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Titrator
DL15
Table of contents
Table of Contents
1. Introduction 5
2. Safety measures 6
3. Standard equipment and Installation 7
3.1 Standard equipment DL15 Titrator 7
3.2 Installation 9
3.2.1 Attaching the titration stand to the titrator 9
3.2.2 Installing the burette 10
3.2.3 Installing the magnetic stirrer 10
3.2.4 Swiveling the titration stand 11
3.2.5 Attaching and removing the titration beaker 12
4. The titrator 13
4.1 Design of the titrator 13
4.2 Connections at the rear of the titrator 13
4.3 The operating concept 14
4.3.1 The display 15
4.3.2 The arrow keys 15
4.3.3 The function keys 15
4.3.4 The input keys 15
4.3.5 The menu keys 16
4.3.6 The Help function keys 17
4.3.7 The Escape key 17
4.3.8 The Reset key 17
4.3.9 The Home screen 18
5. Setup 19
5.1 Opening the Setup menu 19
5.2 Titrants 19
5.2.1 Adding a titrant 20
5.2.2 Modifying a titrant 20
5.2.3 Deleting a titrant 22
5.2.4 Printing a titrant 23
5.2.5 Titer determination from the titrant setup 23
5.3 Sensors 25
5.3.1 Adding a sensor 25
5.3.2 Modifying a sensor 26
5.3.3 Deleting a sensor 28
5.3.4 Printing a sensor 28
5.3.5 Sensor calibration from the sensor setup menu 29
5.3.6 Sensor test from the sensor setup menu 32
5.4 Peripherals 35
5.4.1 Setting up a printer 35
5.4.2 Setting up a balance 36
5.5 Standards 37
5.5.1 Adding a standard 37
5.5.2 Modifying a standard 37
5.5.3 Deleting a standard 39
5.5.4 Printing a standard 39
9. Performing a titration 83
9.1 Preparations 83
9.1.1 Filling the burette (rinsing) 84
9.2 Performing titration method 920 84
10. Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) 89
10.1 Information menu 89
10.2 Sensor 89
10.2.1 Measuring temperature 90
10.2.2 Measuring potential 90
10.2.3 Calibrating a sensor 91
10.2.4 Testing a sensor 91
10.3 Stirrer 91
10.4 Burette 92
10.4.1 Rinsing the burette 92
10.4.2 Rinsing the tip 93
10.4.3 Dispensing 93
10.4.4 Manual titration 93
10.5 Report 95
10.6 Results 95
10.6.1 Displaying and printing results 96
10.6.2 Statistics 96
10.6.3 Terminating the series 98
11. Error messages, malfunctions and hardware tests 99
11.1 Global errors and malfunctions 99
11.2 Hardware tests 100
11.2.1 User interface 100
11.2.2 Communication interfaces 101
11.2.3 Auxiliary I/O 102
11.2.4 pH input value 103
12. Optional accessories and maintenance 105
12.1 Optional accessories 105
12.2 Service and maintenance 107
12.2.1 Cleaning 107
12.2.2 Disposal 107
13. Technical data 109
Appendix: Predefined calibration standards 120
Index 124
1. Introduction
The DL15 Titrator is the ideal solution for all requirements in the food industry, water/
wastewater analysis, and the chemical industry when all that is needed is an endpoint
titration or a pH measurement. The DL15 is mainly used to determine the acid and base
content of a sample.
It features easy-to-understand intuitive user guidance so that, for example, pressing the
Run button twice starts the method you last ran.
The user can assign three other methods to individual function keys, making methods
easy to find and start.
The keys used for the most frequently used manual functions are identified by pictograms.
Titrants and sensors can be selected from the instrument’s database.
Alphanumeric input is easily entered by means of a special keypad, just like with a mobile
phone. There is no need to connect an external keyboard.
The DL15 calculates the analytical results in predefined units and sends an analysis report
to commercially available printers.
2. Safety measures
The titrators have been tested for the experiments and purposes documented in this
Operating Instructions. This does not, however, absolve you from the responsibility of
performing your own tests on the products supplied by us regarding their suitability for the
methods and purposes you intend to use them for. Please adhere strictly to the following
safety measures.
– Make sure that the titration beaker is always securely attached in the titration head!
Corrosive chemicals If the beaker falls out, you could injure yourself when working with poisonous titrants
and solvents, strong bases or acids.
Caution – When using chemicals and solvents, follow the manufacturers' instructions and the
general rules for safety in the laboratory!
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3.2 Installation
3.2.1 Attaching the titration stand to the titrator
When the titration stand is delivered, the spacing ring, clamping ring and threaded ring
are already mounted. The holder for the titration stand still has to be fixed to the titrator
with the corresponding screw. Afterward, the assembled titration stand can be inserted
from above. The diagram below shows how the titration stand is attached to the titrator
and how the titration stand can be assembled and disassembled.
Cap
Titration stand
Spacing ring
Clamping ring
Threaded ring
Screw
Titration beaker
• When you rinse the burette and tubing, place the dispenser tube in a waste contai-
ner!
Magnetic stirrer
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You can swivel the titration stand in and out. To
do this, you lift the titration stand slightly and pull
it upward a little bit out of the holder. Now you
can swivel it to the desired position and then let
it slide back into the holder.
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To remove the titration beaker from the titration stand, loosen the threaded ring about a
quarter to half a turn C, and then carefully remove the titration beaker downward out of
the titration stand.
4. The titrator
4.1 Design of the titrator
Titrator stand
Burette
Sample beaker
Arrestment knob
Magnetic stirrer
Titrant bottle
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mV / pH electrode
Overhead stirrer RS-P42 printer
Reference Balance
electrode
Temperature not assigned
sensor
Rondolino
Polariz. electrode
HP compat.
Magnetic stirrer printer
Power supply
Connection Device
mV/pH mV / pH electrode (sensor)
Ref Reference electrode
PT1000 PT1000 temperature sensor
Pol polarized electrode (sensor)
Overhead Stirrer Overhead stirrer
Magnetic Stirrer Magnetic stirrer
Balance Balance (RS232C)
Rondolino TTL I/O Rondolino, external devices
RS-P42 RS-P42 (GA-42) printer (RS232C)
Computer not assigned
Printer HP-compatible printer (Centronics)
5V/24V DC Power supply
The operating console of the titrator consists of the display in the middle with several
groups of keys arranged around it. The various functional areas are described in the fol-
lowing sections.
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The three black-inverted boxes (E) across the bottom line of the display show the functions
to which the function keys directly below (F1, F2 and F3) are assigned for the menu item
selected.
- Pressing the number key 2 once, for example, writes the letter "a"; pressing it three
time, the letter "c", and so on.
- To obtain large characters, you must press and hold down the Shift key (arrow point-
ing upward) while selecting the character.
- You can delete the last character by pressing the Del key. If you simultaneously press
the Delete key and the Shift key, the entire content of the text box is deleted.
- To insert a space, press the number key 0.
- You can insert special characters by simultaneously pressing the number key 1 and
the Shift key. A screen appears displaying all the available special characters. The
black box indicates the character currently selected.
- Select the desired character using the arrow keys and the < and > keys.
- Press OK to enter the special character in the text area.
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The Setup key opens the Setup menu of the titrator. All the resources such as titrants, sen-
sors, standards and blank values necessary for the titration are stored and managed in
this menu. In addition, you can select the internal titrator settings you require and configure
peripheral devices.
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The Method key opens the Method menu of the titrator. The methods stored in the titrator
are managed in this menu. You can store your own methods, delete and modify them. A
number of methods developed by METTLER TOLEDO are already stored and can be directly
used to perform analyses or be used as templates for new methods.
The resources you want to use for a method must be defined and stored beforehand in
the Setup menu.
The Run key opens the Start menu to perform an analysis. Methods used for different
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determinations can be selected and started.
The Series key opens the start menu to perform a sample series analysis. Methods used
for different determinations can be selected and started
An automation of the series determination can be achived by using a Rondolino sample
changer.
������ This menu lets you measure the pH, potential or temperature of a solution and test and
calibrate pH and ISE sensors.
������� The burette and the burette tip can be rinsed, and any volume you like dispensed. You can
perform a manual titration.
You can view the titrator information and open a menu to test the titrator hardware and
the connected devices.
������� You can view, print and manage the results of your analyses including statistical evalu-
ations.
In the Report menu you can define and print additional reports.
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By pressing the Escape key, you can quit a menu or a selection at any time and discard
the changes you made. You always return to the previous menu and the original values
and names remain the same.
The Home screen appears on the display as soon as you switch on the titrator.
It is the starting point for operating the titrator.
Each time you reset the titrator by pressing Reset, you return to the Home screen.
The screen displays the following important information:
5. Setup
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In this chapter you learn how to set up the titrator for your specific requirements.
To perform a titration, you must first define and configure the resources (titrants, sensor,
peripherals, etc.) used for the method in the titrator.
You can scroll the list upward or downward using the arrow keys on the right next to the
display. The black-inverted line always shows the current selection.
If you press Print, the list with the available entries for the selected resource is printed.
See "5.4.1 Setting up a printer"
If you press OK, the list of the selected resources appears on the display.
5.2 Titrants
- Press Setup to open the Setup menu.
- Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants
stored in the titrator appears.
The titrants used by the METTLER methods are already preset in the titrator. You can delete
titrants, and modify or print the parameters of the selected titrants. Furthermore, you can
determine and store the titer for each titrant using an automatic function.
