HVB - VT - TEC.WI.04.01.27 (Haze)

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HAZE MEASUREMENT BY VOS ROTA 2.

1. PURPOSE
This instruction describes the determination of the turbidity of beer/cider using the turbidity meter
Vos Rota 2.0.
2. WARNING AND SAFETY PRECAUTION
- Avoid the charger contact with water to prevent electrical shock.
- Hydrazinium sulfate is toxic and can cause cancer, must be handled with great care and use
mask and gloves to protect.
3. PRODUCT INTEGRITY REQUIREMENT
N/A
4. SCOPE:
- Object: This instruction is applicable for bright beer/cider tank or packed beer/cider.
- Responsibility: LA, TE
5. REFERENCE DOCUMENTS:
Doc. Nr. Document Title
HMESC: 02.12.03.015 Laboratory Method: Bright Beer – 0 °C Turbidity

HMESC: 02.12.04.030 Laboratory Standard: Brewing Process – Packaged Beer 0 °C


Turbidity
HVB_VT.TEC.SD.01.01.96 Instruction Manual: Turbidity meter Type Vos Rota 2.0
Quality Assurance and Statistics – Care and Adjustment of
HMESC: 02.17.02.002
Apparatus – Turbidity Meter – VOS 4010

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Eff. Date: 30-Mar-2022
HAZE MEASUREMENT BY VOS ROTA 2.0

6. DEFINITION
6.1 Haze (or turbidity) is an important parameter of beer, mainly because turbidity is judged by
customer, its measurement is valuable for process control and can be used for shelf-life
estimation.
6.2 The light dispersion caused by particles in a solution is defined as haze and it is measured in
units of EBC (European Brewery Convention).
7. BACKGROUND
7.1 Turbidity in liquids is an optical phenomenon caused by the presence of suspended particles
which divert light from its regular course.
7.2 The turbidity meter measures the scattered light caused by particles. Particles smaller than 1
μm, such as proteins, mainly cause scattered light and are measured under 90º. Particles larger
than 1 μm, such as diatomaceous earth and yeast, mainly cause forward-scattered light and are
measured under 25º. A red-light source must be used, operating at a wavelength of 650 nm ±
30 nm..
7.3 The Vos Rota 2.0 is designed for measuring the turbidity of beer (and other liquids) in bottles
and cuvettes up to a turbidity of 500 EBC. This instrument is operated by a touch panel and is
made for use in a ventilated room.
8. EQUIPMENT
8.1 Haze meter, type Vos Rota 2.0.
8.2 Cuvette.
8.3 Water Bath 0.0 ± 0.5 oC
8.4 Volumetric flasks, fitted with a ground glass stopper, 100 ml and 200 ml
8.5 Pipettes, 1.0 ml, 2.0 ml, 5.0 ml, 10.0 ml, 20.0 ml and 25.0 ml, accurate to 0.01 ml
8.6 Analytical balance, accurate to 0.1 mg
8.7 AEPA 0.5 EBC
9. REAGENT
9.1 Cleaning agent:
To degrease the turbidity cuvette, use Sodium carbonate 1% (Na 2CO3) which is prepared from
Na2CO3 (Merck, No. 1.06392)
9.2 Calibration solution:
9.2.1 Preparation of a Formazin 1000 EBC standard:
- Solution (I): Dissolve 1g of Hydrazine (Hydrazinium sulfate, Merck, No. 1.04603) in a 100ml
vol. flask with bi-distilled water.
- Solution (II): Dissolve 10g Hexamethylenetetramine (Methenamine, Merck, No. 1.04343) in
100ml vol. flask with bi-distilled water.

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HAZE MEASUREMENT BY VOS ROTA 2.0

- Calibration solution: Mix solution (I) & (II) in a dark bottle, allow the mixture to rest for 48
hours of a temperature of 25 oC. After this period a 1000 EBC standard is ready for use (stored
in a cool dark place in 6 months).
9.2.2 Formazin standard suspension (100 EBC formazin units)
- Mix the “Formazin turbidity concentrate” (1000 EBC formazin units, (9.2.1)) well and pipette
10.0 ml (± 0.01 ml) of the concentrate into a 100 ml graduated glass stoppered volumetric flask.
Dilute to volume with turbidity-free distilled water and mix well.
- This standard suspension, also called the “100 EBC units – Turbidity suspension”, is stable for
one week.
9.3 Prepare a dilution series:
- Pipette respectively 0.0, 1.0, 2.0, 5.0, 10.0 ml of the formazin standard suspension (9.2.2) into
200 ml volumetric flasks and dilute with constant shaking to volume with turbidity bi-distilled
water.
- The turbidities of these suspensions are characterized as respectively 0.0, 0.5, 1.0, 2.5, 5.0 EBC
formazin units. The test suspensions are only stable on the day of preparation, and must be
prepared fresh each time from the formazin standard suspension (9.2.2).

