Milwaukee MI456 User manual

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Milwaukee WMilwaukee W
Milwaukee WMilwaukee W
Milwaukee Wine Line L
ine Line L
ine Lab Minititratorab Minititrator
ab Minititratorab Minititrator
ab Minititrator
Mi456
TT
TT
Titratable Titratable T
itratable Titratable T
itratable Total Aotal A
otal Aotal A
otal Aciditycidity
ciditycidity
cidity
INSTRUCTION MANUAL

Instruction Manual Mi456 TITRATABLE TOTAL ACIDITY Minititrator for wine analysis
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FUNCTIONAL DESCRIPTION ............................................................................... 3
GENERAL DESCRIPTION ..................................................................................... 4
PRINCIPLE OF OPERATION .................................................................................. 6
SPECIFICATIONS ............................................................................................... 7
STARTUP ........................................................................................................... 8
GUIDE TO DISPLAY CODES ................................................................................. 8
GENERAL TIPS FOR AN ACCURATE MEASUREMENT ............................................... 11
PUMP CALIBRATION PROCEDURE ...................................................................... 11
pH CALIBRATION PROCEDURE .......................................................................... 13
MEASUREMENT PROCEDURE ............................................................................. 14
PUMP TUBE REPLACEMENT ................................................................................ 15
FUSE REPLACEMENT ......................................................................................... 16
ELECTRODE CONDITIONING AND MAINTENANCE ............................................. 16
ACCESSORIES ................................................................................................. 18
TABLE OF CONTENTS

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FUNCTIONALDESCRIPTION
FRONT PANEL
A. TITRANT BOTTLE
B. LIQUID CRYSTAL DISPLAY (LCD)
C. KEYPAD
D. ELECTRODE HOLDER
KEYPAD
A. PUMP - to start/stop the pump
B. CAL - to enter pump or pH calibra-
tion mode
C. pH - to enter pH calibration mode
(when CAL tag is active) to modify
the end point value.
D. STIR - to start/stop the stirrer while
in measurement or purging mode
E. START STOP - to start/stop titration
REAR PANEL
E. pH ELECTRODE
F. TEMPERATURE PROBE
G. PERISTALTIC PUMP TUBE
H. BEAKER
I. PERISTALTIC PUMP
J. TEMPERATURE PROBE CONNECTOR
K. BNC ELECTRODE CONNECTOR
L. FUSE
M. POWER CABLE CONNECTOR
N. POWER SWITCH

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GENERALDESCRIPTION
The Mi456 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 preprogrammed analysis method designed for Total
Titratable Acidity measurements on wine.
The Mi456 performs automatic analysis, all the necessary calculations and assures to
the user a simple and effective interface.
The instrument has a powerful and effective built-in algorithm to analyze the shape of the
pH electrode response and to determine the reaction completion.
By simply pressing the START STOP button, the instrument will automatically make the
titration up to the end point. The result is immediately displayed in convenient units, then
the instrument is ready for another titration.
DISPLAY
A. STABILITY INDICATOR: when reading is
unstable or calibration is in progress
B. STIRRER ACTIVE TAGS
C. CALIBRATION MESSAGES
D. PUMP ACTIVE TAGS
E. CALIBRATION MESSAGES
F. “pH” TAG: when a buffer is displayed
on the secondary display
G. FOUR DIGITS AND HALF SECOND-
ARY DISPLAY
H. “Time” TAG: when the time is displayed
on the secondary display
I. FOUR DIGITS AND HALF MAIN DISPLAY
J. “pH” UPPER TAG: when the end point
is modified
K. AUTOMATIC TEMPERATURE COM-
PENSATION: when ATC blinks the
temperature probe is not connected
and the temperature is considered to
be 25 °C

