1.
Objectives:
- Determining the total titratable acid content fruit juices.
2. Principles:
2.1. Acid-base titration using indicator
- Fruit juices often contain organic acids (such as citric acid, malic acid, and
ascorbic acid) that contribute to their sour taste.
- The titration process involves a reaction between the organic acids in the juice and
a strong base (commonly sodium hydroxide, NaOH). The general reaction can be
represented as:
HA + NaOH NaA +H2O
where HA represents the organic acid.
- The titration is performed by slowly adding NaOH standard solution from a
burette or other liquid-dispensing device to a solution of the analyte until the reaction
reach the endpoint, where the amount of titrant added is stoichiometrically equivalent to
the amount of analyte present.
- To detect the endpoint of the titration, a pH indicator (such as phenolphthalein) is
added to the fruit juice sample.
2.2. Acid-base titration using pH meter
- Instead of relying on a visual indicator (phenolphthalein), a pH probe provides a
continuous and precise measurement of the pH of the solution during titration. This
allows for a more accurate determination of the endpoint.
- During the titration, the change of [ H +¿¿ ] follows Henderson – Hasselbalch
equation.
pH = pKa + log ¿ ¿
- The pH probe measures the hydrogen ion concentration in the solution, which
changes as the base is added and the acids are neutralized. As NaOH is added, the pH
will gradually increase. Near the endpoint, where the amount of NaOH added is
stoichiometrically equivalent to the amount of acid present, the pH will rise sharply.
- pH can be monitored by a pH electrode. As the equivalence point is approached,
the denominator [HA] in the Henderson–Hasselbalch equation becomes insignificantly
small and the quotient [A−]/[HA] increases exponentially. As a result, the solution pH
rapidly increases and ultimately .approaches the pH of the titrant
- To detect the endpoint of the titration, plot 2nd order derivative of pH with respect
to VNaOH. At the endpoint, the 2nd order derivative of pH with respect to V NaOH equals to
zero.
3. Procedure:
3.1. Acid-Base titration using an indicator:
Step 1: Sample Preparation for fresh fruits:
- Squeeze the fruits to extract juice.
- Filter the juice using filter paper to remove pulp and solid particles.
- Pipette 10 mL of the filtered juice into a clean conical flask. (dilute the juice with
distilled water if necessary)
Step 2: Preparing the Burette:
- Rinse the burette with distilled water, then with 0.1 N NaOH solution.
- Fill the burette with 0.1 N NaOH and record the initial volume.
Step 3: Performing the Titration:
- Pipette 10 mL of the juice sample (after dilution) into a clean 100 mL conical
flask.
- Add 2–3 drops of phenolphthalein indicator to the juice sample.
- Place the flask on a white surface for better visibility of the color change.
- Slowly add NaOH drop by drop from the burette while swirling the flask
continuously.
- As the endpoint approaches, add NaOH more carefully (dropwise) and observe the
color change.
- The endpoint is reached when the solution changes from colorless to faint pink
and remains for 30 seconds.
- Record the final volume of NaOH in the burette.
Step 4: Data Collection and Repeatability:
- Calculate the volume of NaOH:
V NaOH =final burette−initial burette
- Repeat the titration at least 3 times for accuracy.
Sample V NaOH Titratable acidity (mg/L) Average Stdv
st
1
Fruit juice 2nd
3rd
1st
Commercial 2nd
juice 3rd
- Record and calculate the average volume of NaOH used.
Step 5: Calculation of Titratable Acidity:
0 N ×V 1 × Eq . wt .
acid ( wt ∕ vol )= ×100
0 V 2 × 1000
Where:
- N=normality of titrant , usually NaOH ( mEq
mL )
- V 1=volume of titrant (mL)
- Eq . wt .=equivalent weight of predominant acid ( mEq
mg
)
- V 2=volume of sample ( mL )
- 1000=factor relating mg ¿ grams ( mgg )( 101 = 1000
100
)
3.2. Acid-Base titration using a pH Meter
Step 1: Sample Preparation for fresh fruits:
- Squeeze the fruits to extract juice.
- Filter the juice using filter paper to remove pulp and solid particles.
- Pipette 10 mL of the filtered juice into a clean conical flask. (dilute the juice with
distilled water)
Step 2: Preparing the pH Meter and Setup:
- Calibrate the pH meter according to the manufacturer's instructions (usually with
standard buffer solutions: pH 4.00 and pH 7.00).
- Place a magnetic stirrer under the conical flask.
- Immerse the pH probe in the juice sample, ensuring it is fully submerged.
Step 3: Performing the Titration:
- Slowly add 0.1 M NaOH drop by drop from a burette to the juice sample while
stirring continuously.
- Record the pH value after each small volume of NaOH is added.
- Continue adding NaOH until the pH increases sharply (indicating the endpoint).
- Plot the pH vs. volume of NaOH added to determine the titration curve.
- Find the endpoint: The 2nd derivative of the pH vs. volume curve is used to
determine the exact point where neutralization occurs. The endpoint is where the 2nd
derivative equals zero.
Step 4: Data Collection and Repeatability:
- Record the volume of NaOH at the endpoint.
- Repeat the titration at least 3 times for accuracy.
V NaOH Titratable acidity Average Stdv
1st
2nd
3rd
- Calculate the average volume of NaOH used.
Step 5: Calculation of Titratable Acidity (as we mention the above formula):