Mettler Toledo DL32, DL39 Operating Instructions Manual
Operating Instructions
KF Coulometer
DL32 / DL39
Contents
Page
1 The KF-Coulometer DL32/DL39...................................................................................5
1.1 Where can you find what information? ..........................................................................5
1.2 Coulometric determination of water - principle of measurement ........................................ 6
2 Safety Measures........................................................................................................7
2.1 Measures for your protection ........................................................................................ 7
2.2 Measures for operational safety .................................................................................... 7
3 The Coulometer .........................................................................................................8
3.1 Putting into operation .................................................................................................. 9
3.2 The operating concept ................................................................................................. 9
3.2.1 The arrow keys .........................................................................................................10
3.2.2 The command keys...................................................................................................10
3.2.3 The <Reset> key ....................................................................................................... 11
3.2.4 The <i> key..............................................................................................................11
3.2.5 The menu keys .........................................................................................................11
3.2.6 The auxiliary function keys .........................................................................................12
3.2.7 The enter keys .......................................................................................................... 12
3.3 Changing the language .............................................................................................13
4 Setup ......................................................................................................................14
4.1 Main methods (DL39 only)........................................................................................14
4.2 Peripherals...............................................................................................................15
4.2.1 Printer .....................................................................................................................15
4.2.2 Balance ...................................................................................................................16
4.2.3 Titration stand...........................................................................................................16
4.2.4 Generator electrode ................................................................................................... 17
4.2.5 Computer ................................................................................................................. 17
4.2.6 Oven sample changer Stromboli .................................................................................17
4.3 Settings ...................................................................................................................18
5 Methods..................................................................................................................20
5.1 The KF standard method ............................................................................................21
5.2 KF method parameters ..............................................................................................22
5.2.1 No. (of the method) ..................................................................................................22
5.2.2 Title (of the method)..................................................................................................22
5.2.3 Sample parameters ...................................................................................................22
5.2.4 Speed ......................................................................................................................22
5.2.5 Mix time ..................................................................................................................22
5.2.6 Auto start (DL39 only)...............................................................................................23
5.2.7 Control parameters....................................................................................................23
5.2.8 Termination parameters .............................................................................................23
5.2.9 Blank ......................................................................................................................24
5.2.10 Drift .........................................................................................................................24
METTLER TOLEDO DL32/DL39 1
5.2.11 Result (DL32 only) ...................................................................................................24
5.2.12 Calculation 1 (DL39 only) .........................................................................................24
5.2.13 Calculation 2 / Calculation 3 (DL39 only) ................................................................... 25
5.2.14 Standby ...................................................................................................................25
5.2.15 Report .....................................................................................................................25
5.2.16 Author of the method .................................................................................................25
5.3 Storage procedures ...................................................................................................26
5.4 User and METTLER Methods (DL39 only) .................................................................... 28
5.5 METTLER methods “914 Br index” and “915 Br Blank” (DL39 only) ...............................29
5.6 METTLER Method “912 Stromboli” (DL39 only)............................................................31
6 Analysis (Run).........................................................................................................33
6.1 Starting a method .....................................................................................................33
6.1.1 Menu sequence up to standby mode (KF methods) ...................................................... 34
6.1.2 Standby mode ..........................................................................................................35
6.2 Sample determination................................................................................................36
6.2.1 Weight transfer from a balance ...................................................................................39
6.2.2 Post consumption .....................................................................................................39
6.2.3 Calculations .............................................................................................................39
