub-zero temperature needed for this part of the experiment. Determining the Freezing Point Constant for Cyclohexane In this part of the experiment. metal stirrer. This bath can be prepared by filling an 800 mL beaker with alternating layers of ice and solid NaCl (~100 mL NaCl measured in a beaker). 4. 1. Here. Save the salt-ice-water bath for Part III. this experiment will take an inordinate amount of time. 16 .Part II. After the data has been collected. C6H4Cl2. The sample will have to be frozen and melted three or more times until you obtain good precision in your measurements. you will collect data that will allow you to determine the Kf for cyclohexane. pour the melted mixture into the appropriate waste bottle in the fume hood. Measure the temperature of the ice-salt water bath. Carefully add the solid to the room-temperature cyclohexane. The larger test tube should not need cleaning. Again. Reassemble the freezing point apparatus and stir the solution with the metal stirring rod to ensure complete mixing. and your thermometer with a few milliliters of cyclohexane. a salt-ice-water bath will be necessary. If you let the solution return to room temperature between each trial. then add water to within two cm of the beaker rim. the rate of cooling slows. You can do this by adding a known quantity of solute to the cyclohexane solvent and measuring the freezing point of the mixture. Stir the mixture until the p-dichlorobenzene is completely dissolved. stir more slowly being sure to keep the thermometer bulb submerged in solution.

complete dissolution is essential for molecular mass determination. however. the solute may be slow to dissolve. Calculate an average Kf value. Some unidentified solutes are provided in the laboratory. Rinse out the smaller test tube. Your experimental design will be similar to the procedures used in Part II. There are recommended mass ranges on the bottles. What is that assumption? 2. The salt-ice-water bath may be poured in the sink with copious amounts of water. Calculate the average freezing point of the pure cyclohexane. and your thermometer with a few milliliters of acetone. Determining the Molecular Mass of Solute 1. In Part III. Do not forget this step. Record in your laboratory notebook the number or letter of the unknown solute you use. Using the average freezing point of the cyclohexane. You may need to refresh your salt-ice-water bath. Clean-Up: After the data has been collected. DATA ANALYSIS Parts I & II 1. you will design an experiment to determine the molecular mass of an unknown substance. You will need your solute number or letter for the laboratory write up. 6. The larger test tube should not need cleaning. 4. metal stirrer.Part III. The sample will have to be frozen and melted three or more times until you obtain good precision. 2. pour the melted mixture into the appropriate waste bottle in the fume hood. 3. Furthermore. calculate the Kf of cyclohexane for each trial performed in Part II. since different solutes will require different masses. Explain why salt is added to the ice-water bath in Part II. In calculating Kf you must make an assumption about p-dichlorobenzene. 7. 5. Carefully explain how this works 17 . Calculate the 90% confidence limit of your data collected in Part II. Calculate the standard deviation of the average Kf value.

Include some comments about the sources of error in the experiment that may be responsible for the difference between the values you have obtained and the accepted literature values for the properties you studied in this experiment. 12. calculate the freezing point depression. calculate the molecular mass of the unknown solute. 11. In calculating the molecular mass of the unidentified solute. for each trial. ∆Tf. For each trial. 10. Calculate the 90% confidence limit of your data collected in Part III. ∆Tf. Compose a summary of this experiment. Calculate the standard deviation of the average value.Part III 8. 13. you must make an assumption about the solute. Calculate an average molecular mass of the unknown solute. 18 . What is that assumption? 9. Conclusion. Using the freezing point depression.

We say that a chemical equilibrium is established in this reaction.0 M HF solution certainly does contain the hydrogen (or hydronium) ion and the fluoride ion. It is important to make good observations and carefully consider the results and how they relate to the equilibrium topics you are studying in lecture. This illustrates that chemical equilibrium is dynamic in that reactants are reacting to form products at the same time that products are reacting to form reactants. 19 . a 1. HF(aq) Note the symbol we use to indicate that the acid is not completely dissociated. you were exposed to reactions which essentially went to completion. Study the section on chemical equilibrium in your textbook. the equilibrium point can be established in either direction. That is. One of the important aspects of chemical equilibrium is that it can be established by either starting with reactants or products. all the reactants were converted to products. In fact. We might write this as: H+(aq) + F-(aq). and in all reactions which occur but which do not go essentially to completion.0 M in both the hydrogen ion (or hydronium ion) and the chloride ion. We might write this situation as: HCl(aq) → H+(aq) + Cl-(aq). While a 1. What would happen if you suddenly placed some additional reactant into a system at equilibrium? Clearly this would affect this dynamic balance and cause a change in the resulting chemical equilibrium position. An example of this type of reaction is when HCl is dissolved in water. Chemical equilibrium is thus often thought of as a point of chemical balance between the "reactants" and "products". when these types of experiments are done it is always observed that the equilibrium will shift in such a way to reduce the concentration of the added reactant. that is.Chemical Equilibrium INTRODUCTION In Chemistry 2A. Most reactions do not go to completion but instead stop at a chemical position in which both reactants and products are still present. This behavior was summarized by Henri Louis Le Chatelier in 1884 and is generally referred to as Le Chatelier's Principle: When a stress is applied to a chemical system at equilibrium. In this qualitative experiment you will be exposed to a number of different chemical systems that reach equilibrium and you will observe the effect of an added stress on each system. You know that hydrochloric acid not only dissolves in water but that it also essentially completely dissociates. That is. The analogous situation does not occur when the weak acid HF is dissolved in water. It is the dynamic competition between these two processes that allows the point of equilibrium to be established. or to "relieve the stress" of the added reactant.0 M HCl solution is often described as being 1. the equilibrium shifts in a direction that reduces the effect of the stress. it also contains a significant quantity of HF in solution.

Safety: Remember to wear gloves and use caution whenever handling acids and bases. Wear your goggles. Preparation for Next Lab 1) In preparation for the Strong Acid Titration Experiment, each student must obtain about 4.5 grams of potassium acid phthalate, KHP, in a vial and dry it o in an oven at 110 C for 2 hours. 2) Place the vial of KHP in a small, beaker to keep it from spilling. Label your beaker using a graphite pencil in the white frosted area. 3) Cover the beaker with a watch glass and place it in the oven. After two hours, remove your beaker from the oven. 4) While keeping the watch glass on top of the beaker, let it cool until it is warm but safe to handle. 5) Remove the watch glass and place the beaker containing the uncapped vial in a desiccator.

Work individually on this experiment. The questions for this experiment are integrated with the procedure. Write your answers to these questions in your laboratory notebook as you do the experimental procedure. PROCEDURE Part I. Equilibria of Complex Ions In this procedure, you will study the properties of a chemical system containing a complex ion. Many metal ions will bond with ions and molecules to form species called complex ions. An example of such a system is the combination of iron(III) ion with thiocyanate ion (SCN-). When these two species are mixed they establish an equilibrium in water which can be described as: Fe3+(aq) + SCN-(aq) (pale yellow) Fe(SCN)2+(aq) (deep red)

Thus, the system will change color depending on the quantity of the complex ion present. In this part of the experiment, you will observe the change in the equilibrium position by adding various chemicals. 1. Place 3 mL of 0.1 M KSCN into a 100 mL beaker. Add 3 mL of 0.1 M Fe(NO3)3. Now add 70-80 mL of water to dilute the solution and reduce the resulting color. Observe the color of the solution. Make sure that you can see through the solution; if the color is too dark you will have trouble noting color 20

changes as you proceed. You may continue to dilute the solution if it looks too dark. The volume given here is a general guideline. 2. 3. 4. 5. Place 5 mL of the resulting solution into 4 separate test tubes. To the first test tube add 1.0 mL of 0.1 M Fe(NO3)3 solution. Observe the color change. To the second test tube add 1.0 mL of 0.1 M KSCN solution. Observe the color change. To the third test tube slowly add 6 M NaOH solution drop wise. Observe any changes. You will notice two changes. The color change indicates a shift in the equilibrium, but why is there an equilibrium shift? You should address this in Question A below.

Clean-Up: All solutions can be discarded down the drain.

Question A: Compare the color of the solution in each of the four test tubes. Explain the color changes in terms of the equilibria described above and what you believe happened in Step 5. Part II. Equilibria of Acid/Base Indicators In this procedure, you will study the properties of two acid-base indicators, phenolphthalein and methyl orange. Many indicators are weak acids that establish equilibrium in water: HIn(aq) + H2O(l) H3O+(aq) + In-(aq) (color 1) (color 2) Thus, indicators can be thought of as dyes which change color depending on whether they are in a protonated (HIn) or unprotonated (In-) form. In this part of the experiment you will observe the change in the equilibrium position of the indicators by adding acids and bases to solutions that contain these indicators. 1. Place 3 mL of deionized water into six test tubes. Add two drops of phenolphthalein to three of the test tubes and two drops of methyl orange to the other three test tubes. Observe the color of the solutions. Add two drops of 6 M HCl to one test tube containing each indicator. Observe any color change. Add 4 drops of 6 M NaOH to another test tube containing each indicator. Observe any color change. 21

2. 3.

Question B: What are the colors of the protonated and unprotonated forms of phenolphthalein? Question C: What are the colors of the protonated and unprotonated forms of methyl orange? Question D: Write the equilibrium expression for each indicator as shown above for HIn. Be sure to indicate the color of each form. Use Hph for the protonated form of phenolphthalein and Hmo for the protonated form of methyl orange.

Clean-Up: All solutions may be discarded down the drain and the test tubes should be rinsed with deionized water.

Part III. Equilibria of Weak Acids and Bases In this procedure, you will study the equilibrium properties of weak acids and bases. As described in the chapter on acids and bases, weak acids and bases establish equilibrium with water. In this part you will study this concept by using an acetic acid/acetate ion equilibrium system and the ammonia/ammonium ion equilibrium system. The pertinent equilibria for each system are: HC2H3O2(aq) + H2O(l) NH3(aq) + H2O(l) H3O+(aq) + C2H3O2-(aq) NH4+(aq) + OH-(aq)

In this part of the experiment, you will observe the change in the equilibrium position through the use of the indicators used in Part I. Procedure for the acetic acid/acetate ion equilibrium 1. Place 3 mL of 0.1 M acetic acid into three test tubes. You will make this solution from 6 M stock solution. Add two drops of methyl orange to each test tube. Observe the color of the solutions. To one of these test tubes add 1.0 M NaC2H3O2 a few drops at a time and observe any color changes. Remember to mix the solution well after each addition. To another test tube, add 6M acetic acid a few drops at a time and observe any color changes. Again, mix well after each addition. Repeat this step with another sample to confirm your results.

2.

Question E: Explain your observations using both the equilibria presented above and the one involving the indicator. What color change did you observe? How is the acetic acid/acetate ion equilibrium affected by adding acetate ion? How does this change affect 22

you will again study the properties of a chemical system containing a complex ion. Thus. Mix well after each addition and note any color changes. add 6 M HCl a few drops at a time and observe any color changes. Question G: Explain your observations using both the equilibria presented above and the one involving the indicator.equilibrium? Procedure for the ammonia/ammonium ion equilibrium 3. Add two drops of phenolphthalein indicator to each tube. Temperature Effects on Equilibria In this procedure. To another test tube containing ammonium hydroxide. Observe the color of the solutions. 4.the concentration of H3O+? How does the change the concentration of H3O+ affect the Hmo/mo. Place 3 mL of 0. the system will change color depending on whether heat is added or removed from the system. Remember to mix the solution well after each addition. 23 . Add more 6M ammonium hydroxide to the test tube a few drops at a time.1 M ammonium hydroxide into the other three test tubes. Clean-Up: All solutions can be discarded down the drain. In other words. To one of these test tubes add 1 M NH4Cl a few drops at a time and observe any color changes. Remember to mix the solution well after each addition. 5. You will need to share your hot plate. as the reaction occurs from left to right the system gives off energy in the form of heat. Use a hot plate to heat a beaker of water to boiling. Part IV. The system in this study of the temperature effects on equilibria can be described as: CoCl42-(aq) + 6 H2O(l) (blue) Co(H2O)62+(aq) + 4 Cl-(aq) + heat (red-pink) You will note that "heat" has been shown to be a "product" of the reaction as it is read from left to right. You will make this from 6 M stock solution. Question F: Explain your observations using both the equilibria presented above and the one involving the indicator. In this part of the experiment you will observe the change in the equilibrium position by adding and removing heat. 1.

Place the test tube into a beaker of boiling water until it turns blue.1 M CaCl2 with 4 mL of deionized water in a small beaker. Add 6 drops of 0. dilute the cobalt solution a little. Add 12 drops of 0. C2O42-(aq). 3.2. if you wanted to precipitate the calcium with oxalate. 3. Observe the results. Pull out one of the test tubes and allow it to cool to room temperature. oxalic acid. Slowly immerse this test tube into another beaker containing a water-ice mixture. Why? 24 . would you want the solution to be basic or acidic based on the equilibria described above? Take a guess! Now let's see if you are right.5 M H2C2O4 solution to one of the other test tubes containing calcium chloride. and the weak diprotic acid. 2. For example. The equilibria in water that are important can be described as: Ca2+(aq) + C2O42-(aq) H2C2O4(aq) + H2O(l) HC2O4-(aq) + H2O(l) CaC2O4(s) H3O+(aq) + HC2O4-(aq) H3O+(aq) + C2O42-(aq) Clearly. H2C2O4(aq). However. 1. you will study the properties of two chemical systems involving the oxalate anion. Question H: Explain the color changes in terms of the equilibria described above. Equilibria of Precipitation Reactions In this procedure. Observe the results. this is a more complex system than we have thus far encountered. The chemical sources of the oxalate ion are calcium oxalate. Clean-Up: fumehood.25 M Na2C2O4 solution to one of the test tubes containing calcium chloride. we should be able to qualitatively understand the system. Place 3 mL of saturated solution of cobalt chloride solution into two test tubes. This system is particularly interesting because 3 simultaneous equilibria occur in water. Mix 4 mL of 0. Question I: Even though you added the same stoichiometric amount of oxalate ion to these test tubes you have observed differing amounts of precipitate. reheat it and try again. Observe the color change. Split the resulting solution into three approximately equal portions in three separate test tubes. CaC2O4(s). Place the solution into the metal ion waste container located in the Part V. If you have trouble seeing the color change. Observe the color change.

Observe the results. 25 . 6.4. Likewise. discuss how product concentrations change as equilibrium reactions shift to the left and the right. Clean-Up: All solutions from this part may be washed down the drain. Now slowly add 20 drops of 6 M NH4OH to this test tube until a change occurs. Discuss how your observations illustrated LeChatelier's principle. Discuss how reactant concentrations change as equilibrium reactions shift to the left or the right. Observe the results. Explain using your observations in part V if you would prepare a calcium oxalate precipitate in acidic or basic solution. Question K: Explain the results in terms the equilibria discussed above. Question L: Do you believe the precipitate is calcium oxalate or calcium hydroxide? Explain. Now add 10 drops of 6 M HCl to the solution of calcium chloride and oxalic acid. 5. This can be checked by adding 20 drops of 6 M NH4OH to the solution in the last remaining test tube containing calcium chloride. Question J: Explain the results in terms the equilibria discussed above. You may wonder if the precipitate in Step 5 is really an oxalate or a hydroxide precipitate. Concluding Remarks: Briefly discuss interpretations of your observations and results.

26 .

Note that the equivalence point is slightly different from the endpoint of a titration. This does not always correspond to the equivalence point. you will be utilizing the strong acid. or vice versa. 27 . using the titration skills learned in the earlier parts of this lab.(aq) 2H2O (l) (1) An acid is considered to be strong if it completely ionizes in water. it will slowly rise and level off as an excess amount of base is added. an acid raises the concentration of hydrogen ion. A titration curve is simply a plot of the pH of an acid versus the volume of base added. HCl (aq) + NaOH (aq) NaCl (aq) + H2O (l) (2) The progression of the reaction will be observed using a pH meter and a titration curve will be created using the experimental data. to neutralize the strong base. OH. We start with an exploration of the classic acid-base reaction. hydrochloric acid. In this lab. The titration curve gives a good description of how an acid-base reaction proceeds. According to the Arrhenius concept. Then as the solution becomes more basic. NaOH. The endpoint is when the indicator changes color. In this experiment you will be analyzing the neutralization between a strong acid and a strong base. The pH will start out low and acidic. H+(aq) + OH. The solutions you prepare in the strong acid-strong base experiment will be used as standardized solutions when you explore the additional complexities of a weak-acid titration curve experiment and the titration of a polyprotic acid experiment. As pre-laboratory preparation it is critical that you review the ideas on strong acidstrong base titration presented in your textbook. You will start with a sample containing only the acid and indicator and slowly add your standardized base. When reacted together the acid and base will neutralize each other according to the net ionic equation (1). then increase as it approaches the equivalence point.Strong Acid . sodium hydroxide. H+ while a base increases the hydroxide ion. where the concentration of acid equals that of the base.concentration.Strong Base Titration INTRODUCTION This experiment and the next three permit you to explore most of the important aspects of acid-base chemistry. according to the neutralization reaction below. when dissolved in water. that of a strong acid with a strong base. HCl. Buffers constructed to exploit a property of the weak-acid titration curve are then explored in the fourth of these related experiments.

