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Richard Megna/Fundamental Photographs Experiment 10

Vinegar Analysis

Vinegar is a 4–5% (by mass) solution in acetic acid.

• To determine the percent by mass of acetic acid in vinegar Objective

The following techniques are used in the Experimental Procedure: Techniques

Household vinegar is a 4–5% (by mass) acetic acid, CH3COOH, solution (4% is the Introduction
minimum federal standard). Generally, caramel flavoring and coloring are also added
to make the product aesthetically more appealing.
A volumetric analysis using the titration technique is the method used for determin-
ing the percent by mass of acetic acid in vinegar. A measured mass of vinegar is titrated
to the phenolphthalein endpoint with a measured volume of a standardized sodium
hydroxide solution. Since the volume and molar concentration of the standardized NaOH
solution are known, the moles of NaOH used for the analysis are also known.
mol NaOH
mol NaOH = L NaOH solution (10.1)
L NaOH solution
From the balanced equation:
CH3COOH(aq) + NaOH(aq) —› NaCH3CO2(aq) + H2O(l) (10.2)
mol CH3COOH = mol NaOH (10.3)
The mass of CH3COOH in the vinegar is calculated from the measured moles of
CH3COOH neutralized in the reaction and its molar mass, 60.05 g/mol:
60.05 g CH3COOH
mass(g) of CH3COOH = mol CH3COOH (10.4)
mol CH3COOH
Finally, the percent by mass of CH3COOH in vinegar is calculated:
mass (g) of CH3COOH
% by mass of CH3COOH = 100 (10.5)
mass (g) of vinegar

Procedure Overview: Samples of one or two vinegars are analyzed for the amount Experimental
of acetic acid in the sample. A titration setup is used for the analysis, using a standard-
ized NaOH solution as the titrant and phenolphthalein as the indicator. Procedure

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A standardized NaOH solution was prepared in Experiment 9. If that solution was

saved, it is to be used for this experiment. If the solution was not saved, you either must
again prepare and standardize the solution (Experiment 9, Part A) or obtain about 150 mL
of a standardized NaOH solution prepared by stockroom personnel. Your instructor will
advise you.
Be aware of the number of significant figures when recording data.

A. Preparation of Check with your laboratory instructor to determine if you are to analyze one or two vine-
Vinegar Sample gars. Either obtain 15 mL of a single vinegar or 10 mL of each of two vinegars in sepa-
rate 10-mL graduated cylinders. Clean at least two 125- or 250-mL Erlenmeyer flasks.
1. Calculate the volume of vinegar. Calculate the volume of vinegar that would be
needed for the neutralization of 25 mL of the standardized NaOH solution.
Assume the vinegar has a density of 1 g/mL and a percent acetic acid of 5% by
mass, and the standardized NaOH solution is 0.1 M NaOH. Show the calculation
on the Report Sheet (see Prelaboratory Assignment, question 1).
Data Analysis, A 2. Prepare the vinegar sample. Add the (approximate) calculated volume (from Part
A.1) of one brand of vinegar to a clean dry 125- or 250-mL Erlenmeyer flask with a
previously measured mass (±0.01 g) or a flask that has already been tared on the bal-
ance. Record the tared mass of the vinegar sample. Add 2 drops of phenolphthalein
and rinse the wall of the flask with 20 mL of previously boiled, deionized water.
3. Prepare the buret and titration setup. Rinse twice a clean 50-mL buret with
~5 mL of the standardized NaOH solution, making certain no drops cling to the
inside wall. Fill the buret with the standardized NaOH solution, eliminate all air
bubbles in the buret tip, and, after 10–15 seconds, read and record the initial vol-
ume (see Technique 16C.2). Place a sheet of white paper beneath the flask con-
taining the vinegar sample.

B. Analysis of Record the exact molar concentration of the NaOH solution on the Report Sheet, B.4.
Vinegar Sample
1. Titrate the vinegar sample. Slowly add the NaOH solution from the buret to the
acid, swirling the flask (with the proper hand1) after each addition. Occasionally,
rinse the wall of the flask with previously boiled, deionized water from your wash
bottle. Continue addition of the NaOH titrant until the endpoint is reached.2 See
Courtesy of Thermo Fisher Scientific

Technique 16C.4. After 10–15 seconds, read (Figure 10.1) and record the final
volume of NaOH titrant in the buret (see Technique 16A.2).
2. Repeat with the same vinegar. Refill the buret and repeat the titration at least
once more with another sample of the same vinegar.
3. Consult with your instructor. You are to complete Parts A and B for a second
vinegar to determine its average percent acetic acid or complete a third and/or
fourth analysis of your original vinegar. For the additional analyses, revise the
Report Sheet accordingly.
4. Calculations. Determine the average percent by mass of acetic acid in the vinegar(s).
Figure 10.1 Read the volume of
titrant with a black background.
Disposal: All test solutions and the NaOH solution in the buret can be dis-
carded in the Waste Bases container.

CLEANUP: Rinse the buret twice with tap water and twice with deionized water,
discarding each rinse through the buret tip into the sink. Similarly, rinse the flasks.

1
Review Technique 16C.3 for this procedure.
2
The endpoint (and the stoichiometric point) is near when the color fade of the phenolphthalein indicator
occurs more slowly with each successive addition of smaller volumes of NaOH solution to the vinegar.