6.2.4 Sample series with statistics (DL39 only) ....................................................................40
6.3 Blank determination .................................................................................................. 41
6.4 Drift determination.....................................................................................................41
6.5 Determination of bromine index (DL39 only) ...............................................................42
6.6 Sample determination with the oven sample changer Stromboli (DL39 only) ...................43
7 Auxiliary Functions (Stirrer, Pump, Results)..............................................................45
7.1 Stirrer ......................................................................................................................45
7.2 Pump ......................................................................................................................45
7.3 Results ....................................................................................................................46
7.3.1 All results .................................................................................................................46
7.3.2 Recalculation ...........................................................................................................47
7.3.3 Report .....................................................................................................................48
7.3.4 Calculations (DL39 only) ..........................................................................................48
7.3.5 Statistics (DL39 only) ...............................................................................................49
7.3.6 Statistics series (DL39 only) ...................................................................................... 50
8 Information Menu (<i> key) .....................................................................................51
9 Error Messages and Malfunctions .............................................................................52
9.1 Error messages from the coulometer ........................................................................... 52
9.2 Other errors and malfunctions ....................................................................................54
9.3 Checking hardware ...................................................................................................55
9.3.1 User interface ...........................................................................................................55
9.3.2 Peripheral interfaces ..................................................................................................55
9.3.3 Inputs and outputs ....................................................................................................56
2 METTLER TOLEDO DL32/DL39
10 Installation and Maintenance ...................................................................................57
10.1 Equipping the titration stand .......................................................................................57
10.2 Installing the waste bottle...........................................................................................58
10.3 Attaching the magnetic stirrer, electrodes and devices....................................................59
10.4 Maintenance and servicing ........................................................................................60
10.5 Using TTL inputs and outputs (DL39 only)...................................................................61
11 Standard and optional equipment .............................................................................63
11.1 Standard equipment ..................................................................................................63
11.2 Optional equipment ...................................................................................................64
12 Technical Data.........................................................................................................66
Index ...................................................................................................................................71
METTLER TOLEDO DL32/DL39 3
4 METTLER TOLEDO DL32/DL39
The KF-Coulometer DL32/DL39
1 The KF-Coulometer DL32/DL39
The METTLER TOLEDO DL32/DL39 coulometers are microprocessor controlled analytical instruments which
you can use to perform coulometric Karl-Fischer and bromine index determinations simply, quickly and
dependably.
You can attach a balance, the METTLER TOLEDO GA42 printer and a computer to the appropriate RS-232C
interfaces; an EPSON- or HP-compatible printer can be attached to the Centronics interface and the METTLER
TOLEDO drying oven Stromboli to the TTL-interface of the DL39.
The coulometers have a built-in tutorial, which allows you to quickly become acquainted with the instrument’s
operation and method.
The two coulometers are equal in operation. Differences in hardware and software are mentioned in the
corresponding sections.
These Operating Instructions correspond to software version 1.1 or higher.
1.1 Where can you find what information?
These Operating Instructions and the Help texts integrated in the titrator provide a complete description of
the method of functioning of the two titrators. Explanations of parameters contained in the Help text are
supplemented here when necessary.
On the memo card you can find a short overview of menus and methods.
The Application Brochure explains the theoretical fundamentals of the coulometric Karl-Fischer titration as
well as the METTLER methods that are in the DL39‘s memory.
The Help texts in the coulometer provide you with more information or refer you to the Operating Instructions
or the Application Brochure.
You will find a detailed description of the communication between the titrator and a computer in the Description
for the computer interface.
METTLER TOLEDO DL32/DL39 5
The KF-Coulometer DL32/DL39
1.2 Coulometric determination of water - principle of measurement
When determining the water content according to Karl Fischer, water reacts with iodine and sulphur dioxide
in the presence of an alcohol and a base according to the following reaction:
H2O + I2 + SO2 + CH3OH + 3 RN ➙ [RNH]SO4CH3 + 2 [RNH]I (1).
For a volumetric titration, iodine is added as titrant. In the case of a coulometric titration, the iodine is
generated electrochemically by oxidation at the generator electrode:
2 I- ➙ I2 + 2 e
-
(2).
As long as there is water in the anolyte, the generated iodine will react according to reaction (1). I2 and H2O
react with each other on a 1:1 basis. According to Faraday’s Law, the generated amount of iodine is
proportional to the electric charge (10.72 mC = 1 µg H
O). Current consumption, therefore, is a measuring
2
stick for the amount of water.
As soon as all water has been used for the reaction, a small surplus of iodine will develop in the anodic
compartment. The iodine surplus is detected by the polarized measuring electrode, and the flow of current
to produce iodine is stopped.
METTLER TOLEDO offers generator electrodes with or without diaphragms. In both cases, iodine generation
and detection are equal. The various applicabilities are described in the Application Brochure.
In coulometric bromine index determinations, electrochemically generated bromine reacts with the double
bonds of organic compounds:
Br2 + R1-C=C-R2 ➙ R1-CBr-CBr-R2 (3).