The actual data analyses and the written reports must be done entirely independently of your lab partner or other students. mass the container and the material from which you are going to draw your sample. You will need to calculate and accurately measure out the volume of 6. Calculate the mass removed. Cap and shake the bottle to mix thoroughly and then fill the remainder of the bottle with water. First.2 M HCl. use a polyethylene dropper to dispense it into a 25 mL graduated cylinder. adding each rinsing to the plastic bottle. You will also use a technique called weighing by difference. rinse the graduated cylinder several times with deionized water.Safety: Remember to wear gloves and use caution whenever handling acids and bases. You will need to calculate the volume of 6M NaOH required in this dilution. and then pour the contents of the graduated cylinder into the partially filled plastic bottle. Part II. potassium acid phthalate.2 M HCl.15 M sodium hydroxide solution by diluting the stock solution of 6 M NaOH. Cap the plastic bottle and shake well. invert the bottle at least 30 times in order to completely mix the solution. KHP. and repeat the process until you have removed the mass desired. Weighing by difference is quite simple. Label this bottle 0. For 28 . All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs.15 M NaOH. 1. WEAR YOUR GOGGLES! Work in pairs throughout this laboratory assignment. 2. This is a very important technique to use because it eliminates systematic errors from the balance. Then remove some of the material and place it in a separate container. Calculate the appropriate volume of stock solution. Again. Add the necessary amount of acid to the plastic bottle.0 M HCl needed to make 1 L of 0. Standardizing the base against Potassium Acid Phthalate In this step of the experiment you will standardize your sodium hydroxide solution against the primary standard. Take the second 1 L plastic bottle and label it as 0. Preparing your Solutions You will prepare about 1 L of approximately 0. Clean your graduated cylinder before using it to measure the HCl. Then add the remaining volume of water to bring the total volume to about 1 L. mixing the bottle contents thoroughly. Screw the cap on the plastic bottle and mix the contents thoroughly by inverting the bottle and swirling it repeatedly. Make sure that you avoid unauthorized collaboration and plagiarism. Remeasure the mass of the original container and the remaining material. Rinse the graduated cylinder out with fresh water at least twice. adding the rinsing to the contents of the plastic bottle. Each student must collect data and submit a separate report. Fill it with about 200 mL of deionized water. PROCEDURE Part I. The bottle should be shaken at least 30 times after the last addition. Begin by pouring about 200 mL of deionized water into your (clean) plastic bottle.

and then add water to a total of about 35 mL to each of the four flasks and swirl them gently until the solids dissolve. Holding your buret below eye level. Be careful not to leave drops of the solution on the sidewalls of the flask. Pay attention to the region where the two solutions mix 29 2. Hold the buret at a low enough level that you can safely pour in the needed volume of solution using a funnel. After conditioning. use a folded paper strip to handle the vial. In a previous laboratory period you will have obtained about 6 grams of primarystandard grade potassium acid phthalate (KHP) in a vial. Add three drops of phenolphthalein indicator and a stir bar to the first KHP solution. Using the appearance of this sample as a guide. 3. Do not waste time trying to hit 0.2 gram sample of dry KHP on to a weighing boat. fill the buret with 50 ml of the standardized NaOH. Quantitatively transfer the first sample from the weighing boat into another 500 mL Erlenmeyer flask with the help of a small stream of water from your wash bottle. Add three drops of phenolphthalein indicator to another KHP sample and swirl. Use a laboratory tissue and make one quick stroke downward beginning at the stopcock and ending in the air beyond the buret tip. go a few drops below the zero mark and read and record the actual starting point to the nearest 0. If the masses of KHP are approximately the same then the endpoint of each sample will occur at approximately the same volume. The stir motor control knob is on the left. this will keep oils from your hands from changing the mass of the vial. In what follows. condition and fill a 50 mL buret with the NaOH solution you prepared in Part I and which you will now standardize. Place the flask onto the stir plate underneath the buret and turn on the stirrer and slowly increase the stirring speed. dry 125 or 250 mL Erlenmeyer flasks. 6. Be sure always to wipe off the tip of a buret before you begin a titration. Now you are ready to titrate. pausing every few milliliters to allow the solution to mix thoroughly. . Turn on the stirrer and slowly increase the stirring speed and lower the buret into the flask. 1. dried it in an oven at 110°C for 2 hours. leave the heat control knob turned off. Perform a cursory titration using the KHP sample in the 500 mL Erlenmeyer flask to determine the approximate endpoint of the titration. Please note that the stir plates also have a heat control knob that you will not need and must not use in this experiment. Remember when filling a buret to make sure the stopcock is closed. initially add the titrant fairly rapidly. After you have reached your endpoint for your cursory titration record the buret reading at the endpoint and calculate the volume of NaOH needed to reach the endpoint. 4.02 mL. refill your buret and record the initial buret reading to the nearest 0. be sure to use the same balance so that systematic errors in the balance will continue to be eliminated when you take the difference readings between masses. Rather.00 with the meniscus. Lower the buret tip well into the Erlenmeyer flask.0-1. With the technique described in the Common Laboratory Procedures section of this manual. Accurately weigh a 1. 5. Clean and dry your stir bar for your second titration and gently place it in the flask containing your sample. From your cursory titration you know the approximate position of the endpoint. and stored it in a desiccator for use today. accurately weigh three more such samples by difference into clean.preparation of all additional samples.02 mL.

After completing the experiment. You should throw out the data from the first cursory titration since this titration was performed quickly.00 buffer in three different test tubes. reduce the next amount of titrant added. Standardize the pH meter using the three buffer solutions following the procedure outlined in the Appendix. STORE THE ELECTRODE IN THE STORAGE SOLUTION provided. Treat both pieces of equipment with great care. If it does. Be prepared to stop adding titrant about 1 mL short of this volume. You may wish to record the buret volume of several successive drops as you approach the endpoint in case you discover that you have overshot the endpoint. Always keep the pH electrode in a beaker of tap water or a container of pH 7. 7. then closing the stopcock and washing this ½ drop into the flask. You should frequently wash down the interior sides of the flask to recover any reagent drops that may be clinging to the sides. pH Meter Operating Instructions.00 buffer solution. The pH meter and the accompanying electrode are both very expensive and fragile.and as the indicator color begins to tail out into the solution as you stir. keeping in mind the target volume.2 M HCl solution and 2) to demonstrate the classic titration curve of acid-base chemistry. Additional storage solution is provided in the laboratory if needed. 1. The information you generate in this part of the experiment has two goals: 1) to standardize the approximately 0. You will be doing the titration procedure at least twice. and then resume adding base from the buret but now dropwise. Part III.02 mL. The pH meter will need to be calibrated before starting the experiment. 8. Gently wash down the walls of the flask with water from your wash bottle. Calculate this ratio for your three latter titrations and determine if one of them fails the Q-test.00. and pH 10. When you have three samples that can be retained. It should be clear to you that the ratio of the NaOH titration volume to the mass of KHP being titrated should be a constant. Be careful of the electrode when adding strong base or when stirring the solution. pH 7. Record the final buret reading to the nearest 0. run another sample. 30 . the pink color will increasingly linger. you may begin Part III. Refill the buret and similarly titrate the remaining two KHP samples. As you approach the endpoint. There is no need to recalibrate later during the experiment. The first titration will familiarize you with the critical pH and volumes for your specific solutions’ concentrations after which you may adjust your technique to more accurately locate the endpoint for the specific solutions you are using. Pause after the addition of each drop or ½ drop to allow the solution to mix. A ½ drop may be added by slowly opening the stopcock until a ½ drop forms at the tip. Stop adding base when the entire flask has a faint pink color that persists. When rinsing the electrode use a light stream of deionized water. Place 3 to 4 mL of pH 4. Strong acid-Strong base Titration Curve This part of the experiment requires the use of a pH meter to measure the pH of various solutions. Follow the directions provided very carefully.00.

DO NOT use your wash bottle to rinse down the sides of the beaker as any added volume will change the pH readings and invalidate the titration curve data being collected. You will follow the course of the acid neutralization reaction by monitoring the pH with the pH meter.00 mL volumetric pipet to quantitatively transfer 10.5. With your first sample. The clearances of all this assembly are rather close. Stop the titration when you have reached pH > 11. Allow time for the reaction vessel to become equilibrated and for the pH reading to become stabilized and then record the pH value in your notebook alongside the buret reading. clamp the pH electrode in place below the level of the liquid in the beaker and away from the stir bar. Leave an empty column between the buret reading and the pH in which to place the volume of NaOH added (difference between present buret reading and initial buret reading). Use the previously conditioned buret from Part II filled with the approximately 0. Without measuring precisely. Stop the titration when you have reached pH > 11. For your second titration. Do NOT turn on the heat. You will probably need to position the beaker so that the stir bar is somewhat displaced away from the center of the beaker to allow room for the pH electrode but make sure that the stir bar is above the center of the stir plate. You will now standardize the HCl solution by titrating it with this NaOH solution. Place a magnetic stir plate under a buret clamp that is adjacent to the pH meter you have just standardized near your work area and place the beaker on the stir plate. then 0. add about 40 mL of deionized water to this beaker. For each pH reading. refine your procedure based on your first titration by adding 1 drop of NaOH at a time from well below the endpoint to well above the endpoint. 4. Also adjust the position of the buret tip so that it is inside the beaker. Record your buret readings after the addition of each increment. Using your extension clamp. Record your buret readings after the addition of each increment. . after that add 1 mL increments until pH 11.5. Set up your second titration by repeating step 2.2. Allow time for the reaction vessel to become equilibrated and for the pH reading to become stabilized and then record the pH value in your notebook alongside the buret reading. 31 3.2 M HCl solution you prepared in Part I into a 250 mL beaker.5. away from the side but with the stopcock at a convenient location for you to manipulate.15 M NaOH solution that you standardized in Part II and clamp it in place above the beaker.5. do a quick titration by adding 1 mL increments until you reach pH 2. convert your buret readings to volumes of NaOH added. Examine this data and determine between which volumes the largest change in pH occurs.7. When assembly is complete. The NaOH volumes at both ends of the largest pH change bracket the endpoint. moderate speed and clears the pH electrode. Use your 10.10 mL (2 drops) increments until you reach pH 10. Leave an empty column between the buret reading and the pH in which to place the volume of NaOH added. turn on the stir motor (left knob) slowly so that the stir bar is rotating at a smooth. 5. Repeat the titration procedure as time allows so that you have as many trials as possible to improve the statistics of your standardization of HCl. Place a magnetic stir bar into the beaker gently so no reagent splashes.00 mL of the approximately 0.

NOTE: KHP has the actual chemical formula KHC8H4O4. Carefully clean the buret by rinsing it with a few mL of acetic acid followed by several rinsings with deionized water. How many trials did you perform to determine the titration curve for the neutralization of HCl by NaOH? 8.15 M NaOH? This should be the same volume of 6 M NaOH you used in part I. Calculate the volume of 6 M HCl stock solution required to prepare the 1L of 0. volume of added NaOH solution. 4. Clean-Up: Pour the contents of the beaker and the remaining solution in the buret down the drain. Part III 7.0 L bottles containing your standardized solutions. Calculate the standard deviation of the average molarity of NaOH solution. Calculate the volume of 6 M NaOH stock solution needed to prepare the 1L of 0.23. Rinse all remaining glassware with deionized water. 6. Save both of the 1. Calculate the 90% confidence interval for the reported molarity. Use a spreadsheet program such as Excel to enter your titration data and make your titration curves by plotting pH vs. for subsequent experiments. Calculate the molarity of the NaOH solution as determined by the titration for each of the three acceptable trials. Part II 3. Tightly cap and store the bottles containing the standardized NaOH and HCl solutions for use in later experiments.6.2 M HCl? This should be the same volume of 6 M HCl you used in part I. rinsing with copious amounts of water. 2. Calculate the average molarity of the NaOH solution. Leave four empty columns to the right of each curve for developing the derivative curves in 32 . 5. Enter the volume of NaOH as a column headed V and the pH as an adjacent column headed pH. DATA ANALYSIS Part I 1. formula mass = 204.

pH(1). can help you identify this volume. Head these columns with the labels Vm. Likewise in the next column enter the formula for the volume midway between Vm(i) and Vm(i+1) given by. 33 . V(2). which we will approximate by calculating and plotting forward divided difference curves. Make sure you use the type of plot that will accept both a randomly spaced x value and a corresponding y value. use your spreadsheet program to calculate the forward divided difference approximation to the first derivative (rate of change) of the titration curve and the second forward divided difference approximation to the second derivative (rate of change of the rate of change) of the titration curve. These first and second derivative plots. Vm(i) = (V(i) + V(i+1))/2 The forward divided difference approximation for a series of data points of the type pH(i). enter the formula that will calculate the volume midway between V(i) and V(i+1). perhaps more precisely than you can from the direct plot of pH vs. A property of the equivalence point of an acid-base titration curve is that it is the volume at which the rate of change of pH is greatest (the first derivative reaches a maximum). Following the directions below. What is your best estimate of the volume of NaOH at the endpoint for each of your titration curves based on this plot? 9. In the column immediately to the right of the pH values. The column then is the forward divided difference approximation to the derivative. It is also that volume at which there is an inflection point in the curve (the second derivative will change sign). Here i is one of the data points and i+1 is the next data point in the sequence. NaOH volume. D1. Use this plot to estimate the position of the endpoint (that volume of NaOH which is midway between the two nearly linear asymptotic regions at low pH and at high pH). and V(1) to calculate this forward difference for the first data point in the sequence in a column adjacent to the pH of the first point.question 9. Vd. This formula may then be copied down the column and the spreadsheet will update the references to the correct cells for the pH and Volume for each row automatically. enter the formula for D1. It is easy to set up a formula by referencing the data in the cells for pH(2). Notice that you will not be able to calculate a forward difference for the last row of the data since there are no data values beyond the last row to use for pH(N+1) or V(N+1). Use the plot wizard to create a plot from the first two columns. and D2. Sample data and plots are shown below. The first forward divided difference best represents the derivative or rate of change of the titration curve at the volume midway between volumes V(i) and V(i+1). V(i) is given by: D1(i) = [pH(i+1) – pH(i)]/[V(i+1) – V(i)] In the column to the right of Vm. Such plots are called scatter plots in commonly used spreadsheet programs.

Vm. 0. calculate the molarity of your HCl solution for each trial to four significant figures.02 mL i. Conclusion. 34 . title and label the vertical and horizontal axes. although they will vary because your data will be different from this. 11. The graphs are based on dummy data. The forward divided difference expressions do tend to amplify experimental error (commonly called noise).e. 12.46 mL. the titration curves. what is your best estimate of the equivalence point volume of NaOH for each of your titration curves? You should be able to make this estimate to within 0. of the titration curve. i. Think about the standardization of NaOH. and the standardization of your HCl solution. the forward divided difference approximation (derivative) treatment of the data. You will find some plots at the end of this section of the laboratory manual that work up the first and second forward divided difference plots for some old titration data. These approximations to the first and second derivative illustrate the properties. 32. Your graphs should have the same main features as the following graphs. Your plots should look similar.2314 M HCl. Compose a summary paragraph that describes today’s experiment and your understanding of acid-base neutralization reactions. Vd. Print copies of all your graphs and turn them in to your teaching assistant. Sample Data and Plots Some sample graphs of the first and second derivatives of curves have been provided. Keep the average values of your standardized NaOH and HCl solutions in a prominent place in your notebook and perhaps write the value on the bottle labels.e. and then again to plot the second forward divided difference (D2) vs. Clearly. mentioned above. but your data should be good enough that these plots of the forward divided differences can help you to identify the equivalence point. Using the average molarity of your NaOH solution from Part II. A graph of the titration curve and of the first and second derivative curves of this data have been provided.Vd(i) = (Vm(i) + Vm(i+1))/2 Then in the next and final column to the right. and the equivalence point volume of NaOH determined from the derivative plots. Make sure your name is on each of the graphs. Using the combined representations of the titration curves developed in questions 8 and 9. You can see what the expressions do to the data. You will need these values in subsequent experiments. Calculate the average molarity of your HCl solution. 10. enter the formula for the second forward divided difference approximation to the second derivative (rate of change of the rate of change) D2(i) = [D1(i+1)-D1(i)]/[Vm(i+1) – Vm(i)] Invoke the plot wizard to plot the first forward divided difference (D1) vs.

NaOH Volume (D1 vs. When this plot is made the equivalence point is the value of the volume for which the plot passes through the x-axis. The second derivative plot (D2 vs. When the first derivative vs. 35 . the equivalence point shows up as a large spike on the graph. there is some room for error in estimating the precise volume for the equivalence point. It is because of this difficulty in estimating the equivalence point that the two "derivative" curves are plotted. As you can see.The first curve is just the titration curve. Vm) is plotted. It is based on the data presented on the following page. Both curves are useful in more accurately determining the equivalence point of titrations. In this curve. Vd) is also made for convenience. a strikingly different curve is the result. The equivalence point of the titration is the maximum point on this curve.