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Experiment 10 Prelaboratory Assignment

Vinegar Analysis
Date __________ Lab Sec. ______ Name ____________________________________________ Desk No. __________
1. Assuming the density of a 5% acetic acid by mass solution is 1.0 g/mL, determine the volume of the acetic acid solu-
tion necessary to neutralize 25.0 mL of 0.10 M NaOH. Also record this calculation on your Report Sheet.

2. a. A chemist often uses a white card with a black mark to aid in reading the meniscus of a clear liquid. How does this
technique make the reading more accurate? Explain.

b. A chemist should wait 10–15 seconds after dispensing a volume of titrant before a reading is made. Explain why
the wait is good laboratory technique.

c. The color change at the endpoint should persist for 30 seconds. Explain why the time lapse is a good titration
technique.

3. Lemon juice has a pH of about 2.5. Assuming that the acidity of lemon juice is due
solely to citric acid, that citric acid is a monoprotic acid, and that the density of lemon
Victor de Schwanberg/

juice is 1.0 g/mL, then the citric acid concentration calculates to 0.5% by mass.
Estimate the volume of 0.0100 M NaOH required to neutralize a 3.71-g sample of
Science Source

lemon juice. The molar mass of citric acid is 190.12 g/mol.

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4. Explain why it is quantitatively not acceptable to titrate each of the vinegar samples with the NaOH titrant to the same
dark pink endpoint.

5. a. A commercial vinegar is analyzed for the percent acetic acid present. The data for Trial 1 is listed in the table below.
Complete the table to determine the percent. (See Report Sheet.) Record calculated values with the correct number of
significant figures.

A. Preparation of Vinegar Sample Calculation Zone

1. Mass of vinegar (g) _________

3.06 Part B.5

B. Analysis of Vinegar Sample

1. Buret reading, initial (mL) _________

3.70
2. Buret reading, final (mL) 25.40
_________
Part B.6
3. Volume of NaOH used (mL) _________
4. Molar concentration of NaOH
solution (mol/L) _________
0.0940
5. Moles of NaOH added (mol)
Show calculation. _________
Part B.7
6. Moles of CH3COOH in vinegar (mol)
Show calculation. _________
7. Mass of CH3COOH in vinegar (g)
Show calculation. _________
8. Percent by mass of CH3COOH
Part B.8
in vinegar (%)
Show calculation. _________

5. b. For Trials 2 and 3, the percent CH3COOH in vinegar was 5.01% and 4.66% respectively.
a. What is the average percent of CH3COOH in the vinegar sample? Data Analysis, B.

b. What are the standard deviation and the relative standard deviation (%RSD) for the percent of CH3COOH in the
vinegar sample? Data Analysis, C and D.

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Experiment 10 Report Sheet

Vinegar Analysis
Date __________ Lab Sec. ______ Name ____________________________________________ Desk No. __________

A. Preparation of Vinegar Sample

Calculate the approximate volume of the vinegar sample needed for the analyses (Part A.1).

*Calculations for Trial 1 of the first vinegar sample on next page.

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Calculations for Trial 1.

Discuss briefly a comparison of the two vinegars or for an analysis of a single vinegar, calculate the standard deviation and
the relative standard deviation. Data Analysis C and D.

Laboratory Questions
Circle the questions that have been assigned.
1. Part A.2. A 20-mL volume of previously boiled, deionized water is added to the Erlenmeyer flask to prepare the sample
for titration. Explain why this volume is not critical to the analysis.
2. Part A.2. Previously boiled, deionized water is unavailable. In a hurry to pursue the analysis, deionized water (not
boiled) is added. How does this attempt to expedite the analysis affect the reported percent acetic acid in vinegar: too
high, too low, or unaffected? Explain.
3. Part A.2 and B.1. The 20 mL of water added to the Erlenmeyer flask is to be previously boiled, deionized water. Since
water does absorb CO2 from the atmosphere and since CO2 dissolved in water causes it to be slightly acidic, will the
use of deionized water that has not been previously boiled cause the mass of acetic acid in the vinegar to be calculated
as too high or too low? Explain.
4. Part A.2
a. In determining the percent acetic acid in vinegar, the mass of each vinegar sample is measured rather than the vol-
ume. Explain.
b. If the vinegar were measured volumetrically (e.g., a pipet), what additional piece of data would be needed to com-
plete the calculations for the experiment?
5. Part A.3. The buret is filled with the NaOH titrant and the initial volume reading is immediately recorded without
waiting the recommended 10–15 seconds. However in Part B.1, the 10–15 second time lapse does occur before the
reading is made. Does this technique error result in an increase, a decrease, or have no effect on the reported percent
acetic acid in the vinegar? Explain.
6. Part B.1. The endpoint of the titration is overshot! Does this technique error result in an increase, a decrease, or have
no effect on the reported percent acetic acid in the vinegar? Explain.
7. Part B.1. The wall of the flask is periodically rinsed with the previously boiled, deionized water from the wash bottle.
Does this titrimetric technique result in an increase, a decrease, or have no effect on the reported percent acetic acid in
the vinegar? Explain.
8. Part B.1. A drop of NaOH titrant, dispensed from the buret, adheres to the wall of the Erlenmeyer flask but is not
washed into the vinegar with the wash bottle. Does this error in technique result in the reported percent of acetic acid
being too high, too low, or unaffected? Explain.

148 Vinegar Analysis