Bromine is, thereby, produced at the anode of the generator’s electrode:
2 Br- ➙ Br2 + 2 e
-
(4).
The bromine index [mg bromine / 100 g sample] indicates how much bromine is consumed in the
transformation of a sample according to equation (3).
Generator electrode
without diaphragm
Measuring electrode
Septum
Measuring electrode
Septum
Generator electrode
with diaphragm
Titration cell
Cathode
Diaphragm
Anode
Magnetic stirring rod
6 METTLER TOLEDO DL32/DL39
Magnetic stirring rod
Safety Measures
2 Safety Measures
The titrators have been tested for the experiments and intended purposes documented in these Operating
Instructions. However, this does not absolve you from the responsibility of performing your own tests of the
products supplied by us regarding their suitability for the methods and purposes you intend to use them for.
You should, therefore, observe the following safety measures.
2.1 Measures for your protection
- Ensure that you plug the power cable supplied into a receptacle outlet that is grounded! In
the absence of grounding, a technical fault could be lethal.
Risk of electric
shock
- Never work in an environment subject to explosion hazards! The housing of the instrument
is not gas tight (explosion hazard due to spark formation, corrosion caused by the ingress
of gases).
Risk of
explosion
- When using chemicals and solvents, comply with the instructions of the producer and
the general lab safety rules!
All Karl Fischer reagents are readily flammable and toxic.
- In the case of skin contact, immediately wash off with copious amounts of water!
- If eye contact occurs, rinse intensively with copious amounts of water and consult a
physician!
2.2 Measures for operational safety
- Have the instrument serviced by METTLER TOLEDO Service only!
- Always wipe off splashed liquids immediately! The instrument is not waterproof.
- Exclude the following environmental influences:
Caution
• powerful vibrations,
• direct sunlight,
• atmospheric humidity greater than 80%,
• temperatures below 5 °C and above 40 °C,
• powerful electric or magnetic fields!
METTLER TOLEDO DL32/DL39 7
The Coulometer
3 The Coulometer
Measuring electrode
Generator electrode
Titration cell
Pump button
Keypad
Display
Rear view of instrument with connection diagram
Measuring electrode (Sensor)
External titration stand (DV705)
Cooling fin
External power pack
Waste bottle
Magnetic stirrer
GA42 printer (RS-232C)
Balance (RS-232C)
Computer (RS-232C)
Stromboli (TTL I/O)
Generator electrode
Stirrer
Waste bottle
(Suction fitting)
Pump unit
8 METTLER TOLEDO DL32/DL39
Socket for
external power pack
EPSON- or HP-compatible
printer (Centronics)
On/Off
switch
The Coulometer
3.1 Putting into operation
- Connect the supplied external power pack; switch on the coulometer. A self-test is performed before the
name of the coulometer appears on the display (example DL39).
Hallo!
F3
Arrow keys
(
8
7
[
4
5
1
2
*
.
0
Shift
)
9
]
6
3
CE
Del
Entry keys
<Reset> key
<i> key
Auxiliary function keys
Reset
Stirrer
Pump
Display
i
*
Results
Esc
METTLER TOLEDO
DL39
F1
Setup
Method
Version
F2
Run
Command keys
Menu keys
After the coulometer has been switched on, the command key <F3>, “Hello!”, the <i> key and all menu and
auxiliary function keys can be activated.
3.2 The operating concept
- Press, e.g., the setup key:
Name of the key, i.e., the displayed
list of resources belongs to the
setup menu
Title line
Selection bar
Resources SETUP
Main methods
Peripherals
Settings
Help Print OK
DL32:
“Main methods” not available!
▼
Commands
Now you can also activate the <Reset> key as well as the arrow and command keys.
OK (Press <F3>): The list of selected resources appears.
Print
(Press <F2>): The list of selected resources is printed (if a printer has been selected and defined).
Help (Press <F1>): Information about the selected resource appears.
METTLER TOLEDO DL32/DL39 9
The Coulometer
3.2.1 The arrow keys
▲▼
The arrow appears in the display when there are more lines to the list than are visible. When you
press the arrow keys (∇∆) next to the display, the lines are scrolled downwards or upwards. The
selection bar is fixed. By pressing <Shift>, ∇ or <Shift>, ∆ the lines are moved a page at a time.