00 -0.70 2.07 0.80 19.00 pH level 8.00 -0.39 26.00 5.00 0.40 4 19.15 2.00 10.00 2.50 15.00 16.00 -0.35 0.50 6.80 -208 19.91 11.00 Volume of NaOH added 36 .04 0.62 4.50 28.55 19.00 0.90 3.20 19.56 11.00 28.61 11.78 3.50 2.00 0.50 21.68 11.77 Vm 7.50 2.75 19.50 27.20 3 19.00 25.08 0.11 23.15 19.19 0.04 18.00 30.08 24.90 0.50 16.20 0.11 -0.31 11.00 25.70 -54 19.11 3.00 pH 1.00 22.50 19.50 22.00 -0.87 2.03 1.13 0.04 28.01 Titration Curve (pH vs.35 19.00 24.46 25.90 20.74 0.00 10.02 16.80 2.33 9.00 15.00 19.60 19.00 12.57 11.60 11.50 12.00 0.65455 21.50 26.00 20.10 M NaOH mL NaOH (Vol) 5.05 19.00 21.65 19.37 3.00 35.50 19.00 0.00 0.16 3.60 247 19.10 -17 19.00 -0.00 29.40 19.20 30.63 2.25 19.00 26.10 19.50 23.95 20.04 27.00 15.44 22.50 25.88 10.1 18.70 19.10 2.20 0.23 -2.72 11.04 0.30 19.30 0.50 18.35 10.04 17.00 -0.00 18.30 16 19.00 23.TITRATION EXAMPLE: Titration of 30 mL HCl with 0.07 0.90 25.05 Vd D2 10.50 D1 0.24 7.85 19.80 11.45 19.0052 14.50 4.00 27.00 0.50 37 19.50 24.00 -0.17 0.00 6.09 3.00 17.4 19. vol of NaOH) 14.90 -25 20.00 19.50 17.00 4.00 10.04 0.00 0.93 2.

the species present are the associated species. and H2O. the anion A-. The species present are H3O+. Note that double arrows pointing in opposite directions are used in the chemical equation since this reaction does not go to completion but instead reaches equilibrium.is also considered to be a Brønsted-Lowry base since it can accept a proton. H3O+. we can write an equilibrium constant expression as shown below Ka = [H3O+] [A-] [HA] (3) The equilibrium constant. the associated species. and the chloride ion. Ka.Acid Dissociation Constants and the Titration of a Weak Acid One of the most important applications of equilibria is the chemistry of acids and bases. Cl-. Cl. and H2O. HA and A. In an aqueous solution of HCl. does not exist. The species A. in this reaction HA is the Brønsted-Lowry acid and H2O is the Brønsted-Lowry base. then the equilibrium reaction of a weak acid with water is represented by HA(aq) + H2O(l) H3O+(aq) + A-(aq) (2) Similarly. H+. HCl. H2O and H3O+ also constitute a conjugate acid-base pair where H3O+ is the conjugate acid of H2O. a single-headed arrow pointing to the right is used in the chemical equation. is called the acid dissociation constant. the hydronium ion.as shown by HCl(aq) + H2O(l) → H3O+(aq) + Cl-(aq) (1) In this reaction. Unlike strong acids. HA. If we let HA symbolize a weak acid. Since this reaction essentially goes to completion. In an aqueous solution of HA. In the case of an aqueous solution of a strong acid. Since equation (2) is an equilibrium reaction. such as HCl. The Brønsted-Lowry acid-base theory defines an acid as a species that donates a proton and a base as a species that accepts a proton. Recall that water is not included in the equilibrium constant expression since it appears in the reaction as the 37 . HCl is the Brønsted-Lowry acid and H2O is the Brønsted-Lowry base. formed when HA donates its proton. H3O+. Likewise. The species that make up a conjugate acid-base pair only differ in structure by the presence of a single proton. aqueous solutions of weak acids do not completely dissociate into the hydronium ion and the corresponding anion but instead reach equilibrium.are also referred to as a conjugate acid-base pair where HA is the acid and Ais its conjugate base. the acid reacts completely with the water and dissociates into the hydronium ion.

For example.0 x 10-14.2 x 10-4 and 4. [H3O+] = [A-] and [H3O+] represents the concentration of HA that is lost in the dissociation. H3O+(aq) + A-(aq) HA(aq) + H2O(l) (2) The assumption here is that the amount of hydronium ion resulting from the dissociation of water H2O(l) + H2O(l) H3O+(aq) + OH-(aq) (6) is very small relative to the other sources of hydronium and can be neglected. Once the initial concentration of HA is known. Therefore. at 25°C for this reaction is equal to 1.pure liquid. to a greater extent than does HCN.1 M HCN then the hydronium ion concentration would be higher in the bottle of HF than in the bottle of HCN and. The magnitude of the dissociation constant provides information regarding the degree of dissociation of the acid in water. then the equilibrium 38 . HCN(aq) + H2O(l) H3O+(aq) + CN-(aq) (5) In other words. when a weak acid is titrated with a strong base the equivalence point does not occur at neutral pH. This is a good assumption since the equilibrium constant. If we had a bottle of 0. Furthermore. the pH would be lower in the bottle of HF. the pH then corresponds to the [H3O+] as a result of the dissociation reaction represented by equation (2). Kw. one mole of A. The larger Ka value of HF indicates that the equilibrium reaction between HF and H2O HF(aq) + H2O(l) H3O+(aq) + F-(aq) (4) lies further to the right then the equilibrium reaction between HCN and H2O shown below. and its conjugate base. the concentration of the hydronium ion can be assumed to originate only from the dissociation of the weak acid. You will also find other significant differences between the two titration curves due to equilibrium reactions. therefore. at equilibrium. HF dissociates into hydronium ion. Before any strong base is added to the weak acid. HA. F-. when a strong acid is titrated with a strong base. However. the pH changes that take place when titrating a weak acid with a strong base are significantly different than the pH changes that take place when titrating a strong acid with a strong base. Due to the establishment of equilibrium between a weak acid and its conjugate base in an aqueous medium.1 M HF and a bottle of 0. Let us consider in more detail how pH will change when small amounts of strong base are added to an aqueous solution of a weak acid. respectively. the titration curve of a weak acid has a slightly different shape than the titration curve of a strong acid. H3O+.is produced and one mole of HA dissociates. For example. the Ka values for HF and HCN are 7.0 x 10-10. As a result. for every mole of H3O+ that forms. Therefore. the equivalence point is found to occur at pH = 7.

the only species present will be the conjugate base. divided by the total volume of the mixture. shown by equation (2). other than the equivalence point. HA.concentrations of H3O+. [HA] then is calculated by dividing the number of leftover moles of HA by the total volume of the mixture at this point in the titration. we obtain Ka = [H3O+] and taking the negative log of each side. the Ka value of the weak acid from a measured pH value. A-. then the number of moles of leftover HA will be equal to the original number of moles HA minus the number of moles of OH-. assuming that any [H3O+] formed from the dissociation of water is negligible. Applying this to equation (3). Like HA. Another point of interest. As base is added. as well as. remaining in the solution and thus. and HA can be calculated. At the midpoint. the OH. A-. HA(aq) + OH-(aq) → H2O(aq) + A-(aq) (7) This reaction can be assumed to go to completion followed by the re-establishment of the dissociation equilibrium: HA(aq) + H2O(l) H3O+(aq) + A-(aq) (2) If the equivalence point has not been reached. Therefore. to produce more conjugate base. that has been added.is a conjugate base.produced in the dissociation reaction is negligible. (Again. Since A. is negligible compared to the number of moles of leftover HA. HA. has reacted with all the strong base. the number of moles of A. The midpoint occurs when ½ of the original acid. is the midpoint. at the midpoint. [HA] = [A-]. on a weak acid titration curve. The moles of HA lost in the dissociation reaction. HA. it will accept a proton from water to reform HA and OH. [H3O+] is determined by the number of moles of H3O+ formed in the dissociation reaction and is simply measured by pH. just enough strong base has been added to completely react with all the weak acid. the number of moles of the conjugate base. the Ka of the weak acid can be easily calculated from the measured pH level.is equal to the number of moles of weak acid. A. At the equivalence point. After reaction. shown by equation (7). OH-.ion will react with the major species in solution.formed in the strong base reaction.) [A-] is equal to the number of moles of A.in the equilibrium reaction shown by: A (aq) + H2O(l) The equilibrium constant expression is given by: Kb = [HA] [OH-] [A-] 39 (9) - HA(aq) + OH-(aq) (8) . A-. the equality is expressed as pH = pKa.

OH-. you will use this information to calculate the concentration of the original weak acid solution. Ka of a weak acid and the Kb of the corresponding conjugate base are related to each other by the equilibrium constant. you can determine the concentrations of all three of the species in this equilibrium constant expression. with the strong base. Finally. The amount of OH. 40 .is the same as the concentration of HA. Ka. the excess base determines the pH of the solution. You will then plot all the pH measurements made in this experiment against the quantity of strong base added to form a pH titration curve. In this experiment. sodium hydroxide. acetic acid. Kw. will be in excess. Knowing the original amount of HA placed into the flask. and making the assumption that the concentration of the OH. Beyond the equivalence point in the titration. of acetic acid using several measured pH readings along the titration. Kb. you will be able to re-calculate the value of Ka for the weak acid. Here. You will calculate the acid dissociation constant.The equilibrium constant. the strong base. is called the base dissociation constant. After you find the volume of strong base needed to reach the equivalence point of the titration. measuring the pH. you will be titrating the weak acid. you should be able to calculate the concentration of A.in solution. Kw = KaKb (10) By subtraction. using the relationship shown by equation (10). You will also compare the titration curves of a strong acid titration and weak acid titration.formed from the equilibrium reaction shown by equation (8) is negligible.

let it cool until it is warm but safe to handle. 5) After the sample has cooled. 2) Place the uncapped vial in a beaker. Make sure that you avoid unauthorized collaboration and plagiarism.1 M acetic acid solution by diluting the stock solution of 6 M acetic acid. Weak Acid Strong Base Titration Curve This experiment requires the use of a pH meter to measure the pH of various solutions. you will prepare 200 ml of approximately 0. 4) After removing your sample from the oven. You will need to calculate the volume of stock solution required in this dilution. Do not adjust the temperature on the oven. You will need approximately 1 g of dry sodium carbonate. Do NOT use PAPER labels on your vials or beaker. Make sure that you label the vial! Part I. Be careful not to touch the vial with your fingers. Each student must collect data and submit a separate report. WEAR YOUR GOGGLES! PROCEDURE Work in pairs on this experiment. Cover the beaker with a watch glass. each pair of students needs to dry a sample of solid sodium carbonate. 1) Half fill one vial with pure sodium carbonate. Mix well Part II. The pH meter and the accompanying electrode are both very expensive and fragile. Preparing the Acetic Acid Solution In this step of the experiment. 3) Dry the sample in the oven for 1. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs Preparation for Next Lab Before starting the Weak Acid Titration experiment and in preparation for next week’s Polyprotic Acid experiment. The temperature on the oven has been preset and will heat to the correct temperature when the door remains closed. carefully place the beaker containing the uncapped vial in the desiccator until needed.5 hours. write your name on the white frosted area of the beaker and place it in the oven. The actual data analyses and the written reports must be done entirely independently of your lab partner or other students. Treat 41 . With a graphite pencil.Safety: Remember to always wear gloves when handling all acids and bases.

The pH meter will need to be calibrated before starting the experiment. store the electrode in the storage solution provided.e. 7.00 buffer in three different test tubes. add 3-5 drops of thymolphthalein indicator and without splashing. fill the buret to above the zero mark. 1. and pH 10. Dispense into a 150 mL beaker approximately 30. Follow the directions provided very carefully. Be sure to turn the correct knob. Condition a second buret with your dilute acetic acid solution. later. Turn the stir knob to a low setting until the magnetic field catches the stir bar and begins to spin it. place the buret in the clamp.e.00. pH 7. invert it several times to ensure that your solution is uniform. 3. Place 3 to 4 mL of pH 4.24 mL. carefully. use a funnel when pouring in your sodium hydroxide solution. carefully place a clean magnetic stir bar into the beaker. i. during the experiment. 0. Set up the stir plate underneath the buret containing the sodium hydroxide and place the beaker containing your dilute acetic acid solution onto the stir plate.Strong Base Titration. Titration Set up: 1. lower the buret so that the tip is just below the opening of the beaker.” Before opening the bottle of NaOH. 2. Find your 1L bottle of your standardized NaOH from the previous experiment. Always keep the pH electrode wet when not in use. Gradually increase the speed of the stir bar until it is smoothly stirring the solution. Remember when filling a buret to check that the stopcock is closed. Standardize the pH meter using the three buffer solutions following the procedure outlined in the Appendix. 5.00 mL of the dilute acetic acid solution. there should be no need to recalibrate. While holding the buret at a safe level. Record the initial buret reading to two decimal places.00.both pieces of equipment with great care. When rinsing the electrode. “Strong Acid . pH Meter Operating Instructions. These stir plates also have a knob for heating. 6. Fill the buret with your dilute acetic acid solution. 4. To this solution. and dispel any air bubbles from the stopcock. 42 . Using your extension clamp to hold the pH electrode near the edge of the beaker so that it is submersed in the acetic acid solution but not touching the bottom of the beaker or interfering with the stir bar. After conditioning.02 ml. Record the initial buret reading to two decimal places. i. You may need to center the beaker on the stir plate in order to achieve smooth stirring. Take a 50 ml buret and condition it with your standardized NaOH solution. Record the precise volume to the nearest 0.58 mL. use a light stream of deionized water. Be careful of the electrode when adding strong base or when stirring the solution. After completing the experiment.

First. Allow the solution to mix and equilibrate. allow the solution to equilibrate and the pH to stabilize. Once you are within 2 mL of the estimated midpoint. Find the area of the graph where the change in pH is the greatest. graph a titration curve by plotting the pH level on the ordinate (y-axis) and the volume of NaOH added on the abscissa (x-axis). Carefully add approximately 1 mL of NaOH to the beaker. The Titration 9. Note any color changes that occur alongside your buret and pH readings in your notebook. Before adding any NaOH. Convert your buret readings to volumes of NaOH added. When the solution starts to turn faint blue make a note of the color change alongside the volume of sodium hydroxide added. Continue adding 1 mL increments of NaOH. record the pH of this mixture to two decimal places. 2.34. In your notebook. recording the buret reading and pH after each increment until you reach a pH > 11. Also. Consider the volumes of NaOH that bracket this region and estimate the volume of NaOH needed to reach the equivalence point. volume of NaOH added. 11. Record the pH after each 1 mL addition. begin the titration by adding 1 mL increments of NaOH until you are within 2 mL of the midpoint. 13. After recording the pH of the acetic acid solution. 2. Record the buret reading to two decimal places. in other words. After each addition. The equivalence point is in this region. 10. 12. i. you will need to estimate the equivalence point and the midpoint by graphing pH vs. allow the solution to equilibrate and the pH to stabilize. Do not use your wash bottle to rinse down the sides of the beaker at any time during this titration. Before doing your second titration. The next titration will be performed more precisely to accurately determine the midpoint and the equivalence point. recording the pH of the solution after each addition.e. The only volume changes that may take place must come from added HCl solution. measure and record the pH of the dilute acetic acid solution. i. estimate the volume of NaOH needed to reach the midpoint of the titration. Record the initial buret reading. add your NaOH 2 drops at a time until you are 2 mL beyond the midpoint.34 mL. After the pH meter has stabilized. Continue adding NaOH in 1 mL increments to the acid solution. you will do a quick titration to find the approximate endpoint. where the slope is the highest. After each addition. 43 . Refill your burets with the appropriate solutions and prepare another sample to be titrated following the same set up procedures as with the first titration.e. as the volume of water added during the wash would invalidate the pH readings.8. Record the buret reading and the pH after each 2-drop addition.

Pour down the drain with copious amounts of water. How many trials did you perform to determine the titration curve for the neutralization of HC2H3O2 by NaOH? 3. What volume of 6 M HC2H3O2 stock solution did you use to prepare the 1L of 0.1 M HC2H3O2? Show how you calculated this volume. Return to adding 1 mL increments of NaOH until you are within 2 mL of the endpoint. Using a spreadsheet program such as Excel. enter the volume of NaOH added and corresponding pH levels and plot the pH level on the ordinate (y-axis) and the volume of NaOH added on the abscissa (x-axis) to obtain a titration curve for each set of trial data. DATA ANALYSIS Part I 1. You should still have your 1L bottle of standardized HCl in your locker. Rinse all other glassware. allow the solution to equilibrate and the pH to stabilize. Record the buret reading and the pH after each 2-drop addition. at least one more time. any remaining NaOH solution that is in your 1L bottle. After each addition. rinsing with copious amounts of water. After each addition. At what pH. does the equivalence point occur for each of the graphs? How do the slopes of the titration curves compare? 44 . Save this solution for the Polyprotic Acid Experiment. Clean-Up: Pour the contents of the beaker and the remaining solutions in the buret down the drain. Use these plots to estimate the position of the equivalence point (that volume of NaOH which is midway between the two nearly linear asymptotic regions at low pH and at high pH). Record the buret reading and the pH after each 1 mL addition. Repeat Titration procedure. 16. Part II 2. allow the solution to equilibrate and the pH to stabilize. steps 11. After each addition.16.14. allow the solution to equilibrate and the pH to stabilize. 15. Return to adding 1 mL increments of NaOH until pH > 11. Compare and contrast the shape and trends of this titration curve to the strong acid-strong base titration curve. Record the buret reading and the pH after each 1 mL addition. When you are within 2 mL of the estimated endpoint. What is your best estimate of the volume of NaOH required to reach the equivalence point for each of your titration curves? 4. add your NaOH 2 drops at a time until you are 2 mL beyond the endpoint. Carefully clean the buret containing the NaOH by rinsing it with a few ml of acetic acid followed by several rinsings with deionized water. 17.

