Acid-Base, BT, 8010

Acidity, Phenolphthalein DOC316.53.01149

Sodium Hydroxide with a Buret1 Method 8010

(0 to 10,000 mg/L as CaCO3) Buret Titration
Scope and Application: For water, wastewater and seawater
1 Adapted from Standard Methods for the Examination of Water and Wastewater, 23/0 B (4a).

Test preparation

Before starting the test:

Read the entire procedure before starting the test.

Avoid excessive agitation of the sample to prevent the loss of dissolved gases such as carbon dioxide, hydrogen sulfide or
ammonia.

Six drops of Phenolphthalein Indicator Solution may be substituted for the Phenolphthalein Powder Pillow.

The Methyl Orange and Phenolphthalein Acidity procedures can be run sequentially if both values are desired. First, titrate to
pH 3.7 and record the amount of sodium hydroxide used. Then titrate to pH 8.3.

Phenolphthalein acidity in mg/L x 0.0584 = grains per gallon

Collect the following items:

Description Quantity

Phenolphthalein indicator powder pillow 1

Sodium hydroxide standard solution, 0.020 N varies1

Buret clamp 1

Buret, Teflon plug, Class A 1

Graduated cylinder varies1

Erlenmeyer flask 1

Funnel, Micro 1

Support Stand 1

1 See Consumables and replacement items.

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Buret titration (Method 8010)

See
Table 1

1. Select a sample 2. Use a graduated 3. Transfer the sample 4. Add the contents of
volume from the Sample cylinder or pipet to into a 250-mL Erlenmeyer one Phenolphthalein
volume selection for measure the sample flask. Dilute to about Indicator Powder Pillow.
expected concentration volume. 50-mL with deionized Swirl to mix. (Omit this
table that corresponds to water if necessary. step if you are using a
the expected acidity pH meter.)
concentration in mg/L as
calcium carbonate
(CaCO3).

5. Fill a 50-mL buret to 6. While swirling the 7. Calculate:

the zero mark with 0.020 N flask, titrate the sample mL Titrant × multiplier
Sodium Hydroxide with 0.020 N Sodium used = mg/L
Standard Solution. Hydroxide Standard phenolphthalein acidity
Solution until the solution as CaCO3
color changes from
colorless to a light pink
that persists for 30
seconds (pH 8.3).

Table 21 Sample volume selection for expected concentration

Range
Sample Volume (mL) Sodium Hydroxide Multiplier
(mg/L as CaCO3)

1–1000 50 19353 20
800–2000 25 19353 40
2000–5000 10 19353 100
4000–10000 5 19353 200

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Interferences
Highly colored or turbid samples may mask the color change at the end point. Use a pH meter for
these samples. Titrate to pH 8.3.
Add a drop of 0.1 N Sodium Thiosulfate Standard Solution to remove residual chlorine that may
interfere with the indicator.
Pretreat samples that contain significant amounts of hydrolyzable metals such as iron, aluminum
or manganese as follows:

1. Adjust the sample taken in step 1 of the procedure to pH 4.0 or less (if necessary) by adding
5.0-mL increments of 0.020 N Sulfuric Acid Standard Solution. Record the amount of acid
added. Use a pH meter or appropriate indicator to determine when pH 4.0 is reached. Remove
the pH electrodes after completing this step if a pH meter is used.

2. Using a 1-mL glass serological pipet and pipet filler, add five drops of 30% Hydrogen Peroxide
Solution.

3. Boil the solution for two to five minutes.

4. Cool to room temperature and titrate to pH 8.3 as described in the procedure beginning with
step 3 of the procedure.

5. Subtract the number of milliliters of 0.020 N Sulfuric Acid Standard Solution added from the
number of milliliters of 0.020 N Sodium Hydroxide Standard Solution used in the titration
before multiplying the volume of sodium hydroxide by the multiplier used in step 7 of the
procedure.

Sampling and storage

Collect samples in clean plastic or glass bottles. Fill completely and cap tightly. Avoid excessive
agitation and prolonged exposure to air. Samples should be analyzed as soon as possible after
collection but can be stored at least 24 hours by cooling to 4 °C (39 °F) or below. Warm to room
temperature before analyzing.
Accuracy check
End point confirmation
To determine the correct end point, dissolve the contents of a Buffer Powder Pillow, pH 8.3, in 50
mL of deionized water in a 250-mL Erlenmeyer flask. Add the contents of one Phenolphthalein
Indicator Powder Pillow and swirl to mix. Titrate the prepared water test samples to this same
color.
Standard additions method (Sample spike)
The standard additions method check can be performed as follows:

1. Use a TenSette Pipet to add 0.1 mL of Sulfate standard solution 0.500 N to a prepared sample
titrated to the end point.
2. Swirl to mix and titrate again to the end point. Note the amount of additional titrant used.

3. Make 0.2-mL and 0.3-mL acid additions, titrating to the end point after each addition. The mL
of titrant required should increase by 2.5 mL for each 0.1-mL increment of acid added. If these
increases do not occur, refer to the Water Analysis Guide for Standard Additions.
Standard solution method
Sodium Hydroxide Standard Solution slowly absorbs carbon dioxide when exposed to air, causing
a partial loss of strength. Check the solution frequently (monthly) by titrating 50 mL of Potassium
Acid Phthalate Standard Solution as 100 mg/L CO2and using a Phenolphthalein Indicator Powder
Pillow. The titration should require 5.68 mL of Sodium Hydroxide Standard Solution. If the volume
required for the titration is greater than 5.88 mL, discard the solution and replace with a fresh
supply.

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Summary of method
Acidity is classified by the pH value of the titration end point. Various pH indicators are used
depending on the pH end point selected. Acidity also can be determined by using a pH meter to
follow the solution pH to the correct end point value as the standard base is added.
Consumables and replacement items
Required reagents
Description Quantity/test Unit Catalog number
Phenolphthalein Powder Pillows 1 pillow 100/pkg 94299
Sodium Hydroxide Standard Solution, 0.020 N varies 1L 19353
Water, Deionized varies 500 mL 27249

Required apparatus
Description Quantity/test Unit Catalog number
Buret, Teflon Plug, Class A, 25-mL 1 each 2636540
Buret Clamp, double 1 each 32800
Select one or more based on sample volume:
Cylinder, graduated, 5-mL — each 50837
Cylinder, graduated, 10-mL — each 50838
Cylinder, graduated, 25-mL — each 50840
Cylinder, graduated, 50-mL — each 50841
Flask, Erlenmeyer, 250-mL 1 each 50546
Pipet, volumetric, Class A, 5 mL — each, 1451537
Pipet, volumetric, Class A, 10 mL — each 1451538
Pipet Filler, Safety bulb — each 1465100
Support Stand 1 each 56300
Funnel, Micro 1 each 2584335

Required standards
Description Unit Catalog number
Sulfuric Acid Standard Solution, 0.500 N 100 mL MDB 212132
Buffer Powder Pillows, pH 8.3, 50 mL 25/pkg 89868
Potassium Acid Phthalate Standard Solution, 100-mg/L as CO2 100 mL 226142

Optional items
Description Unit Catalog number
Hydrogen Peroxide Solution. 30 % 473 mL 14411
Meter, pH, SensION 1 with Platinum pH electrode each 5170010
Phenolphthalein Indicator Solution 100 mL MDB 16232
Pipet, 1-mL glass serological pipet each 53235
Pipet Filler each 1465100
Sodium Thiosulfate Standard Solution, 0.1 N 100 mL MDB 32332

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