The commands that can be executed always refer to the line highlighted by the selection bar.
3.2.2 The command keys
The commands, which can be triggered with <F1> ... <F3> change according to the selected menu item.
The following commands require an explanation:
Hello! When the instrument is delivered, the <F3> command in the initial mask “METTLER TOLEDO...”
is assigned to a tutorial menu. This is deleted when you have performed the first titration with
the tutorial.
Note You can call up the tutorial at any time with the <i> key.
OK This command is always a confirmation for what you
• wish to view,
• have viewed or entered,
• wish to adopt from a selection.
Modify When this command appears, a
• submenu can appear, which can or must be modified,
• a selection menu appears from which you can or must accept values or names,
• an existing parameter value or name can be directly replaced.
If a value can be modified or entered only with the keypad, the “Modify” command is missing.
ABC This command always appears when you can select letters or characters, e.g., for a name. In
this case, you cannot enter numbers until you have confirmed “ABC” (press<F1>).
Help Information about the selected resource appears.
The <Esc> key
If you have made changes in the current menu or submenu, they are discarded, i.e., the
Esc
original values/names remain. <Esc> returns you to the previous display.
10 METTLER TOLEDO DL32/DL39
The Coulometer
3.2.3 The <Reset> key
The initial mask “METTLER TOLEDO...” reappears: <Reset> is used to terminate analyses or
Reset
other actions. Data that is not stored is lost.
3.2.4 The <i> key
The value of the current electrolyte capacity, the last drift determination, the last blank value
i
determination for Stromboli (METTLER method 912), the “Hello!” tutorial, and a menu for testing
the titrator hardware are accessible with this key.
3.2.5 The menu keys
In order to analyze a sample automatically, the required data must be stored. On the coulometer, this data
is assigned to task areas (the menus), and can be accessed with the menu keys. Only the interaction
between these menus makes automatic analysis possible.
All resources required for titration such as “Peripherals” and “Settings” are stored in the <SETUP>
Setup
menu and can be changed.
The sample is determined with the aid of a method. All methods necessary for the different
Method
analyses are stored in the <METHOD> menu and can be changed. All resources defined in the
<SETUP> menu are available for these methods.
DL32 Only one method can be stored.
DL39 Fifty user methods can be stored.
The titration is performed in the <RUN> menu. The method called up determines the analysis
Run
sequence.
Note Each menu is subdivided into task areas (submenus), which are designated to menus, lists or
masks in these Operating Instructions.
METTLER TOLEDO DL32/DL39 11
The Coulometer
3.2.6 The auxiliary function keys
To activate the stirrer, the pump or to recalculate results, the required commands are also assigned to
menus. As they are independent of a sample analysis, but can support it, they are called auxiliary functions.
They are accessible under the corresponding keys.
You can switch the stirrer on or off and change the stirring speed.
Stirrer
You can siphon off electrolyte from the cell into the waste bottle. By pressing the <Pump> and
Pump
<F3> keys, “Start” or “Stop” resp., the value of the electrolyte capacity is reset to its initial value.
You can view the result list of analyzed samples, perform recalculations, change the statistical
*
Results
evaluation of a series (DL39 only!) and print out additional reports.
3.2.7 The enter keys
Shift
CE
Del
Shift
Shift
Shift
+
+
+
The <Shift> key activates the characters above the numbers.
CE You delete all entered numbers/characters/letters.
Del You delete the number/character/letter last entered.
7
4
You move the cursor to the right or left (only if letters/characters are selected),
see example:
moves the display up by 3 lines,
moves the display down by 3 lines.
Shift
+
Cursor
User a
abcdefghijklm
nopqrstuvwxyz
ABCDEFGHIJKLM
Help Select OK
12 METTLER TOLEDO DL32/DL39
The Coulometer
3.3 Changing the language
All texts on the coulometer are stored in German, English, French, Spanish, Italian and Russian. If you have
not run the tutorial and understand one of the available languages better than the one displayed, you
should select it:
Setup
Resources SETUP
Main methods
Peripherals
Settings
Help OK
Resources SETUP
Peripherals
Settings
OK
Settings SETUP
Language English
User list
Date 04-09-2001
Modify OK
– Press the <Setup> key.
