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Operating Instructions

KF Titrators

DL31 / DL38

Contents
Page
1

The DL31/DL38 KF titrators .......................................................................................... 5

2
2.1
2.2

Safety measures .......................................................................................................... 6


Measures for your protection .......................................................................................... 6
Measures for operational safety ...................................................................................... 6

3
3.1
3.2
3.2.1
3.2.2
3.2.3
3.2.4
3.2.5
3.3

The titrator .................................................................................................................. 7


Putting into operation .................................................................................................... 8
The operating concept ................................................................................................... 8
The command keys ....................................................................................................... 9
The menu keys ........................................................................................................... 10
The auxiliary function keys ........................................................................................... 10
The <i> key................................................................................................................ 11
The entry and arrow keys ............................................................................................. 11
Changing the language ............................................................................................... 12

4
4.1
4.2
4.3
4.4
4.5
4.5.1
4.5.2
4.5.3
4.5.4
4.6

Setup (<Setup> key).................................................................................................. 13


KF titrants .................................................................................................................. 13
Br No. titrants (DL38 only) .......................................................................................... 15
KF standards .............................................................................................................. 16
Main methods (DL38 only) .......................................................................................... 17
Peripherals ................................................................................................................. 18
Printer ....................................................................................................................... 18
Balance ..................................................................................................................... 19
Titration stand ............................................................................................................. 19
Computer ................................................................................................................... 19
Settings ..................................................................................................................... 20

5
5.1
5.2
5.2.1
5.2.2
5.2.3
5.2.4
5.2.5
5.2.6
5.2.7
5.2.8
5.2.9
5.2.10
5.2.11
5.2.12
5.2.13

Methods (<Method> key) ........................................................................................... 22


The KF standard method .............................................................................................. 23
KF method parameters ................................................................................................ 24
No. (of the method) .................................................................................................... 24
Title (of the method) .................................................................................................... 24
Sample parameters ..................................................................................................... 24
Speed ........................................................................................................................ 24
Mix time .................................................................................................................... 24
Titrant ........................................................................................................................ 24
Volume (for predispensing) .......................................................................................... 25
Wait time (after predispensing)..................................................................................... 25
Auto start (DL38 only) ................................................................................................. 25
Control parameters ...................................................................................................... 25
Termination parameters ............................................................................................... 25
Blank ........................................................................................................................ 26
Drift ........................................................................................................................... 26

METTLER TOLEDO DL31/DL38

5.2.14
5.2.15
5.2.16
5.2.17
5.2.18
5.3
5.4
5.4.1
5.4.2

Result (DL31 only) ..................................................................................................... 26


Calculation (DL38 only) .............................................................................................. 26
Standby ..................................................................................................................... 27
Report ....................................................................................................................... 27
Author of the method ................................................................................................... 27
Storage procedures ..................................................................................................... 28
User and METTLER methods (DL38 only) ...................................................................... 30
METTLER methods "908 Bromine No." and "909 Blank Br No." (DL38 only) ..................... 31
METTLER method "910 Stromboli" (DL38 only) ............................................................. 32

6
6.1
6.1.1
6.1.2
6.2
6.2.1
6.2.2
6.2.3
6.2.4
6.3
6.4
6.5
6.6
6.7
6.8

Analysis (<Run> key) ................................................................................................ 34


Starting a method ....................................................................................................... 34
Menu sequence up to standby mode (KF methods) ........................................................ 35
Standby mode ............................................................................................................ 36
Sample determination .................................................................................................. 37
Weight transfer from a balance ..................................................................................... 40
Post consumption ....................................................................................................... 40
Calculations ............................................................................................................... 40
Sample series with statistics (DL38 only) ...................................................................... 41
Concentration determination ......................................................................................... 42
Blank determination .................................................................................................... 44
Drift determination ....................................................................................................... 44
Bromine number determination (DL38 only) .................................................................. 45
Sample determination with the oven sample changer Stromboli (DL38 only) ..................... 46
KF learn titration ......................................................................................................... 48

7
7.1
7.2
7.3
7.4
7.4.1
7.4.2
7.4.3
7.4.4
7.4.5
7.4.6

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>) ................................... 50


<Stirrer> .................................................................................................................... 50
<Burette>................................................................................................................... 50
<Pump> .................................................................................................................... 51
<Results> .................................................................................................................. 52
All results ................................................................................................................... 52
Recalculation ............................................................................................................. 53
Report ....................................................................................................................... 54
Calculations (DL38 only) ............................................................................................ 54
Statistics (DL38 only) ................................................................................................. 54
Statistics series (DL38 only) ........................................................................................ 55

Information menu (<i> key) ....................................................................................... 56

9
9.1
9.2
9.3
9.3.1
9.3.2
9.3.3

Error messages, malfunctions and hardware tests ....................................................... 57


Error messages from the titrator .................................................................................... 57
Other errors and malfunctions ...................................................................................... 59
Hardware tests ........................................................................................................... 60
User interface ............................................................................................................. 60
Peripheral interfaces .................................................................................................... 60
Inputs and outputs ...................................................................................................... 61

METTLER TOLEDO DL31/DL38

10
10.1
10.2
10.3
10.4
10.5
10.6

Installation and maintenance ..................................................................................... 62


Equipping the titration stand ......................................................................................... 62
Installing the burette .................................................................................................... 63
Installing the solvent and waste bottles .......................................................................... 64
Attaching the magnetic stirrer, electrode and devices ....................................................... 65
Using TTL inputs and outputs (DL38 only) ..................................................................... 66
Maintenance and servicing .......................................................................................... 66

11
11.1
11.2

Standard and optional equipment ............................................................................... 68


Standard equipment .................................................................................................... 68
Optional equipment ..................................................................................................... 70

12

Technical data ........................................................................................................... 73

13

Index ........................................................................................................................ 81

METTLER TOLEDO DL31/DL38

METTLER TOLEDO DL31/DL38

The DL31/DL38 KF titrators

The DL31/DL38 KF titrators

The METTLER TOLEDO DL31/DL38 titrators are microprocessor controlled analytical instruments which you
can use to perform Karl Fischer titrations simply, quickly and dependably.
You can attach a balance, the METTLER TOLEDO GA42 printer and a computer to the appropriate RS232C
interfaces as well as an EPSON- or HP-compatible printer to the Centronics interface and, at the DL38's TTLinterface, the METTLER TOLEDO oven sample changer Stromboli. The METTLER TOLEDO LabX titration
software allows you to control your titrator via a computer.
The titrators have a tutorial stored which quickly enables you to become acquainted with the operation and
method of functioning of the instrument.
The two titrators have the same operation. Differences in the hardware and software are mentioned in the
corresponding sections.
These Operating Instructions correspond to software version 2.0 or higher.

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 texts 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 Karl Fischer titration, the control of
the titration in the DL31/DL38 and documents the METTLER methods stored in the DL38.
The Help texts in the titrator 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 of the computer interface.

METTLER TOLEDO DL31/DL38

Safety measures

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

Caution

Have the instrument serviced only by METTLER TOLEDO Service!


Make sure that every connector is in the correct position! Do not damage the connector
pins of the magnetic stirrer cable! Pins damaged by faulty insertion can cause a short
circuit at the "Stirrer" output. This renders the titrator non-functional.
Always wipe off splashed liquids immediately! The instrument is not water-proof.
Exclude the following environmental influences:
powerful vibrations,
direct sunlight,
atmospheric humidity greater than 80%,
temperatures below 5 C and above 40 C,
powerful electric or magnetic fields!

METTLER TOLEDO DL31/DL38

The titrator

The titrator

Titration stand

Burette

Titrant bottle

Solvent bottle

Arrestment knob
Pump knob
Waste bottle
Keypad

Magnetic stirrer

Rear view

Balance (RS232C)
External stand (DV705)

GA42 printer (RS232C)

Computer (RS232C)
Stirrer output
Stromboli, TBox, etc. (TTL I/O)
Electrode input (KF)
EPSON- and HP-compatible printers
(Centronics)
Pump unit
On/Off switch
Suction fitting
Output fitting

METTLER TOLEDO DL31/DL38

Socket for
external power pack

The titrator

3.1

Putting into operation

Plug the supplied external power pack into the titrators socket, connect to the power supply and switch
on the titrator: A self-test is performed before the name of the titrator appears (example DL38).