Volume of Calibration Volume of vol. flask Standard


solution (100 EBC) (ml) (ml) (EBC)
1.0 200 0.5
2.0 200 1.0
5.0 200 2.5
10.0 200 5

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HAZE MEASUREMENT BY VOS ROTA 2.0

10. DESCRIPTION/ PROCEDURE


10.1. Pre-treatment of sample:
10.1.1 For finished product of clear beer:
- For HARA, OPCO samples, the measurement is done as soon as possible; do not store the
samples in fridge to avoid forming haze particles in cold condition for a long time.
- Finished product samples have to be chilled to 0 oC for 3 hours ± 5 min in an upright position.
The bottles should be completely under water in the 0oC water bath to make sure that the entire
bottle is cold. The temperature measured in the sample, should be 0°C ± 0.5°C.
Notice: After input the samples, if temperature on screen of water bath 0°C ± 0.5°C. Reset &
follow temperature of Min/Max thermometer.
10.1.2 For finished product of wheat beer:
- Finished product samples have to be chilled to 20 oC for 1 hour ± 5 min in an upright position.
The bottles should be completely under water in the 20oC water bath to make sure that the
entire bottle is cold. The temperature measured in the sample, should be 20°C ± 1°C.
- Then samples have to be shaken on the FA shaker at 150rpm for approx. 5 minutes.
10.1.3 Shaking test for finished product:
- This instruction describes a method for the determination of the turbidity of beer/cider by
storing it for 72 hours at 30oC.
- Take two finished products, then shake sample on the FA shaker at 150rpm for approx. 72
hours at 30oC.
10.1.4 For BBT sample:
- The bright beer sample is placed in a cooling bath and after reaching 0.0° C ± 0.5°C the
turbidity is measured. In the situation that bright beer samples have high turbidity (outside the
specification) then the samples have to be placed for 30 minutes at 0.0° C ± 0.5°C to ensure that
the sample is stable.
- Make sure that the sample is submerged under liquid completely.
10.2. Measurement:
- Clean the fill the haze meter with bi-distilled water at room temperature.
- Measure a cuvette of bi-distilled water first to check the cleaning status by pressing “Start”. The
result should be lower than 0.03 EBC.
- Check by AEPA standard solution and the result should be within specification, if the result is
out of specification, drain the water, clean the bath and fill fresh bi-distilled water.
- Pour the sample carefully, to avoid foam formation, into the properly degreased and rinsed
turbidity cuvette.
Notice: The samples should be measure at the middle of bottle to make sure representative
sample.

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HAZE MEASUREMENT BY VOS ROTA 2.0

- When no carbon dioxide bubbles rise to the surface anymore, using bi-distilled water rinse
around the cuvette before place into the measuring chamber, close the cover and press “Start”.
After 2-3 seconds the result will be given on the display.
- Read the degree of turbidity in EBC units directly from the display of the meter.
Caution:
- Samples have to be measured within a minute after taking sample out of water bath.
- Not tare after finishing the last sample and follow the last result display on screen before
measuring next run (because calibration curve may be lost if power cut).
10.3. Cleaning:
Water inside should frequently be renewed to avoid the growth of micro-organisms, a drain
cock is mounted on the back panel.
10.3.1 Daily:
Let measuring chamber drain daily and rinse it out with distilled or demineralized water
- When using recirculation, close the water supply.
- Set the water control button to the “OPEN” position and let the water drain away.
- Open the light cover and rinse out the measuring chamber with a spray bottle of cold
distilled or demineralized water.
- Set the water button to the “CLOSE” position when all the water has drained away.
- If necessary clean the optics with microfiber cloth from the service kit and a little alcohol.
Ensure that you do not damage or scratch the optic while doing this.
10.3.2 Every month:
Cleaning the centering plate and the magnets once a month

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HAZE MEASUREMENT BY VOS ROTA 2.0

- Let the water from the measuring chamber drain away as described under daily cleaning.
- Remove the sealing ring (1) (this is clamped with an O-ring (2)) from the measuring
chamber (5)).
- Remove the four magnets (3) and the centering plate (4) from the measuring chamber.
- Clean the components with cold water and a cleaning agent and use the soft brush or
microfiber cloth from the service kit.
- Remove all traces of the cleaning solution by spraying cold distilled or demineralized water
on the parts.
- Fit all the components back into the measuring chamber.
- Fit the sealing ring last. Where applicable use a little silicon grease from the service kit to
facilitate fitting
10.3.3 Cleaning water control valve:
If the water discharge is blocked or no longer closing properly the water control valve must
be checked for fouling or damage.