– Press <Shift> and the arrow key (-) at the same time in order to scroll
down by two lines, so that “Settings” is selected.
▲
– Press <F3>, “OK”.
▼
–
Press <F2>, “Modify” repeatedly until, e.g., “Español” appears (example).
Settings SETUP
Lengua Español
Lista usuarios
Fecha 04-09-2001
Modif. OK
METTLER TOLEDO DL32/DL39 13
Pressing “OK” or <ESC> returns you to the “Resources” mask.
OK Spanish text appears.
▼
Esc English text reappears.
Setup
4 Setup
In order to perform titrations and to enable data transmission to the peripherals, your coulometer needs to
be setup with the necessary resources. In this menu, you define and store these resources.
When you press the <SETUP> key, the list of resources appears:
Main methods (DL39 only)
Peripherals
Settings
You can select the resources with the arrow keys and open the submenu with <F3>, “OK”.
4.1 Main methods (DL39 only)
When the titrator is delivered, the <F3> command is assigned to the “Hello!” tutorial, i.e., you can select its
sequence immediately. In this menu you can assign methods to command keys <F1>...<F3> or delete
“Hello!”.
With <F3>, “OK”, the following appears (example on delivery of the titrator):
Main methods SETUP
F1: Free
Modify OK
With <F2>, “Modify”, the following appears:
Main methods SETUP
User methods
METTLER methods
OK
You can select a method from the user methods, if available, or from the METTLER methods (e.g., “METTLER
912 Stromboli”:
Main methods SETUP
F1: Method 912
Title: Stromboli
Delete Modify OK
14 METTLER TOLEDO DL32/DL39
Setup
With <F3>, “OK”, the following appears:
Main methods SETUP
F2: Free
Modify OK
You can select a method to configure the <F2> command (Press <F2>, “Modify”). If you confirm this
display with <F3>, “OK”, the following appears:
Main methods SETUP
F3: Hello!
Delete Modify OK
You can either delete “Hello!” with <F1> or overwrite it with another method (press <F2>, “Modify”).
4.2 Peripherals
With <F3>, “OK”, the names of the peripherals you can attach to the coulometer via the RS-232C interfaces
or the Centronics interface appear. You must define these and possibly change the preset settings.
Printer None
Balance None
Titrn stand Internal
Computer Not def.
4.2.1 Printer
With <F3>, “OK”, the name of the printer you connected to the coulometer appears.
HP
GA42
EPSON
None
If you select the METTLER TOLEDO GA42 there is no need for any further settings. If you select an EPSONor HP-compatible printer, you must enter the following settings (standard settings for the printer are printed
in bold).
METTLER TOLEDO DL32/DL39 15
Setup
HP-compatible EPSON-compatible
Type PCL3+ or PCL3 LQ/Stylus or LX/SX
Paper Single sheet Single sheet or Fanfold
Format A4 or 81/2 * 11" A4, 81/2 * 11" or 81/2 * 12"
Automatic feed Yes Yes or No
Type Select “PCL3+”, “PCL3”, “LQ/Stylus” or “LX/SX”.
Paper Select “Single sheet” or “Fanfold.
Format • A4 (width= 21 cm, length= 29,7 cm)
• 81/2 * 11" (width= 81/2 inches, length = 11 inches)
• 81/2 * 12" (width= 81/2 inches, length= 12 inches)
Automatic feed Select “Yes” or “No”.
Yes Each report starts on a new page;
with “Paper: Single sheet”, a footer is printed out on each page.
No The individual reports are separated by a distance of 2 lines.
4.2.2 Balance
Unidirect.
Bidirect.
None
Unidirectional The weight, the balance continuously transfers the current weight value.
Coulometer Balance
Data to Coulometer
Configuration: “Send Cont.”
Bidirectional On requesting the weight, the balance transfers the current weight value when ordered by
the titrator.
Coulometer Balance
Command from Coulometer
Data to Coulometer
Configuration: “Send Stable”
(“Send on Transfer”)
For METTLER TOLEDO balances AB, AG, AT and AX always select “Bidirectional”.