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SIGNIFICANCE OF USE
Acids occur naturally during the growing of grapes and as part of the fermentation process. Wines
show lower levels of acid when there are hot growing seasons or when the grapes come from
hotter regions. In the proper proportion, acids are a desirable trait and give the wine character.
The three predominant acids in wine are tartaric, malic and citric, all of which are intrinsic
to the grape. Tartaric acid is the principal acid in grapes and is a component that promotes
a crisp flavor and graceful aging in wine. A moderate amount of a wine’s acid comes from
malic acid, which contributes to fruitiness, and a small amount comes from citric acid. Wine
also contains trace amounts of other acids. The least desirable acid in wine is acetic acid,
which, when present in more than a nominal amount, gives wine a sour or vinegary aspect.
Total acidity, also called titratable acidity, is the sum of the fixed and volatile acids. In the
United States the total acidity is usually expressed in terms of tartaric acid, even though the
other acids are measured.
Total Acidity directly effects the color and flavor of wine and, depending on the style of the wine,
is sought in a perfect balance with the sweet and bitter sensations of other components. Too
much acidity makes wine tart and sharp; too little makes wines flat, flabby and uninteresting.
Proper acidity in wine is what makes it refreshing and an ideal accompaniment to food.
The proper acid level of a wine varies, with sweeter wines generally requiring somewhat
higher levels to retain the proper balance. For dry table wine the acceptable range is
usually 0.60 to 0.75%; for sweet wine it’s 0.70 to 0.85%.
This meter is supplied with:
• Reagents set for 20 titrations
• One 2000PL automatic pipette
• Two plastic tips for the 2000 PL automatic pipette
• Two 50 mL beakers
• Tubes set with cap
• pH electrode
• Temperature probe
• Stir bar
• Power cable
• One 230 mL bottle of Refill Solution
• One 1 mL syringe
• Instruction manual
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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PRINCIPLE OF OPERATION
The determination of total acids in wine is made according to a neutralization reaction, that
is the reaction between the acids found in wine and a base. This type of reaction forms the
basis of titration methods of analysing acids.
Titratable acidity is measured on a degassed sample at the end-point of 8.20 for Australian
requirements and 7.00 to fulfil the requirements of the European Union. Both results are
expressed as g/L tartaric acid.
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 streching. 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. It is important to calibrate the pump at the pH value you
want to use as the endpoint 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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This instrument is in compliance with CE Directives.
SPECIFICATIONS
Range 0.0 to 25.0 g/L of tartaric acid
Resolution 0.1 g/L
Accuracy 5% of reading
Method Acid-base titration method
Principle End-point titration
pH Calibration One-point in selected end-point: 7.00 pH or 8.20 pH
Sample volume 2 mL
Temperature Automatic from 0.0 to 100.0 °C
Compensation
pH Electrode MA919B/1 (included)
Temperature Probe MA831R (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
Mi556-001 Standard 2 mL
Mi556-002 Titrant
Mi556-003 Buffer pH 7.00 50 mL
Mi556-004 Buffer pH 8.20 50 mL

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PROBE FUNCTIONAL DESCRIPTIONPROBE FUNCTIONAL DESCRIPTION
PROBE FUNCTIONAL DESCRIPTIONPROBE FUNCTIONAL DESCRIPTION
PROBE FUNCTIONAL DESCRIPTION
GUIDE TO DISPLAY CODES
Purging mode message.
Main screen display with stirrer active.
Main screen display.
This screen appears for a few seconds each time the
instrument is turned ON.
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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This screen appears each time the meter enters pump or
pH calibration mode by pressing the CAL button. The
meter is ready to start pump calibration by pressing the
PUMP button. The meter returns to the main screen by
pressing the CAL button.
PUMP CALIBRATION MESSAGES
This screen appears while pump calibration is in progress.
Pressing CAL or PUMP 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.
The used standard solution is wrong.
This error message appears when the input readings
(mV) exceed the input limits (0
y 1000mV).
This error message appears when the sample
concentration exceeds 400 ppm.
This screen appears each time the meter enters pump or
pH calibration mode by pressing the CAL button.
pH CALIBRATION MESSAGES
This screen appears when the pH calibration is started
by pressing the pH button. Pressing again pH or the
CAL button, the pH calibration is aborted and the
instrument returns to the main screen.

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This screen appears each time the minititrator enters
TITRATION mode. Press the START STOP button in order
to stop the titration and return to the main screen.
TITRATION MESSAGES
The titration result, expressed as concentration of tartaric
acid in g/L, is displayed at the end of the titration process.
Press the START STOP button to return to the main screen.
This error message appears when the input reading
(pH, temeprature) exceeds the input limits.
This screen appears when the evaluated concentration
is out of range.
This prompt appears for a few seconds before returning
to the main screen, when the pH calibration is done.
The “WRONG” “” / “WRONG” “ ” tags alternatively
blinking appear when the buffer solution is not correct or
when the probe is wrong. Clean the electrode by following
the Cleaning Procedure or check the quality of the buffer
in order to continue the pH calibration.
Press the CAL or pH button to leave pH calibration mode.
pH END POINT SETUP MESSAGES
This screen appears when the meter is in main screen and the
pH button is pressed. Press the CAL button in order to change
the end-point. Each time the pH button is pressed the end point
value is changed and the meter returns to the main screen.

