Acid Base Titration

 


Purpose: To determine the concentration of a solution of hydrochloric acid using a primary standard (solid Na2CO3) and a secondary standard (aqueous, standardized NaOH).

Procedure:

Preparation of a solution of hydrochloric acid

Each group of 4 students will prepare 1L of 0.1M HCl from concentrated HCl (12M): Fill a 600 mL beaker to the 250 mL mark with de-ionized water. In the hood, add 8.3± .2 mL of con HCl (approximately 12M) to the beaker and stir. (Record the actual volume of con HCl used.) At your desk, transfer the liquid into a 1L volumetric flask using a funnel. Rinse the beaker once with de-ionized water and add the rinse to the flask. Dilute to the 1L mark. Mix thoroughly.

The actual concentration of this solution to 3 significant figures is the unknown in today’s lab.

Titration with a primary standard
  1. Weigh out 0.25 ± .05 g of dry Na2CO3. Record actual mass used to nearest .001 g. Transfer the solid to a 250 mL Erlenmeyer flask, rinse the weigh paper into the flask with a small amount of de-ionized water and dissolve the solid with 25 mL of de-ionized water. Add 3 drops of bromcresol green once the solid is dissolved.
  2. Clean and check the flow rate of a buret (as described in the handbook).
  3. Rinse the buret 3 times with 5 mL of the 0.1M HCl solution to be titrated. Discard the rinses. With the stopcock open and over a beaker, begin filling the buret with 0.1M HCl solution. Have your lab partner close the stopcock once the tip is draining and the volume is above the stopcock. This will prevent bubbles from forming in the stopcock during the filling process. Finish filling the buret to within a few mL of the zero mark. Record this volume as the initial volume in the titration. (Note that this is NOT the volume of liquid in the buret.)
  4. Begin titrating the sodium carbonate solution with the hydrochloric acid solution by adding small increments of the titrant from the buret. Swirl the reaction mixture between additions. Use smaller increments of HCl as you get closer to the expected endpoint (Pre-Lab question 2). The acid-base indicator, bromcresol green, will eventually turn from blue, which indicates an excess of Na2CO3, to yellow, which indicates an excess of HCl. The endpoint will be when the solution remains green, which indicates that the stoichiometric quantity of HCl has been added.
  5. Once the solution is green, bring it to a gentle boil on a hot plate to expel all dissolved carbon dioxide. Remove it from the hot plate to a wire gauze, and rinse the inside surfaces with a small amount of de-ionized water. If the solution stays green, the titration is complete. Record this volume as the final volume of titrant. If it turns blue, allow it to cool, and complete the titration by adding a few drops more of titrant. If the solution is yellow, you have overshot the endpoint and must repeat the titration.
Step 5 is necessary because one of the products of the titration is carbon dioxide. The carbon dioxide will react with water to form carbonic acid which can cause the reaction mixture to become acidic prior to the addition of enough HCl to neutralize the Na2CO3. If this happens, the indicator will change color early, and you will have a "premature endpoint". 6. Flush the neutralized solution down the drain with lots of water. Repeat the titration until you have 3 titrations whose molarity are within ±.0006 of the average.

7. Rinse the buret thoroughly with tap water (3 times) then 3 times with de-ionized water. Verify that the final rinse is neutral by placing a drop from the buret on blue litmus paper. If it is still acidic, the blue litmus will turn pink.
 


Titration with a secondary standard


 
 
  1. Pipet 25 mL of the HCl solution into a 250-mL Erlenmeyer flask. Add 50 mL of de-ionized water and 3 drops of phenolphthalein.
  2. Rinse the buret 3 times with 10 mL of the standard NaOH solution. Discard the rinses. With the stopcock open and over a beaker, begin filling the buret with the NaOH solution. Have your lab partner close the stopcock once the tip is draining and the volume is above the stopcock. This will prevent bubbles from forming in the stopcock during the filling process. Finish filling the buret to near the zero mark. Record the precise concentration of the standard NaOH solution and the Vinitial in your notebook.
3. Start adding the NaOH to the HCl solution in the Erlenmeyer flask, swirling the flask thoroughly between additions. Use smaller increments of NaOH as the color of pink begins appearing in the flask. Add drop-wise when the color seems to last a long time before disappearing. The endpoint is the volume of NaOH needed for the color to remain a pale pink (not fuschia!) Record this volume as the Vfinal. Phenolphthalein, the acid-base indicator, will turn pink at a slight excess of hydroxide ion.

4. Flush the contents of the beaker down the drain with lots of water. Rinse the buret thoroughly with tap water (3 times) then 3 times with de-ionized water. Verify that the final rinse is neutral by placing a drop from the buret on red litmus paper. If it is still basic, the red litmus will turn blue.
 


PROCESSING THE DATA

Part I Titration with a Primary Standard


 
 
For each titration, calculate the molarity of the hydrochloric acid solution using the volume of HCl needed to achieve the endpoint of the titration, the mass of the sodium carbonate and a balanced equation for the reaction. Determine the average and verify that you have three results that are within .0006 of your average. Don’t forget to propagate the error through your calculations!
 
 
Part II Titration with a Secondary Standard

 
 
Calculate the molarity of the hydrochloric acid, using the volume of NaOH needed to reach endpoint, the molarity of the standard NaOH solution, the volume of HCl pipetted and a balanced equation for the reaction. . Don’t forget to propagate the error through your calculations!

Compare the molarity determined using a primary standard and the molarity determined using a secondary standard. Which molarity do you think is the most reliable and why? Use this molarity as your accepted value to calculate the %error.

Pre Laboratory Assignment

Post lab Questions:
  1. Calculate the approximate concentration of a hydrochloric acid solution prepared by diluting 100 mL of 12.3M HCl to 2.00 liter.
  2. Calculate the approximate volume of 0.095 M HCl needed to neutralize 0.25g of sodium carbonate. Hint: Write a balanced equation first.
  3. Calculate the approximate volume of 0.0879 M NaOH needed to neutralize 25.0 mL of 0.095 M HCl. Hint: Write a balanced equation first.
  4. Write an equation (including states) for the reaction between carbon dioxide gas and water. Why is this reaction significant in this experiment?
  5. A student failed to rinse a damp buret with a small amount of the acid before filling it with acid. (p 23 lab handbook). Will more or less titrant (acid) be required to neutralize the sodium carbonate?
Your report should be in the following format:

Purpose: What you are doing in the lab. The question you are answering.

Procedure & apparatus: A description of the procedure. This can be simply the statement: "As given in the lab handout." It should include any modifications to the experiment.

Data: This section contains all observations, including tables with measurements, etc.

Calculations: This section must show samples of all of the different types of calculations. Include any graphs in this section. Show at least one sample calculation for the Na2CO3 titration and one calculation for the NaOH calculation. You may feel free to show the entire square method.

Discussion and errors. A section that describes your results and how good you think your results are. (For example: Although the density of my metal is close to the literature value for gold my results varied widely and the sample did not look like gold.) Although you may have more, you must describe at least 4 sources of error.

The first line in this section could be "My data is good (or bad) because ……)

Another paragraph should be "My errors include..

1.

2.
 
 
 
 

Modifications: Describe at least one modification you would make to improve the accuracy of the procedure. (Presumably it fixes one of the errors you described.)

Conclusion: It is the answer to the problem posed in the purpose In this case, " The concentration of the HCl was _____ from a ....

Answers to the post laboratory questions: Answers to the post laboratory questions.