Display
<Reset> key
<i> key

i
Stirrer

Pump

(
8

)
9

[
5

]
6

CE
Del

METTLER TOLEDO
DL38

Auxiliary function keys

Arrow keys

Reset

Burette

Version 2.0
Hello!

*
Results

0
Esc

F2

F1

Entry keys

F3
Shift

Setup

Method

Run

Command keys

Menu keys

The command key <F3>, "Hello", the <i> key and all Menu and Auxiliary function keys can be activated
after the titrator has been switched on.

3.2

The operating concept

Press, e.g. the <Setup> key:


Title line
Selection bar

Resources

SETUP

KF titrants
Br No. titrants
KF standards

Print
OK

Name of the key, in other words the displayed


list of resources belongs to the Setup menu

Commands

DL31: No "Br No. titrants"!

You can now also activate the arrow key (), the <Reset> key and the Command keys <F2>, "Print" and
<F3>, "OK".

Print
OK

The arrow in the display means that the list contains more resources. If you press the arrow
key (), the lines are scrolled upward, the selection bar is fixed. The commands you can
execute always refer to the line that is selected.
Press <F2>: The list of KF titrants is printed out (if a printer is selected and defined).
Press <F3>: The list of KF titrants appears.

METTLER TOLEDO DL31/DL38

The titrator

3.2.1

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 can not 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, in other words
Esc
the original values/names remain in force. <Esc> always effects a return to the previous display.
The <Reset> key
The initial mask "METTLER TOLEDO..." reappears: <Reset> is used to terminate analyses or
other actions. Data that are not stored are lost.
Reset

METTLER TOLEDO DL31/DL38

The titrator

3.2.2

The menu keys

In order to analyze a sample automatically, the required data must be stored. In the titrator, these data are
assigned to so-called task areas, the menus and can be accessed with the Menu keys. It is only the
coordination between these menus that makes the automatic analysis possible.

Setup

Method

Run

Note

3.2.3

All resources required for the titration such as KF titrants and KF standards are stored in the
Setup menu and can be changed.
The sample is determined with the aid of a method. All methods necessary for the different
analyses are stored in the Method menu and can be changed. All resources defined in the Setup
menu are available for these methods.
DL31: Only one method can be stored.
DL38: Fifty user methods can be stored.
The titration is performed in the Analysis menu. The method called up determines the analysis
sequence.
Each menu is subdivided into task areas (submenus) which are designated menus, lists or
masks in these Operating Instructions.
The auxiliary function keys

To rinse the burette or recalculate results, the required commands are also assigned to menus. As they are
independent of a sample analysis, but can support it, we call them auxiliary functions. They are accessible
under the corresponding keys.
You can switch the stirrer on or off and change the stirring speed.
Stirrer

Pump

Burette

Results

10

You can add or siphon off solvent.

You can rinse the burette and the tip of the dispensing tubing and add a specified volume.

You can view the result list of analyzed samples, perform recalculations, change the statistical
evaluation of a series (DL38 only!) and print out additional reports.

METTLER TOLEDO DL31/DL38

The titrator

3.2.4

The <i> key


The value of the current solvent capacity, the last drift determination, the last blank value
determination for DL38/Stromboli (METTLER method 910), the "Hello!" Tutorial, the KF
learn method and a menu for testing the titrator hardware are accessible with this key.

i
3.2.5

The entry and arrow keys

Shift

With the <Shift> key, you can activate the characters above the numbers.

CE
Del

CE
Del

Shift

Shift

+
+

You delete all entered numbers/characters/letters.


You delete the number/character/letter last entered.

You can move the cursor to the right or left (only if letters/characters are selected), see
example:

User
Cursor

Shift

Shift

abcdefghijklm
nopqrstuvwxyz
ABCDEFGHIJKLM
Help
Select

OK

skips 3 lines of the display upward (page up),


skips 3 lines of the display downward (page down).

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.

METTLER TOLEDO DL31/DL38

11

The titrator

3.3

Changing the language

All texts in the titrator are stored in English, German, 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:

Press the <Setup> key.

Setup

Resources

SETUP

KF titrants
Br No. titrants
KF standards

Print
OK

Resources
Peripherals
Settings

SETUP

OK

Press the <Shift> and Arrow () once, then press only the Arrow key
to select "Settings".

Press <F3>, "OK".

Settings

SETUP

Language
English
User list
Date
20-08-1998
Modify
OK

Press <F2> repeatedly until, e.g. "Espaol" appears.

Settings

SETUP

Lengua
Espaol
Lista usarios
Fecha 20-08-1998
Modif.
OK

12

With "OK" or <Esc> the "Resources" mask reappears.


OK Spanish texts appear.
Esc English texts appear.

METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

Setup (<Setup> key)

In order to perform titrations, the titrator must know the titrants and their concentration. It must know the
settings of the attached instruments to transfer the data. In this menu you define and store these resources:
You set up your titrator.
When you press the <Setup> key, the list of resources appears:
KF titrants
Br No. titrants (DL38 only)
KF standards
Main methods (DL38 only)
Peripherals
Settings

The most commonly used titrants and KF standards are already stored in the titrator. You can not only delete
these or change their parameters, but also define new ones.
All titrants and KF standards needed for the METTLER methods are stored! If you delete
one of these resources, the error message that it is missing does not appear until the start
of the titration.
Print
OK

4.1

Depending on your choice of resource, its list with the corresponding parameters will be printed
out.
The list of the selected resources appears.

KF titrants

With <F3>, "OK" the stored KF titrants appear.


1-comp 5
1-comp 2
2-comp 5
2-comp 2
Pyridine 5
1-comp 5K
...

1 component reagent: 5 mg/mL


1 component reagent: 2 mg/mL
2 component reagent: 5 mg/mL
2 component reagent: 2 mg/mL
Pyridine (1 component reagent): 5 mg/mL
1 comp. reagent for ketones: 5 mg/mL
free line for a new titrant

METTLER TOLEDO DL31/DL38

13

Setup (<Setup> key)

Delete
Print
Modify

The titrant is deleted.


The parameters of the titrant are printed out.
The parameters of the titrant appear:
Name
1-comp 5
Conc.[mg/mL] 5.0000
Type
1 component
Burette
5 mL
Fill rate [%]
100
Batch
Check after [day] 0
Date
00-00-0000
Time
0:00

Name
Conc.
Type
Burette
Batch

Press <F1>, "ABC" to change the name. The titrant with its parameters will be stored under this
name.
You can change the concentration or its range. You should change the concentration only if you
know the correct value!
Select one of the preset titrant types: 1 component, 2 components, Pyridine and Others. The
correct selection is important (see "Control parameters", Section 5.2).
Select the burette (volume) which is used to dispense the titrant.
Press <F1>, "ABC" to enter the batch number specified on the bottle.

Storage procedure
The titrant with its changed parameters is stored when you confirm the parameter list with <F3>, "OK". If
you press the <Esc> key, no changes will be made.
New KF titrant
You add a titrant to the titrant list when you confirm the free line with <F3>, "OK" The parameters always
appear, only the name of the titrant is missing.
Change the parameters as described above.
The name of the new titrant must differ from those already stored, otherwise an existing
titrant will be overwritten!
Note

14

In the DL31 you can store 10 titrants, in the DL38 20.

METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

4.2

Br No. titrants (DL38 only)

With <F3>, "OK" the stored titrants for determination of the bromine number appear:
Br-/BrO3- Bromide/bromate solution
...
free line for a new titrant
Delete
Print
Modify

The titrant is deleted.


The parameters of the titrant are printed out.
The parameters of the titrant appear:
Name
Br-/BrO3Conc. [mol/L] 0.05
Burette
5 mL
Fill rate [%]
100
Batch

Name
Burette
Batch

Press <F1>, "ABC" to change the name. The titrant and its parameters will be stored under this
name.
Select the burette (volume) which is used to dispense the titrant.
Press <F1>, "ABC" to enter the batch number specified on the bottle.

Storage procedure
The titrant with its changed parameters is stored when you confirm the parameter list with <F3>, "OK". If
you press the <Esc> key, no changes will be made.
New Br No. titrant
You add a new titrant to the titrant list when you confirm the free line with <F3>, "OK". The parameters
always appear, only the name of the titrant is missing.
Change the parameters as described above.
The name of the new titrant must differ from the one already stored, otherwise an existing
titrant will be overwritten!
Note

You can store 5 titrants for the bromine number.