4.2.3 Titration stand
Internal
External
You can attach the METTLER TOLEDO DV705 KF titration stand as an external titration stand. Its magnetic
stirrer and pump are controlled via the DV705. For use of the coulometric measuring cell on the external
titration stand, the titration arm must be exchanged (see optional equipment).
16 METTLER TOLEDO DL32/DL39
Setup
4.2.4 Generator electrode
For the generator electrode (with or without diaphragm) there is no need for any further settings.
Note The maximum value of the current pulses of the generator electrode is 400 mA. If the conduc-
tivity of the electrolyte is low and this value can no longer be reached for this reason, the
coulometer limits the current pulses to 200 mA.
4.2.5 Computer
Defined
Not defined
If you connect a computer, you must select “Defined” and possibly change the settings.
Default settings for the computer
Baudrate 4800
Parity Even
Number of data bits8
Number of stop bits1
Character set ASCII
Start/End '{'/CR
Baudrate Select 1200, 2400, 4800 or 9600.
Parity Select “Even”, “Odd” or “None”.
Data bits Select 7 or 8 bits .
Stop bits Select 1 or 2 bit(s).
Character set Select “ASCII” or “DL”.
Note If you select “DL”, you must specify 8 for the number of data bits.
Start/End Select “'{'/CR” or “STX/ETX”.
Note You can find additional information on the communication between coulometer and the computer
in the “Description for the Computer Interface”.
4.2.6 Oven sample changer Stromboli
If you have an oven sample changer Stromboli connected to the DL 39, no further entries are necessary.
METTLER TOLEDO DL32/DL39 17
Setup
4.3 Settings
You can select or define the following settings for the coulometer:
Language English
User list
Date 26-08-2001
Time 10:20
Titrator-ID
Access for Expert
Beep Yes
Capacity [mg] 80
Pumping time [s] 60
Language Select English, German, French, Spanish, Italian or Russian.
User list Press <F2>, “Modify”, and a list of defined names and an empty line appears (“...”)
where you can enter a new name.
Pres “ABC” and you can enter your name. Erase a selected name with “Delete”.
You can then select your name for both the development of a method and the performance
of the analysis.
Date You can set the date and select the format.
Day 26
Month 8
Year 2001
Format 31-08-2001
Format Select “31/08/2001”, “08-31-2001”, “31-Aug-2001” or “Aug/31/2001”.
Time You can set the time and select the format.
Hour 10
Minute 20
Format 24 h
Format Select between “24 h” or “am/pm”.
Titrator ID To enter an identification for your coulometer , press <F1>, “ABC”. The ID is always
reported.
Access for You can decide whether all persons who work with the coulometer should also have
access to the “Setup” and “Method” menus, i.e., have the right to modify resources or
methods.
Expert When the coulometer is delivered, you have access to all menus. To change
this, select “Routine”.
18 METTLER TOLEDO DL32/DL39
Routine You can:
• in the “Setup” menu, only print out the defined resources and view the list
• in the “Method” menu only print out the list of methods (DL39 only) and
• not perform any recalculations or change any statistical data.
• under the <i> key, select neither the “Tutorial” nor the “Hardware test” .
Renewed access for experts is described on the last page of these Operating Instructions.
Beep You can select:
Yes
Minimum
No
Yes In addition to those cases described below under “Minimum”, a beep also
sounds after each keystroke.
Minimum A beep sounds on transition from pretitration to standby, on display of the
results and in the case of error messages.
Setup
of settings
each method.
Capacity You can perform several titrations consecutively in the same anolyte. Its capacity, however,
is limited. In the vicinity of the capacity limit the reaction rate decreases.
You should enter the value for capacity that the producers of the reagents recommend.
When this value is surpassed the message “Capacity exhausted” appears.
The amount of water (in mg) that has been titrated during the analyses and pretitrations
is added up. The difference between the value entered and the titrated water is displayed
under the <i> key. Pressing the <Pump> and <F3> keys, “Start” or “Stop” resp., reset the
value to its initial setting.
Pumping time The defined time is a safety criterion: the pump will shut off after this time if you, e.g.,
leave the coulometer while the pump is running.