Using the combined representations of the derivative graphs developed in questions 4 and 5. NaOH volumes as you did in the previous laboratory report. Using the initial volume of acetic acid. Combine these data with the pH at the midpoint to calculate Ka for each trial. Clearly. 6.46 mL. Then calculate the average value of the molarity of your acetic acid solution and use this value in all subsequent calculations where the molarity of the acetic acid solution is required. calculate the Ka of acetic acid based on your calculated average molarity the initial volume of acetic acid. Then calculate the average value of Ka from the equivalence point determinations. 7.5. Print copies of all your graphs and turn them in to your TA. Average the value of the initial pH of your acetic acid solutions before any NaOH was added. estimate the volume of NaOH required to reach the equivalence point for each of your trials. calculate the volumes and the forward difference approximations for the first and second derivatives using each set of trial data. the equivalence point pH or the midpoint pH? 45 .02 mL i. 9. 10.For each trial. and calculate the Ka of acetic acid based on your calculated average molarity and the average pH of the acetic acid solution before any sodium hydroxide was added. You should be able to make this estimate to within 0. As instructed in questions 8 & 9 of the “Strong Acid-Strong Base Titration” experiment. Calculate the average Ka of acetic acid based on the pH at the midpoint from each of your trials. Which is larger? Which pH has the greater uncertainty. 32. and the pH of your acetic acid solution at the equivalence point. Make sure your name is on each of the graphs. volume is (pH(i) –pH(i-1))/(V(i) – V(i-1) . calculate the molarity of acetic acid you obtained in each of your trials. 11. 12. Find the pH of the midpoint for each of the trials using half the volume of NaOH required to reach the equivalence point for that trial. The rate of change of pH vs. Graph the approximations to the first and second derivatives vs. Use the sum of the initial volume and the volume of NaOH to reach the midpoint as the total solution volume at the midpoint. volume of NaOH at the equivalence point on the weak acid titration curve.e. volume of NaOH at the midpoint to the rate of change vs. the volume of NaOH at the equivalence point and the standardized molarity of your NaOH. Compare the rate of change of pH vs. the volume of NaOH required to reach the equivalence point. 8. title and label the vertical and horizontal axes.

and then compose a summary paragraph that describes today’s experiment and your new understanding of weak-acid titration reactions.1 M HC2H3O2? Explain. Calculate the concentrations of the acetic acid and the acetate ion at the midpoint. Which solution would have a higher pH.1 M HBr or 0. Conclusion Take a moment to reflect on the standardization of acetic acid and the titration curves. 0. At what volume of NaOH did the indicator change color? Does this agree with the volume of NaOH needed to reach the equivalence point? What does this suggest to you about the selection of an indicator for an acid-base titration? 15. How does the weak-acid titration curve differ from the strong-acid titration curve? 46 . 14.13.

We should note here that this buffering action can also be used to your benefit. it is corrosive and does react with metals to form carbonates. Ka1 = 7. and CO32-(aq) is critical for the proper transport of CO2. calculating the concentrations of the species present in a phosphoric acid solution can become quite involved. Carbonic acid is made by dissolving carbon dioxide CO2 in water. In this experiment. Polyprotic acids can generate very complex systems at equilibrium. H2O(l). through the blood stream to be expelled by the lungs. In this experiment. phosphoric acid undergoes three separate dissociations: H3PO4(aq) + H2O(l) H2PO4-(aq) + H2O(l) HPO42-(aq) + H2O(l) H2PO4-(aq) + H3O+(aq) HPO42-(aq) + H3O+(aq) PO43-(aq) + H3O+(aq) For example. In addition to the environmental presence of carbonic acid formed by dissolving the CO2 from the air into water or by acidifying waters that have percolated through formations containing carbonate minerals. This buffering action can make experiments more complicated.08 x 10-3 Ka2 = 6. all but sulfuric acid are monoprotic. carbonic acid H2CO3. For example. Some reactions take place only in a specific pH range. titration of the first endpoint that you encounter establishes a buffer solution that complicates the analysis and determination of Ka for that equivalence point. The equilibrium among CO2(g). detecting the formation of each of the two endpoints of the titration curve using a pH meter. acids that have more than one acidic proton.16 x 10-8 Ka3 = 4.Polyprotic Systems INTRODUCTION Until now you have dealt primarily with monoprotic acids such as hydrochloric and nitric acid in the laboratory. we will start with Na2CO3 and add acid. the carbonic acid system plays another major role in the respiration of all animals. Think about your list of strong acids. 47 . you will trace out the entire titration curve of the diprotic acid. formed in the metabolic cycle inside cells. While carbonic acid is not a strong acid by the dissociation definition. This leaves an entire world of polyprotic acids unexplored. One aspect of polyprotic acids that is different from monoprotic acids is that they always make buffer solutions. Polyprotic acids. HCO3-(aq). In the experiment you are about to perform. including humans.37 x 10-13 Each of these dissociations is an equilibrium reaction with an acid dissociation constant. You will be examining the nature of buffer solutions in the next experiment in the series on acid-base chemistry. and only the first proton of sulfuric acid is considered strong. Nevertheless. are common. you have worked with sulfuric acid and with KHP that comes from diprotic phthalic acid. salts of phosphoric acid are commonly used for the preparation of buffer solutions in biochemical studies. As a result. and buffers can be used to maintain this pH during an experiment.

It occurs at low pH. The dominant species equilibria to be considered are: HCO3HCO3+ + H2O H2O H2CO3 H3O+ + + OHCO32Kb2 = Kw/Ka1 Ka2 We start by writing down the two conditions that are commonly referred to as a mass balance and a charge balance. We then use the two equilibrium expressions listed above and the Kw equilibrium to re-express [H2CO3]. using the discussion as an aid to prove to yourself that the formulas are correct. the solution is identical in composition with a solution of the sodium salt of the bicarbonate ion HCO3. These two conditions are combined into an equality that must be observed. the equilibrium analysis necessary to develop the formulas for reduction of measurements of the pH into the acid dissociation constant are somewhat involved for the second proton equilibrium (the first equivalence point that you will encounter in the titration). but will just describe for you how to find the final formulas.4 x 10-7 We have written the acid dissociation reactions in the reverse of the usual direction to emphasize that we are starting from a solution of Na2CO3.7 x 10-11 Ka1 = 4. Because of the polyprotic nature of carbonic acid. The first proton (Ka1) is encountered as the second equivalence point in the titration. At the second proton equivalence point. The combined equality is then simplified and rearranged to get the result: [ H 3O ] = + K a 2 [ HCO3− ] + K w [ HCO3− ] 1+ K a1 48 . It occurs at high pH. [CO32-] .(except for some extra dissolved NaCl(aq)). We will not go through the details of the development. The mass balance sets the sum of all carbonate containing species equal to the total concentration in the original sample as diluted to the present volume.The important acid-base reactions for carbonate are: H+ + CO32H+ + HCO3HCO3H2CO3 → H2O + CO2(g) Ka2=4. You may want to go through the development on your own. An Equilibrium treatment of the pH of that solution will yield precisely the formulas we need to work with. Also notice that during the titration you will encounter the equivalence point of the second proton (Ka2) of diprotic carbonic acid as the first equivalence point in the titration. The charge balance sets the sum of the concentrations of all positively charged species equal to the sum of the concentrations of all the negatively charged species (including the sodium cation needed for NaHCO3). and [OH-] and insert these into the combined equality. One of the goals of this experiment will be to make your own determinations of the two acid dissociation constants of carbonic acid.

Further. the solution has had two equivalents of protons added to the analyte. Firstly. Consequently. it will be true that [HCO3-] >> Ka1 . K a2 [ H + ][ CO 3 ] = − [ H CO 3 ] 2− Rearranging these expressions: [ H + ][ H CO 3 ] [ H 2 CO 3 ] = K a1 Using substitution: − [ H + ][CO 3 ] . From the equilibrium at the second equivalence point we get the necessary additional information that enables the determination of both acid dissociation constants. the solution is then simply that of carbonic acid H2CO3 (with some extra NaCl in solution that does not affect the acid equilibria). H2CO3(aq) H CO3-(aq) H+(aq) H+(aq) + H CO3-(aq) + CO32-(aq) Ka1 Ka2 A fairly quick solution of these equilibria is available if Ka1 >> Ka2 because then we may assume that the [H+] concentration arises dominantly from the first equilibrium and then [H+] = [H CO3-] .While this formula looks difficult to work with. (1) While this does not give us either of the acid constants directly. [ H CO 3 ] = K a2 − 2− [ H + ]2 [ CO 3 ] [ H 2 CO 3 ] = K a1 K a 2 [ HCO 3 ] K a2 = K a2 Since [H ] = [H CO3 ] . we can use this relationship to determine the other. and solving for [CO3 ] = [H + ] + 2− 2− 49 . for convenient laboratory concentrations. the specific circumstances of the carbonic acid equivalence point simplify it greatly. At the second equivalence point. for those used in this experiment. if we know one of them. and specifically. so that Kw may be neglected in the numerator. it will also be the case that Ka2[HCO3-] >> Kw. For purposes of consideration of the pH equilibria. we may neglect the unity in the denominator. Writing the equilibrium constant expressions: K a1 [ H + ][ H CO 3 ] = [ H 2 CO 3 ] − . Canceling and simplifying then gives: [ H 3O + ] = K a1 K a 2 .

Once Ka1 is found. 50 . ___________________. g = grams of NaCO3 in the titrated sample. we can expect [H CO3-] + [CO32-] << M . Of course in both equations (1) and (2) [H+] = antilog10(-pH). we must have : [H CO3-] + [CO32-] + [H2 CO3] = M [H2 CO3] = M – { [H CO3-] + [CO32-] } Since we are dealing with weak acid dissociation constants. In preparation for the Acid-Base Buffer experiment. obtain your group number for your assigned pH values from your TA. the number of moles of sodium carbonate in the sample. hence [H2 CO3] = M Using the concentrations in the expression for Ka1 [ H + ]2 M + [ H ] = MK a1 K a1 = (2) In the titration. Write your Group number here. M = a/(V + v) . where a = g/105. equation (1) may be used to find Ka2.This reduces the expression for [H2CO3] to: [ H + ]2 [ H 2 CO 3 ] = K a1 Now in a solution that is M molar in H2 CO3. and v is the volume of HCl added to reach the second equivalence point in the titration. V is the original volume of water in which the sample was dissolved.99 .

recording the exact weight in your lab notebook. Handle the sample vial only with a strip of folded paper or with your crucible tongs so that your fingerprints do not produce spurious weighings. You will probably have to place the stir bar somewhat displaced from the center of the beaker so that it will not collide with the pH electrode. Make sure that you avoid unauthorized collaboration and plagiarism. Add a few drops of phenolphthalein indicator to each sample. 2. Standardize the pH meter using the three buffer solutions following the procedure outlined in the Appendix.Safety: Remember to always wear gloves when handling all acids and bases. 5. during the experiment. This should be dried for at least two hours in the oven in the laboratory room the period before you do this procedure.25 grams sodium carbonate by difference into each of three marked 100 mL. 0.15 . Each student must collect data and submit a separate report.197 g. later. Dissolve with 30 mL deionized water. there should be no need to recalibrate. Condition your 50 mL buret with a small amount of your standardized HCl solution saved from the experiment on “Strong acid strong base titration curve” and then properly fill the buret. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs.00 buffer in three different test tubes. Wear your goggles.00. 4. Assemble a stir plate under the buret clamp nearest the pH meter you are using. 1. Accurately weigh 0. put your filled buret into this clamp and put the beaker with the carbonate solution under the buret but atop the stir plate. The magnetic stir bars function using the stir option on the electric hotplates. 3. For this procedure. measured with a clean and conditioned buret.00. The pH meter will need to be calibrated before starting the experiment. pH Meter Operating Instructions. PROCEDURE Work in pairs throughout this experiment. you will need approximately 1 g of dry sodium carbonate. or 250 mL beakers. The volume of water in which you dissolve the sodium carbonate is the initial volume of analyte that was symbolized by V in the equations in the introduction. Record the volume of water as precisely as possible. Place 3 to 4 mL of pH 4.g. A magnetic stir bar will be used during the titration to continuously stir the solution.0. The actual data analyses and the written reports must be done entirely independently of your lab partner or other students. and pH 10. e. Position the buret tip inside the mouth of the beaker with the stopcock in a convenient position to be manipulated. 51 . Do not heat your sample. pH 7. 150 mL.

Take readings for every 1 mL increment until a pH of 9. Be sure to identify the sample and its mass at the top of the page when the titration curve data is copied. you may increase the increment to 1 mL again. 7. leaving a blank column between them to be filled in with the volume of HCl added (present buret reading minus initial buret reading). turn on the magnetic stir bar slowly and increase the setting gradually until you have it rotating at a moderate speed. Each partner needs to have performed all roles. reading the pH after each 1 mL increment addition until pH 5. take readings every 0. 8. so that you have a record of the pH range over which phenolphthalein changes color. Continue past the first endpoint using 0. Do not use your wash bottle to rinse down the sides of the beaker at any time during this titration as the volume of water added during the wash would invalidate the pH readings. When one complete titration is finished. When you have passed the first endpoint by 1 mL. taking readings on the pH meter with measured increments of added HCl solution. alongside the buret readings and pH readings. Titrate your Na2CO3 solution with the standardized HCl.1 mL increments until you have added an additional 1 mL of titrant. DATA ANALYSIS 52 . then record the buret reading and the pH in your notebook. Take notes of the color changes alongside your buret readings and pH readings so that you have a record of the pH range over which bromocresol green changes color. the partner who has been adding the HCl and reading the pH meter will need to copy the recorded data into her own notebook.10 mL (~ 2 drops) until a pH of 7 is reached. When the assembly is ready. Continue taking readings every 0.6 is reached. Then. You may find these general directions need to be slightly adjusted to improve the quality of data for your curve. The titration data is most efficiently collected if one partner is adding the HCl and reading the pH meter while the other records the data. You should modify your technique for the remaining two samples based on your experience with the first one. Add approximately 1 mL of HCl.10 mL until the color changes to yellow. for example by choosing a somewhat different specific pH at which to change the increment sizes. Record the color changes as they occur. Then take readings every 1 mL until another 6 increments of HCl solution have been added. 9. Then take readings every 0. give the system time to equilibrate and the pH meter time to stabilize.5. add a few drops of bromocresol green. The only volume changes that may take place must come from added HCl solution.10 ml until you are 2 mL past the endpoint. the solution should turn clear. During this time. Continue to titrate.6. Once the solution is clear. You will now repeat the titration for the remaining two samples and should exchange roles if you did not trade off during the first titration.

What are the three values of Ka2 that you get from your curves? What is the standard deviation among them? 53 . use equation (2) of the introduction to this experiment to calculate Ka1 from each of the three titration curves. A second divided difference curve is the graph of the change in ∆pH/∆V versus volume or ∆∆pH/∆V∆V versus volume. determine the volume of HCl required to reach the equivalence points in your titrations. Print copies of these plots to turn in to your teaching assistant. From these plots. Prepare plots of your titration data and of the first and second divided differences as was described in the “Strong acid-Strong base Titration” experiment to help you more accurately determine the equivalence point. Title each graph clearly. What are the three values of Ka1 that you get from your curves? What is the standard deviation among them? 6. It approximates the second derivative (rate of change of the rate of change). A first divided difference curve is the graph of the change in pH divided by the change in volume (∆pH/∆V) versus the volume added. It approximates the first derivative (rate of change of pH with volume). Over what pH range did phenolphthalein change color? What was the color change? 4.1. Using the same sequence in which you ordered the masses of Na2CO3. What are the precise masses of Na2CO3 used for each of your three titration curves? 2. Using the data for the second equivalence point (the equivalence point of the first proton dissociation from carbonic acid). Over what pH range did bromocresol green change color? What was the color change? 5. what are your best values for the volumes of HCl required to reach the second equivalence point in the titration (carbonic acid first proton equivalence point)? 3. Use the pH of the first equivalence point (the equivalence point of the second proton dissociation from carbonic acid). equation (1) of the introduction and the values of Ka1 you determined in Question 5 to calculate Ka2 for each of the three titration curves. in the same sequence. label the vertical and horizontal axes. what are your best values for the volumes of HCl required to reach the first equivalence point in the titration (carbonic acid second proton equivalence point) for each of your three titration curves? Again. You may find it convenient to copy and modify the spreadsheet program you prepared to work up the data for that experiment and use it here. and on the second divided difference curve the equivalence point of the titration is where the graph passes through the horizontal axis. and make sure your name is on each of the graphs. On the first divided difference curve the equivalence point of the titration is the maximum point of the graph. Examples of these plots can be found at the end of the laboratory procedure description for the experiment “Strong acidStrong base Titration”.

Conclusion After reflecting on the nature of the titration curve for a diprotic acid. the difference from that of a monoprotic acid. and the complexity of analyzing the data from the titration curve to extract the values of the acid dissociation constants. 54 . Include some comments about the sources of error in the experiment that may be responsible for the difference between the values you have obtained and the accepted literature values for the dissociation constants of carbonic acid. compose a summary of this experiment.

