Acetic Acid Concentration of “JUICY ORCHARD” Apple Cider Collin College Bassam Attili, PhD, Dawn Richardson, PhD and Fred Jury, PhD JUICY ORCHARD, home of the world’s sweetest cider, has contracted us to help with a problem from their past shipment of apple cider. It seems that 30,000 gallons of premium grade A cider has been returned due to taste (acidity) concerns. It will be our task to determine the level of acidity in these samples. Cider becomes more acidic through the formation of acetic acid. Hence, you will be titrating the acetic acid to determine its concentration in the cider samples. To carry out this task, you will need to use the titration process to calculate the concentration of acetic acid. You need to titrate six samples; three for standardizing the NaOH solution to be used to determine the acid in three cider samples. Objectives: The main objective is to determine the concentration of acetic acid in apple cider using a standardized NaOH solution. In addition, you will learn how to prepare solutions. the fundamental concepts associated with titration. the useful technique of titration. how to obtain titration data and perform titration calculations at the end point to determine the molarity of NaOH Materials: NaOH pellets, apple cider, weighing boats, 250 ml volumetric flasks, 50 mL burettes, burette clamps, 250 ml plastic bottles to hold the prepared NaOH solution, ring stands, 3 Erlenmeyer flasks (125 or 250 mL) for each group, 50 mL graduated cylinders, phenolphthalein solution, potassium hydrogen phthalate (KHP). Introduction: Sodium Hydroxide: Many analytical procedures involve comparison of an unknown with a standard. NaOH is not a suitable primary standard. Solid NaOH is highly hygroscopic (it absorbs water from the air). It also absorbs carbon dioxide from the air, forming sodium carbonate and thereby reducing the amount of sodium hydroxide present. When weighing a sample of NaOH, you do not know the exact amount of NaOH in the sample due to the previously stated properties of solid NaOH. This means that an exact known molarity of NaOH cannot be directly prepared. We can only prepare a solution of NaOH that has an approximate concentration. In this case, an acid that can be weighed directly is used as the primary standard to determine the exact concentration of the NaOH solution. The primary standard used here is potassium hydrogen phthalate (KC8H5O4, often abbreviated KHP). Potassium hydrogen phthalate is a weak monoprotic acid. It is available as a pure, stable, fine crystalline solid that can be accurately weighed. A KHP sample of known mass (and, therefore, known moles) can be titrated with the NaOH solution to determine very precisely the concentration of the NaOH. This procedure is called standardizing the NaOH solution. KHP reacts with NaOH as shown below. The stoichiometry of the reaction indicates that one mole of potassium hydrogen phthalate reacts with one mole of NaOH. The acidic solution of KHP is colorless when phenolphthalein indicator is added. When enough NaOH has been added to react stoichiometrically with the acid, the indicator in the solution will be very slightly pink for 30 seconds or longer. This is called the endpoint of the titration. If just one more drop of NaOH (or even a portion of a drop) is added, the solution will possess excess NaOH reactant, which will make the solution appear more intensely pink. At the endpoint, the moles of acid will equal the moles of base added (practically if not exactly). The molarity (M) of the NaOH can then be determined using the moles and the volume of NaOH in the sample used. This is the standardization of a base. M NaOH = [(mol of NaOH) / (L of NaOH solution)] Once this concentration is determined, the average of three trials, the NaOH solution can serve as a standard to determine the concentration of vinegar (acetic acid) in apple cider. Apple cider: The exact volume of apple cider must be accurately measured. NaOH standard solution should be added until the end point; a light pink color appears and stays for 30 seconds or more. Three samples should be titrated and the average should be reported as the concentration of the acetic acid in the cider. Caution: Put on your CHEMICAL SPLASH-PROOF SAFETY GOGGLES! NaOH reacts with the proteins in the top layer of your skin making it feel slippery. You will not feel any pain or itching. When this occurs, simply wash your skin with plenty of soap and water. Keep washing the affected area for no less than 10 minutes. Procedures: Begin by preparing 250. mL of approximately 0.1 M NaOH using a volumetric flask. This solution will be used to titrate a measured mass of KHP (about 0.3 grams). Wash your burette with soap and water till there are no beads of water on the inside of the burette. Rinse the burette with two one-mL portions of your NaOH solution then fill the burette with your NaOH solution up to the zero mark (it need not be exactly at 0.00 mL). Add about twenty milliliters of distilled water to the weighed KHP sample in an Erlenmeyer flask. Stir until all the KHP has dissolved. You may have to slightly heat for all the KHP to dissolve. Add 2-3 drops of the phenolphthalein indicator to the solution. Start titrating the KHP with your prepared NaOH solution. Be sure to record the exact initial burette volume before you begin. Rinse the sides of the flask as you go to make sure all the added NaOH is in solution. The phenolphthalein will change color from colorless to pink when enough base is added. Record the volume of NaOH that you added to obtain a color change of the solution that persists for 30 seconds or longer. Repeat the titration two times, each time with a weighed sample of KHP and refill your NaOH burette. Use the same procedure to titrate thee samples of apple cider (acetic acid) with the standardized NaOH. Pre-lab Questions: 1. Why should the buret be rinsed with NaOH before it is filled? 2. Why does a pink color appear, and then disappear quickly, at the point where the NaOH solution comes in contact with the solution in the flask? 3. What is the concentration of a NaOH solution if 32.47 mL of it are required to neutralize 1.27 g of KHP? 4. Write the balanced chemical equation of the reaction between acetic acid and NaOH. 5. Why must air bubbles be expelled from the burette tip? 6. If the NaOH was diluted to half of its original concentration, what affect would this have on the titration? Post-lab Questions: 1. Determine the number of moles of acid used in each titration. 2. Calculate the molarity (mol/L) of the NaOH solution for each titration as well as the mean molarity for the trials. 3. An impure sample of potassium hydrogen phthalate was titrated to determine the percent composition KHP. What is the percentage of potassium hydrogen phthalate if 2.81 g of the mixture required 35.61 mL of 0.152 mol/L NaOH to reach the end point? 4. Calculations of acetic acid concentration (M) for each trial and calculate the average.