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INSTRUCTION MANUAL
Milwaukee WMilwaukee W
Milwaukee W
Milwaukee WMilwaukee W
Mi455
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ine Line L
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otal Sulphur Dioxideotal Sulphur Dioxide
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otal Sulphur Dioxideotal Sulphur Dioxide
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
TABLE OF CONTENTS
FUNCTIONAL DESCRIPTION ............................................................................... 3
GENERAL DESCRIPTION ..................................................................................... 4
PRINCIPLE OF OPERATION .................................................................................. 6
SPECIFICATIONS ............................................................................................... 7
STARTUP ........................................................................................................... 8
GUIDE TO DISPLAY CODES ................................................................................. 9
GENERAL TIPS FOR AN ACCURATE MEASUREMENT ............................................... 11
PUMP CALIBRATION PROCEDURE ...................................................................... 11
FREE SO
TOTAL SO
PUMP TUBE REPLACEMENT ................................................................................ 15
FUSE REPLACEMENT ......................................................................................... 16
ELECTRODE CONDITIONING AND MAINTENANCE ............................................. 16
ACCESSORIES ................................................................................................. 18
MEASUREMENT PROCEDURE ............................................................... 13
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MEASUREMENT PROCEDURE ............................................................. 14
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FUNCTIONAL DESCRIPTION
DISPLAY
A. HOURGLASS ICON
B. BATTERY STATUS ICON
C. ERROR MESSAGE
D. MEASURE STATUS
E. CALIBRATION MODE INDICATOR
F. MAIN DISPLAY
G. MEASUREMENT UNIT
H. TIMER MODE INDICATOR
I. SECONDARY DISPLAY
FRONT PANEL
A. TITRANT BOTTLE
B. LIQUID CRYSTAL DISPLAY (LCD)
C. KEYPAD
D. ELECTRODE HOLDER
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REAR PANEL
E. ORP ELECTRODE
F. PERISTALTIC PUMP TUBE
G. BEAKER
H. PERISTALTIC PUMP
I. BNC ELECTRODE CONNECTOR
J. FUSE
K. POWER CABLE CONNECTOR
L. POWER SWITCH
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
KEYPAD
A. PUMP - to start/stop the pump
B. CAL - to enter pump calibration mode
C. STIR - to start/stop the stirrer while in
measurement or purging mode
D. START STOP - to start/stop titration or
pump calibration
GENERAL DESCRIPTION
The Mi455 is a low-cost, easy to use, microprocessor-based automatic titrator. It has a
simple and reliable peristaltic pump that ensure high dosing repeatability. By performing
pump calibration with the provided Milwaukee standards, the instrument accuracy is assured.
The instrument comes with a pre-programmed analysis method designed for Free and
Total Sulphur Dioxide measurements on wine samples. The instrument has a powerful
and effective built-in algorithm to analyze the shape of the electrode response and to
determine the reaction completion. This algorithm automatizes the analysis, makes all
the necessary calculations and assures a simple and effective interface for the user.
By simply pressing the START STOP button, the instrument will automatically make the
titration up to the equivalence point. The result is immediately displayed in convenient
units, then the instrument is ready for another titration.
SIGNIFICANCE OF USE
An important reason for adding SO2 is to avoid oxidation. When there is oxygen around,
SO2 itself becomes oxidized before phenol compounds in the wine , and so acts as an oxygen
scavenger. Also SO
problems.
What is really protecting your wine is molecular SO2. When you add SO2, depending of
circumstances, some of it immediately becomes bound. The relationship between the
amount of added SO2 and the amount of SO2 remaining free is complex. It is clear,
however, that it is largely governed by the total SO2 content of the wine. The rate of binding
decreases as the free SO2 concentration increases. The exact relationship between free
and bound (total - free) SO2 will vary from wine to wine.
Below 30-60 ppm, 33% to 50% of SO
called “free” and it is divided in two parts. The larger, and relatively ineffective free part is
suppresses the activity of enzymes that cause browning and other
2
addition becomes bounded. What remains is
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“bisulphite” (HSO3-). The smaller part of the free is the active molecular SO2. The amount
of molecular SO2 in your wine depends both on the level of free SO2 present as well as pH.