• You can add a new titrant by modifying the parameters of an existing titrant and then
storing it under a new name.
• A maximum of 30 titrants can be stored in the titrator.
• You can discard the changes you have made by pressing Esc to quit the selection. In
this case, the titrant is not stored.
• Determine the titer of the new titrant using the automatic titer determination (Titer
key) if you have not already entered it manually. See "5.2.5 Titer determination from
the Titrant setup".
• In any case, first change the name of the titrant. Otherwise the changes you made for
the existing titrant will be effective on pressing the Save key, and no new titrant will
be stored in the titrator!
Minimum The "Minimum" parameter lets you define the lower limit for the
range within which the titer must be.
Maximum The "Maximum" parameter lets you define the upper limit for the
range within which the titer must be.
Standard Here you can select one of the standards defined in the titrator
to determine the titer of your titrant.
Burette Using this parameter you can define the burette volume. Pos-
sible values are 1, 5, 10 and 20 mL.
Charge With this parameter you can record information about the batch
from which the titrant originates.
Fill rate [%] The "Fill rate" indicates how quickly the burette is filled with
titrant. Filling the burette at the highest rate corresponds to a fill
rate of 100%, and at the lowest rate to a fill rate of 30%. The
preset value is 100%
Check after [day] This value is used to calculate the expiration date for the titrant.
A period of 0 to 100 days can be defined. If the parameter has
the value 0, no expiration date is determined.
Date The date of the last titer determination. Each time you store the
titrant, the date is set to 00-00-0000.
Time The time of the last titer determination. Each time you store the
titrant, the time is set to 00:00.
• If you change the name of a titrant and save your changes, a new titrant is created
under the new name.
• If the value for the titer determined by a titer determination or the manually entered
value is outside the range defined by "Minimum" and "Maximum", an error message
appears and the titer must either be determined or entered again.
• When you use a titrant of higher viscosity, it is advisable to reduce the fill rate in
order to prevent air being sucked-in when filling the burette.
• If, at the start of an analysis, the titant has expired (the expiration date has been
exceeded), a message appears to draw your attention to this. If you still want to per-
form the determination, you must confirm the message. In the report, a correspond-
ing line appears that notes that the titrant has expired.
• You can only delete titrants that have not been used in a method.
• Titrants referenced by METTLER methods cannot be deleted.
cactual
t=
cnom
The titer enables the titrator to calculate the results of your analyses corresponding to
the actual concentration of the titrant used. It is therefore essential for you to accurately
determine the actual concentration of the titrant against a reference substance before you
first use it.
The titrator can store the corresponding titer as a parameter for every titrant defined in
the titrator. As long as the titer for a titrant has not been determined, the default value 1
is used.
You can determine the titer yourself, enter the value for the titrant manually in the Setup
menu, or to determine it through automatic titer determination with the titrator.
Before doing this, you should make sure that a suitable standard is already stored in the
titrator for the primary standard you want to use. If this is not the case, you must first define
a new standard in the instrument. See "5.5.1 Adding a standard".
• It is also possible to perform the automatic titer determination from the Analysis
menu. See "8.2 Starting a titer determination using the Run key"
• The concentration of a titrant can change after you have determined the titer. It is
therefore absolutely essential to determine the titer at regular intervals in order to
guarantee constant accuracy of the analysis results. The titrator can also generate a
specific expiration date for each titrant, which requests the user to determine the titer
again after a certain period.
5.3 Sensors
- Press Setup to open the Setup menu.
- Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors
stored in the titrator appears.
Some sensors are already predefined in the titrator. You can add new sensors, change them
or delete them from the list. For pH and ISE sensors you can also perform an automatic
sensor calibration.
You can define:
• mV sensors
• pH sensors
• ion selective sensors (ISE)
• polarized sensors
• To add a new sensor, you must change the parameters of one of the existing sen-
sors and then save it under a new name.
• A maximum of 20 sensors can be stored in the instrument.
• You can discard your changes at any time by pressing Esc to quit the selection. In
this case the sensor is not stored.
• Before using it for the first time, you must calibrate a newly defined pH or ISE sensor
using the automatic calibration function (the Calib. key) if you have not already ma-
nually entered the slope and zero point. See "5.3.5 Sensor calibration from the sensor
setup menu".
• In any case, first change the name of the sensor. Otherwise when you press Save,
your changes will be effective for the existing sensor and no new sensor is stored in
the instrument!
Type This parameter lets you define the sensor type for sensors at the
pH input. There is a choice of pH, mV and ISE.
Unit A possible unit can be selected for the sensor (pH, mV or pX).
This appears only for pH and ISE sensors!
Zero point [pH] The zero point of the pH or ISE sensor used. This value can be
or entered manually or be determined by the instrument during
Zero point [pX] automatic sensor calibration. Prior to the initial calibration, the
default value of 7.00 for pH sensors and ISE sensors is stored
here.
This appears only for pH and ISE sensors!
Slope [mV/pH] The slope of the pH or ISE sensor used. This value can be en-
or tered manually or be determined by the instrument during the
Slope [mV/pX] automatic sensor calibration. Prior to the initial calibration, the
default value of -59.16 for pH sensors is stored here.
This appears only for pH and ISE sensors!
Min. [mV/pH] Min. defines the lower limit for the tolerance range within which
or the slope must be. For a pH sensor, the default value is -65.00.
Min. [mV/pX] The upper limit is correspondingly defined by Max.
This appears only for pH and ISE sensors!
Max. [mV/pH] Max. defines the upper limit for the tolerance range within which
or the slope must be. For a pH sensor, the default value is -50.00.
Max. [mV/pX] The lower limit is correspondingly defined by Min.
This appears only for pH and ISE sensors!
Check after [day] This value is used to calculate the time for the next calibration
of the sensor. A period of 0 to 100 days can be defined. If this
parameter has the value 0, no date is set for the calibration of
the sensor.
This appears only for pH and ISE sensors!
Expiry The "Check after" parameter sets the expiration date for the
sensor, which indicates the time when the sensor has to be
recalibrated. If only the value 0 is entered for the "Check after"
parameter, then no expiration date is calculated.
This appears only for pH and ISE sensors!
Date The date of the last sensor calibration. This date is reset to 00-
00-0000 each time the sensor is stored.
This appears only for pH and ISE sensors!
Time The time of the last sensor calibration. This time is reset to 00:00
each time the sensor is stored.
This appears only for pH and ISE sensors!
Test data Pressing the Test key opens the sensor test data.
This appears only for pH and ISE sensors!
• If you change the name of a sensor and save the changes, a new sensor with a new
name is created.
• The parameters that appear in the list depend on the type of sensor.
• For pH, mV, ISE sensors and the phototrode, the pH input must be chosen; for polar-
ized sensors, the pol. input.
• Prior to the first pH sensor calibration, the date and expiration date are 00-00-0000
and the time 00:00. The value for "Check after" is set to 0 days, and zero point and
slope are set to the default values.
• You can only delete a sensor that has not been used in a method.
E The calibration parameters of a pH electrode are the zero point pH0 (pH at a potential of
0 mV) and the slope.
The theoretical values of a pH electrode are stored in the titrator:
E0
+mv
• Zero point = 7.0 [pH]
pH0 and
0
7 14
pH
• Slope = -59.16 [mV/pH].
-mv
The pH calculation is performed according to the following equation:
mV signal
pH=pH0+
slope
The sensor should be calibrated in order to obtain correct values for your electrode. The
theoretical values are then automatically overwritten with the calculated calibration data
during the calibration.
E
If you only calibrate your electrode with one buffer solution, only the electrode zero point
is recalculated. (Not possible with the titrator.)
+mv
pH0
0 pH
6 7 8 9
MP
-mv
With a two- or multiple-point calibration, the zero point and slope are calculated using
MP
linear regression.
+mv
pH0 (MP)
0 pH
6 7 8 9
-mv
MP
Buff. type The type of buffer solutions to be used for the calibration. You
can select:
pH (to define yourself)
pX (to define yourself)
DIN/NIST
DIN
Fluka
Merck
MT-EU
MT-USA
Fisher
JIS
For the temperature dependencies of the buffers, see
"Appendix A: Predefined calibration standards".
Number of buffers With this parameter you can define the number and type of buffer
solutions to be used for the calibration.
Speed [%] The stirrer speed.
Temp. sensor Either the PT1000 temperature sensor can be selected or the
temperature can be entered manually under the parameter
"Temperature".
Temperature The temperature during the sensor calibration. With this value
the temperature-corrected slope of the pH electrode is used in
the calculation of the pH.
Appears only when the parameter "Temp. Sensor" is set to
"Manual".
dE [mV] During dt, the drift of the electrode potential must be less than
dt [s] dE/dt [mV/s] in order to be accepted as measured value.
This occurs in an interval defined by t(min) and t(max).
- Select "Buff. type" using the arrow keys. Then press Modify and select the buffer
type you are using.
- Select "Number of buffers " and press Modify.
- Add the desired number of buffer solutions to the buffer list using Add. You can
select these from a list and then press OK to include them in the buffer list. (You can
remove buffers again from the list by selecting them and pressing Delete.)
- When you have defined the desired number of buffer solutions, press OK to return to
the setup menu for the calibration.
- Select "Speed [%]" and enter the speed for the stirrer in percent.
- Select "Temp.sensor", press Modify and select the "PT1000" temperature sensor or
"Manual".