METTLER TOLEDO DL31/DL38

15

Setup (<Setup> key)

4.3

KF standards

With <F3>, "OK" the stored Karl Fischer standards appear which you can use to determine the concentration of the KF titrants.
di-Na tartrate
H2O standard 10
H2O standard 1
H2O standard 5
H2O ISO 3696
...

Delete
Print
Modify

di-sodium tartrate . 2 H2O


Water standard : 10 mg/g
Water standard: 1 mg/g
Water standard: 5 mg/mL
pure water following ISO standard
free line for a new standard

The standard is deleted.


The parameters of the standard are printed out.
The parameters of the standard appear:
Name di-Na tartrate
H2O content 15.660
Unit
%
Batch
Type
Mass
Weight [g]0 0.0500

Name
Batch
Type
Weight

Volume

Press <F1>, "ABC" to change the name. The standard and its parameters will be stored under
this name.
Press <F1>, "ABC" to enter the batch number specified on the bottle.
You can select mass or volume. "Weight" changes accordingly to "Volume".
Optimum values for a titrant concentration of 5 mg/mL and a burette volume of 5 mL are stored:
0.05 g for the tartrate standard,
0.75 g for the H2O standard 10,
3.5 g for the H2O standard 1,
0.01 g for the H2O standard ISO 3696,
3 mL for the H2O standard 5.

Storage procedure
The standard with its changed parameters is stored when you confirm the parameter list with <F3>, "OK".
If you press the <Esc> key, no changes are made.
New KF standard
You can add a standard to the list of KF standards if you confirm the free line with <F3>, "OK". The
parameters always appear, only the name of the standard is missing.
Change the parameters as described above.
The name of the new standard must differ from those already stored, otherwise an existing
standard will be overwritten!

16

METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

Note
In the DL31 you can store 10 standards, in the DL38 20.
The Application brochure offers tips on sample preparation, sampling and the optimum amount of sample.

4.4

Main methods (DL38 only)

When the titrator is delivered, the <F3> command is assigned to the Tutorial "Hello!", in other words 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
Main methods

OK

With <F2>, "Modify", the following appears:

SETUP

User methods
METTLER methods
OK
Main methods
F1:
Title

SETUP

Method 910
Stromboli

Delete Modify

OK

Main methods

SETUP

F2:

Free

Modify
Main methods
F3:

Delete Modify

OK

You can select a method from the METTLER methods (or from the user
methods if available), e.g. "910 Stromboli":
With <F3>, "OK", the following appears:

You can select a different method to configure the <F2> command (press
<F2>, "Modify").
If you confirm this display with <F3>, "OK", the following appears:

SETUP
Hello!

OK

METTLER TOLEDO DL31/DL38

You can either delete "Hello!" with <F1> or overwrite it by a different


method (press <F2>, "Modify").

17

Setup (<Setup> key)

4.5

Peripherals

With <F3>, "OK" the names of the instruments which you can attach to the titrator via the RS232C interfaces, the Centronics interface, the stirrer output and the DV705 connection appear. You must define these
and possibly change the preset settings.
Printer
Balance
Titrn stand
Computer

If you have the METTLER TOLEDO oven sample changer Stromboli connected to the TTL I/O interface, no
further entries are necessary.
4.5.1

Printer

With <F3>, "OK" the names of the printers which you can attach to the titrator appear.
HP
GA42
EPSON
None

Select the attached printer.


With an EPSON or HP printer change the type and possibly the settings with <F2>.
Type
Select "PCL3+", "PCL3", "LQ/Stylus" or "LX/SX"
Paper
Select "Single sheet" or "Fanfold" (see "Feed")
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
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.
If you select an EPSON- or HP-compatible printer, you must enter the following settings:
Standard settings for the printer are printed in bold
HP-compatible

EPSON-compatible

Type

PCL3+ or PCL3

LQ/Stylus or LX/SX

Paper

Single sheet

Single sheet or Fanfold

Format

A4 or 8 /2 * 11"

A4, 81/2 * 11" or 81/2 * 12"

Automatic feed

Yes

Yes or No

18

METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

4.5.2

Balance

Unidirectional
Bidirectional
None

Unidirect. On request for the weight, the balance continuously transfers the current weight value.
Titrator

Balance
Data to titrator

Bidirect.

Configuration: "Send Cont."

On request for the weight, the balance transfers the current weight value when ordered by the titrator.
Titrator

Command from titrator


Data to titrator

Balance

Configuration: "Send Stable"


("Send on Transfer")

With METTLER TOLEDO balances AB, AG, AT and AX always use the setting "Bidirectional" and the following
settings on the balance:
Baud rate: 2400, Data bits: 7, Parity: Even, Handshake: No.
4.5.3

Titration stand

Internal
External

As an external titration stand you can attach the DV705 KF Titration Stand from METTLER TOLEDO whose
magnetic stirrer and pump are controlled via the DV705 connection ("External stand").
4.5.4

Computer

Defined
Not defined

If you attach a computer, you must select "Defined" and possibly change the settings.
Baud rate
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".

METTLER TOLEDO DL31/DL38

19

Setup (<Setup> key)

Default settings for the computer


Baud rate
Parity
Number data bits
Number stop bits
Character set
Start/end

4800
Even
8
1
ASCII
'{'/CR

Note
The METTLER TOLEDO LabX titration software allows you to control your titrator via a computer.
You will find additional information on the communication between titrator and computer in the Description
of the computer interface.

4.6

Settings

You can or must select or define the following settings for the titrator:
Language
User list
Date
Time
Titrator ID
Access for
Beep
Solv. capac.[mL]
Pumping time [s]

Language
User list

Date

Select English, German, French, Spanish, Italian or Russian.


Press <F2>, "Modify", and a list of defined names and an empty line ("") appears
where you can enter a new name. Press "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.
You can set the date and select the format.
Day
Month
Year
Format

Time

Format
Select "31-08-1998", "08/31/1998", "31-Aug-1998" or "Aug/31/1998".
You can set the time and select the format.
Hour
Minute
Format

Format

20

26
8
1998
31-08-1998

10
20
24 h

Select "24 h" or "am/pm".

METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

Titrator ID
Access for

Beep

To enter an identification for your titrator, press <F1>, "ABC". The ID is always reported.
You can decide whether all persons who work with the titrator should also have access to
the Setup and Method menus, in other words have the right to modify resources or methods.
Expert
When the titrator is delivered, you have access to all menus. To change this,
select "Routine".
Routine
You can
in the Setup menu only print out the defined resources and view the list of
settings.
in the Method menu only print out the list of methods (DL38 only) and
each method.
in the Results menu not perform any recalculation and not change any
statistical data.
under the <i> key, select neither the Tutorial, the KF learn titration nor the
Hardware tests menu.
Renewed access for experts is described on the last page of these Operating Instructions.
You can select:
Yes
Minimum
No

Solv. capac.

Pumping time

Minimum A beep sounds on transition from pretitration to standby, on display of the


results and in the case of error messages.
Yes
A beep also sounds after each keystroke.
You can perform several titrations in the same solvent in succession, but its capacity is
limited. In the vicinity of the capacity limit, the reaction rate decreases.
You should enter a value for the maximum titrant volume which is suitable for your
sample determinations. If this value is exceeded, the error message "Solvent capacity
exhausted" appears.
Only the titrant volume which is consumed during the analysis is summed. The volume
which is added, e.g. using the auxiliary function "Dispense" is not taken into account.
The difference between the defined value and the titrant consumption is shown under the
<i> key.
The defined time is a safety criterion: the pump will shut off after this time if you, e.g.
leave the titrator while the pump is running.

METTLER TOLEDO DL31/DL38

21

Methods (<Method> key)

Methods (<Method> key)

The titrator automatically performs analyses with the help of predefined methods. On delivery of the instrument

in the DL31 the KF standard method specified by us


is stored. You can modify this method and save it
under a number.
Methods

METHOD

Methods

KF standard method

Help

in the DL38 the KF standard method specified by us


and 11 METTLER methods are stored. You can modify
these methods and save them as user methods.
METHOD

User methods
METTLER methods
KF standard method
Help
Print
OK

Modify

Method
No.
of the method
Help

Print The list of methods you have developed is


printed out.
OK The user methods with their defined numbers
and titles appear (example):

METHOD
0

OK
Methods

When you have modified and saved the method,


the following appears (example):
Methods

METHOD

METHOD

22 Coffee
33 Tea
113 Powdered milk
Delete Print Modify

123 Cellulose
KF standard method
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 titrator as parameters which determine
the progress of an analysis.
You modify a method
by changing its parameters.

