Titration Lab

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Acid-Base Titration
Titration is a laboratory technique that can be used to determine the concentration of certain solutions by chemical reaction. A standard solution of known concentration is titrated against (reacted with) a solution of unknown concentration. An indicator can signal the completion of the reaction (by color change) and the concentration of the unknown solution can be determined. Any chemicals that react in solution can be titrated with each other. Since acids and bases are usually found in solution, they are commonly involved in titrations. Titrations involving a strong acid or a strong base involve the neutralization reaction between hydrogen ions and hydroxide ions. These ions combine to form the neutral water molecule: H+ + OH- H2O When carrying out an acid-base titration, you must be able to recognize when to stop adding the standard solution. You must stop exactly when neutralization is reached: this is the equivalence point. At this point, the number of hydrogen ions added from the acid equals the number of hydroxide ions added from the base. The indicator mentioned above helps you stop at just the right time. A sudden change in color of the indicator signals that neutralization has occurred and you must end the titration. Thus, the point of color change is called the end point. The indicator must be carefully chosen so that the end point corresponds with the equivalence point. If the wrong indicator is used, the color change may occur too early or too late and you will have added too little or too much of the second chemical. When the endpoint is reached, the volume of the known and unknown solutions used are carefully determined. These volumes and the known concentration of the known solution can be used to calculate the concentration of the unknown solution by stoichiometry. There are many ways to perform the titration calculation, but they are all based on stoichiometry. Thus, the balanced reaction that occurs must be known! PURPOSE: 1. To determine the molarity of a solution of NaOH by titrating it with a known solution of HCl. 2. To verify the molar mass of oxalic acid by titration. 3. To practice single and double buret titrations EQUIPMENT / MATERIALS: two 50 mL burets one 250 mL beaker (for rinsing and titration) ring stand two or three 100 or 150 mL beakers (for acid, base, and extra) butterfly buret clamp HCl (known concentration) phenolphthalein NaOH (unknown concentration) oxalic acid (part II) ** SAFETY AND LAB TIPS - Acids and bases are corrosive and can cause severe injury. Be very careful with these chemicals.

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If any should spill on you, begin rinsing the affected area immediately and report the incident to your instructor. It is especially important to rinse your eyes as soon as possible if they come into contact with your eyes. Also immediately report spills to your instructor. They may need to be neutralized and cleaned up with spill pillows. - Always be sure your buret stopcocks are closed before pouring in any acid or base. - Always use a small beaker or graduated cylinder to pour acid or base into a buret. - Careful control of the buret stopcock is critical to efficient and accurate titration.
PRE-LAB 1. Write the equation for the neutralization reaction between NaOH and HCl. 2. What is the chemical formula of oxalic acid? Calculate its molar mass. 3. When performing titrations, why should the beaker be constantly swirled? 4. Why is it good to perform a titration 3 or 4 times? 5. How will you know when the HCl has been neutralized in part 1? 6. What is the difference between the end point and the equivalence point? How are they related to the indicator? 7. Describe the safety procedure to be used in the event that acid spills on you or on the lab counter or on the floor.

PROCEDURE, PART 1. Double buret titration- unknown NaOH. 1. Obtain two burets, a butterfly buret clamp, and ring stand and set up in the appropriate fashion. (See figure, this page) One buret is for acid and one for base. Fill your 2 small beakers with 6065 mL of acid or base. Be sure to record the known concentration of the acid! 2. Clean out both burets by filling with tap water from a beaker and draining it all out. Make sure the stopcock works at this time. 3. Rinse the acid buret by adding about 5-10 mL of HCl solution and swirl while slowly emptying the buret (from the large opening). 4. Rinse the base buret by adding about 5-10 mL of NaOH solution and swirl while slowly emptying the buret (from the large opening). 5. Add HCl solution to your acid buret to about the 0 mL mark or above. Using the stopcock, draw off liquid until air bubbles are gone and the level (bottom of the meniscus) is just below the 0 mL marking. Take your initial reading. Record in your data table. 6. Add NaOH solution to your base buret to about the 0 mL mark or above. Using the stopcock, draw off liquid until air bubbles are gone and the level (bottom of the meniscus) is just below the 0 mL marking. This is your initial reading. Record in your data table. 7. Obtain a 250 mL beaker to perform the titration. Add to this approximately 10-15 mL of HCl