For instance, at pH 3.2, the amount of free SO2 for 0.8 ppm molecular SO2 is 22 ppm. At
pH 3.5, you will need 43 ppm free - essentially double.
Free SO
concentration (ppm) for 0.8 ppm molecular SO2:
2
Hp 0.31.32.33.34.35.36.37.38.39.3
418122825344559678901
OSeerF
2
In most situations, 0.8 ppm molecular SO
you with adequate protection from oxidation and bacterial action. This includes prevention
during bulk storage and at bottling will provide
2
of malolactic bacteria as well.
It is important to remember that the amount of free SO2 in the wine depends on three
things: how much is added, how much was present before the addition and how much of
your addition promptly becomes bound.
The level at which molecular SO
This is also the level which is needed for maximum protection of your wine. This is
can be detected by the human senses is about 2.0 ppm.
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particularly true in the case of sweet, and most notably, botrytised wines.
The Milwaukee Mi455 offers the possibility to test free or total SO
including the red ones, that are difficult to test with manual methods because the color
in all the wines
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changes are hardly seen.
This meter is supplied with:
• Reagents set for 20 titrations
• Two 50 mL beakers
• Two 20 mL beakers
• Tubes set with cap
• ORP probe
• Stir bar
• Power cable
• One 230 mL bottle of Refill Solution
• One 1 mL syringe
• Instruction manual
• Warranty code
Note: Save all packing material until you are sure that the instrument works correctly.
Any defective item must be returned in its original packing.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
PRINCIPLE OF OPERATION
Determination of sulphur dioxide in wine samples is made by titration of the sulphur
dioxide present in wine with iodate. In this procedure an excess of iodine is added to the
wine sample and it is titrated with iodate.
For precise results it is very important to know the exact sample volume, titrant volume and
concentration.
The peristaltic pump has a good repeatability but the dosing volume depends on many
factors as the diameter of the tube or the tube stretching. To compensate for all this errors,
the pump need to be calibrated. The calibration of the pump is also needed in order to have
high precision of the titrations.
The calibration procedure is in fact the analysis of a known solution. By doing this, the
instrument makes a differential analysis between the standard and the wine sample. The
pump volumetric debit and the real concentration of the titrant is compensated. Only the
sample volume has to be precisely known.
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SPECIFICATIONS
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Range 0 to 400 ppm SO
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Resolution 1 ppm
Accuracy 5% of reading
Method Ripper titrimetric method
Principle Equivalence point redox titration
Sample volume 50 mL
ORP Electrode MA924B/1 (included)
Pump debit 0.5 mL/min
Stirring speed 1500 rpm
Environment 0 to 50 °C (32 to 122 °F) ; max 95% RH non-condensing
Power supply 220V/50Hz; 10VA
Dimensions 208 x 214 x 163 mm (8.2 x 8.4 x 6.4") (with beaker)
Weight 2200 g (77,6 oz.).
Required Reagents
Code Description Quantity/test
Mi555-001 Standard (for Free & Total SO
Mi555-002 Titrant (for Free & Total SO
Mi555-003 Alkaline Reagent (for Total SO
Mi555-004 Acid Reagent (for Total SO
Mi555-005 Acid Reagent (for Free SO
Mi555-006 Stabilizer (for Free & Total SO
) 50 mL
2
)
2
)5 mL
2
)5 mL
2
)5 mL
2
) 1 packet
2
This instrument is in compliance with CE Directives.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
STARTUP
• Place the instrument on a flat table. Do not place the instrument on direct sun light.
• Connect the titrator to mains socket with ground connection and the correct voltage
and frequency. See the label on the instrument rear for this.
• Place the peristaltic pump tube on the pump. See the Pump Tube Replacement section
for the procedure.
• Remove the reagent bottle cap and place the bottle cap of the tubes set. Place the
reagent bottle in the appropriate place on the titrator top.