- If you have selected "Manual" for "Temp.Sensor", select "Temperature" and enter the
temperature in the corresponding units.
- Select "dE [mV]" and enter the millivolt number for the determination of the maxi-
mum drift dE/dt [mV/s] of the electrode potential.
- Select "dt [s]" and enter the time in seconds for the determination of the maximum
drift dE/dt [mV/s] of the electrode potential.
- Select "t(min) [s]" and "t(max) [s]" one after the other and define the time at which
the measured value at the earliest (tmin) and at the latest (tmax) is to be accepted.
- Select "Report" and select "none" or "printer" for the report printout using Modify.
- Start the sensor calibration by pressing Start.
- For the selected number of buffer solutions, a message appears each time reques-
ting you to prepare the corresponding buffer solution. You must confirm this by
pressing OK to start the measurement with the corresponding buffer solution.
- After all buffer solutions have been measured, a summary of the calibration results
appears on the display with the following information:
• Name of the sensor
• Calibration "OK" / "not OK"
• measured slope [mV/pH]
• measured zero point [pH]
If the measured slope is outside the limits defined for the sensor Min. [mV/pH] and
Max. [mV/pH], "Calibration not OK" appears and the calibration results are not ac-
cepted.
- If the measured slope lies within the limits defined for the sensor, the slope and zero
point for the sensor can be accepted by pressing Save. The date and time for the
calibration are automatically updated.
- If "Printer" was selected for the "Report" parameter, a report of the sensor calibration
is printed on the printer.
- Quit the display that follows by pressing Esc. in order to prevent the date and time
from being set to 00-00-0000 and 00:00.
• The sensor calibration can also be opened using the Sensor Help function key. (See:
"10.2.3 Calibrating a sensor")
• For storing into Setup, the slope is converted to 25 °C.
Buff. type The type of the buffer solutions to be used for the test. You
can select:
pH (to define yourself)
pX (to define yourself)
DIN/NIST
DIN
Fluka
Merck
MT-EU
MT-USA
Fisher
JIS
Number of buffers This parameter lets you define the number of buffer solutions
to be used for the sensor test.
Two buffer solutions must be selected.
Max. drift [mV/min] The maximum allowable drift in [mV/min]. Determines the
maximum value for the drift determined by the test in [mV/
min].
Temp. sensor You can select the PT1000 temperature sensor or enter the
temperature manually under the parameter "Temperature".
Temperature The temperature during the sensor tests. This value is used
to correct the slope of the pH electrode for temperature and is
taken into account in the calculation of pH.
It appears only if the parameter "Temp. sensor" is set to
"Manual".
dE [mV] During dt, the drift of the electrode potential must be less than
dt [s] dE/dt [mV/s] in order to be accepted as a measured value.
This occurs in a period defined by t(min) and t(max).
t(max) [s] The measured value is in any case accepted after t(max).
- Using the arrow keys, select "Buff. type". Then press Modify and select the buffer
type you are using.
- Select "Number of buffers " and press Modify.
- Add two buffer solutions to the buffer list using Add. You can select these from a list
and then press OK to include them in the buffer list. (You can remove the buffers
again from the list by selecting them and then pressing Delete.).
- Press OK to return to the setup menu for the sensor test.
- Select "Speed [%]" and enter the speed for the stirrer in percent.
- Select "Max. Drift [mV/min]" and enter a value in [mV/min] that the drift must not
exceed.
- Select "Temp. sensor", press Modify and select the "PT1000" temperature sensor or
"Manual".
- If you have selected "Manual" for "Temp. Sensor", select "Temperature" and enter the
temperature in the corresponding units.
- Select "dE [mV]" and enter the millivolt number for the determination of the maximum
drift dE/dt [mV/s] of the electrode potential.
- Select "dt [s]" and enter the time in seconds for the determination of the maximum
drift dE/dt [mV/s] of the electrode potential.
- Select "t(min) [s]" and "t(max) [s]" one after the other and define the time at which
the measured value at the earliest (tmin) and at the latest (tmax) is to be accepted.
- Start the sensor test by pressing Start.
- For the two selected buffer solutions a message appears each time requesting you to
prepare the corresponding buffer solution. You must confirm this by pressing OK to
start the measurement with the corresponding buffer solution.
- After the measurements have been performed for both buffer solutions, the drift is
determined for a period of 60 seconds.
If you have selected "Printer" under the menu item, the results of the sensor test are
recorded on the printer. There follows the summary of the results of the sensor test on
the display with the following information:
• Name of the sensor
• Drift "OK" / "not OK"
• Slope "OK" / "not OK"
• Drift [mV/min]
• Zero point [pH]
• Slope [mV/pH]
If the measured slope or the measured drift is outside the limits defined for the sen-
sor, then "Drift not OK" or "Slope not OK" appears.
- The sensor test was successful if "OK" appears for both for the drift and the slope.
• The sensor test can also be opened using the Sensor Help function key. (See
"10.2.4 Testing a sensor")
5.4 Peripherals
- Press Setup to open the Setup menu.
- Select "Peripherals" using the arrow keys and press OK to confirm. The setup menu
for the peripherals that can be connected to the titrator appears.
If you have connected an HP compatible printer, you can also define the paper format for
this printer.
- Select "HP compatible" and press Modify.
- In the menu that follows you can select the appropriate paper from the list of entries
by pressing Modify.
The following paper formats for HP compatible printers can be selected:
• 8 1/2 * 11"
• 8 1/2 * 12"
• A4
• If your titrator is not connected to a printer, select "Not defined" and confirm by pres-
sing OK.
• If your titrator is not connected to a balance, select "Not defined" and confirm with
OK.
• For the METTLER TOLEDO AE, AG, AT, AX and XS balances, use the setting "Bidirec-
tional" and the following balance settings: Baud rate: 2400, Data bits: 7, Parity:
even, Handshaking: no.
5.5 Standards
- Press Setup to open the Setup menu.
- Select "Standards" using the arrow keys and press OK to confirm. The setup menu
for the standards stored in the titrator appears, or "Template" if no standards are
stored in the titrator.
In this menu you can define and store primary standard substances using different pa-
rameters. These standards are needed by the titrator for the automatic titer determination
and can be changed and also deleted again.
Name Here you can enter the name under which the standard is to
be stored.
Entry type As entry type you can select mass or volume, depending wheth-
er you want to add the standard as a weighed quantity or a
measured volume during the automatic titer determination.
Minimum [g] / With "Minimum" and "Maximum" you can define a range for
[mL] the quantity of the standard to be added. Minimum defines the
lower limit of this range.
Depending on the selected entry type, Minimum is given in
[g] or in [mL].
Maximum [g] / Using "Minimum" and "Maximum" you can define a range for
[mL] the quantity of the standard to be added. Maximum defines the
upper limit of this range.
Depending on the selected entry type, Minimum is given in
[g] or in [mL].
• If you change the name of a standard and save your changes, a new standard is cre-
ated under the new name.
• You can only delete standards that are not referenced by a titrant.
In this menu you can determine and store all the blank values for the solvents you use.
These blank values are used for the calculation of the results of your analyses and can be
changed or deleted here.
• You can enter the blank value of the solvent manually or by means of the automatic
blank value determination. See "5.6.5 Blank value determination from the blank
values setup menu".
- Press Modify.
- The list of the parameters of the selected blank value appears. Individual parameters
can be selected and then changed.
- Press Save to accept your changes and to quit the menu, or press Esc to discard
your changes and quit the menu.
Solvent Here you can enter the name of the name of the solvent whose
blank value is to be stored.
Blank value The blank value of the solvent. This value can either be entered
[mmol] manually or determined by the titrator during the automatic
blank value determination. If the blank value is automatically
determined, the date and the time are automatically updated.
Minimum [mmol] "Minimum" and "Maximum" let you define a range in which the
blank value of the solvent must be. "Minimum" defines the lower
limit of this range.
Maximum [mmol] "Minimum" and "Maximum" let you define a range in which
the blank value of the solvent must be. "Maximum" defines the
upper limit of this range.
Blank This parameter indicates whether the blanc value was automa-
tically determined ("Determined") or manually entered ("Edi-
ted").
Check after [day] This value is used to calculate the expiration date for the blank
value. A period of 0 to 100 days can be defined. If the value of
this parameter is 0, no expiration date is calculated.
Expiry The expiration date for the blank value. If no other value than
0 is given for the parameter "Check after", then no expiration
date is calculated.
Date The date of the last blank value determination. Each time the
blank value is stored the date is set to 00-00-0000.
Time The time of the last blank value determination. Each time the
blank value is stored the time is set to 00:00.
• If you change the name of a blank value and store your changes, a new blank value
is created under the new name.
• You can only delete blank values that are not referenced by a method.
5.6.5 Blank value determination from the blank values setup menu
- Press Setup to open the Setup menu.
- Select "Blank values" using the arrow keys and press OK to confirm. The list of blank
values stored in the titrator appears, or the entry "Template" if no blank values are
stored in the titrator.
- Select the blank value whose value you want to determine.
- Press Modify.
- Press Blank.
- In the display that follows, the methods are shown that reference the blank through
the parameter "Solvent".
- Select one of the methods shown and press Start.
- The blank value determination is performed according to the preset conditions of the
method you use. (See "6.3 Modifying a method")
- If "Printer" was selected for the parameter "Report", a report of the blank value deter-
mination is printed on the printer.