Titration Lab

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from the acid buret. Now add one or two drops of phenolphthalein solution. 8. From your base buret add NaOH and gently swirl the beaker so the solution will mix. Continue to add the NaOH until a very pale pink color lasts throughout the solution for a period of 15 seconds. To find the end point, back titrate by adding acid one drop at a time until one drop of acid removes the pink. At this point, about one drop either way should change the color. Now take your final buret readings (both burets!). Discard the neutralized solution in your sink. 9. First trial only: subtract your initial and final readings and have your teacher check your result to make sure you are in the ballpark. 10. Without refilling your burets, take your new initial readings and repeat procedures 7 & 8 for three more times. If you do not disturb your burets after one trial, your final readings for that trial will be the same as the initial readings on the next trial. 11. If continuing on to part II, save your base, but dispose of your acid in the waste container. If not doing part 2, place all untitrated solutions in waste containers, rinse and brush all equipment and clean your area. all units mL initial reading final reading volume used known concentration of acid: ____________ LAB PROCEDURE PART 2: Single buret titration. 1. Keep the same base buret from part 1. If you have at least 15 mL of base go on to step 2. If you have less than 15 mL, add some more base to the buret. 2. Mass out between 0.2 and 0.25 gram of oxalic acid, H2C2O4. Record the exact mass of acid used. 3. Dissolve the acid in approximately 50 mL of water. Once dissolved, carefully measure the volume of the acid solution. 4. Place all of the acid solution in a beaker or Erlenmeyer for titration. 5. Now titrate the acid with the base. Use the skills you developed in Part 1 of this lab. You must also be very careful because you have no acid buret to back titrate. 6. Place all untitrated acid or base solutions in waste containers, rinse and brush all equipment, and clean your area. Buret readings initial (NaOH) final volume used Trial 1 HCl NaOH Trial 2 HCl NaOH Trial 3 HCl NaOH Trial 4 HCl NaOH

if given known concentration of base: ____________

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mass of oxalic acid used: ___________

volume of oxalic acid solution: ______________

PROCESSING: (complete on a separate sheet) Part 1: 1. Determine the molarity of the base in each trial and calculate the average molarity of the base. (Show calculations clearly at least once). See processing hints at the end of the handout. Part 2: 2. Using the molarity of your base (use the value given by your teacher if available, if not use your answer from processing part 1), determine the molarity of the acid solution you made through titration calculation. Do not use the molar mass of oxalic acid! 3. The molar mass of the acid can be calculated by dividing the measured mass of acid by the moles that were calculated as part of the previous question. Calculate the molar mass of the oxalic acid. 4. The accepted value for the molar mass of oxalic acid is actually 126.1 g/mol. Calculate your percent error.

ADDITIONAL QUESTIONS: 1. Which solution of known concentration would you use when titrating against a solution of vinegar: acid or base? Why? (Hint: what is vinegar?) 2. How would your final result for the concentration of the base in part I have differed if you did the experiment with H2SO4 (a strong diprotic acid) instead of HCl? Explain. 3. If 30.0 mL of 0.500 M KOH are needed to neutralize 10.0 mL of HCl of unknown concentration, what is the molarity of the HCl? 4. How many mL of 0.100 M NaOH are needed to titrate 20.0 mL of 0.100 M H2SO4? Use a balanced equation for the neutralization reaction and explain your calculations. Extra credit: 1) Assume you calculated the molarity of the sodium hydroxide solution just as you did in the lab, but you made the following errors in the experiment. Explain clearly what each of the following would mean about the molarity of NaOH calculated in part 1 compared to the true value. Are your calculations too high, too low, or unaffected? a. the actual concentration of HCl was lower than stated b. You spilled a drop of base during titration (it wasnt collected in the titration flask).

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c. Extra water was left in the acid buret before you added the acid. d. An air bubble was initially present in the base buret and escaped during the titration. 2) Describe the idea of hydrates and water of crystallization and use it to explain why the given molar mass of oxalic acid does not match your prelab value. As always, cite your sources!

Processing guide for titrations:

0.0268 L Ca(OH) 2

2 mol HNO 3 0.40 mol Ca(OH) 2 = 0.214mol HNO 3 1 L Ca(OH) 2 1 mol Ca(OH) 2
Mole it ratio it done!

3) Put it all together: Molarity =

mol (HNO3) = 0.214 mol = 5.76 M L HNO3 solution 0.0372 L