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The South African Breweries Section : 10.

7
Page : 1 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

1. INTRODUCTION
a) During fermentation fermentable sugars are converted into alcohol and carbon
dioxide (CO2). Some of the CO2 remains dissolved in the beer and some is
released, collected for purification and re-introduced via carbonation to achieve
brand specific levels in package.
b) Bulk measurements are conducted on beer in Bright Beer tanks and storage
vessels, and, may be conducted on fermenting vessels, if so required.
c) The method involves filling an apparatus with beer from a vessel against a
counter pressure so that there is no loss of CO 2. With caution a defined
headspace is created. The apparatus is then shaken vigorously allowing CO 2
(from the beer) to enter the headspace until an equilibrium is established in the
temperature and pressure within the apparatus. A temperature vs pressure
chart is used to determine the volumes of CO2 per volume of beer.
d) The ASBC chart giving volumes of CO2 (at 0°C and 760 mm Hg) per volume of
beer was adopted experimentally for beer from Henry’s law for the solubility of
CO2 in water to give results agreeing with chemical methods of CO 2
determination in beer. The factor is non-linear and the chart can therefore not
be easily metricated. (In addition the equipment is non-metric). Where metric
equipment is used to determine temperature and pressure it must be accurately
converted into degrees Fahrenheit and pounds per square inch before using
the chart.
e) References:
i) ASBC, Methods of Analysis, 8 th edition 1992.
ii) Zahm and Nagel, Manufacturer’s instruction manual.

2. HEALTH AND SAFETY

2.1 HAZARDS

2.2 SAFETY REQUIREMENTS


a) Safety shoes.

2.3 PRECAUTIONS
a) Safety shoes must be worn in production areas.
b) Adhere to production area safety requirements.
The South African Breweries Section : 10.7
Page : 2 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

3. APPARATUS
3.1 EQUIPMENT REQUIRED
a) Zahm volume meter, model “SS-60”.
b) Zahm aspirator bulb or aspirator pump.
c) Zahm clamping device or rubber pressure tubing (OD approx. 1,25 cm, ID
approx. 0,6 cm and length  10 cm).
The Zahm volume meter is fitted with a Fahrenheit thermometer and a
pressure gauge, usually 30 p.s.i. Obtainable from:
CC Imelmann (Pty) Ltd
34 Nelson Road
Booysens (Gauteng)
d) Water bath set at about 60°C.
e) Refrigerator maintaining a maximum temperature of 5°C.
f) Barometer (see Vol. X, Section 7.9).
g) Dead weight (gauge) tester.

3.2 PREPARATION
a) Ensure that the barrel and bore of stopcocks (valves) are clean and
greased with a thin layer of silicone grease.
b) Ensure that the pressure gauge and thermometer are calibrated.
c) Thoroughly wash the inside of the volume meter with a mild detergent and
water below 25°C.
Note: Do not use water with a temperature greater than the
thermometer’s maximum temperature.
d) Attemperate the volume meter to a constant temperature below 5°C.

3.3 MAINTENANCE
a) Lubricate all cocks and the piston weekly as described above and as per
manufacturer’s recommendations.
b) Regularly inspect and replace ‘O’-rings and gasket.
c) After use, thoroughly rinse the volume meter with purified water, drain and
close all valves.
d) Check the instrument for leaks. Establish a 10 p.s.i. pressure inside the
volume meter. If the pressure drops within 10 minutes use Snoop and trace
the leak.
The South African Breweries Section : 10.7
Page : 3 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

3. APPARATUS (Continued)
3.4 CALIBRATION
a) Calibrate the pressure gauge at least daily against a dead weight tester or
manometer.
b) Check the thermometer at least once per month.

3.5 STORAGE
a) When not in use store the volume meter in a refrigerator.

4. CHEMICALS
4.1 CHEMICALS REQUIRED
a) Decon (detergent).
b) Snoop (soapy solution).
c) Laboratory grade silicone grease.