- By pressing Stat. you can view the statistics of the current sample series.
- If the blank value determined is within the defined limits, the value (or the mean va-
lue of the results if you have performed the blank value determination several times)
can be accepted by pressing Save. The date and time for the blank value determina-
tion are then automatically updated.
- Quit the display that follows by pressing Esc. to prevent the date and time from being
set to 00-00-0000 and 00:00.
• You can also perform the automatic blank value determination from the Analysis
menu. See "8.3 Starting a blank value determination using the Run key"
Using the "Main methods" setup function, a total of three methods (METTLER or User
methods) can be assigned to the function keys F1, F2 and F3.
These methods can then be started directly from the Home screen by pressing the function
keys.
Methods can be assigned to the function keys in the setup menu for the main methods;
the assignment can be changed or deleted.
In the "User management" setup menu, titrator users can be added or changed on a user
list.
The active user can be defined here; the user’s access rights (Expert or Routine) can be
changed. (See "5.8.4 Defining access rights")
• As long as no user is entered in the user list, the entry "No user" appears instead of
the user name.
• By pressing Inactive you can deactivate the active user. "No user" appears again on
the display.
5.9 Settings
- Press Setup to open the Setup menu.
- Select "Settings" using the arrow keys and press OK to confirm. The Settings setup
menu appears.
In this menu you can change different titrator settings such as date, time and language.
• Language
• Date
• Time
• Temperature unit
• Titrator ID
• Report header
• Beep
• 31-11-2004
• 11/31/2004
• 31-Nov-2004
• Nov/31/2004
- Press OK to accept your changes and quit the menu, or press Esc to discard your
changes and quit the menu.
- Press OK to accept your changes and quit the menu, or press Esc to discard your
changes and quit the menu.
- Select the menu item "Stand" with the arrow keys and press Modify to change to
your desired setting "Internal", "Extern" or "Rondolino".
• "Internal": With this setting the titrator controls the internal titration stand.
• "Extern": The titrator can communicate with external devices (e.g. Kjeldahl distilla-
tion units of different manufacturers, pumps, etc.). See "13. Technical data".
6. Methods (Method)
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Pressing the Method key opens the method editor.
The titrator automatically performs analyses with the aid of predefined methods. In this
chapter you learn how to open methods and how to define your own methods.
A number of METTLER methods are already stored in the titrator. These methods have been
developed by METTLER TOLEDO for certain applications and can be used directly for the
corresponding analysis. See "6.7 Predefined methods".
You can modify METTLER methods according to your requirements and store them as
User methods.
A complete titration method consists of sample preparation, stirring or waiting times, the
actual titration itself, result calculation and a report. In the titrator, these steps are defined
as functions. They are performed one after the other in an analysis. The individual func-
tions consist of parameters whose values you can change.
Each method has a name and a three-digit number that uniquely characterizes each me-
thod. For User methods, the method identification number (method ID) can be between
1 and 899. The range 900 to 999 is reserved for METTLER methods.
You can create a new method by modifying the parameters of the functions of an existing
method and storing them under a new method ID.
The method editor can be opened by pressing the Method key. It allows you to create,
modify, delete, print and start methods.
If you do not know the method ID of the method that you want to execute, you can use the
arrow keys to select the method from a list using its name and method ID:
- If you press Modify, the functions of the selected method are shown on the display.
- Modify the individual functions according to your requirements. (See "6.3 Modifying
a method")
- Select "Title" and enter a title for the new method using the keypad.
- Select "Method ID" and enter a method ID (range 1-899) for the new method.
- Press OK.
- A summary of the new method with method ID, title, author, date of creation and
time appears on the display.
- Press OK to store the new method.
- In the display that follows, you can use the arrow keys to select the desired method
with its name and method ID from a list.
- If you press Modify, the functions of the selected method are shown on the display.
- Modify the individual functions according to your requirements. (See "6.3 Modifying
a method")
- Select "Title" and enter a title for the new method using the keypad.
- Select "Method ID" and enter a method ID (range 1-899) for the new method.
- Press OK.
- A summary of the new method with method ID, title, author, date of creation and time
appears on the display.
- Press OK to store the new method.
To modify the parameters of a method, you must first select the method:
- Press Method to open the method editor.
- The Methods menu appears with the following items:
• Method ID
• User methods
• METTLER methods
- Select the method whose parameters you want to modify.
- If you press Modify, the functions of the selected method are shown on the display.
- Modify the individual functions according to your requirements.
- Press OK to store the new method.
The parameters of the following functions are explained in the sections that follow:
• 6.3.1 Sample
• 6.3.2 Stirring
• 6.3.3 Measuring
• 6.3.4 EP titration
• 6.3.5 Calculation
• 6.3.6 Report
6.3.1 Sample
This function defines the request for sample information or the input of sample data such
as weight, density and equivalent number, and temperature.
Request ID [Yes/No]
This defines whether the ID of the sample is to be requested at the beginning of an analysis,
"YES", or as a parameter in the method, "No".
Select from the possible settings using Modify
ID
If "No" was selected, you can enter the sample ID here.
The ID can be entered using the keypad.
Weight [g]
The weight of the sample. Appears only if "No" was selected for "Request sample" and
"Mass" was selected as "Entry type".
The desired value can be entered using the keypad.
Volume [mL]
The volume of the sample. Appears only if "No" was selected for "Request sample" and
"Volume" was selected as "Entry type".
The desired value can be entered using the keypad.
Density [g/mL]
The density of the sample substance. Appears only if "No" was selected for "Request
sample" and "Mass" or "Volume" was selected as "Entry type".
The desired value can be entered using the keypad.
Weight [g/pc.]
The weight per piece of the sample substance. Appears only if "Number of pieces." as
"Entry type" was selected.
The desired value can be entered using the keypad.
Number [pcs.]
The number of sample units in a "piece". Appears only if "No" was selected for "Request
sample" and "Number of pieces" as "Entry type" was selected.
The desired value can be entered using the keypad.
Mol.m. [g/mol]
The molar mass of the sample substance in [g/mol]
The desired value can be entered using the keypad.
Equival. number z
The equivalent number of the sample substance.
The desired value can be entered using the keypad.
Request [Yes/No]
Indicates whether the temperature at the start of the analysis is to be requested or stored
in the method. Appears only if "Manual" was selected for "Temp. sensor".
Select from the possible settings using Modify.
Temp.
The temperature during the determination. Appears only if "Manual" was selected for "Temp.
sensor" and "No" was selected for "Request temperature".
The temperature unit is the unit that was selected in the Setup.
The desired value can be entered using the keypad.
6.3.2 Stir
The parameters of the Stir function let you determine the speed of the overhead or magnetic
stirrer during the analysis and whether the stirring time is to be requested before beginning
the titration or defined in the method.
Speed [%]
The speed (rpm) of the stirrer during the analysis in %. (0%, stirrer does not rotate, 100%,
stirrer rotates at the highest speed)
The desired value can be entered using the keypad.
Time [s]
The stirring time. Appears only if "No" was set for "Request time".
The stirring time indicates how long the stirrer has to stir to homogenize the solution before
the titration or the measurement is started.
The desired value can be entered using the keypad.
6.3.3 Measure
The Measure function enables you to measure the potential of a solution under defined
conditions.
The following parameters can be set:
Sensor
Using Modify, you obtain the list of sensors from which you can select the desired sensor.
Press OK to confirm. The unit (pH, or mV) is adapted for the other parameters according
to the sensor selected.
dE[mV]
The drift of the electrode potential must be less than dE/dt during dt in order to be accepted
as a measured value. This occurs during an interval defined by t(min) and t(max).
The desired value can be entered using the keypad.
dt[s]
The drift of the electrode potential must be less than dE/dt during dt, in order to be accepted
as a measured value. This occurs during an interval defined by t(min) and t(max).
The desired value can be entered using the keypad.
t(min) [s]
t(min) defines the earliest possible time that the measured value is accepted.
The desired value can be entered using the keypad.
t(max) [s]
t(max) defines the latest possible time after which the measured value is in any case
accepted.
The desired value can be entered using the keypad.
6.3.4 EP titration
Titr.
Using Modify, you obtain the list of titrants from which you can select the desired titrant.
Press OK to confirm. The concentration of the titrant from the Setup is used.
Conc. [mol/L]
The concentration of the titrant. You cannot change this parameter; the concentration of
the titrant is used as defined in the Setup.
Sensor
Using Modify, you can access the list of sensors from which you can select the desired
sensor. Press OK to confirm. The unit (pH, or mV) is adapted for the other parameters
according to the sensor selected.
• pX sensors are used like mV sensors in the method. The calibration parameters in
the Setup are used to perform calculations for measured values in [ppm] or [mol/L]
in the method.
Value [mmol]
This parameter allows you to enter a blank value in the method. The desired value can be
entered using the keypad.
Appears only if "Entry" was selected for the parameter "Blank value".
Solvent
Using Modify, you obtain the list of blank values stored in the titrator. From there you can
select a blank value and confirm by pressing OK.
Appears only if "From list" was selected for the parameter "Blank value".
Vol.[mL]
With this parameter you can enter a volume for predispensing in [mL]. The desired value
can be entered using the keypad.
Appears only if "No" was selected for the parameter "Request predisp.".
Determin. [Normal/Cautious/Fast/User]
Using the Determination parameter you can select a criterion for performing the titration.
The possibilities are "Normal", "Cautious", "Fast" and "User".