22

METTLER TOLEDO DL31/DL38

Methods (<Method> key)

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 DL38, 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 the method" always appears
in its own mask.
The method is always shown with the following default parameters. The parameters which you can modify
are listed in Section 5.2.
No. of the method 0
Title of the method
Sample parameters
ID
Type
Mass
Minimum [g]
0.0000
Maximum [g]
5.0000
Entry
Before
Speed [%]
35
Mix time [s]
10
Titrant
2-comp 5
Volume [mL]
for predisp. 0.0000
(Wait time [s]
after predisp.
0)
Auto start
No
Control parameters
Current [A]
20
End point[mV]
100
Vmin [L]
0.5
Vmax [L]
8.0
Vmax factor [%] 30
Start
Cautious
Termination param.
Max. time [s]
600
Drift stop
Rel.
Drift [g/min]
15
Vmax [mL]
10.000
Blank [g]
0
Drift
Online

DL38 only

Result
%
Calculation 1
%
R1 =
x [%]*f1
f1 =
1.0000
Unit
%
Decimal places
2
Statistics
Yes
Max. srel [%]
0.00
Calculation 2
R2 = No calculation
f2 =
1.0000
Unit
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

DL31 only

DL38 only

The METTLER methods 900 910 and specific parameters for automation with the METTLER TOLEDO oven
sample changer Stromboli are described in a separate chapter.

METTLER TOLEDO DL31/DL38

23

Methods (<Method> key)

5.2

KF method parameters

The following parameters can be changed. This will either cause some parameters to appear or disappear.
5.2.1

No. (of the method)

The method is stored under this number. The numbers 900 999 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 for every sample
("Request").
Type
Select "Mass", "Fixed mass", "Volume", "Fixed volume", "Pieces" or "Fixed pieces".
Weight
appears when "Fixed mass" is selected.
Volume
appears when "Fixed volume" is selected.
Number
appears when "Fixed pieces" is selected.
Density
appears when "Volume" or "Fixed volume" is selected.
Minimum/Maximum
appears when "Mass", "Volume" or "Pieces" is selected. The unit depends on the type of sample:
g, mL or pcs.
<F1>, "Help"
For a fixed or variable amount of sample you can have the titrator calculate
and enter values if you know the approximate water content of your sample.
Entry
of the amount of sample before or during the actual titration. "Entry" is faded out when "Fixed
mass", "Fixed volume" or "Fixed pieces" is selected.
DL38:
If you select "Yes" for the parameter "Auto start", on storage "Before" is automatically
set to "During".
5.2.4

Speed

Stirring should guarantee quick and thorough mixing of the electrolyte. We rocommend the setting: 40%.
The magnetic stirring rod should not "jump". Only use the magnetic stirring rod included in the delivery.
5.2.5

Mix time

This value for time is an empirical value and can be entered specific to the samples ("Request").
5.2.6

Titrant

You can select from the titrants stored in the Setup menu.

24

METTLER TOLEDO DL31/DL38

Methods (<Method> key)

5.2.7

Volume (for predispensing)

A predispensing shortens the titration time and can be entered specific to the sample ("Request").
Note
In the user and METTLER methods the parameter is called "Predis.".
5.2.8

Wait time (after predispensing)

The parameter does not appear in the KF standard method if you have entered "0" for the predispensing.
This parameter always appears in the user methods.
5.2.9
Yes

Auto start (DL38 only)


The DL38 begins analysis as soon as a sample has been added. The time for adding a sample
may not exceed 30 seconds or the instrument will revert to its "Standby" mode. You should
select "Yes" for determinations in which, e.g. side-reactions could occur during the titration.

5.2.10 Control parameters


The following holds for all control parameters: You should not modify the preset default values for the
different reagent types until you have evaluated the titration curve of your sample (see Application brochure).
1 component

2 components

Pyridine

Current

20 A

20 A

20 A

End point

100 mV

100 mV

100 mV

Vmin

0.5 L

0.5 L

0.5 L

Vmax

4.0 L

8.0 L

3.0 L

Vmax factor

100%

30%

100%

Note

Vmin and Vmax depend on the burette volume; the values listed apply to the 5 mL burette.

In the Tutorial and KF standard method these default values are automatically entered for the selected titrant
and hence the type. This does not apply to user methods: When you select a titrant whose type differs from
the previous one, you should also adapt the control parameters.
Current
Select 1, 2, 5, 10, 15, 20, 30 or 40 A for polarization current.
5.2.11 Termination parameters
To terminate the titration you must define "Vmax" and "Drift stop" ("Delay" respectively) as a condition; the
maximum time is an additional termination condition. The titration is terminated when the first of the
selected conditions is met.

METTLER TOLEDO DL31/DL38

25

Methods (<Method> key)

Vmax

The maximum volume is intended as a safety precaution: It avoids dispensing an unnecessarily


large amount of titrant if the titration is faulty.
Drift stop Select "Relative", "Absolute" or "No".
Relative Termination when actual drift is less than the drift measured before the titration (D0)
plus the entered value (Di): D < D0 + Di.
Absolute Termination when the drift is less than the entered value (Di): D < Di.
No
"Drift [g/min]" disappears and "Delay [s]" appears.
Delay
If you enter "0" for the delay time, the titration is terminated as soon as the end point is reached.
5.2.12 Blank
For the entry of a correct value, you should perform a determination.
[g]
You can enter a value in the method.
Request Before each titration, the value is requested individually for each sample.
5.2.13 Drift
The drift value is needed for calculation of the result.
[g/min] You can enter a value in the method.
Request Before each titration, the value is requested individually for each sample.
Online
The moisture which enters the titration vessel is always measured, evaluated and displayed in
the standby mode.
Determin. Some standard operating procedures require insertion of the value of a drift determination. If
you have performed a drift determination, the result is stored under the <i> key and used in the
calculation.
5.2.14 Result (DL31 only)
The water content is calculated with the appropriate formula by selection of the unit:
[mg], [g], [%], [ppm], [mg/pc], [mg or g] and [% or ppm].
[mg or g], [% or ppm]
With the following limit values, the result is automatically set from one unit to the other:
mg

ppm

less than 0.1

99...

less than 0.1

999...

0.1..

greater than 100

0.1..

greater than 1000

5.2.15 Calculation (DL38 only)


Calculation 1
R1
Result of the first calculation. The water content is calculated with the appropriate formula by
selection of the unit: [mg], [g], [%], [ppm], [mg/pc], [g/kg], [mL], [min], [ppm]ext.extr.,
[ppm]ext.soln., [%]ext.extr., [%]ext.soln..

26

METTLER TOLEDO DL31/DL38

Methods (<Method> key)

[mL]
Titrant consumption up to the end point.
[min]
Duration of the titration.
[ppm]ext.extr., [ppm]ext.soln., [%]ext.extr., [%]ext.soln.
Special calculation for samples which are used after an external extraction or external
dissolution. The second and third calculation are needed (see Application brochure).
Unit
You can enter a nonselectable unit, e.g. "g" if you define a factor of 0.001 for the calculation of
the H2O content in "mg".
Statistics To obtain the mean value "x", the standard deviation "s" and the relative standard deviation "srel"
of a sample series, you must select "Yes". You can terminate a sample series using the auxiliary
function "Results" (<Results> key).
Max. srel If the entered value for the max. relative standard deviation is exceeded, a message appears.
Calculation 2 / Calculation 3
The available parameters are the same as for Calculation 1. Instead of a formula, you can select "No calculation".
The following units are missing: [ppm]ext.extr, [%]ext.extr., [ppm]ext.soln, [%]ext.soln.
Note
You can not determine samples from an external extraction or dissolution in the routine mode
as you must enter the amount of sample for the extraction/dissolution and the amount of
solvent under calculation 2 and 3.
5.2.16 Standby
Yes
No
[min]

After a titration, the titration vessel is kept anhydrous. We recommend allowing the standby
titration to run even during lengthy pauses so that you can start the next titration at any time.
After a titration the start mask of the Analysis menu reappears.
After the sample determination, a switch is made to the "Standby" mode. The subsequent rate
of consumption is displayed and printed out during the defined time.

