ENGINEERING SCIENCE DEPARTMENT

Water and Environmental Technology Program

Name _________________
SPRING TERM

Aquatic Chemistry II, WQT-134

Laboratory #1
Acidity Modified from STM 2310
Purpose: In this lab you will perform an acidity test on a water/waste water sample. This
procedure determines the mineral acidity of a sample. Acidity results from carbon dioxide in the
atmosphere, from biological oxidation of organic matter, or from industrial waste discharges.
The acidity of a water or wastewater sample is its quantitative capacity to neutralize a strong
base to a pH of 8.3. Titrating with 0.02 N sodium hydroxide measures the concentration of
mineral acids (such as sulfuric acid), hydrolyzing salts, and total acidity. The end point of the
titration may be detected using a pH meter or phenolphthalein indicator methods (Operation of
Wastewater Treatment Plants. Chapter 16. Laboratory procedures and chemistry).

Acidity levels in wastewater indicate its corrosive properties and can take a leading role
in regulating biological processes as well as in chemical reactions (such as chemical
coagulation and flocculation). While both acidity and alkalinity are related to pH, they
should not be confused with pH, nor should the terms be used interchangeably. Acidity is a
measure of a solutions capacity to react with a strong base (usually sodium
hydroxide, NaOH) to a predetermined pH value. This measurement is based on the total
acidic constituent of a solution (strong and weak acids, hydolyzing salts, etc.). It is
possible to have highly acidic water but have moderate pH values. Likewise, the pH of a
sample can be very low but have a relatively low acidity. Acidity is similar to a buffer in
that the higher the acidity, the more neutralizer is needed to counteract it
(http://www.lagoonsonline.com/laboratory-articles/acid.htm).
Acidity of a water is its quantitative capacity to react with a strong base to a designated pH.
The measured value may vary significantly with the end-point pH used in the determination.
Acidity is a measure of an aggregate property of water and can be interpreted in terms of specific
substances only when the chemical composition of the sample is known. Strong mineral acids,
weak acids such as carbonic and acetic, and hydrolyzing salts such as iron or aluminum sulfates
may contribute to the measured acidity according to the method of determination.

Acids contribute to corrosiveness and influence chemical reaction rates, chemical speciation,
and biological processes. The measurement also reflects a change in the quality of the source
Advantages
Very useful/common procedure but not required by NPDES permit
Commonly done to assess performance of a wastewater anaerobic digestor: A ratio of
10:1 acidity to alkalinity = good digestor, 5:1 ratio= bad digestor.
Visual results a color change to purple using the phenolphthalein indicator at pH 8.3
Disadvantages/Interferences
Variable sample volume that requires a procedural trial and error
Dissolved gases contributing to acidity or alkalinity, such as CO2, hydrogen
sulfide, or ammonia, may be lost or gained during sampling, storage, or titration.
Oily matter, suspended solids, precipitates, or other waste matter may coat the glass
electrode and cause a sluggish response.
Presence of ferrous or ferric iron, aluminum, and manganese may cause drifting end
points.
Turbidity
Residual free available chlorine in the sample may bleach the indicator (remove with
sodium thiosulfate).
Sample collection: According to EPA sampling and preservation guidelines, samples for both
acidity and alkalinity measurements can be collected in a borosilicate glass or plastic bottles and
stored at 4 degrees Celsius for up to fourteen days. However, its always best to analyze fresh
samples collected with no headspace.
SUPPLIES/SAFTEY:
Please wear lab coats, safety goggles, and gloves at all times for this lab procedure.

REAGENTS/STORAGE:

Modified from Acidity STM 2310

Distilled water. pH 4 and 7, calibration solutions .

Potassium hydrogen phthalate solution, approximately 0.05N
Crush 15 to 20 g primary standard KHC8H4O4 to about 100 mesh and dry at 120C for 2 h. Cool
in a desiccator. Weigh 10.0 0.5 g (to the nearest mg), transfer to a 1-L volumetric flask, and
dilute to 1000 mL.
*Standard sodium hydroxide titrant, 0.1N: use for sample with acidities that are greater then
1,000 mg/l CaCO3

*Standard sodium hydroxide titrant, 0.02N, use for sample with acidities that are less then 50
mg/l CaCO3
Dilute 200 mL 0.1N NaOH to 1000 mL and store in a polyolefin bottle protected. Standardize
against KHC8H4O4 using 15.00 mL KHC8H4O4 solution and a 50-mL buret. Calculate
normality as above: 1 mL = 1.00 mg CaCO3.
Dechlorinating reagents: A number of dechlorinating reagents may be used to remove residual chlorine
prior to distillation. Sodium thiosulfate (1/70 N): Dissolve 3.5 g Na 2S2O3 5H2O in distilled water and
dilute to 1 liter. One mL of this solution will remove 1 mg/L of residual chlorine in 500 mL of sample.