4.2 REAGENT PREPARATION

4.3 STANDARDISATION

4.4 DISPOSAL

5. METHOD
5.1 SAMPLE PREPARATION

5.2 TEST METHOD


a) Note the following requirements:
i) Ensure that the thermometer and pressure gauge are calibrated.
ii) The meter is clean and airtight.
iii) The meter is attemperated to about the test beer temperature.
b) Close the lower inlet cock.
c) Lock the piston in the IN position.
d) With the top vent cock (outlet) open, establish the required counter pressure
and close the top vent cock.
Note: The counter pressure in the instrument should be slightly less
than the pressure of the tank plus the hydrostatic head pressure
of the beer above the sample cock, e.g if the pressure is 8 p.s.i.
and the beer level is 6 ft above the sample cock or
approximately 3 p.s.i. then 11 p.s.i counter pressure is required.
The South African Breweries Section : 10.7
Page : 4 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

5. METHOD (Continued)
5.2 TEST METHOD (Continued)
e) Attach the meter to the tank sample cock ensuring an airtight fitting.
f) Open the inlet cock wide and then open the tank cock wide.
g) Crack open the top vent cock only when the pressure is constant so that the
pressure gauge does not drop by more than 1 p.s.i. Allow beer to slowly fill
the meter until it overflows at the goose neck.
h) Open the vent cock fully to allow the beer flow to remove air bubbles.
Note: Allow beer to flow through the meter for about 1-2 minutes to
ensure temperature equilibrium.
i) Close the top vent cock and then the inlet cock on the meter.
j) Close the tank cock and remove the meter from the tank.
k) Open the top vent cock keeping the meter vertical to reduce the false
pressure. Allow the gauge pressure to drop to approximately the
equilibrium pressure expected.
Note: Do not shake the meter while reducing the false pressure.
l) Close the top vent cock.
m) Turn the piston handle to the release position.
Note: i) Do not manually pull the piston out, but allow the internal
beer pressure to force the piston out as the sample is
shaken.
ii) It may be necessary to raise the temperature by about 2-3°F.
n) Shake until equilibrium temperature and pressure is established.
o) Read and record the temperature and pressure once stable.
Note: Tap the gauge slightly before reading the gauge pressure.
p) Read and record the barometric pressure in mm Hg (mercury) pressure.
q) After use, open both cocks (inlet and top vent) and blow the beer out with
air.
r) Rinse the meter thoroughly with purified water, invert to drain and return to
the refrigerator if no longer required.

5.3 CALCULATIONS
a) Pressure correction for Altitude:
Correction factor = (760-ABP) x 0,2
( 10 )
Where ABP = actual barometric pressure:
Note: 0,2 p.s.i. is subtracted for every 10 mm Hg below the standard
pressure i.e. 760 mm Hg.
The South African Breweries Section : 10.7
Page : 5 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

5. METHOD (Continued)
5.3 CALCULATIONS (Continued)
b) Subtract the altitude correction factor from the recorded gauge pressure
(step (O) above).
Note: Correct the recorded temperature if the thermometer contains a
correction factor.
c) Read off the volumes of CO2 from temperature and corrected pressure from
Table 1, Vol. X, Section 6.4.
Note: The CO2 chart (Table 1) relates to the solubility of Carbon
Dioxide in beer as derived from the temperature-pressure
relationship at 0°C and 760 mm Hg.
d) Report CO2 volumes to two decimals.
e) If required, the percentage CO2 is calculated as follows:
% CO2 = Vols of CO2 x 0,197
Relative density of the sample
f) Example of calculations:
Given:
Barometric pressure = 625 mm Hg
Temperature = 37,3°F
Gauge pressure = 13,6 p.s.i.
Relative density = 1,00578
Thermometer correction = + 0,2°F
Calculate as follows:
i) Altitude correction factor = 760-625 x 0,2
10
= 2,7
ii) Corrected gauge pressure = 13,6-2,7 = 10,9 p.s.i.
iii) Corrected temperature = 37,3 + 0,2 = 37,5°F.
iv) From the chart: (see Appendix A)
37,5°F @ 10 p.s.i. = 2,40 vols.
37,5°F @ 11 p.s.i. = 2,50 vols.
Therefore 0,1 p.s.i. = (2,50-2,40)  10 = 0,01
Thus 0,9 p.s.i. = (9x0,01) = 0,09
Therefore 37,5°F @ 10,9 p.s.i. = 2,40+0,09 = 2,49
= 2,49 vols CO2
Percentage CO2 = 2,49 x 0,197 = 0,488
1,00578
= 0,49% CO2
The South African Breweries Section : 10.7
Page : 6 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

5. METHOD (Continued)
5.3 CALCULATIONS (Continued)
g) Useful Conversions:
i) Degrees Centigrade into Fahrenheit
°F = (°C x 9) + 32
5
ii) Pounds per square inch x 6,89476 = Kilopascals
(e.g. 20,7 Kpa  6,89476 = 3,00228 e.g. 3,00 p.s.i.)