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HAZE MEASUREMENT BY VOS ROTA 2.0

- Check that water bath is emply and the voltage of the equipment is turned off
- Unscrew the Torx screw (14) on the front
- Remove the metal handle (13)
- Unscrew the two hexagon socket screws (12)
- Valve components (9), (10) and (11) can be removed from the instrument
- Remove O-rings (6), (7) and (8)
- Clean the components and check for any damage
- Remove O-rings (6), (7), (8) and smear a little silicon grease onto the O-rings
- Replace the components in the instrument in the reverse order
- Check the correct operation of the handle
10.3.4 Cleaning of water inlet and water outlet
If the water supply and/or discharge is blocked or leaks are shown this must be checked for
fouling or damage.

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HAZE MEASUREMENT BY VOS ROTA 2.0

- Check that the electrical power supply of the instrument is turned off, the water bath is
empty and the water supply and discharge hoses have been disconnected
- Remove water outlet connection (18) and water inlet (23/(27) connection
- Dismantle the flow control by unscrewing inlet connections (23) and (27) from one another
- Remove any fouling particles or deposits with a clean cloth and rinse them with clean water
and replace components (19), (20), (21) and (22)
- Replace damaged or deformed O-rings (15), (16) and (17) and smear a little silicon grease
onto the O-rings and the housing of the internal cabinet
- Assemble the flow control of the water inlet in the reverse order and check that the flow
direction of flow element (21) is correctly positioned
- Assemble the water outlet and water inlet connection
10.4. Calibration:
10.4.1 Calibration procedure

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HAZE MEASUREMENT BY VOS ROTA 2.0

EBC standard: 0.5 – 1 – 2.5 – 5 – 10 Cuvette

- Fill bi-distilled water inside the machine and turn on the machine.

- Click “Menu” icon in screen.

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HAZE MEASUREMENT BY VOS ROTA 2.0

- Click to “Login” and enter Supervisor code “6848”


- Click “calibration” icon to create new calibration:
o Select a curve number
Note: This instrument is provided on receipt with an extensive factory calibration.
This is shown in curve 1. This curve cannot be overwritten.
o Choose range
o Color: Choose “transparent”
o Container: Choose “Cuvette”
o Diameter: Choose “60 mm”
- Follow the instructions on the display to carry out the calibration
- If a calibration standard is measured you are asked if you want to save this measurement or
carry it out again
- After the last measurement the software determines a calibration curve from the points
recorded
- In a table the accuracy of the recorded calibration curve is shown
- Press save if you want to save the new calibration curve
10.4.2 Verification procedure
- This is a verification of the calibration procedure 10.4.1
- Prepare another Formazin standard suspension (100 EBC formazin units, see 9.2.2) and
another dilution series 0.5, 1.0, 2.5, 5.0 EBC (see 9.3) by a second analyst.
- Click “Configuration” and then click “Measure”.

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HAZE MEASUREMENT BY VOS ROTA 2.0

o Curve: Select curve chosen in 10.4.1


o Cuvette: 60mm
o Unit: EBC
o Rotation: Rotate
- Measure again all dilution series. Acceptable deviations are:
Curve Maximum permitted deviation
0 ÷ 1.0 EBC ± 0.02 EBC
0 ÷ 2.5 EBC ± 0.05 EBC
0 ÷ 5.0 EBC ± 0.10 EBC

- If the results are good, the instrument is ready for use. If not, start calibration again.
- Measure AEPA solution 0.5 EBC 10times, calculate the mean value and standard deviation
(s), specification of AEPA solution is mean value + 2s.
11. REPORT AND RECORDS:
Record the results directly from the screen in the Qualass software, worklist and calibration result
into logbook.
Doc. Nr. Document Title
HVB_VT.TEC.RE.04.01.04 Worklist analysis - BBT
HVB_VT.TEC.RE.04.01.07 Worklist - Main process analysis for haze and 7days test
HVB_VT.TEC.RE.04.01.08 Worklist analysis of haze 3 & 6 & 9 months
HVB_VT.TEC.RE.04.01.18 Worklist main process finished product Cider
HVB_VT.TEC.RE.04.01.20 Worklist - filtered cider base analysis
HVB_VT.TEC.RE.04.01.21 Worklist of bright cider tank
HVB_VT.TEC.RE.01.01.24 Logbook for Haze Vos rota

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