The South African Breweries Section : 9.

12
Page : 1 of 4
BREWING MANUAL 1st Issue : Dec 1997
Vol. X - Analytical Methods Rev. Date :

SECTION 9.12 : DETERMINATION OF SULPHITE (SO3)

1. INTRODUCTION
a) Sodium sulphite is added to the boiler feed water as an oxygen scavenger to
remove any dissolved oxygen in the water which is corrosive towards the boiler.
b) This test is based on the titration of a boiler water sample containing sulphite
against a standard potassium iodate solution. Free iodine is produced when the
sulphite has been completely oxidised, which gives a blue colour with the starch
indicator, when this blue colour appears, the end-point has been reached.
c) The method is applicable only to boilers where sodium sulphite has been added
as an oxygen scavenger.
d) Reference:
i) Standard Methods for the Examination of Water and Waste Water, 14th edition,
1975, p508.

2. HEALTH AND SAFETY

2.1 HAZARDS
a) Sulphuric acid is highly corrosive.
b) Potassium iodate is an oxidising substance.
c) Sampling of boiling hot water from a boiler.
d) Handling boiling hot samples.

2.2 SAFETY REQUIREMENTS

a) Protective clothing such as: safety glasses, face shield, safety shoes, dust
coat, heat protective gloves and acid proof apron and gloves are required.

2.3 PRECAUTIONS
a) Wear a face shield, acid proof gloves and apron when handling sulphuric
acid.
b) Store sulphuric acid in an acids cupboard.
c) Sulphuric acid reacts violently with water.
Note: Do not add water to this acid but add the acid slowly and
cautiously to the water and keep cold.
d) Store potassium iodate away from organic materials and reducing agents.
Contact with combustible materials must be avoided, much heat is
produced and may result in a fire.
e) Wear safety glasses and surgical gloves when working with potassium
iodate.
f) Wear a face shield and heat protective gloves during sampling and handling
not sample containers.
g) Use a pro-pipette when pipetting the 50% sulphuric acid solution.
 The South African Breweries Section : 9.12
Page : 2 of 4
BREWING MANUAL 1st Issue : Dec 1997
Vol. X - Analytical Methods Rev. Date :

SECTION 9.12 : DETERMINATION OF SULPHITE (SO3)

3. APPARATUS
3.1 EQUIPMENT REQUIRED
a) Oven set at 120°C.
b) Desiccator and desiccant.
c) Analytical Balance.
d) Drying dish with lid.
e) Burette, grade A, 50 ml.
f) Pipette, grade A bulb, 1 and 50 ml.
g) Erlenmeyer flask, 250 and 500 ml.
h) Sample bottles. Wide mouth polyethylene, 500 ml. (To include a
polyethylene screw on cap).
i) Measuring cylinder, 100 ml.
j) Volumetric flask, 100 ml.
k) Reagent bottles (amber), 250 and 1000 ml.
l) Water bath set at ± 20 ± 0,5°C.
m) Pro-pipette.

3.2 PREPARATION

3.3 MAINTENANCE
a) Desiccant, ensure it remains dust free and dry.

3.4 CALIBRATION

3.5 STORAGE

4. CHEMICALS
4.1 CHEMICALS REQUIRED
a) Potassium iodide (KI), AR.
b) Potassium iodate (KIO3) anhydrous, AR.
c) Sulphuric acid (H2SO4), 98% AR.
d) Sodium hydrogen carbonate (NaHCO3), AR.
e) Vitex (starch) indicator.
f) Soluble starch powder, AR.
 The South African Breweries Section : 9.12
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BREWING MANUAL 1st Issue : Dec 1997
Vol. X - Analytical Methods Rev. Date :

SECTION 9.12 : DETERMINATION OF SULPHITE (SO3)

4. CHEMICALS (Continued)
4.2 REAGENT PREPARATION
4.2.1 Sulphuric acid, 50%.
a) Cautiously measure out 100 ml sulphuric acid in a measuring cylinder.
b) Add 100 ml purified water to a 500 ml erlenmeyer flask.
c) Slowly and cautiously add the sulphuric acid to the purified water in the
erlenmeyer flask. Mix thoroughly and keep cold.
d) Transfer to a labelled (amber) reagent bottle.
4.2.2 Starch Indicator (only if Vitex is not available)
a) Weigh out 1 g soluble starch.
b) Dissolve in a little hot purified water.
c) Make up to 100 ml with purified water.
d) Boil for 5 minutes and cool to room temperature.
Note: This indicator must be prepared fresh when required.
4.2.3 Potassium Iodide-Iodate Solution, 0,0125N.
a) Dry approximately 1 g of anhydrous potassium iodate for 2 hours at
120°C an oven.
b) Cool in a desiccator to room temperature.
c) Separately weigh out the following:
 Dried amhydrous potassium iodate – 0,4485 g.
 Potassium iodide - 4,35 g.
 Sodium hydrogen carbonate – 0,31 g.
d) Pour approximately 500 ml purified water into a 1000 ml volumetric
flask.
e) Add the potassium iodate and dissolve.
f) Add the potassium iodide and dissolve.
g) Add the sodium hydrogen carbonate and dissolve.
h) Make up to volume with purified water and mix thoroughly.
i) Transfer to a labelled (amber) reagent bottle.
Note: i) Shelf life is one month.
ii) Store in the dark.

4.3 STANDARDISATION

4.4 DISPOSAL
 The South African Breweries Section : 9.12
Page : 4 of 4
BREWING MANUAL 1st Issue : Dec 1997
Vol. X - Analytical Methods Rev. Date :

SECTION 9.12 : DETERMINATION OF SULPHITE (SO3)

5. METHOD
5.1 SAMPLE PREPARATION
a) Note the following sampling requirements:
i) Refer to Vol X, Section 3.2.
ii) Sample in air-tight polyethylene containers.
iii) Brim fill the container to exclude air in the headspace before sealing.
b) Place the sample in a water bath and attemperate to approximately 20-
25°C.
Note: i) Do not filter.
ii) Conduct the test as soon as possible when cold.

5.2 TEST METHOD

a) Pipette 1 ml 50% sulphuric acid solution into a 250 ml erlenmeyer flask.
b) Pipette 50 ml (cold) sample into the erlenmeyer flask and mix.
c) Add about 0,2-0,3 g Vitex indicator and mix.
d) Titrate with 0,0125N potassium iodide-iodate titrant until a faint permanent
blue colour develops in the sample.
e) Record titrant volume used as A ml.

5.3 CALCULATION
a) Sulphite (SO3) mg/l = A x N x 40 000
Sample Volume
Where : A = ml of titrant used.
N = normality of the titrant (0,0125N).
or
Sulphite (SO3), mg/l = A x 10 if 50 ml sample was used.
b) Record sulphite to one decimal only.

6. VERIFICATION
Refer to Verification Routines Vol X, Section 3.12.

7. COMPETENCY TEST