6. VERIFICATION
i. Refer to Verification Routines Vol. X, Section 3.12.
ii. Calibration and maintenance records.

7. COMPETENCY TEST
The South African Breweries Section : 10.7
Page : 7 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

7. COMPETENCY TEST

FORMATIVE ASSESSMENT CHECKLIST

Date: Candidate Name :


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

Assessment 1 2 3

CHECKLIST COMPETENT NOT YET NOT


COMPETENT ASSESSED

1.0 PRODUCT
I’d know that the end product is right and as
manualised if:-
1. Calibration status records of the equipment are valid
and current.
2. Maintenance records of the equipment are valid and
current.
3. Service record of the dead weight (gauge) tester is
available and current..
4. The SS60-Volumeter, when not in use, is stored filled
with water and at 1-5°C.
5. A “Change Management” record is available and
current.
6. Updated record of results is available and current.
Range of Variables:
1. Calibration equipment = pressure gauge, thermometer, barometer and dead weight tester.
2. Maintenance equipment = SS60 volumeter, barometer and dead weight tester.
2.0 PROCESS
If the candidate does the job as manualised the
correct way she/he would:-
1. Adhere to Health and Safety:
1.1. Sampling: mains and tanks are under pressure.
1.2. Production areas H&S regulations and attire.
The South African Breweries Section : 10.7
Page : 8 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

7. COMPETENCY TEST (Continued)

CHECKLIST COMPETENT NOT YET NOT


COMPETENT ASSESSED

2.0 PROCESS (Continued)


2. Prepare the SS60 volumeter

2.1 Check gauge calibrate.


2.2 Use a cold instrument.
2.3 Check that the piston is free moving.
2.4 Check for leaks on the instrument.
2.5 Establish and set a counter pressure on the
meter.
3. Analyse the sample:

3.1 Attach the inlet hose securely to the sample cock


(no leaks) and place the outlet in a drain.
3.2 Open cocks in the following order: inlet cock,
sample cock, crack open vent cock to allow beer
to slowly fill the meter.
3.3 Open the vent cock fully and allow beer to run
through the meter for 1-2 minutes (temp.
equilibration of meter).
3.4 Close cocks in the following order, top vent, inlet
cock and sample cock.
3.5 Remove the false pressure.
3.6 Turn the piston handle to the release position.
3.7 Shake gently until equilibrium pressure and
temperature values are obtained.
3.8 Read and record temperature and pressure.
3.9 Determine the barometric pressure
4. Calculate the CO2-content:
4.1 Calculate and correct of altitudes pressure.
4.2 Read off the CO2-content from the corrected
pressure and temperature using the CO 2-chart.
5. Drain the sample, rinse the meter and store cold at 1-
5°C.
6. Verify and validate the result(s).
7. Record, report and communicate results.
The South African Breweries Section : 10.7
Page : 9 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

7. COMPETENCY TEST (Continued)

CHECKLIST COMPETENT NOT YET NOT


COMPETENT ASSESSED

3.0 KNOWLEDGE
A candidate who does this job should be able to:
1. Define Henry’s Law on which the CO2 measurement
is based.
2. Discuss the impact of altitude
3. Describe how and why a gas space is created inside
the meter when it contains the sample.
4. Discuss the solubility of CO2 in beer as compared to
in water.
5. Explain the term “equilibrium” pressure as in this
determination.
6. State why CO2 determinations are made on the
product during the various proces stages.
7. Define the gas law conditions relevant to the CO 2-
chart.
8. Name three ways in which CO2-content can be
expressed.
9. Describe how a pressure gauge can be calibrated if a
deadweight tester is not available.
10.State what other equipment may be used if a SS60
volumeter is not available.
The South African Breweries Section : 10.7
Page : 10 of 10
BREWING MANUAL 1st Issue : Nov 1997
Vol. X - Analytical Methods Rev. Date : Feb 1999

SECTION 10.7 – DETERMINATION OF CARBON DIOXIDE IN BEER IN


BULK WITH ZAHM NAGEL EQUIPMENT

7. COMPETENCY TEST (Continued)

Competent : Not Yet Competent:


Comments :

Action Plan Follow up


Dates

Assessor 1 Candidate
Sign. Sign.

Assessor 2
Sign.

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