5.2.17 Report
Output
Type

Select "Printer", "Computer" or "Print.+Comp." as output device.


DL31:
Select "GLP", "Short-form" or "None".
DL38:
Select "GLP", "GLP+curves", "Short-form" or "None".
Curves can be printed out only on an EPSON or HP-compatible printer.
(GLP report: All data which are required by the rules of Good Laboratory Practice.)

5.2.18 Author of the method


The selection of your name documents that you are responsible for the development of the method.

METTLER TOLEDO DL31/DL38

27

Methods (<Method> key)

5.3

Storage procedures

The following always appears as the last parameter of a method:


Method

METHOD

Author
of the method
Help

Modify

OK

The modified method is stored when you confirm by pressing <F3>, "OK".
Examples:
DL31
DL38
Methods

METHOD

Methods

METHOD

123 CaCl2
KF standard method

4 H3PO4
31 Oil

Help

Delete Print Modify

Print Modify

If you have not entered any or a wrong method no., the following appears:
Error
No/invalid value
Min:
1.00000
Max:
899.000
OK

Confirm the error message by pressing <F3>, "OK".


Method

METHOD

No.
of the Method
Help

OK

Enter the new number and confirm by pressing <F3>, "OK". The method is stored.

28

METTLER TOLEDO DL31/DL38

Methods (<Method> key)

If you have entered a method No. which already exists, the following appears:
DL38
Method 22
METHOD
Method No. exists
Change number
Overwrite method
OK

Change number
Overwrite method

"No. of the method" reappears.


The new or modified method is stored, that with
the same number deleted.

While you are modifying a user or a METTLER method, you can press the <Run> key (the <Setup> and
Auxiliary functions keys are blocked).
a. If you have not yet modified any parameter of the method, the start mask of the Analysis menu appears.
b. If you have already modified a parameter of the method, the mask "Author of the method" appears. The
method is stored with "OK" and the start mask of the Analysis menu is displayed.

METTLER TOLEDO DL31/DL38

29

Methods (<Method> key)

5.4

User and METTLER methods (DL38 only)

The following methods have been developed by METTLER TOLEDO and can be performed immediately (see
Application brochure).
900
901
902
903

Standard 10
Na tartrate
Toluene dry
Ketone

904
905
906
907

Homogenizer
Ext. Extr.
KF Oven
Gas

908
909
910

Bromine No.
Blank Br No.
Stromboli

You can modify METTLER methods, but in this case you must always give them a number (1-899) so that
they are stored as user methods.
You can print out the selected methods by pressing <F2>, "Print".
User methods can be deleted (only in expert mode).
Methods

METHOD

22 Coffee
33 Tea
113 Powdered milk
Delete Print Modify

If you press <F1>, "Delete", the following appears:


Delete?

METHOD

Yes
No
OK

Yes Pressing <F3>, "OK", will delete the method.


No Pressing <F3>, "OK", will bring up the list of methods.
The method is not deleted.

METTLER methods cannot be deleted.


Methods

METHOD

900 Standard 10
901 Na tartrate
902 Toluene dry
Print Modify

30

METTLER TOLEDO DL31/DL38

Methods (<Method> key)

5.4.1

METTLER methods "908 Bromine No." and "909 Blank Br No." (DL38 only)

If you wish to develop a bromine number determination to meet your requirements, you can modify
METTLER method 908 or 909 and store as user methods. The "909 Blank Br No." method's result serves
as blank value for the bromine determination.

No.
908
Title
Bromine No.
Sample parameters
ID
Request
Type
Mass
Minimum [g]
0.2000
Maximum [g]
0.4000
Entry
Before
Speed [%]
30
Mix time [s]
120
Titrant
Br-/BrO3Predisp. [mL] 0.0000
Wait time [s]
0
Control parameters
Current [A]
2
End point [mV]
150
Vmin [L]
1.0
Vmax [L]
20.0
Vmax factor [%] 100
Start
Normal
Termination param.
Max. time [s]
6000
Delay [s]
15
Vmax [mL]
20.000
Blank
Request

Type
Weight
Volume
Density
Min./Max.
Entry

Calculation 1
R1 =
x[Br No.]*f1
f1 =
1.0000
Unit
Decimal places
2
Statistics
Yes
Max. srel [%]
0.00
Calculation 2
mL
R2 =
x [mL]*f2
f2 =
1.0000
Unit
mL
Decimal places
3
Statistics
No
Max. srel [%]
0.00
Calculation 3
R3 = No calculation
f3 =
1.0000
Unit
Decimal places
2
Statistics
Yes
Max. srel [%]
0.00
Report
Output Print.+Comp.
Type
GLP
Author of the method

Select "Mass", "Fixed mass", "Volume" or "Fixed volume".


appears when "Fixed mass" is selected.
appears when "Fixed volume" is selected.
appears when "Volume" of "Fixed volume" is selected.
appear when "Mass" or "Volume" is selected. The unit depends
on the type of sample: [g] or [mL].
of the amount of sample before or during the actual titration.
"Entry" is faded out when "Fixed mass" or "Fixed volume" is
selected.

METTLER TOLEDO DL31/DL38

No.
909
Title
Blank Br No.
Sample parameters
ID
Request
Type
Fixed volume
Density [g/mL] 1.000
Volume [mL]
50
Speed [%]
30
Mix time [s]
120
Titrant
Br-/BrO3Predisp. [mL] 0.0000
Wait time [s]
0
Control parameters
Current [A]
2
End point [mV]
150
Vmin [L]
1.0
Vmax [L]
5.0
Vmax factor [%] 100
Start
Cautious
Termination param.
Max. time [s]
6000
Delay [s]
15
Vmax [mL]
10.000
Calculation 1
mmol
R1 =
x [mL]*f1
f1 =
0.0500
Unit
mmol
Decimal places
4
Statistics
Yes
Max. srel [%]
0.00
Calculation 2
R2 = No calculation
f2 =
1.0000
Unit
Decimal places
2
Statistics
Yes
Max. srel [%]
0.00
Calculation 3
Report
Output Print.+Comp.
Type
GLP
Author of the method

31

Methods (<Method> key)

R1

Result of the first calculation. The bromine number or bromine index is calculated using the
appropriate formula by selection of [Br No.] or [Br index].
[mL]
Titrant consumption up to the end point.
[min]
Duration of the titration.
Bromine number and bromine index are quantities without dimension.
The bromine number is the amount of bromine in [g] reacting with 100 g of sample.
The bromine index is the amount of bromine in [mg] reacting with 100 g of sample.
"Author of the method" only appears if you change the method.

Unit

Author

5.4.2

METTLER method "910 Stromboli" (DL38 only)

If, according to your needs, you wish to develop an automated determination of water content of thermally
stable liquids or solids, then you can modify the METTLER method "910 Stromboli" and store it as a user
method.
No.
910
Title
Stromboli
Sample parameters
Type
Mass
Minimum [g]
0.0000
Maximum [g]
5.0000
Speed [%]
40
Mix time [s]
300
Set temperature 150
Titrant
1-comp 5
Control parameters
Current [A]
5
End point [mV]
100
Vmin [L]
0.5
Vmax [L]
4.0
Vmax factor [%] 100
Start
Cautious

Sample parameter
Mix time
Auto start
Set temperature

32

Termination param.
Max. time [s]
600
Driftstop
Rel.
Drift [g/min]
10
Vmax [mL]
10.000
Blank
Auto
Drift
Auto
Calculation 1
ppm
R1 =
x [ppm]*f1
f1 =
1.0000
Unit
ppm
Decimal places
3
Statistics
Yes
Max. srel [%]
0.00
Calculation 2
Calculation 3
Report
Output Print.+Comp.
Type
GLP
Author of the method

The sample parameters "ID" and "Enter" are not applicable, because the sequence
of the sample series is controlled automatically.
The time (in seconds) during which the water in the sample evaporates completely
and dissolves into the solvent in the titration vessel.
This parameter does not apply because the sequence of the sample series is
controlled automatically.
Enter in C at the desired temperature at which the water determinations are to be
performed. The set temperature can be selected between 50 C to 300 C. This
setting cannot be changed during a series. The set temperature is noted in the
titration protocol.
METTLER TOLEDO DL31/DL38

Methods (<Method> key)