• Connect the tubes with the peristaltic pump (inlet tube is connected with the reagent
bottle, outlet tube is connected with the dosing tip).
• Turn the instrument ON using the power switch from the rear panel of the instrument
and wait until it displays dashes.
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PROBE FUNCTIONAL DESCRIPTIONPROBE FUNCTIONAL DESCRIPTION
PROBE FUNCTIONAL DESCRIPTION
PROBE FUNCTIONAL DESCRIPTIONPROBE FUNCTIONAL DESCRIPTION
GUIDE TO DISPLAY CODES
This screen appears for a few seconds each time the
instrument is turned ON.
Main screen display.
Main screen display with stirrer active.
Purging mode message.
PUMP CALIBRATION MESSAGES
This screen appears each time the meter enters pump
calibration mode. The meter is ready to start pump
calibration by pressing the START STOP button.
This screen appears while pump calibration is in progress.
Pressing CAL or START STOP button, the minititrator
returns to the main screen.
This screen appears for a few seconds before returning
to the main screen, when pump calibration is done.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
This error message appears when the sample
concentration exceeds 400 ppm.
The used standard solution is wrong.
This error message appears when the input readings
(mV) exceed the input limits (0÷1000mV).
TITRATION MESSAGES
This screen appears each time a titration is running.
When the START STOP button is pressed the minititrator
returns to the main screen.
The titration result, expressed as concentration of sulphur
dioxide in ppm (mg/L), is displayed at the end of the titration
process. Press the START STOP button to return to the main
screen.
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This error message appears when the input reading
exceeds the input limits (0÷1000mV).
This screen appears when the sample concentration
exceeds 400 ppm.
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GENERAL TIPS FOR AN ACCURATE MEASUREMENT
The instructions listed below should be carefully followed during testing to ensure
best accuracy.
• Purge the peristaltic pump to have fresh titrant when starting a new analysis or
calibration.
• Calibrate the peristaltic pump before performing an analysis.
• Analyze the wine immediately after the sample is obtained.
PUMP CALIBRATION PROCEDURE
Warning: The calibration of the pump must be performed each time the pump tube, the
reagent bottle or the pH electrode is changed. It is recommended to perform the pump
calibration before each set of measurements.
• Using a clean pipette, fill the 50 mL beaker
up to the 50 mL mark with Mi555-001
Standard.
Note: Failure to use clean pipettes will result
in erroneus readings.
• Place the stir bar in the beaker and put the
beaker in the minititrator top.
• Fill the 20 mL beaker up to the 5 mL mark
with the Mi555-005 Acid Reagent and add
the content to the 50 mL beaker.
• Place the beaker into the beaker holder.
Place the probe holder on the top of the
beaker and secure by turning clockwise.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
• Open refill cap on the ORP electrode and
immerse the electrode approximately 2 cm
(0.8”) into the sample to be tested. Do not
touch stir bar with the tip of the electrode.
• Ensure there is titrant in the dosing tip. If
not, hold the dosing tip over an empty
container and press PUMP for a few seconds
until the titrant is in the dosing tip.
• Add the contents of one powder packet of
Mi555-006 Stabilizer into the beaker.
• Press CAL button. The meter enters in pump
calibration mode.
• Press START STOP in order to start the
system calibration.
• At the end of the calibration, DONE appears
for a few seconds and the meter returns to
the measurement mode.
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FREE SO2 MEASUREMENT PROCEDURE
• Using a clean pipette, fill the 50 mL beaker
up to 50 mL mark with the wine sample.
Note: It is important to be accurate in your
measurements of Wine sample. Pipettes are
recommended.
• Place the stir bar in the beaker and put the
beaker in the minititrator top.
• Fill the 20 mL beaker up to the 5 mL mark
with the Mi555-005 Acid Reagent and add
the content to the 50 mL beaker.
• Place the probe holder on the top of the
beaker and secure by turning clockwise.
