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Titration Analysis of Various Unknown Acids Purpose In this experiment, a solution of NaOH, an approximate molarity, will be standardized using

potassium hydrogen phthalate, and the standardized solution of NaOH will be used to determine the concentration of a hydrochloric acid solution of unknown molarity. Background Students will prepare a solution of sodium hydroxide (NaOH) with an approximate concentration of 0.100 M. In order to make accurate determinations based on this solution, it must be standardized. The primary standard used in this experiment will be potassium hydrogen phthalate, also known as potassium acid phthalate, or simply as KHP. The molecular structure of KHP can be seen in Figure 1.

Figure 1. Potassium hydrogen phthalate (KHP)

The hydrogen in KHP is slightly acidic, and it is often used as a primary standard for acid-base titrations because it is solid and air-stable, making it easy to weigh accurately. It is, however, slightly hygroscopic and is generally kept in a desiccator before use. A solution of KHP will be titrated with the NaOH solution that is prepared in the first portion of this experiment. The results of the titration will be used to calculate the exact molar concentration of the NaOH solution. The standardized NaOH solution will then be titrated into a solution of hydrochloric acid (HCl). The amount of NaOH required to completely neutralize the acid (Reaction 1) will then be used to calculate the exact molar concentration of the unknown acid solution.

HCl( aq) NaOH ( aq) NaCl ( aq) H 2 O(l )


Reaction 1. Neutralization of hydrochloric acid with sodium hydroxide

Procedure Preparation of Sodium Hydroxide Solution 1. Weigh out between 1.900-2.100 g of NaOH on the analytical balance. Transfer the solid NaOH to a test tube. Add 5 mL of DI water to the solid NaOH in order to dissolve. CAUTION: The dissolving of sodium hydroxide (NaOH) in water is extremely exothermic! 2. Filter the concentrated NaOH solution into a 500 mL polyethylene bottle. Be sure to wash the inside of the test tube with several portions of DI water. These washings should be sent through the filter as well. CAUTION: Concentrated sodium hydroxide (NaOH) is extremely caustic! Do not get any of the solution on your hands or clothes. It is highly recommended that you wear gloves when handling this reagent! 1|Page

Titration Analysis of Various Unknown Acids

CHEM 1412

3. Fill the remainder of the polyethylene bottle with DI water. Do not completely fill the bottle. Stop when the liquid level reaches the fill mark on the side of the bottle. Securely cap and shake the bottle to ensure that the solution is homogeneous. Standardization of Sodium Hydroxide Solution 1. For this experiment you will again work in pairs. Condition your buret by rinsing with several portions of the NaOH solution and discarding the rinse solution. 2. After conditioning fill the buret with NaOH to above the 0.00 mark and then open the stop cock fully to remove any air bubble from the buret nozzle. You want to remove any air bubble from the nozzle since that can cause an error if the bubble is dislodged during the titration. Lower the liquid level below the 0.00 mark. 3. In a desiccator, you will find a weighing bottle or beaker with some previously dried primary standard KHP. Using an analytical balance weigh out three trials between 0.6 and 0.7 grams of KHP into separate 150 mL Erlenmeyer flasks. You should not be so concerned with a specific amount, but you must record the mass to 0.001 grams. 4. Once you have the KHP samples weighed, add 50 mL DI water to the Erlenmeyers and allow the KHP to completely dissolve before starting the titrations. KHP is soluble in water but will dissolve more quickly if you stir and swirl the solution. Figure 2. Buret diagram 5. Once the KHP is dissolved, add several drops of Phenolphthalein indicator to the flask and rinse down the sidewalls of the flask with DI water. 6. Record the initial volume of NaOH. Then, titrate the KHP solution to the faintest pink you can see that is persistent for several minutes. The fainter the pink the better. You will want to repeat the experiment until at least 3 reliable trials are obtained. 7. Using your data, calculate the molarity of the NaOH for each trial to make sure your results are reliable. Remember the mass of KHP will vary slightly for each trial so you cant determine how consistent your results are by observing the titration volumes. 8. Calculate and record the average molarity of the NaOH solution. Determination of Unknown Hydrochloric Acid Solution Concentration 1. Once you have obtained reliable data for the molarity of the NaOH, collect 150 mL of an unknown HCl solution in a 250 mL Erlenmeyer or other similarly sized container. Keep the top of the Erlenmeyer covered with parafilm. 2. Condition a pipet by rinsing with the solution several times making sure the pipet drains properly. Pipet 25 mL of the HCl solution into another 150 mL Erlenmeyer flask. Add several drops of Phenolphthalein indicator. 3. Titrate the HCl with the standardized NaOH solution to a pink endpoint as was done during the standardization procedure. The best endpoint will not persist more than several minutes. 4. Repeat the titration to obtain 3 reliable results. Calculate the molar concentration of the unknown acid solution based on each of the 3 reliable titrations.