Blank

Drift

Standby
Protocol
Author

The blank [g] is made up of the water content of the purge gas (time-dependent) and the
water content of the sample vessel (independent of time). The determination is performed as
a "normal" sample determination with the defined method parameters and, therefore, can be
integrated into the series sequence. The product of drift and duration (Drift * Duration) is
subtracted from the result, so that the blank is an absolute value independent of time. The
blank for the Stromboli can be viewed at any time by pressing the <i> key.
Request
The value is retrieved prior to the series.
Auto
The value is determined automatically prior to the sample series ("Blank"
position on the sample rack). The result is stored under the <i> key
and automatically integrated into the calculations.
Determination The most recently stored value is used.
Note
A one-time blank determination can be used for various sample series. In order
to do this, a method with the method parameter "Blank: Auto" is developed. In
the request for the sample parameters enter "0" for the number of samples. The
resulting blank value is stored and can be viewed at any time by pressing the
<i> key, i.e., it is available for all ensuing sample series.
The drift [g/min] can be determined at any time in the STANDBY mode (press <F1>, "Drift")
or automatically prior to a sample series.
Request
The value is retrieved prior to the series.
Auto
The value is determined automatically prior to the sample series ("Drift"
position on the sample rack). The result is stored under the <i> key
and automatically integrated into the calculations.
Determination The most recently stored value is used.
This parameter does not apply as no post consumption measurements are performed.
The results are printed out at the end of a series.
"Author of the method" only appears if you change the method.

At the beginning of a sample series, the following parameters need to be entered, provided you chose
"Request" in the method:
Mix time [s]
Blank [g]
Drift [g/min]
ID [Text]
No. of samples [max. 13]
Sample parameters (mass, volume, amount, etc.)

METTLER TOLEDO DL31/DL38

33

Analysis (<Run> key)

Analysis (<Run> key)

You perform titrations with a selected method. The required data are stored in the Method and Setup menu.
You prepare your sample, titrate and obtain the result.
While an analysis is running, all menus and auxiliary functions are blocked.

6.1

Starting a method

Preparations
Press the <Burette> key. Rinse the burette and fill ensuring that there are no air bubbles in the burette and
tubing.
Press the <Pump> key and fill the titration vessel with approx. 40 mL solvent.
When you press the <Run> key, the start mask appears:
DL31
DL38
Start
Method
Title
User
Help

RUN
No.

22

OK

Start
Method No.
Title
User
Help Modify

RUN
22

OK

As method number
"0" is entered if no method (DL31) or no user method (DL38) is stored.
in the DL31 case always that of the stored method is automatically entered together with the title.
in the DL38 case the number which you enter directly or accept it with <F2> from the METTLER or user
methods is entered.
Note
You can select the user name. The name which was selected in the analysis last performed remains
stored.
If you have defined an expiry date for the titrant and this has been passed, an appropriate message
appears before the pretitration starts. You should then first perform a concentration determination.
DL38: The start mask always shows the number of the method with which an analysis was last performed, e.g. Method No. 22. If you delete this, "Method not available" appears when you confirm the
mask with "OK".

34

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

Start
Data

6.1.1

RUN
transfer..

The titrator also accepts methods which are stored in the attached
computer: When you enter a number whose method is not stored in
the titrator, the method is requested from the computer (see Description of the computer interface). If it is available, the pretitration is
started immediately following transfer; if it is not available, "Method
not available" appears.

Menu sequence up to standby mode (KF methods)

Example:
Start

RUN

Method No.
22
Title
Coffee
User
C. De Car
H e l p M o d i f y OK

PRETITRATION

RUN

DL31: "Modify", is missing.


The pretitration starts with <F3>, "OK": It is always executed with the
control parameters of the selected method. The length of the solid bar
reflects the addition of the titrant. The vertical bar represents the threshold for the transition to the standby mode.

Help

STANDBY

RUN

Active
method:22
Potential
[mV]74
Drift g/min]
[
2
D R I F T CONZ Sample

This arrow indicates that you can start a determination.


Wait, drift still decreasing!
Wait, drift increasing again!

Press <F1> to start the drift determination,


<F2> to start the concentration determination,
<F3> to start the sample determination.
Note If the pretitration lasts longer that 10 minutes, a message appears. After confirmation with "OK", a
pretitration again starts. In such a case, you should check whether, e.g. all connections of the
titration stand are tight.

METTLER TOLEDO DL31/DL38

35

Analysis (<Run> key)

6.1.2

Standby mode

During standby, the following menus are blocked or selectable:


Blocked
<Setup>, <Burette>, <Pump> and under the <i> key: "Hello!", "KF learn titration" and "Hardware
tests".
Selectable <Stirrer>, <Results>, <Method>, <Run> and <i> key (except "Hello!", "KF learn titration" and
"Hardware tests").
Note
If you press the <Run> key, the sample determination is started!
To switch to the Analysis menu from the selected menu/selected auxiliary function, press the <Run> key.
Stirrer (<Stirrer> key)
You can change the speed. This is reported for the subsequent sample determination.
Results (<Results> key)
The menu is not shown until you have performed the first measurement or a result is available.
Method (<Method> key)
You can modify all methods. With the active method you can not modify the following parameters:
Titrant
Polarization current
End point
The modified parameters are adopted for the next sample. For documentation conforming with GLP, you
should print out the method before you switch back to the Analysis menu.
Note (DL38 only) If you modify the parameters of the active method, a sample series will be terminated.
If you restart a method, the results of the current series are deleted.

36

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

6.2

Sample determination

With <F3>, "OK", or <Run> you start a sample determination. According to th selected method, the following
masks may appear.
In succession, specific parameters are requested if defined in the method as "Request".
Example:
ANALYSIS
Mix

time

RUN
[s]

10

OK

Then one of the follwing mask appears:


ANALYSIS
RUN
H 2 O exp. [%] 2 . 0 0
Weight
[g]
0
Minimum [g] 0 . 3 7 5 0
Maximum [g] 0 . 8 7 5 0
H e l p B a l . * OK

The mask for the sample entry appears if a variable


amount of sample is defined with "Entry: Before".

ANALYSIS
Please
0.3750
Help

RUN

add sample
g 0.8750 g
OK

The mask for sample addition appears if a variable


amount of sample is defined with "Entry: During"
(example: mass).

Note
If you take longer than 5 minutes for the entry of samples or sample-specific parameters, the titrator
switches back to the standby mode.
If you add a sample while the titrator is in the standby mode without first pressing the <Run> key, the
titrator will begin a pretitration to titrate all the water in the sample. Immediately pressing the <Reset> key
and thereafter pressing the <Shift> and <Run> keys simultaneously can prevent this. By doing this, the
pretitration and standby mode is skipped and one of the above masks appears. In this manner your
sample is not "lost".

METTLER TOLEDO DL31/DL38

37

Analysis (<Run> key)

Sequence of the sample determination


Example (with "Entry: Before"):
ANALYSIS
RUN
H 2 O exp. [%] 2 . 0 0
Weight
[g]
0
Minimum [g] 0 . 3 7 5 0
Maximum [g] 0 . 8 7 5 0
H e l p B a l . * OK

The values for the expected water content and the limits for the weight are
adopted from the defined sample parameters of the method. The limits are
recalculated if you change the value for "H2O exp.".
*

Appears only if a balance is defined.

ANALYSIS
RUN
Add sample or
confirm
addition
0.3750 g 0.8750
Help
OK

If you have entered the weight value or have it transferred from a balance,
the mask shown appears.

Pressing <F3>, "OK", confirms addition of the sample and starts the analysis.

ANALYSIS

RUN

In the graph, the bar fills and empties in accordance with the drift. The
vertical bar represents the end point of the titration.
** Appears only if you have not yet entered the amount of sample. With <F1>, "Sample", the parameter

Sample** D r i f t

"Weight [g]" is displayed to enter the value.

During the titration you can switch between three different displays:
ANALYSIS

RUN

ANALYSIS

RUN

Drift:
Content:
9500 g/min 42.0012 mg

ANALYSIS

RUN

Consumpn: 1.2010 mL
D u r a t i o n : 0:31 mi

Sample C o n t . G r a p h SampleConsum G r a p h Sample D r i f t G r a p h

38

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

The titration is ended in accordance with the defined termination parameters. In the background the titrator
switches to the standby mode or the start mask. If you have not yet entered the amount of sample, the
parameter "Weight [g]" appears.
Report

RUN

The result is reported before it is displayed.

Printing...