For the "Normal", "Fast" and "Cautious" settings, corresponding sets of parameters are
stored in the titrator. You can view these parameters by printing the method. No other
parameters need to be adapted. The "User" setting gives you the possibility to individually
adapt all the parameters with regard to the addition of titrant and the measure mode.
The following parameters "Addition" and "Measure" with the corresponding subparameters
are only available if you have selected "User" for the parameter "Determination".
Addition [Incremental/Dynamic]
By using this parameter you can set whether the addition of the titrant is to be performed
incrementally or dynamically. If you select "Incremental", the same volume increment is
always added throughout the entire titration; if you select "Dynamic", the volume increment
added during the titration is adapted dynamically within the preset limits to the course of
the titration in order to obtain a constant potential difference per increment.
Using Modify, you obtain the next screen on which you can select "Incremental" or "Dyna-
mic" and define the subparameters using Modify. (For faster titrations, you should select
"Incremental".)
dV [mL]
Defines the size of the volume increment that is added in each dispensing step. This
volume increment remains constant throughout the entire titration. The value in [mL] can
be entered using the keypad.
dEnom [mV]
Here you can enter the desired potential difference in [mV] per titration step.
dVmin [mL]
This value defines the minimum size of the volume increment. The value in [mL] can be
entered using the keypad.
dVmax [mL]
This value defines the maximum size of the volume increment. The value in [mL] can be
entered using the keypad.
• The range defined by dVmin and dVmax should be chosen as large as possible and
the titrant addition controlled by dEnom.
Using Modify, you obtain the next screen where you can select "EQU controlled" or " Fix
time" and define the subparameters using Modify.
The wait time to the next incremental addition also depends on the definition
As soon as the change in potential of the solution is less than the defined equilibrium
(dE/dt), the titrator accepts the measured value and adds the next increment.
This can occur at the earliest at tmin and occurs at the latest at tmax. At tmax the measured
value is in any case accepted even if the equilibrium condition is not met.
This measure mode has the result that the incremental addition is fast in the flat part of the
titration curve, and slow in the steep part.
The following parameters are available:
dE [mV]
Defines the maximum change in potential per time interval dt in [mV]. The desired value
can be entered using the keypad.
dt [s]
Gives the time interval for the calculation of the calculation dE[mV]/dt[s]. The desired value
can be entered using the keypad.
t(min) [s]
Defines the wait time in [s] after which measured value acquisition occurs at the earliest.
The desired value can be entered using the keypad.
t(max) [s]
Defines the wait time in [s] after which the measured value is in any case accepted. The
desired value can be entered using the keypad.
dt [s]
Defines the wait time dt in [s] after each incremental addition. The desired value can be
entered using the keypad.
6.3.4.2 Recognition
The Recognition function lets you set the tendency for endpoint recognition. You can access
the parameters of this function using Modify.
Tendency [Positive/Negative]
Select "Positive" if you want the endpoint to be detected only for a positive tendency; select
"Negative" if you want the endpoint to be detected only for a negative tendency. You can
select from the possible settings using Modify.
• If the start potential already exceeds EP, the titration is terminated without the addi-
tion of titrant.
• For a relative EP the tendency describes the position of the EP related to the measu-
red start potential.
Vmax [mL]
The maximum volume of titrant dispensed during the determination. This parameter is a
safety measure to prevent unnecessary addition of titrant if a malfunction occurs during
the titration. The desired value can be entered using the keypad.
At tmax [Yes/No]
This parameter lets you define whether the titration is to be terminated after a certain time,
"Yes", or not "No".
t(max) [s]
This parameter lets you define the time interval after which the titration is terminated. The
desired value can be entered using the keypad.
This parameter appears only if "Yes" was selected for the parameter "At tmax".
6.3.4.4 Evaluation
The Evaluation function lets you define which endpoint of the titration is to be evaluated.
You can access the parameters of this function using Modify.
Potential 1 [pH/mV]
The value for Potential 1. The unit depends on the sensor used, pH or mV. The desired value
can be entered using the keypad.
Appears only if "1" or "2" was selected for the parameter "Numb. EPs".
Potential 2 [pH/mV]
The value for Potential 2. The unit depends on the sensor used, pH or mV. The desired value
can be entered using the keypad.
Appears only if "2" was selected for the parameter "Numb. EPs".
6.3.5 Calculation
You can define three different calculations per analysis (Calculation 1-3). The following
parameters are available for this:
• It is not sufficient, under the function EP-Titration to request or enter a blank value
or back value for it to be included in the calculation. In addition, you must set the
parameter "Type" in the calculation function accordingly.
Formula
For user-defined calculations, you can select a formula to calculate the results. (See
"6.3.5.1 Table of formulas for the calculation of results".)
Select from the possible settings using Modify.
This parameter only appears if you have selected "User def." for the parameter "Calcula-
tion".
C
For user-defined calculations, you can enter a constant to convert the results to the desired
unit.
The desired value can be entered using the keypad.
This parameter only appears if you have selected "User def." for the parameter "Calcula-
tion".
• The constant C is only included in the calculation if C is also present in the calcula-
tion formula.
Factor
For user-defined calculations, you can enter a factor to recalculate the results.
The desired value can be entered using the keypad.
This parameter only appears if you have selected "User def." for the parameter "Calcula-
tion".
Name
For user-defined calculations, you can enter a name that appears later in the report.
The desired name can be entered using the keypad.
This parameter only appears if you have selected "User def." for the parameter "Calcula-
tion".
Unit
You can select the desired unit for the result. The possibilities depend on the parameter
Calculation.
Select from the possible settings using Modify.
Calculation: Content [g/L] [mg/L] [mol/L] [eq/L] [meq/L] [mg/g] [%] [ppm]
[mol/kg] [mmol/kg] [mmol/g] [mmol/L]
Calculation: Consumption [mL] [mmol]
Calculation: Measured value [ppm] [mmol/L] [g/L] [mol/L] [mV] [pH] [pX]
Calculation: User-def. Can be freely chosen, depends on the formula for the
calculation of the results.
For user-defined calculations, the unit can be entered using the keypad.
Which EP
The parameter indicates for which number EP the result is calculated. Does not appear for
determinations of the type "Measurement".
The following possibilities are available for EP:
1, 2, Start value
Select from the possible settings using Modify.
Decimal places
You can enter the number of decimal places for the result of the calculation.
The desired value can be entered using the keypad.
Minimum
Enter the lower limit for the calculated result.
Appears only if you have selected "Yes" for the "Result limits".
The desired value can be entered using the keypad.
Maximum
Enter the upper limit for the calculated result.
Appears only if you have selected "Yes" for the "Result limits".
The desired value can be entered using the keypad.
• If the result of a titration is outside the defined result limits, the result is marked with
an exclamation point and a message appears on the display.
Statistics [Yes/No]
This parameter lets you define whether the statistics of the analysis is included in the
report, "Yes", or not, "No".
Select from the possible settings using Modify.
The following table summarizes the formulas on which the individual calculations are
based.
Calculation: Titer Calculation: Calculation: Calculation: measured Calculation: content Calculation: user. def.
blank value consumption value default formula:
R = Q*C/m
R = m/(VEQ*c*C) R=Q mL: R = VEQ mV: R = E %: C = M/(10*z) R = Q*C/m (default formula)
Liquid standards: mmol: R = Q pH: zero point[pH] + mg/g: C = M/z R = (Q-Bl)*C/m (default for-
C = 1/(cst*z) Q = VEQ*c*t E[mV]/slope[mV/pH] mula including the blank value)
Solid standards: pX: zero point[pX] + g/L: C = M/z R = (Ba-Q)*C/m (default for-
C = M/(1000*z) E[mV]/slope[mV] mula including the back value)
ppm: R = pw(-pX)*1000 ppm: C = M*1000/z mL: R = VEQ
mmol/L: mg/L: C = M*1000/z mmol: R = Q
R = pW(-pX)*1000 Q = VEQ*c*t
g/L: R = pW(-pX) mol/L: C = 1/z mV: R = E
mol/L: R = pw(-pX) mol/kg:C = 1/z R = pw(-pX)*1000
(mmol/L, ppm or other unit of
measure, depending on the
position of the zero point)
mmol/g:C = 1/z R = pw(-pX)
(mol/L, g/L or other unit of
measure, depending on the
position of the zero point)
mmol/L: C = 1000/z
mmol/kg: C = 1000/z
eq/L: C = 1
meq/L: C = 1000
R = (Q-Bl)*C/m (con-
tent with blank value)
R = (Ba-Q)*C/m (con-
tent back titration)
The following table summarizes the symbols used and their meaning:
6.3.6 Report
This function lets you determine whether a report is to be printed or not and defines the
size of the report.
You can define the following parameters:
Output [Printer/None]
Determines whether a report is to be printed "Printer", or not "None".
Select the setting you want using Modify.
Results [GLP/None/Short]
Determines the size of the presentation of the results in the report.
"GLP" Good Laboratory Practice - comprehensive.
"None" No presentation of the results.
"Short" Brief presentation of the results.
Select the setting you want using Modify.
E - V curve [Yes/No]
Determines whether a titration curve (potential plotted against volume) is to be included
in the report, [Yes], or not, [No]. Appears only for measurements
Select the setting you want using Modify.
7. Series
Pressing the Series key opens the Series menu. From this menu you can perform any type
of series determination (sample, titer or blanc value).