Indicators
*Phenolphthalein indicator solution, alcoholic, pH 8.3 indicator.
Lab Materials:

Use any commercial pH meter or electrically operated titrator that uses a glass electrode
and can be read to 0.05 pH unit. Standardize and calibrate according to HACH
manufacturers instructions (note: use pH 7 first , then pH 4). Check calibration
efficiency by re-measuring pH 7 indicator solution.
Titration vessel: 205 ml beaker
Magnetic stirrer
Pipets, volumetric
Flasks, volumetric, 1000-, 200-, 100-mL
Burets, borosilicate glass, 50-, 25-, 10-mL
Polyolefin bottle, 1-L.
SUMMARY PROCEDURE
Modified from Acidity STM 2310

Acidity Measurement: Acidity comprises a simple titration. Basically, acidity is determined by

titrating the sample with sodium hydroxide to a pH of 8.3 (often called the phenolphthalein
acidity this term dates back to the time before electronic pH meters). Standard Methods for the
Examination of Water and Wastewater, 20th Edition, section 2310.
Determine sample acidity from the volume of standard alkali required to titrate a unknown
sample to a pH of 8.3 (phenolphthalein acidity). Titrate at room temperature using a properly
calibrated pH meter, electrically operated titrator, or color indicators.

Step-by-step Procedure
Modified from Acidity STM 2310
Part 1 Determine Normality of Sodium Hydroxide
1. Please work with me to make to make a 0.05N of Potassium hydrogen phthalate solution.
2. Add 50 ml of what should be 0.02 N Standard sodium hydroxide to a clean 250 ml beaker
(titration vessel) that contains a magnetic stir bar on a stir plate with a pH probe inserted
in the vessel. Position titration vessel below a 50 ml buret containing 50.00 mL of 0.05 N
KHC8H4O4 solution.
3. Titrate to the inflection point which should be close to pH 8.7--( ~15-18 ml).
4. Calculate normality of NaOH where:
Normality = _____ N NaOH
Normality = A X B
204.2 X C
A = g KHC8H4O4 weighed into 1-L flask (should be 10 g),
B = mL KHC8H4O4 solution taken for titration, and
C = mL NaOH solution used (should be 50 ml).
Use the measured normality in further calculations; 1 mL = 1.00 mg CaCO3.
Part 2 Titration to pH 8.3 endpoint
1. Measure pH of your sample record value __________________
2. Add 200 ml of sample to a clean 250 ml beaker (titration vessel) that contains a magnetic
stir bar on a stir plate with a pH probe inserted in the vessel. Position titration vessel
below a 25 ml buret containing Standard sodium hydroxide titrant, 0.02N. Note: If free residual
chlorine is present add 0.05 mL (1 drop) 0.1M Na2S2O3 solution.

3. Add 0.2 mL (5 drops) Phenolphthalein indicator solution, alcoholic pH 8.3 indicator

solution to the sample.
4. Add Standard sodium hydroxide titrant, 0.02 N in 1 drop increments, such that a change
of less than 0.2 pH units occurs per drop (note: it may take ~2-3 ml to reach the endpoint,
if your initial unknown sample is pH ~7.0 and clean).
5. Continue adding titrant and record ml amount added each time as well as record pH
after each addition, until pH 8.3 is reached (it will be colorless). Slow down as you
approach pH 8.3 (note: it may take 2-3 ml to reach the endpoint).

Part 3 Potentiometric titration curve

6. Measure pH of your sample record value __________________
7. Add 200 ml of sample to a clean 250 ml beaker (titration vessel) that contains a magnetic
stir bar on a stir plate with a pH probe inserted in the vessel. Position titration vessel
below a 25 ml buret containing Standard sodium hydroxide titrant, 0.02N.
8. Add Standard sodium hydroxide titrant, 0.02 N in 1 drop increments, such that a change
of less than 0.2 pH units occurs per drop (note: it may take ~2-3 ml to reach the endpoint,
if your initial pH is ~7.0 and clean).
9. Continue adding titrant and record ml amount added each time as well as record pH
after each addition, until pH 9 is reached.
10. Construct the titration curve by plotting observed pH values versus cumulative milliliters
titrant added (i.e. add the data to the Excel spreadsheet in front of the class and graph (I
will help you))
11. View titration curve it should be smooth. Determine acidity relative to a particular pH
from the curve.

Environmental Chemistry II, - WQT 134

Acidity
Sample Location

Sample Date

Sampled by

Sample Time

Analyzed by

Date

Sample Type

______

Method

Original pH ________________________ pH after indicator____________________

pH

ml 0.02 N NaOH

Calculations
Table1. Drop conversion to ml additions
20 drops ~1ml
10 drops ~0.45 ml
5 drops ~0.2 ml
2 drops ~0.10 ml
Acidity CaCO3/L= (A X B) X 50,000
ml of sample
A = mL NaOH titrant used,
B = normality of NaOH,
Report pH of the end point used, as follows:
The acidity to pH _______ = _______ mg CaCO3/L.
If a negative value is obtained, report the value as negative. The absolute value of
this negative value should be equivalent to the net alkalinity.

Example Problem
A sample of wastewater plant effluent was collected and tested for acidity. The results are as
follows:
1. Sample size , ml = 50 ml
2. NaOH normality, N = 0.02 N
3. ml NaOH titrant used A = 8.9 ml
E: Calculations
Acidity CaCO3/L= (8.9 ml X 0.02 N) X 50,000
50 ml of sample
A = mL NaOH titrant used,
B = normality of NaOH,
Report pH of the end point used, as follows:
Acidity mg/L as CaCO3 = __178__ mg CaCO3/L.