This is especially true of many biological systems in which the pH must be maintained in very narrow ranges if the organism is to survive. -log Ka = -log [H3O+] – log [A ] [HA] + - A-(aq) + H3O+(aq) 55 . Buffers are solutions that simultaneously contain relatively large amounts of acid/base conjugate pairs. Additionally. a buffer works best when the pH is about the same as the pKa for the acid component of the buffer.Acid-Base Buffers INTRODUCTION In this experiment we will focus on the topic of acid-base buffers. An example that you are already familiar with is the acetic acid/acetate ion conjugate pair. however the pH will change very little if the amounts of added base or acid is small relative to the concentration of the buffer conjugates already present in the solution. To illustrate this. A solution containing both of these substances will be a buffer because the weak acid will react with added base to produce the conjugate base via: HC2H3O2(aq) + OH-(aq) C2H3O2-(aq) + H2O(l) and the conjugate base present will react with added acid to produce the conjugate acid via: C2H3O2-(aq) + H3O+(aq) HC2H3O2(aq) + H2O(l) In both cases the pH will change with the addition of acid or base. An acid-base buffer is a solution that resists pH change. consider the reaction: HA(aq) + H2O(l) for which the Ka expression is: Ka = [H3O ] [A ] [HA] If we take the –log of both sides then we have. Buffers are very important in chemistry since many reactions will only occur in certain pH ranges.

Name of Acid Acetic acid Hydrogen carbonate ion Dissociation Reaction HC2H3O2(aq) + H2O(l) HCO3-(aq) + H2O(l) H3O+(aq) + C2H3O2-(aq) H3O+(aq) + CO3-2(aq) pKa 4. If the pH is the same as the pKa. the contribution of the logarithm must be small. You will graph these pH changes against volume and make comparisons to the previous experiments. Then you will make small additions of acid and base to the buffer solutions and observe the pH changes that occur. In fact. Table 1.or pH = pKa + log [A ] [HA] Considering the second term in the above equation. For each of the buffers you will calculate the amounts of the conjugates required to prepare the buffer solutions. you will prepare two buffers and study the effects of adding acid and base. As preparation for this experiment. one can then find the concentration and thus a mass or volume required of the unspecified conjugate to complete the buffer solution.74 10. as strong acids or bases are added. The above equation can also be used to determine the conjugate acid-base concentrations required to make a buffer of specified pH. we can expect a buffer solution to work best at stabilizing the pH when [A-] = [HA]. We can rearrange this equation to express the conjugate acid-base concentration ratio in terms of pH. pKa values for Acids used in the experiment.33 In this experiment. Therefore. study the section on Acid-Base Buffers in your textbook. we see that in order for the pH change to be minimal. it follows that [A-] = [HA]. 56 . - [A -] = 10(pH − pK [HA] a ) Given a target pH for the buffer and a desired concentration for either the conjugate acid or base. We do this by subtracting pKa from both sides of the equation then taking the antilog of both sides. Recall that the antilog function is 10x. Table 1 contains a list of useful pKa values needed for this lab. the logarithm will be zero if [A-] = [HA] since the log 1 = 0.

0 10.5 10.2 10. 57 .1 Basic Buffer 9. pH of Buffer Solutions Group 1 Group 2 Group 3 Group 4 Group 5 Group 6 Group 7 Group 8 Acidic Buffer 4.4 4.6 4.0 5.9 5. Table 2. (You were asked to write it down in your lab manual immediately following the introduction of the Polyprotic System Experiment.) Table 2 identifies the assigned pH values by group numbers. For this reason you are required to prepare for this experiment by calculating the needed amounts of your reagents to make your buffer solutions at the assigned pH values.3 10.1 10. If you do not complete the calculations before the laboratory session you may not have time to complete this experiment.6 You must have the calculation checked by the teaching assistant before you can begin the laboratory experiment.9 10. You should have been assigned a group number during the previous laboratory session.8 4.7 4.Pre-Lab Preparation The calculations for this experiment are not trivial.5 4.4 10.

. You will need to share your glassware. Add about 100 mL of deionized water to the 250 volumetric flask and mix. You will also need to condition this glassware between measurements. After preparing the solutions you will measure the pH level of the solution and adjust the levels by adding either strong acid or strong base as needed. Transfer this volume to your 250 mL volumetric flask. The acidic buffer will be prepared from a 6 M acetic acid solution and 2. Each group is to prepare the 2 buffer solutions at the designated pH values given in Table 2. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs. place the buffer solution into a clean and appropriately labeled 250 mL or 400 mL Erlenmeyer flask. The actual data analyses and the written reports must be done entirely independently of your lab partners or other students. Preparing your Buffers Working in groups of two. Calculate the volume of 6 M stock acetic acid solution you need to make 250 mL of the buffer solution to the designated pH. Wear your goggles! You will be working in groups of two for this experiment. you will be preparing two 250 ml buffer solutions. Add this volume of 6 M acetic acid to your 250 mL volumetric flask that contains the sodium acetate solution. and the other group member prepare 250 mL of the basic buffer at the designated pH values. an acidic and basic buffer. Use the appropriate volumetric pipet to measure this volume. 1. Preparation of Basic Buffer: Calculate and weigh out the grams of solid sodium hydrogen carbonate needed to prepare 250 mL of 0. 58 2.20 M sodium acetate. Now. 3. Transfer this mass to a clean 250 mL volumetric flask and add about 100 mL of deionized water to the volumetric flask.Safety: Remember to always wear gloves when handling all acids and bases. Make sure that you avoid unauthorized collaboration and plagiarism.5 M sodium acetate solution needed to prepare 250 mL of 0. You may use your graduated cylinder to measure this volume. PROCEDURE Part I. Group Member Assignments: The TA will assign your group a number between 1 and 8.5 M sodium acetate trihydrate.1 M sodium hydrogen carbonate solution. Each student must collect data and submit a separate report. The basic buffer solution is prepared from solid sodium hydrogen carbonate and solid anhydrous sodium carbonate. Question: What is meant by conditioning? Preparation of Acidic Buffer: Calculate and measure the volume of 2. Have one group member prepare the 250 mL of the acidic buffer. After you have mixed the buffer solution well. add sufficient deionized water to the volumetric flask to bring the total volume to 250 mL.

there should be no need to recalibrate. 5.Calculate the mass of anhydrous solid sodium carbonate required to make the basic buffer to the designated pH. Using a disposable pipet. After you have mixed the buffer solution well. pH 7. later. Now.00 buffer in three different test tubes. add either 6 M HCl or 6 M NaOH to adjust the pH until it is equal to the assigned pH. Standardize the pH meter using the three buffer solutions following the procedure outlined in the Appendix.02 pH unit. during the experiment.) Stir the solution and record the pH to the nearest 0. For each of the buffer solutions: Measure the pH. place the buffer solution into a clean and appropriately labeled 250 mL or 400 mL Erlenmeyer flask. add sufficient deionized water to the volumetric flask to bring the total volume to 250 mL.00. pH Meter Operating Instructions. 59 . 4. The pH meter will need to be calibrated before starting the experiment. (See Table 2 above.00. Weigh out and add this mass of anhydrous sodium carbonate to your 250 mL volumetric flask that contains the diluted sodium hydrogen carbonate. Place 3 to 4 mL of pH 4. and pH 10. Always store the pH electrode when not in use. Rinse and wipe the electrode before placing it in a new solution.

Start gently rotating the stir bar.2 M HCl In this part of the experiment each group will treat each of their two buffer solutions with 0. Addition of 0.2 M HCl solution in a labeled 250 mL Erlenmeyer flask. Gently. 5. 3. 2. 3. Record the initial buret reading and pH meter reading. You will then plot the pH vs. stir plate. Store half of the 0. Stir the solution and measure the pH. Place 50 mL of the acetic acid/acetate ion buffer in a clean and dry 250 mL beaker.02 mL. 1.2 M HCl solution. You may use your graduated cylinder to measure the 6 M HCl volume.2 M NaOH. Record the pH to the nearest 0. Set up the beaker containing the buffer.2 M HCl solution and the other buret with 0. 2.5 pH units. place a stir bar into the 250 mL beaker containing buffer solution.2 M acetic acid solution in a labeled 125 Erlenmeyer flask. Label the buret and flask. Condition and fill two 50 mL burets. Repeat step 3 until the pH of the buffer solution decreases by 1.2 M HCl to 0.2 M HCl from the 6 M HCl stock solution using a 250 mL volumetric flask. You may use your graduated cylinder to measure the 6 M acetic acid volume. 4. added volume of HCl to graphically observe the pH changes that occur. Record the buret reading to the nearest 0.2 M NaOH solution in a labeled 250 mL Erlenmeyer flask. 60 .02 pH unit when the reading has stabilized.Part II. Store the 0. Record the initial volume of HCl and NaOH to the nearest 0. Save this solution for use in step 7 in Part IV. electrode under the buret containing the 0. Store the 0. You may use your graduated cylinder to measure the 6 M NaOH volume. disposing the rest down the sink. Part III. 4.2 M NaOH from the 6 M NaOH stock solution using a 250 mL volumetric flask.2 M acetic acid solution. Preparing your Reagents 1.02 mL.2 M acetic acid from the 6 M acetic acid stock solution using a 250 volumetric flask. You will also explore the effect of adding 0.2 M HCl solution. Prepare the 250 mL of 0. one with the 0. Prepare the 250 mL of 0. After each addition you will measure the pH of the solution. Prepare the 250 mL of 0. Add approximately 2 mL of HCl to the buffer.

02 pH unit when the reading has stabilized. added volume of NaOH to graphically observe the pH changes that occur. Repeat steps 1-4 using a fresh sample of your second buffer. Start gently rotating the stir bar. Record your volumes and pH levels carefully. 1. stir plate.2 M acetic acid solution in a clean and dry 100 mL beaker. place a stir bar into the 250 mL beaker containing buffer solution.2 M NaOH solution. Repeat steps 2-4 using the 0. You do not need to save this solution. You will also explore the effect of adding 0. 3.6.2 M NaOH In this part of the experiment you will treat each of the two buffer solutions with 0. Gently. Repeat steps 2-4 using the 0. After each addition you will measure the pH of the solution. hydrogen carbonate ion/carbonate ion solution.2 M acetic acid solution instead of a buffer solution. Add approximately 2 mL of NaOH to the buffer. You do not need to save this solution. electrode under the buret containing the 0. Stir the solution and measure the pH. It is important that your beakers are clean and not contaminated with buffer/HCl mixture. Part IV. Record the buret reading to the nearest 0.2 M NaOH to 0. Addition of 0. Gently place a stir bar into the 250 mL beaker containing the acetic acid/acetate ion buffer and HCl mixture reserved from step 5 of Part III.2 M acetic acid solution instead of a buffer solution. Repeat step 3 until the pH of the buffer solution increases by 1. You do not need to save this solution. hydrogen carbonate ion/carbonate ion solution.5 pH units. Gently. 7. You will then plot the pH vs.2 M NaOH solution. Record your volumes and pH levels carefully. 5. You do not have to save this solution. Record your volumes and pH levels carefully. Place 50 mL of the 0.2 M acetic acid solution.02 mL. Place a fresh 50 mL sample of the 0. Record your volumes and pH levels carefully. 4. place a stir bar into the 100 mL beaker containing acetic acid solution. 61 2. Place a fresh 50 mL sample of the acetic acid/acetate ion buffer in a clean and dry 250 mL beaker. Record the pH to the nearest 0. 6. You may need to clean out your 250 mL beaker or use a 150 mL beaker. You do not need to save this solution. 7. . Set up the beaker containing the buffer. Gently place a stir bar into the 100 mL beaker containing acetic acid solution.2 M acetic acid solution in a clean and dry 100 mL beaker. Repeat steps 1-4 using your second buffer.

2 M NaOH? 62 . What was your assigned pH value of your basic buffer? 6. What mass of anhydrous sodium carbonate was required to make the 250 mL hydrogen carbonate ion/carbonate ion buffer at that pH? Show your calculations.5 M sodium acetate was needed to make 250 mL of the acetic acid/acetate ion buffer that has an acetate ion concentration of 0. Clean-Up: All solutions can go down the drain with copious amounts of water. What volume of the 6 M HCl stock solution is needed to prepare 100 mL of 0. Note that it is critical to store the electrode in this solution at the end of the laboratory period. What mass of sodium hydrogen carbonate was needed to make the buffer solution 0. 9. 1. What volume of the 6 M acetic acid solution was needed to prepare the 250 mL acetic acid/acetate ion buffer solution? 5. Record your volumes and pH levels carefully.0 pH units. Be sure to rinse the electrode with deionized water before placing it in the storage solution. 3.2 M HCl? Show your calculation. Part II 10. 7. Provide reasons as to why the measured pH level is different from the calculated value. 8. What volume of the 6 M NaOH stock solution is needed to prepare 100 mL of 0. DATA ANALYSIS Part I.Repeat steps 2-4 using this solution but adding NaOH until the pH increases by about 3. What volume of 2. What was your assigned pH value of your acidic buffer? 2. What was the concentration of the sodium carbonate in the hydrogen carbonate ion/ carbonate ion buffer solution? Show your calculations. What was the concentration of the acetic acid in the 250 mL acetic acid/acetate ion buffer solution at your assigned pH? 4.20 M at that pH? Show your calculations.1 M in sodium hydrogen carbonate? Show your calculations. 11.

You should have 3 separate graphs when you are finished. added volume of HCl for both buffer solutions and the 0. At corresponding pH values. compare how much HCl or NaOH is added before ∆pH = 1. Line up these two graphs along the pH axis (y-axis) and the volume axis (x-axis). When is the buffer capacity at its maximum? 18.Part III 12. Hopefully your graph paper is “see through. 63 . 17. Buffer capacity is defined as the amount of acid or base that can be added to a buffer before any substantial change in pH. You should now have a curve that looks like an “S” laying on its side and one of the graphs will be face down. 14. Label each graph appropriately. take the two graphs of the acidic acid buffer. keeping the pH axis aligned. Using a spreadsheet program. Repeat the procedure described in question 17 for graphs involving the basic buffer. Plot pH vs. Plot pH vs. compare the slopes of the curve of each graph at corresponding points. the volume axis will be lined up end-to-end. What are the differences. Plot pH vs.2 M acetic acid solution. What is the buffer range for the basic buffer? 16. How do these graphs compare to the graphs of the acetic acid/acetate ion buffer? For example. b. Repeat the procedure described in question 17 for the graphs involving the 0. Considering the ranges of pH of each buffer.” What is the pH range over which the buffer effectively neutralizes the added acid and base and maintains a reasonably constant pH? This is referred to as the buffer range. added volume of NaOH for the acetic acid/acetate ion buffer and HCl mixture used in step 8 of Part IV. 13. You should have 3 separate graphs when you are finished. Let’s begin comparing corresponding graphs.2 M acetic acid solution. First. Label each graph appropriately.2 M acetic acid solution. Label the graph appropriately. After the flip. write an equation in terms pH and pKa that defines buffer range. if any? How do the buffer ranges compare? 15. c. One graph will be on top of the other. added volume of NaOH for both buffer solutions and the 0. Compare the acidic buffer graph constructed in question 17 to the graph you made in question 16c. Flip the top graph 180°. a. such as Excel make the following graphs.

where is the buffer region? If not.19. Consider the titration curve you plotted for the “Titration of a Weak Acid” experiment. why not? Conclusion After reflecting on the nature of buffer solutions and their effectiveness over different pH ranges. compose a summary of this experiment. 64 . How does the titration curve compare to the graph involving the acetic acid/acetate ion buffer in this experiment? Does the titration curve include a buffer region? If so.

you will be able to calculate the concentration of 65 . Thus. The presence of this species is easily observed by its reaction with starch indicator to form a deep blue complex. With the two concentrations you can easily calculate the solubility product constant. In this process you will add excess iodide ion to solution that is known to contain iodate ion in the presence of acid. I3-. In the second part of this experiment you will be able to observe the "common ion effect". Once you determine the concentration of iodate by the method described above. The iodate reacts with the iodide by the following reaction: IO3-(aq) + 5 I-(aq) + 6 H+(aq) → 3 I2(aq) + 3 H2O(l) The I2 thus produced will then react via a titration with thiosulfate by the reaction: I2(aq) + 2 S2O32-(aq) → 2 I-(aq) + S4O62-(aq) I2(aq) + I (aq) - I3 (aq) - It should be noted that the progress of this latter reaction can be followed because the iodine formed reacts with the excess iodide ion to form the triiodide ion. one mole of calcium ion forms. In this part of the experiment you will be given a saturated solution of calcium iodate in a 0.Solubility Products INTRODUCTION This experiment involves the determination of a solubility product constant. of the calcium iodate will be equal to the concentration of the calcium ion since for every mole of calcium iodate that dissolves. in the presence of starch. Thus. the endpoint of this latter titration is when the deep blue color disappears.01 M potassium iodate solution. Once the concentration of the iodate has been determined you can easily calculate the concentration of the calcium ion and then the Ksp for the system. if you can obtain the concentration of one ion you can calculate the concentration of the other ion. s. You shall determine the concentration of the iodate ion via what is known as an iodometric titration. The calcium iodate chemical system to be analyzed is described by the reaction: Ca(IO3)2(s) = Ca2+(aq) + 2 IO3-(aq) with a solubility product of: Ksp = [Ca2+] [IO3-]2 In the first part of the experiment you will determine the solubility of calcium iodate in pure water. The solubility. Recall that the iodate ion concentration will be twice the calcium ion concentration in solution.

but is not necessarily equal to the concentration. Because the equilibrium constant expressions using concentrations in place of activity are rigorously correct in the limit of dilute concentration. Based on this reasoning. any time you add an inert soluble salt to a solution of a sparingly soluble salt you will increase the solubility of the sparingly soluble salt. you have only considered the common ion effect. however. Lastly as part of the data workup of this experiment.3 x 10-18 for the dissolution of mercury(I) iodate. This turns out to be a general observation. However. when you have determined the effect of other dissolved ions on a specific equilibrium. 66 . we commonly discuss equilibria and equilibrium constants using the concentrations. they are conceptually parallel with the use of activities. Using the concentration of the two ions you will be able to calculate the solubility product constant for this system. if you were to saturate a 0. (i) (ii) Hg2(IO3)2(s) Hg22+(aq) + 2 IO3-(aq) K = 1. we will recognize that the true expressions are in terms of activities. including the effect that polarity can have on the solubility of solids.05 M potassium nitrate with mercury(I) iodate you would find that the solubility of the mercury(I) iodate has increased by about fifty percent. Based on the equilibrium constant of 1. You have discussed some of the effects of the polarity of water. Because the results are useful. In this experiment. The thermodynamic activity is a function of concentration. you would not predict that potassium nitrate in solution would have any effect on the solubility of mercury(I) iodate.9 x 10-7 M So far. it is true that in the limit of extremely dilute solutions.9 x 10-7 M in mercury(I) ion. you will incorporate activity effects in the calculation of the solubility product from your data. The higher the charge on an ion in solution. The correct incorporation of activity effects makes the treatment of equilibria and equilibrium constants more rigorous. However. Equilibrium constants are properly defined in terms of thermodynamic activity rather than concentration.iodate from the dissolution of the calcium iodate and thus calculate the concentration of calcium ion in solution. By comparing the two parts you will note the dramatic effect that the iodate ion from the potassium iodate has on the solubility of calcium iodate. you would expect a saturated solution of the salt to be 6. if not exactly correct. the activity is equal to the concentration. These interactions can be significant enough that they cannot be ignored when salt concentrations exceed hundredth molar values. It should not be surprising to find that water interacts with various ions differently and that a more highly charged particle has a greater interaction with water molecules. the greater will be the interaction of the ion with the dipole of the water molecule and with other ions in the solution.3 x 10-18 K = [Hg22+][IO3-]2 = s(2s)2 s = [Hg22+] = 6.