An Important prerequisite for performing an analysis with the titrator is that you have
properly set up all the necessary resources in the setup menu (See "5 Setup") and that the
methods you need are available. You can create or modify the methods using the method
editor (See "6 Methods").
Furthermore you have the possibility to automatize your series determination by using
a Rondolino sample changer. Up to nine samples can be analyzed automatically. It is
required to choose „Rondolino“ as titration stand if you use a Rondolino sample changer.
(See „5.10 Titration stand“)
• You can enter the method ID of an existing method (User method or METTLER me-
thod) in the "Method ID" box and then confirm this by pressing Start.
8. Analysis (Run)
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Pressing the Run key opens the Analysis menu. From this menu, you can perform any
type of determination (sample, titer or blank value determination).
An Important prerequisite for performing an analysis with the titrator is that you have
properly set up all the necessary resources in the setup menu (See "5 Setup") and that the
methods you need are available. You can create or modify the methods using the method
editor (See "6 Methods").
• You can enter the method ID of an existing method (User method or METTLER me-
thod) in the "Method ID" box and then confirm this by pressing Start.
• You can facilitate starting the three most frequently used methods by defining them
as main methods in the Setup menu. The method ID of these main methods then
appear on the Home screen and can be started from there by pressing the corre-
sponding function key. (See "5.7 Main methods".)
- You can view the statistics of the current sample series by pressing Stat..
- If the blank value is within the defined limits, you can accept the result of the blank
value determination (or the mean result if you have performed the blank value deter-
mination several times) by pressing Save. The date and time of the last blank value
determination are automatically updated.
- Quit the display that follows by pressing Esc. in order to prevent the date and time
being set to 00-00-0000 and 00:00.
9. Performing a titration
This chapter explains the general procedure for performing a titration method, using a
simple acid-base titration as an example. The method for determining the acid content
is stored as a METTLER method under the method ID 900 entitled "Acid Content EP". The
purpose of the method is to determine the acid content of an aqueous solution using an
endpoint titration.
The following determination is performed:
9.1 Preparations
– Make up solutions of hydrochloric acid and sodium hydroxide in the concentrations
given above. The sodium hydroxide must be free of carbonate.
– Prepare the burette for the sodium hydroxide and attach it to the titrator (see "3.2.2
Installing the burette").
– To protect the sodium hydroxide from CO2, mount a drying tube on the burette holder
of the NaOH bottle.
– Attach a titration beaker to the titration stand and insert the NaOH dispensing tube
into one of the smaller openings of the titration head.
– Connect the stirrer to the appropriate connection, and check that the stirrer is cor-
rectly configured under the settings for the titration stand. (See "5.10 Titration stand")
If you use an overhead stirrer, attach it to the titration stand.
If you use a magnetic stirrer, make sure that the titration arm is swiveled in and that
the titration beaker is positioned above the magnetic stirrer.
– Fill the burette (see next page).
• A printer and/or a balance can be optionally connected to the titrator. (See "5.4
Peripherals")
�������
- Press the Burette key.
- The menu of the Burette auxiliary function menu appears.
- Select "Rinse" using the arrow keys and press Start to start the rinsing process.
- The main menu of the Burette auxiliary function appears on the display again:
- Repeat the rinsing process twice to make sure that the burette is completely filled and
the tubing has been well rinsed.
– Press the Reset key. The start screen appears.
• Make sure that the dispensing tube of the burette is attached to the titration stand and
is inserted in the titration beaker.
- Press Start.
- Now enter the weight of the sample (for this example, approx. 5g) using the keypad.
- If a balance is connected to the titrator and is configured in the Setup menu, you can
also transfer the sample weight directly from the balance.
- Press Balance in the Request sample display.
���
- Press OK or the Run key to start the titration.
- An appropriate message appears on the display while the burette is being filled.
- After the burette has been filled, the sample is stirred for the duration of the mixing
time to make sure the solution is homogeneous.
The duration of the mixing time can be defined in the method. (See "6 Methods
(Method)")
- During the titration, you can display the titration curve (measured potential plotted
against dispensed volume) using Graph. A line shows the zero point of the y-axis (0
mV/ pH 7).
- You can return to the measured values display by pressing Values.
- You can terminate the titration by pressing Abort. Values already measured are ho-
wever not lost.
- At the end of the titration, the result is shown on the display and at the same time the
analysis report is sent to the printer.
- If you confirm the result by pressing OK, the start screen of the Analysis menu ap-
pears.
- As long as the printout of the report on the printer is still in progress, the message
"Reporting" appears on the display; the titrator does not return to the start screen of
the Analysis menu until the printout is finished.
- If you perform the determination several times, you can display the statistical evalua-
tion of your results by pressing Stat..
- You can view the result of your titration using the Results auxiliary function. (See
"10.6 Results")
- If you have not set up a printer in Setup, an error message is given at the end of the
analysis, which you must confirm by pressing Abort.
- The result is then shown on the display.
- If you have connected a printer, the following report is printed:
================================================================= EP titration
METTLER TOLEDO DLXX 26-01-2005 15:21
----------------------------------------------------------------- -----------------------------------------------------------------
SNR ----- V1.00 ID Method ID 920 Sample No. 1
26-01-2005 15:21 User Meyer 25-01-2005 12:05 Sample ID HCl
================================================================= -----------------------------------------------------------------
EP titration
-----------------------------------------------------------------
Method ID 920 Title Acid content EP
25-01-2005 12:05 Author Meyer
Titer 1.03523
-----------------------------------------------------------------
Titrant NaOH 0.1 Sensor DG115
Conz. [mol/L] 0.1 Unit pH
-----------------------------------------------------------------
Sample 1
Sample ID HCl
Entry type Mass
Mass [g] 5.2354
Minimum [g] 1.2
Maximum [g] 6.5
Density [g/mL] 1.0
Mol.m. [g/mol] 36.46
Equival. number z 1
Predis. [mL] 1.000
Mixing time [s] 3
Init.pot. [mV] 275.3
Consumption [mL] 5.224
Duration [min:s] 2:00
Temp. [°C] 25.0
Abort All points reached
Blank [mmol] 0.00
Back value [mmol] 0.00
Statistics report
Result n x s Unit srel
-----------------------------------------------------------------
1 1 0.363 0.000 [%] 0.00 [%]
• The auxiliary function keys are locked during an analysis that is running and the
corresponding menus cannot be opened.
System information
This function lets you view the system information for the titrator.
System test
This function lets you test the titrator hardware and any connected peripheral instruments,
such as a balance or a printer.
(See "11.2 Hardware tests")
Service
(This menu can only be accessed by service specialists.)
10.2 Sensor
������ If you press the Sensor key, the list of sensors stored in the titrator appears.
• You can also start the measurement directly by pressing Start after selecting the
temperature sensor. The setting last used is used for the stirrer speed.
• You can change the temperature unit in the "Settings" setup menu. (See "5.9.4 Defin-
ing the temperature unit")
• You can also start the measurement by pressing Start directly after selecting the
sensor without changing the settings beforehand with Modify. The settings last used
are then adopted.
The calibration is performed in the same way as described in the setup section for sensor
calibration from the setup menu. (See "5.3.5 Sensor calibration from the sensor setup
menu")
10.3 Stirrer
������� If you press the Stirrer key, the Stirrer menu appears.
This menu lets you switch a stirrer on and off (an overhead or a magnetic stirrer) and
change its speed:
• The Stirrer auxiliary function always refers to the stirrer that was selected in the "Titra-
tion stand" setup menu. To change from an overhead stirrer to a magnetic stirrer, you
must make the corresponding settings in the setup menu. (See "5.10 Titration stand")
10.4 Burette
������� If you press the Burette key, the Burette auxiliary functions menu appears.
• A lower fill rate is recommended for reagents of high viscosity in order to prevent air
being sucked in.
• Make sure in rinsing processes that the waste container under the dispensing tube is
sufficiently large.
• You can also start the rinsing process at the rinsing rate shown by selecting "Rinse"
and pressing Start.
• Make sure during the rinsing processes that the waste container under the dispens-
ing tube is sufficiently large.
10.4.3 Dispensing
- Press Burette to open the Burette auxiliary functions.
- Select "Dispense" using the arrow keys.
- Press Modify to change the settings for the dispensing process.
- Under "Volume", enter the volume in [mL] that you want to dispense.
- Select "Burette", and using Modify, select the volume of the burette you are using
(1 mL, 5 mL, 10 mL or 20 mL).
- Select "Fill rate [%]" to change the speed at which the burette is filled. Enter a value
for the fill rate.
- Press Start to start the rinsing process.
• A lower fill rate is recommended for reagents of high viscosity in order to prevent air
being sucked in.
• You can also start the dispensing process by selecting "Dispense" and pressing
Start. The settings last used are adopted for the fill rate and the burette volume.
• The volume of the manual dispensed increments depends both on the volume of the
burette used and the numeric key. Press "1" to dispens the lowest volume depending
on the burette used up to "0" to dispens the highest volume.
The following table displays the volume of increments in mL for different burette sizes.
10.5 Report
If you press the Report key, Report auxiliary functions menu appears. This enables you to
print additional reports of the determination or measurement you performed last.
• If no analyses or measurement results are stored in the titrator, only the message
"No results" appears on opening the Report menu and you cannot perform any set-
tings in this menu.
• "Meas. val. table", "E-V curve" and "dE/dV curve" are not available for reports of
measurements.