Result
Method 22
Sample 1
R1 = 1.98%

RUN

DL31: R = 1.98%
OK

If you confirm "OK", either


the standby mask (method parameter "Standby: Yes") appears or
the start mask (method parameter "Standby: No"), or
the post consumption mask (method parameter "Standby: [min]").
The result is now stored under the auxiliary function "Results" (<Results> key) so that you can, e.g.
recalculate it.
Note If, after the sample addition, the elapsing mixing time is shown and no amount of sample has been
entered, you can also press <F1>, "Sample", to enter the amount of sample.

METTLER TOLEDO DL31/DL38

39

Analysis (<Run> key)

6.2.1

Weight transfer from a balance

ANALYSIS
>

1.3245

If you press <F2>, "Balance", in the corresponding mask, the value


displayed on the balance appears. It is transferred with <F3>, "OK".

RUN
g

OK

6.2.2

Post consumption
If you have selected "Standby [min]" in the method, the subsequent
measurement of the drift is performed directly after the sample determination and a drift value automatically printed out every minute (not on
HP-compatible printers).

STANDBY
RUN
Post
consumption:
D u r a t i o n :0:34 min
Drift:
6 g/min
Stop

6.2.3

Calculations

DL31 (without Auto start) / DL38 ("Auto start: No")


If you press <F3>, "SAMPLE", or the <Run> key in the standby mode, measurement of the time needed for
calculation of the drift compensation starts. It is stopped as soon as the titration is at an end.
Sample
addition
Confirm Sample

Requests

Mix time

Predisp.

Wait time

Titration

Measured value acquisition


Standby

Time measuremnet (duration)

DL38 ("Auto start: Yes")


In the case of an automatic start of the titration, the titrator does not start the time measurement until you
have entered the sample.
Sample
addition
Confirm Sample

Requests

Mix time

Predisp.

Wait time

Titration

Measured value acquisition


Standby

40

Time measuremnet (duration)

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

Calculation formulae
H2O [mg]

= (consumption [mL] * CONC [mg/mL]) ((drift [g/min] * duration [min]) + blank [g]) * 10-3 [mg/g]

Note

H2O [%]

For the H2O content in g, the formula is multiplied by 1000.

H2O [mg] * 0.1 [% * g/mg]


weight [g]

Note

H2O [mg/pc.] =

For the H2O content in ppm, the formula is multiplied by 10000,


for the H2O content in g/kg by 10.

H2O [mg]
number [pc.]

These parameters are listed on every GLP report to allow you to check the result using the formula.
6.2.4

Sample series with statistics (DL38 only)

If you have selected "Statistics: Yes" in the method under Calculation 1, 2 or 3, results and statistical data
of the sample or concentration determinations are stored under the auxiliary function <Results>.
The series is terminated if you
enter the appropriate command,
switch off the titrator or an attached Stromboli,
modify the method parameters of the active method,
select another method.
A sample series is also terminated if you
select the concentration determination in the standby mode,
change the current titrant in the Setup menu after a Reset.
A conc. series is also terminated if you
select the sample determination in the standby mode,
change the KF standard during the determinations,
change the current standard in the Setup menu after a Reset.
The series is not terminated if you stop a determination with <Reset> and perform the next determination
with the same method.
Note You can perform a series with maximum 99 samples. The last 60 results are stored. (This is not the
case if operating a Stromboli!)

METTLER TOLEDO DL31/DL38

41

Analysis (<Run> key)

After, e.g. the third sample determination, the following appears:


Result
Method 22
Sample 3
R1 = 1.91 %

RUN

OK

<F1>

You can switch between the result and statistics displays.

Statistics
RUN
Method 22
R1 n = 3
x = 1.95 %
s = 0.021095 %
Result
OK

Note The mean value is calculated after two samples, the absolute and relative standard deviation after
three samples.

6.3

Concentration determination

For the correct determination of the water content of a sample, you should determine the concentration of
the titrant with Karl Fischer standards (see Application brochure).
The concentration is always determined with the control and termination parameters of the active method.
A predispensing and wait time defined in the method are not performed, a defined blank value is not
incorporated in the calculation and the selection of "Standby: No" is not taken into account. After a concentration
determination, a switch to the standby mode is always made to allow duplicate or multiple determinations.
Calculation formula

CONC [mg/mL]

H2O content [mg/g] * weight [g]


consumption [mL]

42

drift [g/min] * duration [min] * 10-3 [mg/g]


CONC "old" [mg/mL]

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

With <F2>, "CONC" appears:


CONC
RUN
KF
standard:
di-Na
tartrate

Help Modify

You can select one of the standards stored in the Setup menu with <F2>,
"Modify".

OK

CONC
RUN
di-Na
tartrate:
Batch
H2O
content 1 5 . 6 6 0
Unit
%
ABC
OK

A batch number defined in the Setup menu is entered here. If you change or
enter this for the first time, it will be adopted for the current concentration
determination.

CONC
Mix

RUN
time

[s]

10

Irrespective of the mixing time you have defined in the method, you can
enter this according to the standard.

OK

CONC
RUN
di-Na
tartrate:
Weight
[g]
0
Proposal
[g]
0.0500
Help

Bal.*

OK

This mask appears when "Entry: Before" is defined in the method. If


"Entry: During" is defined, the sample addition mask appears immediately.
*

Appears only if a balance is defined.

ANALYSIS
Please
0.0500
Help

RUN

add sample
g
(approx

The amount of sample suggested in the previous mask is displayed.


The further progress corresponds to that of the sample determination.

OK

METTLER TOLEDO DL31/DL38

43

Analysis (<Run> key)

DL31
Each result is entered in the parameter list of the titrant, in other words the second overwrites the first etc.
Result
Method 22
Sample 2
C o n c . = 4.9892

RUN

If you calculate the mean value of the results and then enter this in the list,
date and time are deleted; this means the shelf life date can not be checked.

mg/mL
OK

DL38
The first result is entered in the parameter list of the titrant and is overwritten by the calculated mean value
of two then three results etc..
Result
Method 22
Sample 2
C o n c . = 4.9892

mg/mL

OK

6.4

RUN

As in the sample determination, you can switch between the statistics and
result displays.

Blank determination

If you have dissolved a sample in a solvent with a H2O-content unknown to you, run an analysis with only
the solvent and without the sample. The obtained value can be entered as a blank befor each titration
("Request") or can be entered automatically ("Determination"). This blank value is included in the calculations.
The blank value of the METTLER method "910 Stromboli" is stored under the <i> key.

6.5

Drift determination

You must determine the drift when a value is required for the calculation of the water content which has been
obtained by a titration. With <F1>, "DRIFT", appears:
DRIFT

RUN

The length of the solid bar represents the elapsed time.


D u r a t i o n :4:24
Help

min

After 5 minutes, the result is reported and displayed. At the same time, the value is stored under the <i> key.

44

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

6.6

Bromine number determination (DL38 only)

The course of the determinations corresponds to the sample determination of a KF titration. This also applies
to the performance of a sample series.
Start

RUN

If method parameters are defined with "Request", they are displayed before
the sample entry mask appears (example "Type: Mass" and "Entry: Before").

Methode No.
123
T i t l e Bromine
No
User
R. Hube
H e l p M o d i f y OK

ANALYSIS

RUN

Weight
[g]
0
Minimum [g] 0 . 2 0 0 0
Maximum [g] 0 . 4 0 0 0
H e l p B a l . * OK

ANALYSIS

Appears only if a balance is defined.

RUN

Consump:
2.3450
mL

When you have confirmed the sample addition, the titration starts.

Sample**

** Appears only if you have not yet entered the amount of sample. With <F1>, "Sample", the parameter
"Weight [g]" is displayed to enter the value.

Result
Method 123
Sample 2
Bromine No.=

RUN

After the end of the titration, the result is reported before it is displayed.
If you confirm "OK", the start mask reappears.