Instead of looking only at the concentration of a species in solution. aW a X Following this procedure for our example solubility problem. The activity of an ion includes both concentration and how susceptible the ion is to the kinds of effects described in the preceding paragraph. but employing activity in positions in the equation where you were previously using concentration: q aYp a Z K= m n . Substituting these 2 3 expressions into eq. Thus the mercury(I) iodate becomes more soluble. The definition of the equilibrium constant represented in equation (ii) above does not take this phenomenon into account. (ii) becomes: 2 K = aHg 2 + aIO − 2 3 (iii). 2 3 2 3 ( )( ) 2 67 . To incorporate these and other effects arising from molecular and ionic interactions in solution. When a mercury(I) ion comes close to an iodate ion surrounded by potassium ions. and γ IO − are the activity coefficients for Hg22+ and IO3. preventing it from combining with the iodate ion and precipitating out of solution. A convenient way to quantitatively account for the molecular interaction part of the activity is to express the activity as the product of an activity coefficient times the concentration. eq.The explanation for the observed increase in solubility is that the positively charged potassium ions can cluster around the negatively charged iodate ions. and the negatively charged nitrate ions cluster around the positively charged mercury(I) ions. the positive charge on the potassium ions will repel the positive charge on the mercury(I) ion. The general way for incorporating activities into equilibrium constants for the general reaction: mW + nX pY + qZ is to form the equilibrium constant in the usual way. For example the mercury iodate equilibrium requires the activities: 2 aHg 2 + = γ Hg 2 + [ Hg 2 + ] 2 2 aIO − = γ IO − [ IO3− ]. we simply use the activity of the ion in place of the concentration in the equilibrium constant expression. the activity of that species should be examined when equilibrium is considered. (iii): 2 2 2 K = γ Hg 2 + [ Hg 2 + ] γ IO − [ IO3− ] = γ Hg 2 + γ IO − [ Hg 2 + ][ IO3− ]2 .. 3 3 Where γ Hg 2 + .

g.05 M potassium nitrate.05 M potassium nitrate it becomes very clear that the ionic strength of the solution in pure water is vastly different from the solution in 0. 2 µ = (4[ Hg 2 + ] + [ IO3− ] + [ K + ] + [ NO3− ]) 1 2 Because mercury(I) iodate is so sparingly soluble.05 . various theoretical and empirical methods for consistently separating the observed mean ionic activity coefficients into individual ion coefficients have been developed.From this form we can see that expressing the equilibrium constant using concentrations alone is identical to assuming that the activity coefficients are equal to 1. which is defined by the expression: 1 µ = 2 Σ ciZi2 i where ci is the concentration of the ith species and Zi is its signed charge in multiples of the elementary charge (e. In the example contrasting the solubility of mercury(I) iodate in pure water and in 0. However. Instead their product 2 3 is replaced by γ ± . This sum extends over all ions in 2 3 solution. 3 2 K = γ ± [ Hg 2 + ][ IO3− ] 2 . Because it is impossible to get a solution containing just the cation or just the anion. These methods are by no means perfect. This assumption is also called the ideal solution approximation. It has been found that a convenient quantity to use when expressing the functional dependence of the activity coefficients of ions on concentration is the ionic strength of the solution. Since they account for molecular and ionic interactions. in the solution containing potassium nitrate: In pure water 2 µ = (4[ Hg 2 + ] + [ IO3− ]) . Z Hg 2 + = +2 and Z IO − = −1 ).0 . 1 2 2+ − Since Hg 2 and IO3 are the only ions in solution. the values of activity coefficients change as the concentration of the solution changes. it is impossible to experimentally determine γ Hg 2 + and γ IO − individually. but they often give much better 68 . µ = 0. in pure water.05 M potassium nitrate when we apply this definition. the mean ionic activity coefficient. calculations will give the result that.0 whereas in 0. raised to the power equal to the sum of the exponents of the individual ion activity coefficients. While it is impossible to experimentally determine the values of individual ion activity coefficients. µ = 0.

J.095 0.872 0. Cu2+. HPO42Al3+.485 0.928 0.1 0. CN-. as in the earlier ionic strength calculation.445 0. CrO42-.45 0. 1675 (1937) As an example of how to use activities.results than the alternative very simple assumption that the solutions are ideal.38 0.868 0. HCO3-. SCN-.31 0. MnO4-.965 0. Cs+. I-.505 0. Cl-. Ag+ Mg2+.05 0. presents results for one such method of representing individual ion coefficients as a function of the ionic strength of the solution.9 x 10-11 K = (aCa2+) (a2F-) = (γCa2+ [Ca2+]) (γ2F.675 0. Fe3+.900 0.01 0. SO32Hg22+.405 0.005 0.36 0. Chem.898 0.967 0. S2Pb2+.445 0.395 0.924 0. Kielland.001 0. Ba2+.755 0. its 69 .964 0.964 0. M) Ion H+ Li+ Na+. Br-.926 0. Mn2+ Sr2+. Be2+ Ca2+.738 0.71 0. Since the equilibrium constant for the dissolution of calcium fluoride is quite small.929 0.76 0. IO3-.899 0.72 0.81 0.665 0.660 0. The concentration of calcium is going to depend on how much calcium fluoride dissolves. ClO4K+. Table 1.775 0.867 0. Cr3+ PO43Sn4+ 0..925 0.37 0.902 0.255 0.41 0.588 0.742 0.749 0.355 0. The ionic strength is due to the dissolved magnesium sulfate and the dissolved calcium fluoride.67 0.81 0. Cd2+. Zn2+.69 0.755 0. Table l. F-.33 0.964 0.80 0.77 0.740 0. SO42-.10 0.725 0.465 0. NO3Rb+. Soc. assume that. CO32-.86 0. here is a calculation of the concentration of calcium ion in a 0.35 0.76 0.52 0.805 0. H2PO4OH-.0125 M solution of magnesium sulfate MgSO4 saturated with calcium fluoride CaF2.867 0.82 0. Hg2+.73 0.75 0.870 0.83 0.54 0.16 0. 59.455 0.744 0.065 0.80 0.15 0.964 0. it is necessary to know the ionic strength of the solution.933 0.835 0.066 0.[F-]2) = (γCa2+ [x]) (γ2F.15 0.048 Source: Data from J.245 0. so the chemical equilibrium and initial set-up of interest is CaF2(s) Initial: Final solid solid Ca2+(aq) + 2F-(aq) 0 x 0 2x K = 3.914 0. Amer.907 0.x 3 In order to look up the activity coefficients in the table.30 0.[2x]2) = 4γCa2+ γ2F. Activity Coefficients for Aqueous Solution at 25o Ionic Strength (µ.18 0. NH4+.

contribution will be negligible, and the only ions that need to be considered are the magnesium and sulfate ions. This gives an ionic strength of 0.050 M: µ = 1/2([0.0125] * 22 + [0.0125] * (-2)2) = 0.050 M Using this value for the ionic strength, the activity coefficients for calcium and fluoride ions are 0.485 and 0.81 respectively. Plugging into the equilibrium constant equation and solving for x gives 3.9 x 10-11 =[x]0.485[2x]20.812 x = [Ca2+] = 3.1 x 10-4 M If you had neglected the activity of the ions in solution you would have calculated the calcium ion concentration to be 2.1 x 10-4 M. This is a thirty-two percent error. In this experiment you will examine the effect of activities in determining an equilibrium constant, the solubility product. You will do a calculation similar to the example given, but you will determine the concentrations of the species in solution, and you will use these to calculate the solubility product both with and without including activity effects. Your solutions are not likely to have an ionic strength exactly equal to one of those given in the table. While more sophisticated interpolation between values in the table are possible, it is sufficient for this experiment to simply use the tabulated value for that ionic strength that is closest to the value you calculate for your solution of interest. If your solution has an ionic strength exactly midway between two tabulated values, then use the value for the lower ionic strength.

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Safety: Remember to always wear gloves when handling all solids. WEAR YOUR GOGGLES! PROCEDURE Work in pairs on this experiment. Each student must collect data and submit a separate report.
The actual data analyses and the written reports must be done entirely independently of your lab partner or other students. Make sure that you avoid unauthorized collaboration and plagiarism. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs.

Part I. Preparation of a Potassium Iodate Solution

In this procedure you will prepare a standard potassium iodate solution for use in standardizing a sodium thiosulfate solution. 1. Using a volumetric flask, accurately prepare 250 mL of a solution approximately 0.01 M KIO3. Note that this will need to be made as accurately as possible since this solution will serve as the primary standard for the experiment. The solid will take a few moments to dissolve. While you are waiting, go on to Part II.

Part II. Preparation of a Sodium Thiosulfate Solution

In this procedure you will prepare and standardize a sodium thiosulfate solution. You will use the standard KIO3 solution prepared in Part I to standardize the sodium thiosulfate solution. The sodium thiosulfate solution will then become a secondary standard. 1. Using your clean 1 L plastic bottle, prepare about 500 mL of a 0.05 M Na2S2O3 solution. You should do this using the 1.0 M Na2S2O3stock solution provided. Some calculations are required here.

Part III. Standardization of the Sodium Thiosulfate Solution

Standardize the sodium thiosulfate solution with the potassium iodate solution you have prepared. You should use the iodate-to-iodine and iodine-to-iodide reactions given in the introduction of the experiment. You will have to plan how to best perform this experiment. Here are some tips:

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1.

For the first reaction you will need excess potassium iodide and hydrochloric acid. If you were using a 10 mL sample of the standard potassium iodate solution it would require about 2 g of potassium iodide and about 3 mL of 6 M hydrochloric acid. Begin by dissolving the potassium iodide in about 50 mL of water in your titration flask. Next, accurately add 10.0 mL of potassium iodate using volumetric glassware. Finally, add the hydrochloric acid. The solution will turn brown due to the formation of iodine. Now immediately titrate the solution with the sodium thiosulfate solution until the solution in the titration flask becomes a light brown color indicating only a limited amount of iodine present. At this point add 1 mL of the starch indicator. The starch will react with the I3 to form a complex that is dark blue in color. Continue the titration until the dark blue color just disappears. Do at least three acceptable titrations so that you can calculate a meaningful average sodium thiosulfate concentration, standard deviation and 90% confidence limit for your data. An acceptable trial is one that passes the Q-test.

2.

3.

Titration Tips

- Do not use assembly line techniques when preparing flasks for titration; prepare a flask, titrate it, and then prepare the next flask. If you do not begin the titration immediately iodine may crystallize out of solution and your titration results will be inaccurate. - Do not add the starch indicator until the brown solution has lightened to light brown or yellow. - Do not waste chemicals. You should be using no more than a couple of grams of potassium iodide and a few milliliters of acid in each titration. - Do not waste time. Only your limiting reagent needs to be measured out with volumetric glassware. The other reagents in the iodate-to-iodine reaction can be measured out reasonably roughly without affecting your results. - Do not contaminate your reagents. If the solutions in the bottles are brown they have been contaminated. Return these bottles to the stockroom.
Part IV. Solution Solubility and Solubility Product from a Saturated Calcium Iodate

Determine the iodate concentration in a saturated solution of calcium iodate using your standard sodium thiosulfate solution. You should use the same procedure you developed for the thiosulfate standardization, but this time you will use a saturated calcium iodate solution instead of a potassium iodate solution when performing the first reaction. 72

Pour out enough sample in a beaker so that you can conveniently but not wastefully use your 10. Solubility and Ksp from a Saturated Calcium Iodate Solution in 0. Part V. This solution will also be provided by the stockroom. Again. If there is time remaining in the lab come back and repeat this titration. Pour out the required amount carefully so that you do not disturb the solid Ca(IO3)2 settled at the bottom of the bottle. Pour out enough sample in a beaker so that you can conveniently but not wastefully use your 10. After you have done a second titration for Part IV do a second titration for this part of the experiment if time permits. Add the same amount of KI and 6 M HCl in 50 mL of DI water that you did to standardize the thiosulfate solution.00 mL of saturated Ca(IO3)2 solution for the titration. and for this part of the experiment you are interested in the solution that has only calcium iodate dissolved in water. You do NOT want any of the solid Ca(IO3)2 in your Erlenmeyer flask. You do NOT want any of the solid Ca(IO3)2 in your Erlenmeyer flask. then add the 10. 73 . Clean-Up: All solutions can go down the drain.010 M KIO3 solution for the titration.010 M KIO3 Determine the iodate concentration in a saturated solution of calcium iodate in 0. read the label carefully. there are two calcium iodate solutions.010 M KIO3 using standard sodium thiosulfate solution. Do one titration then go back to Part IV. This saturated solution is prepared by dissolving enough potassium iodate in water to make it 0.010 M in iodate and then saturating the solution with calcium iodate. Pour out the required amount carefully so that you do not disturb the solid Ca(IO3)2 settled at the bottom of the bottle. You may only have time for a single titration for this part of the experiment. Clean up your glassware and your work area and complete any other cleanup tasks to which you have been assigned.00 mL of saturated Ca(IO3)2 in 0.The saturated calcium iodate solution will be provided by the stockroom.00 mL pipet to transfer the sample to an Erlenmeyer flask for the titration. do not confuse this solution with the saturated calcium iodate solution you used in the previous part of this experiment. Make sure you read the labels on the bottles provided carefully. You only have time to do a single titration for this part of the experiment. then add the 10.00 mL pipet to transfer the sample to an Erlenmeyer flask for the titration. Do one titration then move on to Part V. Add the same amount of KI and 6 M HCl in 50 mL of DI water that you did to standardize the thiosulfate solution. Clean and return all burets to the proper location at the back of the room.

What is the molarity of the Na2SO3 that you calculate for each of your three trials in the same order in which you entered the volumes? 7. What was the mass of KIO3 that you dissolved in 250. what is the solubility of Ca(IO3)2 in the saturated solution in pure water? 74 . For each of your three trials. Based on the number of moles of IO3.05 M Na2S2O3? Part III 4. that is the number of moles of Na2S2O3 reacting with one mole of KIO3? 5.were present? If you performed multiple trials. What is the average molarity and the standard deviation of the Na2SO3 solution based on your three trials? Part IV 8. what volume of Na2S2O3 was required to reach the endpoint? 6.in the saturated solution of Ca(IO3)2 in pure water solvent? 9. what was the average number of moles of IO3present? 12. For each of the trials you performed. how many moles of IO3.0 mL of de-ionized water to make your primary standard solution? 2. What was the resulting molarity of your primary standard solution of KIO3? Part II 3. For each of the trials you performed. What volume of 1 M Na2S2O3 stock solution did you use to prepare 500 mL of 0. How many trials were you able to complete for the determination of IO3. What is the stoichiometric factor.present in your sample(s) and the volume of that sample. What volume of the saturated solution of Ca(IO3)2 in pure water did you use as a sample for titration with Na2SO3? 10. what volume of standardized Na2SO3 was required to reach the endpoint? 11.DATA ANALYSIS Part I 1.

