The South African Breweries Section : 9.

6
Page : 1 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

1. INTRODUCTION
a) Chlorination is the process of adding chlorine to water in order to destroy disease
producing organisms. In addition it also destroys nuisance organisms which cause taste
and odour problems.
b) Chlorination in the presence of nitrogenous compounds leaves residuals of various forms.
They are hypochlorous acid (HOCl 2); monochloramine (NH2Cl); dichloramine (NHCl2)
and nitrogen tri-chloride (NCl3). Dichloramine and nitrogen tri-chloride have unpleasant
tastes even at trace levels.
c) For the purpose of brewing these combined residuals must be removed. This is down by
a process called dechlorination. The most common method in breweries is by passing
the water through a bed of granular activated carbon.
d) The analysis of free available chlorine and combined chlorine gives a measure of level of
chlorination and efficiency of dechlorination.
e) In this method free and total chlorine levels are measured separately, using two of the
three reagents in combination.
When reagents Cl2-1A and Cl2-2A are combined, total residual chlorine is determined,
when Cl2-1A and Cl2-3A are combined; free residual chlorine is measured and the
difference between total and free is bonded chlorine.
f) Applicable to the analysing of water.
g) References :
i) Merck SQ 118 Photometer Manual.
ii) Merck Spectroquant chlorine test kit pamphlet.

2. HEALTH AND SAFETY

2.1 HAZARDS
The glassware in which the colours were developed may contain chloramine a harmful
substance to the eyes, respiratory system and skin.
 The South African Breweries Section : 9.6
Page : 2 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

2.2 SAFETY REQUIREMENTS

Surgical gloves.

2.3 PRECAUTIONS
a) After use the cuvette must be rinsed thoroughly with tap and purified water.
b) Surgical gloves must be worn when :
 Conducting the test.
 Handling the chemicals and reagents.
 Washing the cuvette.
c) The chlorine test kit containers (chemicals and reagents) must be kept tightly closed.

3. APPARATUS
a) Merck SQ 118 photometer.
b) Tissues.
c) Test tubes.
d) Pipette, 10 ml (bulb).
e) Glass cuvette, 10 mm (dedicated).

3.1 EQUIPMENT PREPARATION

3.2 EQUIPMENT MAINTENANCE

3.3 CALIBRATION

3.4 STORAGE

4. CHEMICALS
4.1 CHEMICALS REQUIRED
Merck spectroquant chlorine test kit, Cat No.14828.
Note: The formulation of the test kit chemicals and reagents correspond to the
normal DPD chemicals and reagents.
 The South African Breweries Section : 9.6
Page : 3 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

4.2 PREPARATION REQUIRED

None.

4.3 STANDARDISATION
None.

4.4 DISPOSAL

5. METHOD
5.1 SAMPLING
Adhere and comply to the Quality requirements of Sampling Vol. X, Section 3.2.

5.2 SAMPLE PREPARATION

None.

5.3 TEST METHOD

5.3.1 Total Residual Chlorine
a) Press 0 1 8 on the keyboard to call up the chlorine method.

b) Press to enter. The following will be displayed:

018 CHLORINE Cl2 14828

0, 05 - 1,50 mg/l

c) Pipette 10 ml purified water into a second test tube (blank).

d) Pipette 10 ml purified water into a second test tube (blank).

e) Add 2 micro-spoonfuls of Cl2-1A chemical to each of the test tubes and

dissolved immediately.

f) Immediately add 4 drops of Cl2-2A reagent to each tube and mix.

g) Press the blank value key 0 .

Note: Wait until “Reaction time” or “Measure blank” appears on the
display.

h) Press the timer key.

Note: The reaction time of 1 minute begins.
 The South African Breweries Section : 9.6
Page : 4 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

5.3 TEST METHOD (Continued)

5.3.1 Total Residual Chlorine (Continued)
i) When the timer bleeps, transfer the blank solution into the 10 mm curvette.
j) Place the blank into the cell compartment.
k) Press the key.
Note: The blank value is displayed.
l) Remove the blank from the cell compartment.
m) Rinse the cuvette with sample and fill with the sample.
n) Insert cuvette (sample) into the cell compartment.
m) Press the key.
n) The result will appear on the display.
o) Record the total residual chlorine value in mg/l.
p) The result will appear on the display.
q) Record the total residual chlorine value in mg/l.