• Open refill cap on the ORP electrode and
immerse the electrode
(0.8”) into the sample to be tested. Do not
touch stir bar with the tip of the electrode.
• Insert dosing tip into holder. Ensure there is
titrant in the dosing tip. If not, hold the
dosing tip over an empty container and press
PUMP for a few seconds until the titrant is in
the dosing tip. The tip should be below the
pump to ensure gravity flow.
Note: Be aware of any air bubbles in the
tube it could effect the results.
approximately 2 cm
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• Add the contents of one powder packet of
Mi555-006 Stabilizer into the beaker.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
• Press START STOP in order to start titration.
The display will show “----” during titration,
along with stirrer and pump tags blinking on
the LCD.
• At the end of the titration, the Sulphur Dioxide
concentration is displayed in mg/L (ppm).
TOTAL SO2 MEASUREMENT PROCEDURE
• Fill the 50 mL beaker up to 50 mL mark with
the wine sample.
Note: It is important to be accurate in your
measurement of wine sample. Pipettes are
recommended.
• Place the stir bar in the beaker and put the
beaker in the minititrator top.
• Fill the 20 mL beaker up to the 5 mL mark
with the Mi555-003 Alkaline Reagent and
add the content to the 50 mL beaker.
• Swirl the beaker and wait for 15 minutes.
• Using a clean pipette, fill the 20 mL beaker
up to the 5 mL mark with the Mi555-004
Acid Reagent and add the content to the 50
mL beaker.
• Open refill cap on the ORP electrode and
immerse the electrode approximately 2 cm
(0.8”) into the
sample to be tested. Do not
touch stir bar with the tip of the electrode.
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• Insert dosing tip into holder. Ensure there is
titrant in the dosing tip. If not, hold the
dosing tip over an empty container and press
PUMP for a few seconds until the titrant is in
the dosing tip. The tip should be below the
pump to ensure gravity flow and minimize
the chance of air bubbles in the tube.
• Add the content of one powder packet of
Mi555-006 Stabilizer into the beaker.
• Press START STOP button to start titration.
The display will show “----” during titration,
along with stirrer and pump tags blinking on
the LCD.
• At the end of the titration, the Sulphur Dioxide
concentration is displayed in mg/L (ppm).
PUMP TUBE REPLACEMENT
To remove the tube of the peristaltic pump follow next steps:
• Detach the old tube system from the reagent bottle.
• Grasp one fixing ring of the peristaltic pump tube.
• Pull the tube until it’s taken out from its location.
• Remove the other side of the tube.
To mount the new peristaltic pump tube follow next steps:
• Position one peristaltic pump fixing ring on its location.
• Stretch the tube over the peristaltic pump cylinders.
• Fix the second pump fixing ring on its location.
• Attach the tube to the reagent bottle.
Note:Purge the peristaltic pump until drops of reagent appears on the dosing tip by
pressing the PUMP button.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
FUSE REPLACEMENT
To change the fuse follow next steps:
• Disconnect the power cord from the rear panel
of the instrument.
• Pull out the fuse holder located near the power
cord connector.
• Replace the fuse with a similar one.
• Push the fuse holder with the fuse in the
appropriate place.
ELECTRODE CONDITIONING & MAITENANCE
PREPARATION PROCEDURE
Remove the protective cap of the ORP electrode (MA924B/1).
DO NOT BE ALARMED IF SALT DEPOSITS
ARE PRESENT. This is normal with electrodes. They will disappear when rinsed
with water.
During transport, tiny bubbles of air may
form inside the glass bulb affecting proper
functioning of the electrode. These bubbles
can be removed by “shaking down” the electrode as you would do with a glass
thermometer.
If the bulb and/or junction is dry, soak the
electrode in MA9015 Storage Solution for at
least one hour.
If the filling solution (electrolyte) is more
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than 2½ cm (1”) below the fill hole, add MA9011 3.5M KCl Electrolyte Solution. For
faster response, unscrew the fill hole screw during measurements.
STORAGE PROCEDURE
To minimize clogging and assure a quick response time, the glass bulb and the junction of
the electrode should be kept moist and not allowed to dry out.