When you do this calculation.Part V You will now calculate the concentration of the iodate present in your final solution. appropriate for the ionic strength of the saturated Ca(IO3)2 in pure water. how many moles of IO3.in the saturated solution of Ca(IO3)2 in the solution containing 0.01M potassium iodate KIO3? 14. For each of the trials you performed.01 M KIO3? Comparison of solubility values 18. Using the activity coefficients from TABLE I. What volume of the saturated solution of Ca(IO3)2 in 0. What is the ionic strength of the saturated solution of Ca(IO3)2 in 0. 13. For each of the trials you performed. Examine the values you have obtained for the solubility of Ca(IO3)2 in pure water and in 0. what volume of standardized Na2SO3 was required to reach the endpoint? 16.01 M KIO3 did you use as a sample for titration with Na2SO3? 15. what is the value of Ksp that you calculate using the expression in concentrations alone? 20. What is the ionic strength of the saturated solution of Ca(IO3)2 in pure water? 22.01 M KIO3? 75 .were present? If you performed multiple trials.present in your sample(s) and the volume of that sample. Using the concentration of Ca(IO3)2 that you determined in the saturated solution in 0. Based on the number of moles of IO3. How many trials were you able to complete for the determination of IO3.01 M KIO3? Explain any difference you may observe. what is the solubility of Ca(IO3)2 in the saturated solution in 0. Calculating Ksp based on concentration 19. calculate the value of Ksp that you calculate using the expression in concentrations alone? Calculating Ksp based on activity 21.01 M KIO3.010 M iodate present that does not come from the dissolved Ca(IO3)2. Is the value of solubility significantly different in pure water and in 0. make sure that you account for the fact that there is 0. calculate Ksp using activities? 23.01 M KIO3. Using the concentration of Ca(IO3)2 that you determined in the saturated solution in pure water. what was the average number of moles of IO3present? 17.

Is the value of Ksp significantly different in pure water and in 0.01 M KIO3 solution. calculate Ksp using activities? Comparison of Ksp values 25. appropriate for the ionic strength of the saturated Ca(IO3)2 in 0. commenting upon the common ion effect and its influence on solubility.01 M KIO3 both recognizing the presence of activity effects and based upon concentrations alone. Using the activity coefficients from TABLE I. Examine the values you have obtained for Ksp for Ca(IO3)2 in pure water and in 0.24. Then write a summary paragraph comparing your results. and commenting upon activity effects and their influence on the Ksp 76 .01 M KIO3 ? Is any difference you calculate affected by the recognition of activity effects? Conclusion Reflect on the experimental procedures you have undertaken and the possible sources of error.

APPENDIX .

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that is. in order to pass this course. Data Collection All data must be recorded in ink directly into your laboratory notebook. the experiment name. 2. the TA's name. If a student needs more unknown. a student must complete all of the assigned laboratory work. The note should contain the student's name. Any student without this preparation completed at the beginning of the laboratory period is deemed unsafe and must leave the laboratory until the pre-laboratory write up is complete and the supervising TA is convinced that you are prepared to begin the experiment. After preparing the laboratory notebook. Pre-Laboratory Preparation Many of the Chemistry 2 laboratory experiments are intricate and use chemicals that could present a hazard if used improperly. they must know the name of the experiment and unknown. the laboratory section number. Students must be explicit in their request for an unknown. Thus. 4. Therefore. 1. Post laboratory exercises are due one week after the completion of the laboratory. Title: The report should have a title that concisely describes the experiment. students will complete the on-line pre-laboratory presentation and must pass the pre-laboratory quiz. Unknowns Students will obtain all unknowns from the TA. Writing A Laboratory Report Below is the suggested format that your report should follow.A) General Experimental Guidelines The laboratory is a critical component of your study of chemistry. 3. A-1 . "Writing a Laboratory Report". Below is a general outline of a common format that is often used in science laboratory courses. and the name of the unknown.& off-line postlaboratory exercises. students are required to judiciously prepare for each experiment by carefully reading the experiment and writing a Title. Discuss this format with your TA during the first laboratory period so that you clearly understand what will be expected. you must turn in a copy of your data sheet to your TA before you leave the laboratory. Procedure (brief outline). the student's locker number. including all on. Portions of the report should be written in your laboratory notebook and others will be submitted on-line as part of the post laboratory exercises. Purpose. At the completion of the experiment. A detailed description of each section is described below under. and Data (outline) section before arriving at the laboratory. they should notify the TA who will then write a note of explanation that the student can take to the dispensary.

A-2 . A severe penalty will be imposed for pencil or transcribed data entries. Students will not be granted extra time to complete the laboratory. It is also important to organize and prepare the format of the Data section before coming to the laboratory so that you will only need to neatly record your data and observations during the experiment. Results & Conclusions: Report the outcome of the experiment. especially in the Data section. you should also cite the literature or laboratory manual. Do not erase mistakes. If you are using a published procedure. Simply draw a line through the error and record the correction. You must prepare for each experiment by writing the Title. All data must be recorded in ink directly into the notebook at the time it is collected. A date should be indicated on each report. The following sections are to be submitted on-line as part of the post-laboratory exercise: Calculations: This section generally includes any complicated calculations that are involved in the experiment. If it is not completed the student must finish it and the TA will deduct 30% of earned points from the post-laboratory exercise for first time offenders (70% for repeat offenders). It is important that this section be as neat and as organized as possible. State the purpose of the experiment in the form of a complete sentence. Be sure to note any problems or unexpected occurrences. it is important to use foresight when organizing this section. and Procedure before coming to the laboratory. Do not start with the word "To. Questions: All assigned questions are answered in this section. Your notebook should be organized and written in such a manner that another chemist could read it and repeat the experiment in precisely the same way. Again. Any pertinent chemical reactions are generally indicated. The use of tables will often help in this regard. Your notebook is subject to examination at any time. It is also important to complete the report as soon as possible after the completion of the experiment as this is much more efficient than waiting until the night before the experiment is due.Purpose: A brief and concise statement that describes the goals of the experiment and the methods employed. All reports must be written in non-erasable ink." Procedure: A brief and concise outline of each step of the experiment should be included. Purpose. A drawing of the apparatus may also be included. Data and Observations: Report all measurements and observations that are pertinent to the experiment. Each section should be clearly marked with a proper heading.

The standard deviation. and a relative deviation. a 90% confidence limit of ± 2. σ. Clearly the more precise a set of data. Examples are a difference in readings by different observers.0 of the calculated average of a limited collection. or the fluctuations in equipment due to electrical noise. Random or Indeterminate Errors are due to limitations of measurement that are beyond the experimenter's control. Statistical Treatment of Data Every measurement made in the laboratory is subject to error. in other words.0 indicates that there is a 90% probability that the true average of an infinite collection of data is within ± 2. Although you should try to minimize error. a standard deviation. Data that is highly accurate suggests that there is little systematic error. a 90% confidence limit. a small confidence interval is always the goal of any experiment. Another related term is precision. For example. These errors cannot be eliminated and lead to both positive and negative fluctuations in successive measurements. You will be graded by your ability to obtain accurate results. Examples are errors due to a miscalibrated piece of glassware or a balance that consistently weighs light. In an effort to describe and quantify the random errors which will occur during the course of the Chemistry 2 laboratory you will be asked to report an average. You may also have to analyze multiple trials to decide whether or not a certain piece of data should be discarded. the measurements are more precise. Thus. Average and Standard Deviation The average or mean. Systematic or Determinate Errors are those errors which are reproducible and which can be corrected. In General Chemistry you will be required to calculate the 90% A-3 .x)2 N-1 The smaller the value of σ the more closely packed the data is about the mean.5. The following sections describe these procedures. Data of high precision indicates small random errors and leads experimenters to have confidence in their results. is defined by Σxi x = N where each xi is one measurement and N is the number of trials or samples. or. two types of errors will occur. the smaller the confidence interval. Confidence Limits Confidence limits provide an indication of data precision. Accuracy describes how close your result is to the true value. Precision describes how close your results from different trials are to each other. A well-designed experiment (and a well-trained experimenter) should yield data that is both precise and accurate. The standard deviation for small samples is defined by σ = Σ (xi . measures how close values are clustered about the mean. x.

t = 6. The values in the table below are given for the 90% confidence level. with all data that are of high quality. Next. Relative Deviation The relative average deviation. This number is generally expressed as parts per thousand (ppt). a) Calculate the average. d) Divide that average of the deviations by the mean of the good data. or test. x. |xi . Analysis of Poor Data: Q-test Sometimes a single piece of data is inconsistent with other data. t = 2. given by gap QData = range and compare the value to that given in the table below. The advantage of a relative deviation is that it incorporates the relative numerical magnitude of the average. The relative average deviation. and t = 2. like the standard deviation. For the 90% confidence limits you are asked to calculate. is useful to determine how data are clustered about a mean. t = 2. You will then calculate the QData.314 when N = 2.132 when N = 5. Number of Trials 3 4 A-4 QCritical 0.confidence interval for all experimental collections of data. You should always report your result as the average ± the 90% confidence limit. d.x|. you calculate the magnitude of the total spread of the data by calculating the difference between the data in question and the data furthest away in value (this is called the "range"). Many tests have been developed for this purpose. t = 2. You can do this by simply multiplying by 1000.015 when N = 6. Please report the relative average deviation (ppt) in addition to the standard deviation in all experiments. One of the most common is what is known as the Q test. b) Calculate the deviation.920 when N = 3.353 when N = 4. You need a method to determine. To determine if a data should be discarded by this test you first need to calculate the difference of the data in question from the data closest in value (this is called the "gap"). d. The formula to do this is: tσ N Confidence Limit = where t varies with the number of observations.94 0. c) Calculate the average of these deviations. If the QData is greater than the QCritical then the data can be discarded with 90% confidence (the value has a less than 10% chance of being valid). of each good piece of data. if the data in question is so poor that it should be excluded from your calculations.76 . is calculated in the following way.

However.ucdavis. beware of discarding data that do not meet the Q test.html 2) Near the bottom of the page. Plan ahead. Keep in mind that you also always have the right to discard a piece of data that you are sure is of low quality.& Post-Laboratory Procedures The Department of Chemistry is introducing on-line pre-& post-laboratory activities. Prior to doing any activities.5 6 0. The purpose of the pre-laboratory presentations is to aid the student in preparing for the laboratories. 1) Go to http://email. Accessing the Website Each time you access the On-Line Chemistry 2 Laboratory website you must do so by logging into MyUCDavis. All registered students have a UCD login with kerberos password in order to access the site.56 While the Q test is very popular. 1. You may be discarding your most accurate determination! B) On-line Pre. then you will not be able to take the pre-lab quizzes or do the post-lab exercises. A UCD login and kerberos password may be obtained from IT Express located in Shields Library. Each post-laboratory exercise is designed to guide you through the calculations or concepts that apply. Read your Laboratory Manual and complete your pre-laboratory write up before viewing on-line pre-laboratory presentation. Prior to coming to the laboratory class.edu/forms/forms.64 0. all students are required to complete the Safety Quiz online after watching the online safety videos. If you do not log in through your Chemistry 2 Course Webpage on MyUCDavis. That is. the prelaboratory exercises are to be viewed and the pre-lab quiz must be completed on-line. when you are aware of a poor collection. Do not wait until the last minute to complete any of the required on-line activities. (If you are registered – proceed to item c below) b.” A-5 . Have laboratory notebook and calculator with you when viewing the on-line prelaboratory presentation or completing the post-laboratory exercises. a. it is not always useful for the small samples you will have (you will generally only do triplicate trials). the on-line activities may take time to complete. click on “Temporary Affiliate Form. Concurrent students need to contact the Head TA to request guest access to the website in addition to obtaining a UCD login with kerberos password. As with any computer activity.

4) Fill out your portion of the form indicating that your affiliation will be expected to terminate at the end of the current quarter. 6) Take the form to room 108 Chemistry for Departmental Approval to be signed by George Hague. contact your Head TA with your UCD email address so that the Head TA may give you MyUCDavis access to Chemistry 2. Logging in 1) Go to http://my.ucdavis. Chemistry Department MSO. 5) Take the form to your Head TA to sign as the sponsor. c.edu. Please note that George Hague will not accept your form until your Head TA has signed. 7) Take the completed form to IT Express in room 182 Shields Library and follow their instructions to obtain your UCD login and email accounts. 8) Once you have your UCD login and email account activated. A-6 .3) Download and print this form.

2) In the upper right-hand corner of the MyUCDavis Welcome page is a “Students. and Staff” link. be sure to place the CD in your CD Drive before proceeding. Click on it and log in using your UCD login ID and kerberos password. 4) If you are using a modem or a slow DSL connection. A-7 . Faculty. 3) Select the “My Classes” tab located near the top of the frame. 5) Click your Chemistry 2 class.

” Click on this link. you will find a blue link named. Please follow the instructions to correct your settings and/or install the correct software.6) Following the course description paragraph. A-8 . 7) You may see the screen below. This is checking your computer to make sure you have all the software and settings needed to view the course materials. then there is no guarantee that you will be able to view all the videos and slides. “Course Website. If you decide to bypass these tests.

does not necessarily install them. you may see the following screen.e. If you do not see the movie on the Welcome page. Flash player. If you do not have the correct Flash player installed. Please follow the instructions to download and install the Flash Player. A-9 .8) The Welcome Page tests whether the Flash plug-in is working. i. then there is no guarantee that you will be able to view all videos and slides. Be sure to check the website you are downloading from for specific instructions on installing the plug-in. Keep in mind that downloading the plug-ins.

” it will take you to the Pre-Laboratory Presentation screen as seen below. you have the option to use the CD that accompanies this course or the no-CD option. then make sure you select the right drive for your CD-Rom drive. A-10 . There is a brief tutorial in the “Getting Started” Presentation. you may do so at this page. Whichever CD option you choose. the program will use it as the default option for subsequent logins. If you click on “Pre-Laboratory Presentations.edu. At the “My Profile” page. NOTE: If you run into difficulty with any of these steps. You can change this option any time. Viewing the Pre-laboratory Presentations. 2. If you choose to use the CD. please contact mwwebhelp@ucdavis. a. If you would like to change your password.9) Click on “My Profile” to enter your personal information.

A passing score of 100% (correct answers to all three questions) is required before you will be allowed to perform the laboratory experiment. Audio is provided but not essential. review the laboratory material again and be prepared to take another prelaboratory quiz at the beginning of laboratory class given by your TA. or view any slide in the presentation by selecting it in the Slide Menu. Because the questions are chosen randomly. 3. d. Note you may review any slide at any time. Choose the appropriate laboratory quiz. The entire text for each slide may be viewed by moving the slider directly to the right of the text frame. Taking the Pre-laboratory Quiz After viewing the lab session. it will be counted as one of your two attempts even if you do not hit the submit A-11 . If you fail the quiz on the first attempt. you may receive different questions on your second attempt. Pre-lab quizzes are timed quizzes. go back to the Chemistry 2 Laboratory Presentation Home Page by clicking at the top of the page. so it is a good idea to review the pre-lab session prior to your second attempt. You may also view the laboratory session while you are taking the prelaboratory quiz. Each pre-lab quiz must be completed at least 1 hour prior to attending your scheduled lab class. you may take the quiz a second time. Sequentially view the slides by either clicking on “Prev” and “Next” buttons. Presentations Menu Slide Menu Text Frame c.b. You have twenty minutes to take the quiz. All the information is conveyed in the text and the main frame. a. once you open a window to take a quiz. If you fail to pass the quiz on a second attempt. b. Click on pre-laboratory quizzes. Furthermore.

c. There are also multiple-choice questions and free response questions posed in the post-lab exercises. A-12 .6 grams. then a value in a range of 0. The program also allows for rounding differences.236 may be accepted. For your calculation entries.232 – 0. 0. For your data entries. For example. 4. the program will check to see if your data entry falls within a range such as 1 . if you are asked to weigh approximately 3 g of a substance. In order to receive your 2 points for the prelaboratory quiz you must complete it successfully at least 1 hour before your laboratory class is to begin. An on-line text box will be provided for you to write any concluding remarks discussing and explaining your experimental results.button before closing the window. For example. you will be asked to enter your data and the results from your calculations. based on your data. Completing the Post-Laboratory Exercises.234. if the program is expecting the entry. Only start the pre-lab quiz when you are ready to take it. the program is designed to verify that your calculation is correct based on your previously entered data. the post-lab exercises are designed to check that your data is sensible. In the post-laboratory exercises. You will need to complete all the on-line post-laboratory exercises for each lab in order to receive credit for the laboratory portion of the course.

You may need to reference this material when discussing a calculation with a TA. a scroll down window appears at the bottom of the screen. You should keep a detailed record of your data entries and the resulting calculations in your laboratory notebook. You will need to have your laboratory notebook and a calculator or spreadsheet program to complete the exercises. See below. This summary is the post-lab data summary. b.a. You may refer to this summary to verify the values you entered that are used in subsequent calculations. Click on post-laboratory exercises. c. Choose the appropriate laboratory exercise and follow the instructions. As you proceed through your post-lab exercise. and it contains your accepted entries and the number of points awarded for each question. A-13 .

you must have data for at least 3 trials to complete the post-lab exercises. Data Entry – No Scoring Simply enter your experimental value. you will receive one point for completing the question and you will be informed of the correct answer. You will receive a minimum of one point if you answer correctly on the third or subsequent tries. If you are unable to proceed after repeated attempts to enter a correct response. you cannot go back and change your answer to a previous question.d. The program will verify that your entry is within the expected range for the experiment. Scoring Scheme: 3-2-1-1 These are typically multiple-choice questions with three alternatives. The notation used and an explanation of each is provided below: 1. Once you proceed to the next question. Some hints are provided for the first few incorrect responses. The possible points earned are then reduced by one point on each try and a hint is provided. Scoring Scheme: 2–1 These are typically questions that have only two alternative answers. the program will begin with the same question that you were answering when you exited. In contrast to the pre-lab quizzes. 2. g. If you select the incorrect answer. Points are not awarded until you click the submit button. If you select the correct answer. you will not be able to proceed to the next question until you have correctly answered the previous question. but no awarding of points is involved. When asked to collect data for multiple trials. you may exit the post-laboratory exercise at any time and re-enter as many times as you wish. you will receive two points. When entering data or calculated values. The single exception to this is Part III of the Vitamin C laboratory. you will receive three points. The first line of text on each question contains a terse notation describing the scoring for that question. If you select the correct answer on the first try. please contact your TA. 3. In many cases. Upon reentry. f. A-14 . Scoring Scheme h. Be careful and deliberate about your entries. do not include unit symbols e.