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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.
PUMPCALIBRATIONPROCEDURE
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.
• Use the 2000 PL automatic pipette to add
exactly 2 mL of Mi556-001 Standard to the
50 mL beaker.
• Fill the beaker up to the 50 mL mark with
deionized water, place the stirrer bar into
the beaker and then place the beaker in the
appropriate place on the minititrator top.
• Place the electrode holder on the top of the
beaker and secure by turning clockwise.

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• Immerse the pH and the temperature probe
approximately 2 cm (0.8“) into the sample
to be tested while paying attention to not
touch the stir bar.
• Insert the dosing tip in the appropriate holder
place and pay attention to not be immersed
into solution.
• After sample preparation, press the CAL
button to enter the pump calibration mode.
The CAL tag will start blinking.
• Press PUMP in order to start the pump
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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pH CALIBRATION PROCEDURE
The pH calibration must be performed each time the pH electrode is changed.
• Turn the instrument ON using the power
switch from the rear panel of the instrument.
• Fill the 50 mL beaker up to the 50 mL mark
with Buffer Solution 1 (7.00 pH) or Buffer
Solution 2 (8.20 pH).
• Place the pH electrode into solution and
press the CAL button. The CAL tag will
appear blinking.
• Press pH in order to start the electrode
calibration.
• At the end of the calibration procedure “done”
appears for a few seconds and then the meter
automatically returns to measurement mode.
or
7.00 pH 8.20 pH

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MEASUREMENT PROCEDURE
• Use the 2000 μL automatic pipette to add
exactly 2 mL of wine sample to the 50 mL
beaker.
• Fill the beaker up to the 50 mL mark with
deionized water, place the stirrer bar into
the beaker and then place the beaker in the
appropriate place on the minititrator top.
• Place the electrode holder on the top of the
beaker and secure it by turning clockwise.
• Immerse the pH and the temperature probe
approximately 2 cm (0.8“) into the sample
to be tested while paying attention to not
touch the stir bar.
• Insert the dosing tip in the appropriate holder
place and pay attention to not be immersed
into solution.
Warning: Make sure the instrument has been calibrated (pH and pump calibration) before
performing a wine sample analysis.

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• Press the START STOP button to start the
titration. The display will show “----” during
titration, along with stirrer and pump tags
blinking on the LCD, and 7.00 or 8.20 pH
buffer on the secondary display.
• At the end of the titration, the Total Titratable
Acidity concentration is displayed in g/L.
Note:If the end-point is not reached or it is not
recognized because of the noisy solution,
an error message will be displayed.
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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FUSEREPLACEMENT
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 pH elec-
trode (MA919B/1).
DO NOT BE ALARMED IF SALT DEPOSITS
ARE PRESENT. This is normal with elec-
trodes. They will disappear when rinsed
with water.
During transport, tiny bubbles of air may form
inside the glass bulb affecting proper func-
tioning 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
than 2½ cm (1”) below the fill hole, add

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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 thor-
oughly 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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ACCESSORIES
REAGENT SETS
MA9015 Electrode storage solution (220 mL)
MA9016 Cleaning solution (220 mL)
MA9011 Electrode filling solution (230 mL)
Mi456KIT Reagent set
Mi556-001 Calibration standard (100 mL)
Mi556-002 Titrant solution (100 mL)
Mi556-003 Buffer solution 1 pH 7.00 (100 mL)
Mi556-004 Buffer solution 2 pH 8.20 (100 mL)
OTHER ACCESSORIES
MA919B/1 pH electrode with 1 m cable
MA831R Temperature probe
Tube set with cap for titrant bottle and tip
Mi0022 2000 PL pipette
Mi0023 Pipette tips for 2000 PL pipette (4 pcs.)
Mi0009 Stir bar (5 pcs.)
Mi0020 Beaker 50 mL (4 pcs.)
Power cable
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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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.
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.

THANK YOU FOR CHOOSING
Sales and Technical Service Contacts:
Milwaukee Electronics Kft.
Alsókikötősor 11.
6726, Szeged, Hungary
Tel: [phone]
Fax: [phone]
e-mail: [email protected]
Milwaukee Instruments, Inc.
2950 Business Park Drive Rocky Mount, NC
27804 USA
Tel: [phone]
Fax: [phone]
e-mail: [email protected]
www.milwaukeeinst.com
MANMI456 11/06