10.6 Results
������� Pressing Results leads you into the menu of the Results auxiliary function. This function
enables you to
• If no analyses or measurement results are stored in the titrator, only the message
"No results" appears on opening the Results menu and you cannot perform any set-
tings in this menu.
• If no analyses or measurement results are stored in the titrator, the message "No
results" appears on opening the Results menu, and you can not perform any settings
in this menu.
• To select an individual result from a list of all the stored results, select "Number of
samples" and press List. You can then select any result using its sample number,
and view it by pressing Show.
• To print the method with which the sample series was performed, select "Method"
and press Print.
• While the results are shown on the display, you can view the following or the pre-
vious results using Next and Back.
10.6.2 Statistics
In the Statistics menu you can view and print a statistical evaluation of the results of your
current sample series. A sample series is always a series of analyses with the same (un-
changed) method. It does not matter whether the analyses consist of a series of blank
value determinations, titer determinations, or sample determinations.
You can exclude individual samples from the statistical evaluation by deleting them from
the statistics memory. You can still view deleted samples in a list of the deleted results and
return them to the statistics if desired.
• To select an individual result using its sample number, select "Results samp. no."
and enter the sample number using the keypad. You can view the result by pressing
Show and then if necessary remove it from the statistics using Del..
• To select an individual result using its sample number, select "Results samp. no."
and enter the sample number using the keyboard. You can view the result by pres-
sing Show and then if necessary add it to the statistics with Add.
• If no analyses or measurement results are stored in the titrator, the message „No
results" appears on opening the Results menu and you can not perform any settings
in this menu.
You can now select and open the following functions by using the arrow keys and pressing
OK.
Screen test
The screen alternately shows a full and then an empty display. This enables you to iden-
tify faulty pixels on the display. The test mode automatically switches off after about 10
seconds.
Keypad test
As soon as you press a key, a number code assigned to this key appears so that you can
identify a faulty key (see following table).
Key codes
KeyCode Key Code Key Code
Reset 101 Run 114 3 51
i 105 F1 650 4 52
Stirrer 116 F2 651 5 53
Report 112 F3 652 6 54
Sensor 110 ∇ 607 7 55
Burette 98 Δ 606 8 56
Results 117 Shift 0 9 57
Setup 115 0 48 Del 8
Method 109 1 49 . 46
Series 97 2 50
Beeper test
You can check the internal beeper: press Start to switch it on, and Stop to switch it off.
Interface test
To test the RS-232C interfaces, you must plug the test connector 51107288 into the bal-
ance or RS-P42-interface.
To test the Centronics interface, you must plug the Centronics cable into the Centronics
interface and plug the test plug 51107287 into the Centronics socket of the cable.
- Then select the interface you want to test using the arrow keys and press Start.
- After the test, the message "Test successful" or "Test failed" appears on the display.
- Press OK to return to the menu.
- After the test, the message "Test successful" or "Test failed" appears on the display.
- If the test was successful, the letters and characters available in the titrator are
printed.
Balance test
To perform the balance test, a weight must first be placed on the balance. When you press
Start, the weight shown on the balance must appear on the titrator display.
TTL-I/O
- Before starting the test, plug the test plug 51107723 into the TTL-I/O interface.
After the test, the message "Test successful" or "Test failed" appears on the display.
Overhead stirrer
This test allows you to check whether the overhead stirrer operates properly at different
speeds.
- Select "Overhead stirrer" using the arrow keys and then press OK to confirm.
- On the display that follows, you can enter a speed and switch on the overhead stirrer
by pressing Start.
- Press Stop to switch off the stirrer again.
Magnetic stirrer
This test allows you to check whether the magnetic stirrer operates properly at different
speeds.
- Select "Magnetic stirrer" using the arrow keys and then press OK to confirm.
- On the display that follows, you can enter a speed and switch on the magnetic stirrer
by pressing Start.
- Press Stop to switch off the stirrer again.
���
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Sensors
DM140-SC
Combined platinum ring electrode
for redox titrations
DM141-SC
Combined silver ring electrode for
argentometric titrations
DM143-SC
Double-pin platinum electrode
12.2.2 Disposal
In conformance with the European Directive 2002/96/ EC on Waste Electrical and Electro-
nic Equipment (WEEE) this device may not be disposed of in domestic waste. This also
applies to countries outside the EU, per their specific requirements.
Please dispose of this product in accordance with local regulations at the collecting point
specified for electrical and electronic equipment.
If you have any questions, please contact the responsible authority or the distributor from
which you purchased this device.
Should this device be passed on to other parties (for private or professional use), the
content of this regulation must also be related.
Thank you for your contribution to environmental protection.
5
9 RxD (In) 2
4 Data to titrator
8 TxD (Out) 3 Data from titrator
3 �470��
7 DTR +12 V 4 Handshake from titrator ready for operation
2
6 GND 5 Signal ground, galvanically coupled to titrator electronics
1
Centronics socket
1. Basics
The TTL interface of the titrator is used to communicate with external devices via several signals. Not only the Rondolino
sample changer can be controlled by using the interface but also several third party devices ( e.g. Kjeldahl distillation units,
pumps, etc.)
2. Hardware
The interface consists of 4 output lines (Out1, Out2, Out3, Out4) and 2 inputs (In1, In2). They are provided on a 9 pin D-Sub
connector using the following scheme:
3. Functionality
3.1.1 Out2
This signal is activated on initializing a titration. Its rests active until return to the home state. On handling a sample series
using Rondolino a follwing sample must be initialized within 1 second, otherwise Rondolino returns to ist home position
(beaker 0).
The signal Out2 is always set, irrespective of the selected titration stand setting.
3.1.2 Out4
An active pulse of about 200ms on Out4 after initialization of a titration indicates a request of a ready signal on In1. On
handling a series using a Rondolino this pulse raises about 600ms after activation of Out2, otherwise it raises after input of
the sample data is done by the user.
The signal Out4 will only be activated if selection of titration stand setting ist Rondolino or External.
3.1.3 In1
After the pulse on Out4 has raised, the titrator expects the activation of signal In1. This will be done by Rondolino or an external
titration stand, declaring the sample is now ready to be analyzed. Using Rondolino this means the beaker is reached an dipped
in. In1 rests active till a following activation on Out1.
The signal In1 will only be expected if selection of titration stand setting ist Rondolino or External.
3.1.4 Out1
The start of the titation in the inner sense is indicated by a pulse of 200ms on Out1. At this time the stirrer will be started an
the mixing time starts counting down.
The signal Out2 is always set, regardless of the selected titration stand setting.
3.1.5 Illustrations
The following illustration shows the above described sequence of signals handling a Rondolino series of 3 samples.
The following illustration shows some details of the one above. On the left side it can be seen, that 600ms after activa-tion of
Out2 a pulse of 200ms raises on Out4, by which Rondolino starts moving to the next position. The arrival of this position is
indicated after about 8s by activating In1. By this the titrator is stimulated to start titration and to raise a pulse on Out 1. Seeing
this pulse on Out1 Rondolino deactivates In1.
The following sample shows a sequence of signals using an external titration stand. After activation of Out2 the pulse on Out4
does not raise until the user has put the sample data in..
This illustration shows the sequence of signals using an internal titration stand. The pulses on Out4 und In1 do not raise. After
the user has put he sample data in, the start of the titration is just indicated by a the pulse on Out1.
including software and accessories were developed, tested and successfully validated according to the international
ISO9001:1994 based Life cycle rules of Mettler-Toledo AG, Analytical.
Life cycle checkpoint details were reviewed and approved by the Project Supervisory Group (PSG). The products/sys-
tems were tested to meet functional and performance specifications and release criteria at release to shipment. In
order to support GLP and validation requirements, we will make the following documents available to an authorized,
governmental or regulatory agency for inspection.
• Performance Specifications
• Software Specifications
• Quality Plan
• Project Management System
• Test Plan
• Customer Requirements
• Review Reports
• Source Code
Mettler-Toledo AG, Analytical will maintain possession of all documents and their reproductions and may require a
non-disclosure agreement to be provided by those requiring access to these documents.
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EC - DECLARATION OF CONFORMITY
EG-Konformitätserklärung
KD-Nr.: 51107749 A Doku-Nr.: 20010111
The undersigned, representing the following manufacturer
Die Unterzeichnenden vertreten das folgende Unternehmen
certified model: --
Modell für Eichprüfung
is in conformity with the provisions of the following EC directives (incl. all applicable amendments)
mit den folgenden EG-Richtlinien (Inkl. Änderungen) übereinstimmt
Last two digits of the year in which the CE marking was affixed: 01
Die letzten zwei Zahlen des Jahres der Erst-CE-kennzeichnung des Produkts mit dem CE Zeichen.