Analysis (1 to 5 points possible) In some of the laboratories. In these three laboratories. 6.4. Scoring Scheme: 3-3-2-1 These are typically questions that require you to do calculations based upon previously entered experimental data. but may also be multiple choice questions with 4 or more alternatives. In the Redox and EDTA laboratories you will find a mass percent and in the Qualitative Analysis laboratory you will be identifying the metal ions present in a mixture. If you respond correctly on either of the first two tries. Your points for these questions will appear in your on-line score sheet. Your TA will read your responses and award you your points accordingly. 5. Each post lab exercise has a date/time stamp to indicate the date and time of completion. The last report each quarter is due at the A-15 . Late Reports Laboratory reports are due at the beginning of the period after the one allocated for the completion of the experiment. The point value for each question will be indicated. you will receive three points. The possible score is reduced by one point for each of the next two tries and remains one point for a correct response on any subsequent try. you will need to enter your locker series number. Due Date/ Late Submission of Post-lab Exercise. you will analyze a sample of unknown content. NOTE: If you run into difficulty with any of your post-laboratory entries. please contact your TA. The post-laboratory exercises must be completed by the next normally scheduled laboratory meeting. Free Response (1 or 2 points possible) Some of the laboratories contain questions where you will write your answer in a text box. The last post-laboratory exercise is due the last day of instruction. In order for the on-line program to identify which sample you were assigned to analyze. C) Late Reports & Make-Up Policy 1. you will be awarded 1 to 5 points for accuracy. Late submission of your post lab exercise will be met with a 5-point deduction for every calendar day it is late.

and allow you to do the lab. If you miss a lab. No further opportunity for make-up will be provided to the student who fails to make up the lab by the following week. If you cannot present this proof. Typically. Failure to make up a lab may result in a failing grade for the course. the teaching assistant will allow you in the lab.time indicated by the TA. the actual data analyses and the written reports must be done entirely independently of your lab partner or other students. No laboratory make-ups will be offered after the last day of laboratory. time and room number where you made up the laboratory. it must be made up before the end of the following week of laboratory. If there is room in the class. Plagiarism and Unauthorized Collaboration Some of your experiments will be done with lab partners. However. See the schedule below for exceptions to this policy. Students who have missed making up the lab within the allotted time period but can present proof of an extended illness or family emergency must contact the head teaching assistant as soon a possible to make arrangements regarding the missed labs. you may receive a failing grade in the course. unlock your locker. All suspected violations of the Code of Academic Conduct will be referred to Student Judicial Affairs. Laboratory Make-Up Policy Students must attend the laboratory class for the section in which they are enrolled. other students and the TAs. Make sure that you avoid unauthorized collaboration and plagiarism. A-16 . Make sure to record the teaching assistant's name. If a student misses the last lab of the quarter. you must make it up by attending another scheduled laboratory section. it must be made up immediately. 2. date. 4. You must be on time for the start of the lab period. If a student misses a laboratory class. Have the TA collect your data sheet and he or she will give it to your regularly assigned teaching assistant. laboratory classes end one or two days before the end of the quarter. Consult the Class Schedule and Room Directory for a listing of rooms and times. You are encouraged to discuss your data and its analysis and interpretation with your lab partner. No laboratory report will be accepted without a valid copy of the data sheet. Go to the selected laboratory section and ask the teaching assistant if you may be admitted to make up a lab. 3. Laboratory Make-up Procedure You are required to complete all labs in order to pass the course and it is your responsibility to make up any missed labs promptly. Late reports will be met with a 5-point deduction for every calendar day the report is late.

turn off the balance by raising the tare bar. turn it on by pushing the tare bar down. A diagram of a balance is shown in Figure 1. Using the Balance A balance is used to measure the mass of an object. Open one of the sliding doors and be sure the balance pan and surrounding area is clean. You can clean it with a balance brush or Kimwipe. To do this simply place the weighing paper on the balance pan and be sure it is not touching the side.. A-17 . At the end of the period. To use the balance. Next shut the doors and press the tare bar to set the balance at zero.000 g.001 grams. Press the tare bar on the right side and the balance will then read 0. Now simply place the object to be weighed on the balance and measure the mass to 0. Now add the desired mass of solid and record the mass. The electronic readout should then be lit. Always clean the balance carefully after use. Each laboratory room contains two electronic balances that are very easy to use.D) Common Laboratory Procedures 1. Figure 1: The Balance Always use weighing paper when weighing solids to protect the balance. Always use the balance with extreme care as it is very expensive.

Never use a contaminated spatula. however the techniques shown in the Figure are still useful and should be carefully examined. never remove more solid from a bottle than is necessary. Simply discard it. Handling Solids Use a clean spatula to transfer solid from bottles.2. In the Chemistry 2 laboratories we are presently using weighing boats rather than weighing paper. Also. Figure 2: Solid Transfer A-18 . Below in Figure 2 is an illustration of how to properly weigh and transfer a solid using weighing paper. never return unused solid to the reagent bottle. To avoid waste.

always remove the cap/stopper and hold it in your hand. Never place the cap/stopper on the bench or contamination could result. Figure 4: Capping a Flask A-19 .3. as is shown below in Figure 3. Handling Liquids When transferring liquids from a reagent bottle. Capping a Flask During many experiments you will have to cap a flask to protect the contents from contamination. You may find the use of a glass rod helpful. Figure 3: Liquid Transfer 4. Figure 4 illustrates the proper method using Parafilm. Pour the liquid slowly and carefully to avoid spillage.

A graduated cylinder of the appropriate size can be used for measurements of moderate accuracy. While twirling the buret by the tip. Figure 5 shows the use of a card with a dark strip on it to sharpen the image of the meniscus. Next. this time also opening the stopcock when the buret is inverted to allow most of the water to drain back out of the tip. A pipet is commonly used to transfer an accurately known volume of a liquid from one container to another. Then. Repeat this operation two more times. While it is still upside down. Burets: With practice. empty the buret out the top by inverting it swiftly. add enough of the new solution to bring the liquid level up to about the 48 mL mark. fill the buret above the zero mark and drain the excess out the tip until the meniscus is within the calibrated portion of the buret. slowly empty it through the top. Be sure that no air A-20 . Open the stopcock and drain about 5 mL out of the tip. at the sink. First. cradle the top of the buret between the thumb and index finger of one hand. blot/wipe off the top of the buret with a laboratory tissue. Wait about 30 seconds for drainage and then close the stopcock. Figure 5: Reading the Meniscus You should always use the following procedure when changing the solution in a buret. Erlenmeyer flasks and graduated cylinders are usually filled/read by raising them to your eye rather than by squatting down to bring your eye level to the bench top.02 mL. and using a clean. However. you should take a moment to study its calibrations to insure that you know how to read them properly. In making any volume measurement. and then repeat the water washing. close the stopcock.5. Finally. the bottom of the meniscus will be very easy to see. being careful to wet the entire interior wall with the new solution. You will find by experiment that if the top of the strip is positioned slightly below the level of the liquid in the buret. turn the buret horizontal. the accuracy of such a transfer is only as good as the technique of the operator will allow. Before using a piece of glassware to make a volume measurement. the position of the meniscus of a liquid in the 25 mL burets used in the Chemistry 2 labs can be estimated to within 0. A beaker or Erlenmeyer flask can be used for rather rough measurements. drain part of the liquid out of the tip into a waste receiver. Then turn it upright. empty the buret out the top and half-fill it with deionized water. dry beaker for the transfer. and wipe off the tip with a laboratory tissue. While holding it by the tip with your other hand. Over the sink. The liquid level in a pipet is always lowered to the mark while the mark is held steady at eye level. the liquid level should always be the same as your eye level. Measuring Liquid Volumes Many glassware items have volume marks printed on them.

you can't get a good seal. except that you must use a bulb to suck the small doses of water or the new liquid into the pipet rather than pouring them in from a beaker. You might try conditioning your index fingertip first by rubbing it gently in the palm of the other hand. If your finger is too wet.bubbles are trapped in the tip. If you keep the pipet bottomed. since the 0. Do not attempt to bring the meniscus to 0. the illustrations in Figure 6 and some hands-on practice using deionized water should help you to become proficient fairly quickly. you can then remove the bulb and quickly seal the pipet mouth with the index finger of your "better" hand before the liquid level falls below the mark. In what follows. and touch the pointed tip of the pipet to a dry spot on its sidewall. we assume that the pipet has been pre-rinsed with the solution you want to transfer following essentially the same procedure as that described above for burets. Raise the over filled pipet vertically out of the vessel from which you are taking the measured sample and quickly put a beaker or some other waste receiver under it. Figure 6: Using a Pipet To begin a pipetting operation hold the pipet vertical and rest the pointed end on the bottom of the container from which you want to transfer a sample. The following instructions. tilt the receiver slightly. use a rubber bulb fitted with an Eppendorf tip to draw the liquid a few centimeters above the mark on the pipet. Raise the mark on the pipet to your eye level.00 line may not be in precisely the right place.00. Pipets: Students often experience some initial difficulty in using a pipet. With your least-dexterous hand. and if it is too dry. This method is both time consuming and unwise. you can't create a small enough crack (see below). (In this step some individuals have more success by slowly rotating the pipet using the thumb and the other fingers on the hand A-21 . If you now slightly rock your index finger you can open and close a tiny crack at the mouth of the pipet and thereby allow the liquid level in the pipet to fall exactly to the mark on its shaft.

6.) Be patient because if you overshoot the mark you must begin the whole process again. leaving the solid behind. You want to avoid splashing as much as possible. this setting may vary depending on the hot plate so you will have to experiment. and then remove it from the receiver. Once the paper has set. transfer the solution to be filtered. What this really means is that you should never blow the last drops out of them. that is. Always be careful to avoid burns and never heat a material too quickly or explosive "bumping" can occur. Keep the tip of the pipet in contact with the flask sidewall for at least 30 seconds after it looks empty. you will carefully pour out the liquid. this is shown in Figure 7. Figure 7: Fluting the Filter Paper You will then set the paper in the funnel using your wash bottle. Slowly add water to the sides with a circular motion to avoid air bubbles between the paper and the funnel. Never overwhelm the filter. place its tip against the receiver wall so that when take your finger off of the pipet mouth. Filtration You will often need to separate a liquid from a solid. At other times you will need to filter the solution. You must first flute the paper in order to accelerate the process. always use a A-22 . 7. Remove the accurately filled pipet from its container and while still tightly sealing its top with your finger. and then wash the solid as directed by the experimental procedure. To do this you will use filter paper and a funnel. Transfer the solid using a wash bottle and rubber policeman. Heating You will use both a hot plate and a Bunsen burner to heat solids and solutions.holding it. When using a hot plate always begin at the setting indicated in the manual. liquid will flow smoothly down to the bottom of the vessel. At times you will simply decant. If the solid has settled. To do this simply place the paper into the funnel and add a small amount of water to the bottom of the filter. However. Tilt the final receiver slightly and while holding the pipet vertical. The pipets in the Chemistry 2 laboratories are calibrated "to deliver" the specified quantity of liquid rather than "to contain" it. quickly dry the lower portion of the shaft with a single downward stroke of a laboratory tissue. In using a Bunsen burner. don't add the solution too quickly and never come to within one centimeter of the top of the paper. decant the liquid through the filter first in order to save time.

Figure 8: The Bunsen Burner 8. This measurement must be converted to mmHg. Control the heat transfer by adjusting the distance from the burner to the object. Note that the distances suggested in the manual are measured from the hottest part of the flame to the object.00 inch = 25.tight blue flame as shown in Figure 8. Barometric Readings and Unit Conversions There are barometers placed in each laboratory room that give the barometric pressure readings in inches of Hg. A-23 .4 mm. The conversion factor is 1.

pH Meter Operating Instructions.9. A-24 .

E) Maps A-25 .

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Additional containers may also be obtained from the dispensary. be sure to bring the empty containers to the dispensary. c. b. it is your responsibility to replace them before the lab starts. obtain the missing items from the surplus items in the laboratory. If for some reason you are not able to bring the broken item. Refilling of Chemical and Supply Containers When replacing or refilling general laboratory chemicals or supplies. Dispensing Policies The following outline concisely describes the various stockroom dispensary procedures that will be used this quarter. Please read this over carefully. In the case of chemical containers. a. Locker Supplies There will be a two-week grace period for filling out dispensing room slips when checking out supplies from the dispensary for your locker. you must bring the broken item or a representative portion thereof to the dispensary and fill out a dispensing slip for a replacement. Policies at the End of the Quarter Surplus Stores Any item you may have in surplus should be placed in the area set aside for surplus items in the laboratory (a box at the back of the lab). and discuss any questions you may have with your TA. Waste Containers Full waste containers may be exchanged for empties located below the fume hoods. you must fill out a dispensing room slip and have your TA sign it before you may obtain a replacement. Make sure that you have everything on your locker list by the end of the second week of instruction. If the missing item is not in the surplus area.F) Dispensary Procedures 1. Policies During the Quarter Locker Supplies If a locker item is broken after the initial two-week period. A-27 . be sure to return the tops or caps with the containers. Equipment on Loan from the Dispensary All equipment that is on loan from the dispensary must be returned to the dispensary at the end of each laboratory period. Policies at Beginning of Quarter Goggles You must use the approved goggles given to you in Chemistry 2A. Filling Locker Requirements If your locker is short of any items when you are checking your locker equipment against your locker list. If you have lost those goggles. obtain it from the dispensary.

Have your TA check the contents of the locker and if everything is present and clean then they will lock the drawer. Return all extra equipment to the extra glassware box in the lab.Preparing Your Locker for Check-In Clean and dry all equipment. A-28 . Replace all broken or missing items by checking them out from the stockroom.

2. Chem 2C Experiment Qualitative Analysis Chemical Waste Composition: Chloroform. Acetone WASTE ONLY Label is BLUE and is used only in Chem 2B A-29 . Zinc WASTE Label is WHITE and is used in all Chem 2 courses. Chromium. Dithizone. Lead Manganese. Waste Labels Chem 2 Experiments Cation Metal Waste Chemical Waste Composition: Bismuth. Cobalts. Copper. Silver.

Benzophenone. p-Dibromobeneze. p-Dichlorobenzene. Acetone.Chem 2B Experiment Colligative Properties Chemical Waste Composition: Cyclohexane. Naphthalene. WASTE ONLY Label is YELLOW and is used only in Chem 2B A-30 . Diphenyl.

non-mercury 2 25 ml Volumetric Flask 1 250 ml Volumetric Flask 1 5 ml Volumetric Pipet 1 10 ml Volumetric Pipet METAL EQUIPMENT 1 Beaker Tongs 1 Crucible Tongs 1 Scoopula 1 Test Tube Clamp CHEMISTRY 2 LOCKER LIST PORCELAIN 1 Small Casserole 1 Large Casserole 1 Evaporating Dish 2 Crucible 2 Crucible Cover PLASTIC WARE 1 250 ml Washing Bottle 1 25 ml Graduated Cylinder (may be glass) 1 Short Stem Funnel (may be glass) 2 1 L Bottle. Only safety goggles which have been approved by the Chemistry Department are acceptable GLASSWARE 1 100 ml Beaker 1 150 ml Beaker 1 250 ml Beaker 1 400 ml Beaker 1 800 ml Beaker 1 50 ml Erlenmeyer Flask 2 125 ml Erlenmeyer Flask 2 250 or 300 ml Erlenmeyer Flask 2 500 ml Erlenmeyer Flask 1 100mm Watch Glass 2 Glass Stir Rod 10 Test Tubes (rounded end) 6 Centrifuge Tubes (pointed end) 2 Thermometer. Return all extra equipment to the extra glassware box in lab. Locker Inventory Procedure for beginning of quarter (1) Replace broken or missing items in your locker in the first two weeks. Alkacid Test Paper 1 Sponge 2 Rubber Policeman 1 Wire Triangle. (2) Replace all broken or missing items by checking them out from the stockroom. Student Name ____________________________________________________ T.3. ____________ (print) (initial) A-31 . square 1 Desiccator 1 Pipet bulb w/ Tip 1 Plastic Test Tube Rack OTHER 1 Centrifuge Tube Brush (pointed end) 1 Test Tube Brush (rounded end) 2 Match Books 1 Vial. They may be checked out from the stockroom (Room 1060). Pipe Stem Covered 1 Wire Gauze Square COMMUNITY SUPPLIES SHELVES 50 ml Buret AT LAB BENCH Bunsen Burner w/ Silicone Rubber Tubing Procedure for end of Quarter COMMUNITY LOCKERS 8" Extension Clamp Clamp Holder Small Support Ring Large Support Ring (1) Clean and dry all equipment. (3) Have your TA check your equipment and initial below.A. They must be worn AT ALL TIMES when in the laboratory. All excess equipment should be placed in the extra glassware box (red) in the lab room. including during locker check out. (2) One pair of SAFETY GOGGLES will be supplied to each Chem 2A student.

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