METTLER TOLEDO DL32/DL39 19
Methods
5 Methods
The coulometer automatically performs analyses with the help of predefined methods. On delivery of the
instrument
in the DL32, the KF standard method specified by
us is stored. You can modify this method and save it
under a number.
Methods METHOD
KF standard method
Help Modify
Methods METHOD
No. 0
of the method
Help OK
When you have modified and saved the method, the
following appears (example):
Methods METHOD
111 Methanol
KF standard method
in the DL39 the KF standard method specified by us
and 5 METTLER methods are stored. You can modify
these methods and save them as user methods.
Methods METHOD
User methods
METTLER methods
KF standard method
Help Print OK
Print The list of methods you have developed
is printed out.
OK The user methods with their defined
numbers and titles appear (example):
Methods METHOD
22 Toluene
33 Silicon oil
111 Methanol
Delete Print Modify
Help Print Modify
A complete titration method comprises sample preparation, mixing and wait times, the actual titration,
result calculation and a report. These partial steps are defined in the coulometer as parameters which
determine the progress of an analysis.
You modify a method
by changing its parameters.
20 METTLER TOLEDO DL32/DL39
Methods
5.1 The KF standard method
You can use the KF standard method to develop your own method. In this you are guided from one
parameter to another in the specified order. Exceptions are sample, control, termination and report parameters,
which are shown as a group in a mask. In the case of the DL39, this also applies to the calculation
parameters.
With the user and METTLER methods, all parameters appear as a list in a mask. Exceptions are again the
above-mentioned groups.
The last parameter of a method, “Author of a method”, always appears in its own mask.
The method is always shown with the following default parameters.
No. of the method
Title of the method
Sample parameters
ID
Type Mass
Minimum [g] 0.0000
Maximum [g] 5.0000
Entry Before
Speed [%] 40
Mix time [s] 10
Auto start No
Control parameters
Pol. current [µA] 2
End point [mV] 100
Gen.speed Normal
Termination param.
Max. time [s] 300
Drift stop Rel.
Drift [µg/min] 3
Blank [µg] 0
Drift Online
Result
→→
→ DL39 only
→→
→→
→ DL32 only
→→
Calculation 1 ppm
R1 = x [ppm]*f1
f1 = 1.0000
Unit ppm
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Calculation 2
R2 = No calculation
f2 = 1.0000
Unit → DL39 only
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Calculation 3
R3 = No calculation
f3 = 1.0000
Unit
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Standby Yes
Report
Output Print.+Comp.
Type GLP
Author of the method
METTLER TOLEDO DL32/DL39 21
Methods
5.2 KF method parameters
The following parameters can be changed. This will either cause some parameters to appear or disappear.
The METTLER methods 911 – 915 and specific parameters for automation with the METTLER TOLEDO oven
sample changer Stromboli are described in a separate chapter.
5.2.1 No. (of the method)
The method is stored under the number. The numbers 911– 915 are reserved for METTLER methods.
5.2.2 Title (of the method)
You can give the method a specific name.
5.2.3 Sample parameters ID You can enter an identification for the sample(s) now or just before the titration (“Request”)
for every sample.
Type Select “Mass”, “Fixed mass”, “Volume”, “Fixed volume”, “Pieces” or “Fixed pieces”.
Minimum/Maximum
appears when “Mass”, “Volume” or “Pieces” is selected. The unit depends on the
type of sample: [g], [mL] or [pcs]..
Help You can calculate and enter values for a fixed or variable amount of sample.
Entry of the amount of sample “Before” or “During” the actual titration. “Entry” appears when
“Mass”, “Volume” or “Pieces” is selected.
DL39: If you select “Yes” for the parameter “Auto start” (see below), “Before” is automatically
converted to “During” when storing.
Density appears when “Volume” or “Fixed Volume” is selected.
Weight appears when “Fixed Mass” is selected.
Volume appears when “Fixed volume” is selected.
Number appears when “Fixed pieces” is selected.
5.2.4 Speed
Stirring should guarantee quick and thorough mixing of the electrolyte. We recommend the setting: 40 %.
The magnetic stirring rod should not “jump”.
Only use the magnetic stirring rod included in the delivery (see equipment).
5.2.5 Mix time
The time is an empirical value and can be entered individually for the samples (“Request”).
22 METTLER TOLEDO DL32/DL39
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