CH-8603 Schwerzenbach
09.03.2005
Bernhard Grob Rolf Truttmann
General Manager Manager Business Area AnaChem
EMC standards:
EN61326:1997+A1:98+A2:01 (class B)
EN61326:1997+A1:98+A2:01 (Industrial environments)
Metrological standards:
--
IP standards:
--
Standards for Canada, USA and Australia
CAN/CSA-C22.2 No.1010.1-92
UL Std. No. 3101-1
FCC, Part 15, class A
AS/NZS4251.1, AS/NZS4252.1
release: 9.12.2004 / ATL Seite 1 von 2 printed: Mrz. 2005
EC - DECLARATION OF CONFORMITY
EG-Konformitätserklärung
KD-Nr.: 51107749 A Doku-Nr.: 20010111
Type code
Typenschlüssel
DL 38 Software
Remarks
Bemerkungen:
Name of METTLER METTLER DIN MERCK FLUKA (Ref. FISHER DIN JIS Z 8802
the list TOLEDO TOLEDO (19266) (Ref. 20°C) 20°C) (Ref. 25°C) (19267) (Ref. 25°C)
(Ref. 25°C) USA (Ref. /NIST (Ref. (Ref. 25°C)
25°C) 25°C)
2.00 1.68 1.680 1.00 1.00 1.00 1.09 1.679
Contained 4.01 4.01 3.557 2.00 2.00 2.00 3.06 4.008
calibration 4.60 7.00 3.775 3.00 3.00 3.00 4.65 6.865
standards 7.00 10.01 4.008 4.00 4.00 4.00 6.79 7.413
9.21 6.865 4.66 5.00 5.00 9.23 9.180
10.00 7.416 5.00 6.00 6.00 12.75 10.01
11.00 9.184 6.00 7.00 7.00
10.014 6.88 8.00 8.00
12.454 7.00 9.00 8.991
8.00 10.00 10.00
9.00 11.00 11.00
9.22 12.00
10.00 13.00
11.00
12.00
13.00
Temperatur
2.00 4.01 4.60 7.00 9.21 10.00 11.00
°C
0 2.03 4.01 4.66 7.12 9.52 10.65 11.90
5 2.02 4.01 4.65 7.09 9.45 10.52 11.72
10 2.01 4.00 4.64 7.06 9.38 10.39 11.54
15 2.00 4.00 4.63 7.04 9.32 10.26 11.36
20 2.00 4.00 4.62 7.02 9.26 10.13 11.18
25 2.00 4.01 4.60 7.00 9.21 10.00 11.00
30 1.99 4.01 4.61 6.99 9.16 9.87 10.82
35 1.99 4.02 4.62 6.98 9.11 9.74 10.64
40 1.98 4.03 4.63 6.97 9.06 9.61 10.46
45 1.98 4.04 4.64 6.97 9.03 9.48 10.28
50 1.98 4.06 4.66 6.97 8.99 9.35 10.10
55 1.98 4.08 4.67 6.98 8.96 9.22 9.92
60 1.98 4.10 4.69 6.98 8.93 9.09 9.74
70 1.99 4.16 4.71 7.00 8.88 8.96 9.56
80 2.00 4.22 4.73 7.04 8.83 8.83 9.38
90 2.00 4.30 4.75 7.09 8.79 8.70 9.20
95 2.00 4.35 4.77 7.12 8.77 8.57 9.02
Index
A
Accessories, optional 105 Design of the titrator 13
Analysis 79 Display 15
Starting a blank value determ. using the Run key 80 Disposal 107
Starting a blank value determ. using the Series key 77
Starting a sample determ. using the Run key 79 E
Starting a sample determ. using the Series key 75
EP titration 61
Starting a titer determ. using the Run key 80
Control param. 62
Starting a titer determ. using the Series key 76
Evaluation 66
Arrow keys 15
Recognition 65
Assignment of a function key 44
Termination param. 65
Attaching and removing the titration beaker 12
Error messages 99
Attaching the titration stand to the titrator 9
Escape key 17
Auxiliary functions 89
Expert 47
Auxiliary I/O 102
F
B
Function keys 15
Balance, setting 36
Assignment of a function key 44
Beeper sound, setting 50
Changing the assignment of a function key 44
Blank values 40
Deleting the assignment of a function key 45
Adding a blank value 40
Blank value determ. from the blank values setup menu 43 G
Deleting a blank value 42
Modifying a blank value 40 Global errors and malfunctions 99
Printing blank values 42
Blank value determination using the Run key 80 H
Blank value determination using the Series key 77 Hardware tests 99,100
Burette 92 Auxiliary I/O 102
Dispensing 93 Magnetic stirrer 102
Rinsing the burette 92 Overhead stirrer 102
Rinsing the tip 93 TTL-I/O 102
Burette intallation 10 Communication interfaces 101
Balance test 102
C Interface test 101
Calculation 67 Printer test 101
Calibration standards, predifined 120 pH input value 103
Centronics socket 111 User interface 100
Changing the assignment of a function key 44 Beeper test 101
Cleaning 107 Keypad test 100
Communication interfaces 101 Key codes 100
Connections at the rear of the titrator 13 Screen test 100
Connection possibilities for peripheral instruments 110 Help function keys 17
Home screen 18
D
I
Date, setting 48
Defining access rights 47 Information menu 89
Expert 47 Service 89
Routine 47 System information 89
Deleting the assignment of a function key 45 System test 89
Input keys 15 O
Entering character strings into text boxes 15
Entering numbers into number boxes 16 Operating concept 14
Installation 9 Optional accessories 105
Attaching and removing the titration beaker 12
Attaching the titration stand to the titrator 9
P
Installing the burette 10 Performing a titration 83
Installing the magnetic stirrer 10 Performing titration method 920 84
Swiveling the titration stand 11 Preparations 83
Introduction 5 Filling the burette (rinsing) 84
Peripherals 35
L Setting up a balance 36
Language, setting 48 Setting up a printer 35
pH input value 103
M Potential, measuring 90
Predefined calibration standards 120
Magnetic stirrer installation 10 Predefined methods 74
Main methods 43 Printer, setting 35
Assignment of a function key 44
Changing the assignment of a function key 44 R
Deleting the assignment of a function key 45
Malfunctions 99 Report 71,95
Manual titration 93 Report header, enter 50
Measuring potential 90 Reset key 17
Measuring temperature 90 Results 95
Menu keys 16 Displaying and printing results 96
Methods (Method) 53 Statistics 96
Creating a method 55 Adding a result to the statistics 98
Selecting a method from the methods list 55 Displaying or printing a sample series 97
Selecting a method using its method ID 55 Removing results from the statistics 97
Deleting methods 72 Terminating the series 98
Selecting a method from the methods list 72 Routine 47
Selecting a method using the method ID 72 RS232C connector 111
Modifying a method 56 Run 79
Calculation 67 Starting a blank value determination using the Run key 80
Table of formulas for the calculation of results 70 Starting a sample determination using the Run key 79
EP titration 61 Starting a titer determination using the Run key 80
Control param. 62
Evaluation 66
S
Recognition 65 Safety measures 6
Termination param. 65 Measures for operational safety 6
Measure 60 Measures for your protection 6
Report 71 Sample 58
Sample 58 Sample determination using the Run key 79
Selecting a method from the methods list 57 Sample determination using the Series key 75
Selecting a method using a method ID 56 Sensor 89
Stir 60 Calibrating a sensor 91
Predefined methods 74 Measuring potential 90
Printing a method 73 Measuring temperature 90
Selecting a method from the methods list 73 Testing a sensor 91
Selecting a method using the method ID 73 Sensors 25
Printing a methods list 73 Adding a sensor 25
Starting a method 54 Deleting a sensor 28
Starting methods from the method editor 54 Modifying a sensor 26
Printing a sensor 28
Sensor calibration from the sensor setup menu 29 Titer determination from the titrant setup 23
Performing sensor calib. from the sensor setup menu 30 Performing the titer determ. from the Titrant setup 24
Zero point and slope 29 Titration 83
Sensor test from the sensor setup menu 32 Performing titration method 920 84
Series 75 Preparations 83
Starting a blank value determ. using the Series key 77 Filling the burette (rinsing) 84
Starting a sample determination using the Series key 75 Titration stand 50
Starting a titer determination using the Series key 76 Titrator ID, enter 49
Service and maintenance 107 TTL I/O socket 111
Settings 47 TTL interface description 112
Defining the temperature unit 49
Entering a report header 50 U
Entering the titrator ID 49 User interface 100
Setting the beeper sound 50 User management 45
Setting the date 48 Adding a user 45
Setting the language 48 Defining access rights for active users 47
Setting the time 49 Defining an active user 46
Setup 19 Deleting a user 46
Opening the Setup menu 19
Standards 37
Adding a standard 37
Deleting a standard 39
Modifying a standard 37
Printing a standard 39
Standard equipment 7
Start
Starting a blank value determ. using the Series key 77
Starting a blank value determination using the Run key 80
Starting a sample determination using the Run key 79
Starting a sample determination using the Series key 75
Starting a titer determination using the Run key 80
Starting a titer determination using the Series key 76
Statistics 96
Stir 60
Stirrer 91
Swiveling the titration stand 11
T
Technical data 109
Centronics socket 111
Connection possibilities for peripheral instruments 110
RS232C connector 111
TTL I/O socket 111
Temperature, measuring 90
Temperature unit, define 49
Terminating the series 98
Time, setting 49
Titer determination using the Run key 80
Titer determination using the Series key 76
Titrants 19
Adding a titrant 20
Deleting a titrant 22
Modifying a titrant 20
Printing a titrant 23
Worldwide service. Our extensive service network is among the best in the
world and ensures maximum availability and service life of your product.
European conformity. The CE conformity mark provides you with the assurance
that our products comply with the most recent EU directives.
On the Internet. You will quickly find lots of essential information about our
products, our services, and our company at
http://www.mt.com
*P51710354*
© Mettler-Toledo AG 2005, 2006 ME-51710354A Printed in Switzerland 0610/2.12