Replace the solution in the protective cap with a few drops of MA9015 Storage Solution
or, in its absence, Filling Solution (MA9011). Follow the Preparation Procedure before
taking measurements.
Note: NEVER STORE THE ELECTRODE IN DISTILLED OR DEIONIZED WATER.
PERIODIC MAINTENANCE
Inspect the electrode and the cable. The cable used for connection to the instrument must
be intact and there must be no points of broken insulation on the cable or cracks on the
electrode stem or bulb. Connectors must be perfectly clean and dry. If any scratches or
cracks are present, replace the electrode. Rinse off any salt deposits with water.
Probe Maintenance
Refill the reference chamber with fresh electrolyte (MA9011). Allow the electrode to
stand upright for 1 hour. Follow the Storage Procedure above.
CLEANING PROCEDURE
• Wine deposits Soak in Milwaukee MA9016 cleaning solution for 1 hour
• Wine stains Soak in Milwaukee MA9016 cleaning solution for 1 hour
IMPORTANT: After performing any of the cleaning procedures, rinse the electrode thoroughly with distilled water, refill the reference chamber with fresh electrolyte and soak the
electrode in MA9015 Storage Solution for at least 1 hour before taking measurements.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
ACCESSORIES
REAGENT SETS
MA9011 Electrode filling solution (230 mL)
MA9015 Electrode storage solution (220 mL)
MA9016 Cleaning solution (220 mL)
Mi555-001 Calibration standard (500 mL)
Mi555-002 Titrant solution (100 mL)
Mi555-003 Alkaline reagent (100 mL)
Mi555-004 Acid reagent for Total SO
Mi555-005 Acid reagent for Free SO
Mi555-006 Stabilizer reagent (40 pcs.)
OTHER ACCESSORIES
MA924B/1 ORP probe with 1 m cable
Mi0009 Stir bar (5 pcs.)
Mi0010 Titrator tube (2pcs.)
Mi0020 Beaker 50 mL (4 pcs.)
Mi0021 Beaker 20 mL (4 pcs.)
determination (100 mL)
2
determination (100 mL)
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Recommendations for Users
Before using this product, make sure that it is entirely suitable for your specific application
and for the environment in which it is used.
Operation of this instrument may cause unacceptable interferences to other electronic
equipments, this requiring the operator to take all necessary steps to correct interferences.
Any variation introduced by the user to the supplied equipment may degrade the instrument
EMC performance.
To avoid damages or burns, do not put the instrument in microwave ovens. For yours and the
instrument safety do not use or store the instrument in hazardous environments.
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For your Safety don’t use or store the instrument in hazardous environments. To avoid
damages or burns, do not perform any measurement in microwave ovens.
WARRANTY
This instrument is warranted against defects in materials and manufacturing for a period of
2 years from the date of purchase. Electrodes are warranted for 6 months.
If during this period the repair or replacement of parts is required, where the
damage is not due to negligence or erroneous operation by the user, please return
the intrument, electrode and probe to either distributor or our office and the repair
will be effected free of charge.
Damage due to accidents, misuse, tampering or lack of prescribed maintenance is
not covered by the warranty.
Milwaukee/Martini instruments reserves the right to make improvements
in design, construction and appearance of its products without advance
notice.
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Instruction Manual Mi455 FREE & TOTAL SULPHUR DIOXIDE Minititrator for wine analysis
THANK YOU FOR CHOOSING
Sales and Technical Service Contacts:
Milwaukee s.r.l.
C.so Leonardo da Vinci 48/50
21013 Gallarate (VA) ITALY
Tel: +39 0331 26 80 09
Fax: +39 0331 26 80 33
e-mail: sales@milwaukee.191.it
Milwaukee Instruments, Inc.
2950 Business Park Drive Rocky Mount, NC
27804 USA
Tel: +1 252 443 3630
Fax: +1 252 443 1937
e-mail: milwaukee@vol.com
2020
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MANMI455 12/07
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