5.3.2 Free Residual Chlorine

a) Repeat steps (a) and (b) of 5.3.1 (if necessary).
b) Pipette 10 ml sample into a test tube.
c) Pipette 10 ml purified water into a second test tube (blank).
d) Add 2 micro-spoonfuls of Cl2 - 1A chemical to each of the test tubes and
dissolve immediately.
e) Immediately add 4 drops of Cl2 - 3A reagent to each tube and mix thoroughly.
f) Press the blank value key 0
Note: Wait until “Reaction time” or “Measure blank” appears on the
display.
g) Press the timer key.
Note: The reaction time of 1 minute begins.
h) When the timer bleeps, transfer the blank solution into the 10 mm cuvette.
 The South African Breweries Section : 9.6
Page : 5 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

5.3 TEST METHOD (Continued)

5.3.2 Free Residual Chlorine (Continued)
i) Place the blank into the cell compartment.
j) Press the key.
Note: The blank value is displayed.
k) Remove the blank from the cell compartment.
l) Rinse the cuvette with sample and fill with the sample.
m) Insert cuvette (sample) into the cell compartment.
n) Press the key.
o) The result will appear on the display.
p) Record the free residual chlorine value in mg/l.

5.4 CALCULATIONS
No calculations are required, the photometer is programmed to perform the calculations.

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

7. COMPETENCY TEST
 The South African Breweries Section : 9.6
Page : 6 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

7. COMPETENCY TEST

FORMATIVE ASSESSMENT CHECKLIST

Date : Candidate Name :

Position : Department Name :
Unit :
Element :
Assessor 1 : Assessor 2 :

Assessment 1 2 3

COMPETENT NOT YET NOT

CHECKLIST COMPETENT ASSESSED

1.0 PRODUCT
I’d know that the end product is right and as
manualised if:-
1. Maintenance record of the photometer is available
and current.
2. Service record of the photometer and details of
services conducted is available and current.
3. The test kit is maintained as per Supplier's
instructions.
4. A 'Change Management' record is available and
current.
5. Updated record of results is available.
2.0 PROCESS
If the candidate did the job the correct way as
manualised he/she would:-
1. Adhere and comply to Health and Safety i.r.o:
1.1 The reagents are harmful - wear safety
glasses and surgical gloves throughout the
analysis and glassware cleaning.
1.2 After use rinse the glassware thoroughly with
both tap and purified water.
2. Use dedicated glassware in this test.
3. Identify samples and glassware clearly for
traceability.
 The South African Breweries Section : 9.6
Page : 7 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

7. COMPETENCY TEST (Continued)

FORMATIVE ASSESSMENT CHECKLIST (Continued)

COMPETENT NOT YET NOT

CHECKLIST COMPETENT ASSESSED

2.0 PROCESS (Continued)

4. Prepare the photometer:
4.1 Switch on and enter the method code
( 0 1 8 )
4.2 Verify the display to show:
018 CHLORINE CL2 14828
0,05 - 1,50 mg/l

5. Analyse the sample:

5.1 Pipette 10 ml purified water into a test tube
(Blank).
5.2 Pipette 10 ml sample into a second test tube.
5.3 Add 2 micro-spoonfuls of chemical Cl2-1A to
each tube and dissolve.
5.4 Immediately add 4 drops of reagent:
5.4.1 Total chlorine: Cl2-2A to blank and
sample.
5.4.2 Free chlorine: Cl2-3A to blank and
sample.
5.5 Press the blank value key 0 and wait
for "Reaction Time" or "Measure blank" to be
displayed.
5.6 Start timer and allow 1 minutes reaction time.
5.7 Transfer the blank into the 10 mm cuvette
when the time is over, place it in the cell
compartment and press the key.
5.8 Transfer the sample to the 10 mm cuvette,
place it in the cell compartment and press the
key.
5.9 Record the displayed result.
 The South African Breweries Section : 9.6
Page : 8 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

7. COMPETENCY TEST (Continued)

FORMATIVE ASSESSMENT CHECKLIST (Continued)

COMPETENT NOT YET NOT

CHECKLIST COMPETENT ASSESSED

2.0 PROCESS (Continued)

6. Demonstrate sound Techniques and Practices:
6.1 Pipetting.
6.2 Adhering to reaction times.
6.3 Rinsing the cuvette.
6.4 Avoiding cross contamination of test
solutions.
7. Verify and validate results against verification
routines.
8. Record, report and communicate results.
9. Clean used glassware.
3.0 KNOWLEDGE
A candidate who does this job should be able to:
1. Explain what chlorination is and why it is conducted.
2. Discuss the effects of chlorine on the brewing
process.
3. Explain how chlorine levels can be determined if
the SQ 118 is unavailable.
4. Discuss the hazards of the analysis.
5. Describe how the total bonded chlorine is
determined in this method.
 The South African Breweries Section : 9.6
Page : 9 of 9
BREWING MANUAL 1st Issue : Sep 1996
Vol. X - Analytical Methods Rev. Date : Jan 2000

SECTION 9.6 : DETERMINATION OF FREE RESIDUAL AND

TOTAL RESIDUAL CHLORINE : SQ 118 PHOTOMETER

7. COMPETENCY TEST (Continued)

Competent : Not Yet Competent:

Comments :

Action Plan Follow up Dates

Assessor 1 Candidate
Sign. Sign.

Assessor 2
Sign.