Introduction to Titration

1. Standardization of NaOH with Potassium Hydrogenphthalate (KHC₈H₄O₄)

1. To begin, the titrant, sodium hydroxide, must be standardized. Prepare a stock NaOH solution by dissolving about 4 g of NaOH pellet in 100 mL of deionized water. Note that NaOH is a hazardous chemical which is corrosive to skin and irritant to eye, be cautious and wear proper personal protection equipment (PPE) to avoid skin or eye contact.
2. Make a 1:10 dilution of the sodium hydroxide solution by adding 25 mL of the stock sodium hydroxide solution to a 500-mL bottle. Sodium hydroxide absorbs carbon dioxide. It is important to prevent this by making sure to use boiled, deionized water, an oven-dried bottle, and to cap the bottle quickly. Make the solution up to 250 mL with the deionized water and shake to mix.
3. Dry 4–5 g of the primary standard acid, KHC₈H₄O₄ at 110 °C for 4 h in a drying oven and then cool the solid in a desiccator for 1 h.
4. Dissolve about 4 g of dried KHC₈H₄O₄ in 250 mL of deionized water. Record the mass accurately. Calculate the molar concentration of the KHC₈H₄O₄ solution.
5. Pipette 25 mL of KHC₈H₄O₄ into a clean and dry Erlenmeyer flask. Add 2 drops of phenolphthalein, and swirl gently to mix well. Note that phenolphthalein is toxic and irritant, be cautious to avoid skin or eye contact.
6. Clean a 50-mL burette and a funnel thoroughly with detergent and water. Flush the burette with water and rinse 3x with deionized water. Rinse the burette with the diluted NaOH solution 3x, making sure that the NaOH wets the entire inner surface and drain the waste through the tip. Mount the washed burette on a ringstand with a clamp and ensure that it stands vertically.
7. Fill the clean burette with the diluted NaOH solution. It should be noted that the amount of the diluted NaOH needs not be exactly at the zero mark but should be within the scale and sufficient for at least one titration. Air bubbles may affect the accuracy of volume reading. Carefully check the burette for air bubbles, and gently tap the burette to free them and open the stopcock to let a few mL of titrant to flow through and at the same time releasing any trapped air. Read the volume by viewing the bottom of the meniscus after 10 s. Record this initial volume. Pay attention to the significant figures of the reading. Record the value to two decimal places in mL.
8. Place the Erlenmeyer flask containing potassium hydrogen phthalate (KHC₈H₄O₄) under the burette and adjust the height of the burette properly. Titrate the KHC₈H₄O₄ solution by slowly adding NaOH solution in 1–2 mL increments using one hand to control the flow rate by adjusting the stopcock, and the other swirling the flask.
9. When close to the endpoint, begin adding the titrant drop by drop. The endpoint is reached when the solution turns a faint, persistent pink color. Record the final volume of the diluted NaOH in the burette.
10. Repeat the titration at least twice more to obtain consistent data. Calculate the molar concentration of the diluted NaOH solution.

2. Titration of Vinegar with Standardized Sodium Hydroxide Solution

1. The sodium hydroxide solution is now standardized and can be used as a titrant to analyze vinegar. To reduce the pungent aroma of vinegar, dilute 10 mL of the vinegar solution to be tested in a 1:10 ration to a total volume of 100 mL.
2. Pipette 25 mL of analyte, to a clean and dry Erlenmeyer flask (noted as V_A). Add 2 drops of phenolphthalein.
3. Fill the burette with the standardized NaOH solution from the first part of the Procedure. Record the initial volume of titrant (V₁).
4. Progressively add the standardized NaOH solution to the vinegar. When the volume of titrant approaches the expected value, adjust the stopcock to add the titrant drop by drop. Continue to swirl the flask with one hand and keep the other hand ready to close the stopcock. Once the analyte solution changes to light pink color, swirl for a few seconds to see whether the color will fade. If the color persists, the titration reaches the end point. Record the final volume of titrant (V₁^'). If the solution color fades, add one more drop of titrant. Wash the bottom tip of the burette using the wash bottle. Collect the washed mixture and watch the color change of the analyte solution. Continue the titration till the end point. Record the amount of titrant needed (V_t1 = V₁' V₁).
5. Repeat the titration at least twice until three concordant values that are within 0.1 mL of one another is obtained (V_t2 and V_t3).
6. Calculate the mean value of titrant volume using the three values obtained in three different titrations: V_t = (V_t1 + V_t2 + V_t3)/3. The molar concentration of acetic acid in vinegar can be thus calculated using Equation 3.