OK

Calculation formula

Bromine No. [g bromine/100 g sample] =

Note

Molar mass Br2:

METTLER TOLEDO DL31/DL38

(consumption [mL] * CONC [mmol/mL] blank [mmol]) * 100 * 0.1598 [g/mmol]


weight [g]

159.8 [g/mol] = 0.1598 [g/mmol]

45

Analysis (<Run> key)

6.7

Sample determination with the oven sample changer Stromboli (DL38 only)

The oven sample changer Stromboli is used in combination with the DL38 titrator to automatically determine the water content of thermally stable liquids and solids. For this purpose, the sample is heated in the
oven and the evaporated water is transported into the titration vessel by means of a dry inert gas stream.
The DL38 controls all of Strombolis functions via the METTLER Method "910 Stromboli". Using this method
as point of departure, user methods can be developed allowing automatic determination of sample series
with up to 13 samples as well as drift and blank determinations. Prior to determination, Stromboli automatically inserts the sample vials on the sample rack into the oven.
The result of a sample determination with Stromboli is made up of the samples water content, blank value
(water content of an empty sample vial) and drift (sum of the water content of the rinsing vessel over the
measuring time "Duration").
The drift determination is automatically performed if "Drift: Auto" was selected in the method. Drift can be
determined manually at any time in the standby mode (press <F1>, "Drift"). In both cases the determination is performed with the sample vial in the "Drift" position. The vial is inserted into the oven and the
determination is performed for three minutes after the set temperature entered in the method has been
reached. The result is stored (i.e., it is available for subsequent sample series) and can be viewed by
pressing the <i> key (including date and time of determination).
The blank determination is automatically performed if "Blank: Auto" was selected in the method. The determination is performed with the sample vial in the "Blank" position (empty sample vial). The determination
is performed as a "normal" sample determination with the defined method parameters and, therefore, can
be integrated into the series sequence. The blank value is defined as sample "0" without any content
parameters and the default parameter "ID: Blank". The result of the blank determination is stored and can be
seen under sample number "0" in the titration report or viewed by pressing the <i> key (including date and
time of determination).
Sequence of a sample series
When starting a method from the idle state, the entered, desired temperature is conveyed to the oven. The
sample vial in position "Drift" is inserted into the oven and the oven heats to the set temperature during
pretitration, i.e., in the standby mode. The temperature display flashes on the Stromboli and the display
alternates between current temperature and set temperature. After reaching a constant drift at the set temperature, the sample series can be started from the standby mode by pressing <Run> or <F3>, "Sample".
ANALYSIS
#01 RUN
ID
Weight
[g]
0
Minimum [g] 0 . 0 0 0 0
Maximum [g] 5 . 0 0 0 0
B a l . * S t a r t OK

46

When starting a sample series the parameters are requested for which
"Request" has been selected in the method. The entries are stored by pressing
<F2>, "Start" and then the display for the next sample (#...) appears.
Pressing <F2>, "Start" begins the sample series even if not all of the sample
data have been entered. The analysis will only begin when the oven has
reached the set temperature. Until the set temperature has been reached
(approx. 1-2 min), the message "Waiting for Stromboli" appears.

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

No.ID
Status
0 Blank
Done
1
Active
2
Ready
3
Ready
M o d i f y OK

Sample 1
RUN
ID
Weight
[g]
0
Minimum [g] 0 . 0 0 0 0
Maximum [g] 5 . 0 0 0 0
H e l p B a l . * OK
*

By pressing <F1>, "Sample" during a series, the current status (ready,


active or done) of the samples is displayed. Pressing <F2> "Modify" allows you to alter or complete your entry. After each sample the result is
calculated and reported, and the sample series is continued without displaying the results. If a printer is installed, the result is printed out after each
sample.
At the end of a sample series the results of the final sample and the series
statistics (press <F1>, "x") are displayed. In standby mode, the results
and statistics can be viewed by pressing the <Results> key.

Appears only if a balance is defined.

Note
If the input of the sample specific parameters takes longer than 5 minutes, the titrator will return to
Standby mode. The inputs to this point will then be lost. With a sample series and a Stromboli method,
the sample data for the first sample can be entered and the analysis started. The sample data for the
remaining samples can be entered while sample 1 is being analyzed by pressing <F1>, "Sample".
If an analysis is terminated by the termination parameter "Max. time" even though the entire amount of
water has not been titrated yet, then the Strombolis sample rack returns to its basic position ("Drift"
position below the oven) and remains there even during pretitration of the next sample. The Stromboli
only moves on to the next sample after the DL38 has gone into standby mode.
In the following cases the sample series will be interrupted:
When one of the following messages appears: "Weight [g] 0", "No titration!", "Capacity exhausted!",
"No drift determination performed!", "Blank determination not yet performed!", "CONC determination due!".
When the calculated value for "srel" is above the value entered in the method.
In order to continue the series, the message on the display has to be confirmed by pressing <F3>, "OK",
on the titrator.
At the beginning of the next series, results and statistics of a series are automatically erased as soon as
the message "Series aborted!" is confirmed by pressing <F3>, "OK".
As soon as a Stromboli is attached to a DL38 and switched on, each titration is started automatically,
regardless of whether "Auto start" has been set to "Yes" or "No". The Stromboli must be switched off for
a KF method without Stromboli!

METTLER TOLEDO DL31/DL38

47

Analysis (<Run> key)

6.8

KF learn titration

If you are unsure what parameters should be entered for your sample, select the learn titration stored under
the <i> key. The titrator calculates the range for the amount of sample you need to enter as well as control
and termination parameters, stores these and prints them out after the titration.
The learn titration is blocked when an analysis or auxiliary function is running. The learn titration cannot be
used with a Stromboli.
If you confirm "KF learn titration" with "OK", the following appears:

Method

KF-L

No.
of the

55
method

Help

OK

If you enter a number under which a method is already stored, an appropriate message appears:
DL31: Although the method is overwritten, you should enter a different
number (documentation of the method!).
DL38: The method is stored as a new user method with a different number.

Method

55

Type
of the

KF-L

mass
sample

Modify

OK

Method

55

Calculation

Modify

KF-L
1

DL31:

Instead of "Calculation 1", "Result" appears.

OK

Start
KF-L
KF
learn
titrat
T i t r a n t 1-comp 5
Type
1 componen
User
V.
Mlle
H e l p M o d i f y OK

Correct selection of the titrant used is important: The control depends on


the titrant type!
The pretitration starts with <F3>, "OK".

STANDBY

KF-L

Active
method 55
Potential
[mV]87
Drift g/min]
[
2
Help
SAMPLE

48

Wait until the drift is completely stable before you confirm <F3>, "SAMPLE"!

METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

The masks for the entry of mixing time and sample ID appear before the amount of sample is requested.
Analysis
Weight

[g]

Help

Bal.*

KF-L
0

OK

Appears only if a balance is defined.

ANALYSIS
KF-L
Add sample or
confirm
addition
1.2345 g
Help

Appears if you have already entered the amount of sample.


Otherwise, "Please add sample" appears.

OK

Result

KF-L

R1 = 0.61% !
Calculated
parame
ters
are
stored
OK

After the end of the titration, the result and the "learned" parameters are
printed out before the result is displayed. The result is always marked
with an exclamation mark (!).

STANDBY

RUN

Active
method:55
Potential
[mV]87
Drift g/min]
[
2
D R I F T CONC. SAMPLE

The standby mask of the Analysis menu with the active method number
appears so that you can determine the next sample with the "learned" method.

The following parameters are calculated:


Minimum and maximum for the amount of sample to be entered,
Vmin, Vmax, and Vmax factor (control parameters),
Drift value (termination parameter).

METTLER TOLEDO DL31/DL38

49

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

With the aid of the Symbol keys you can execute functions which are independent of a titration method, but
which can support or expand it. While an analysis is running, all auxiliary functions are blocked; in standby
mode (KF titrations) you can activate only the functions of the <Stirrer> or <Results> key.

7.1

<Stirrer>

You can switch the stirrer on and off and change its speed. Start and stop the stirring with <F3>.
Stirrer
Speed

STIRRER

[%]

35

Start

The stirrer stirs at the defined rate.

Start
Stirrer
Speed

STIRRER

[%]

35

OK

7.2

To change the speed in the standby mode in KF titrations,


press the <Stirrer> key, change the speed and confirm with "OK": The
stirrer stirs at the new speed.
Press the <Run> key to return to the Analysis menu.

<Burette>

The following functions are possible under this menu.


Rinse
Rinse
tip
Dispense

Rinse
Start and stop the rinsing process with <F3>.
Burette

BURETTE

Rinse
(rate:
100%
Rinse
tip
Dispense: 0.010 m
Help Modify S t a r t

Rate

Start

With <F2> you can change the rate at which the burette should
be filled. For the two-component reagents we advise always setting 60%. They outgas easier than the one-component reagents.
The titrator delivers 1 burette volume. The piston of the burette
moves below the zero position to ensure that air bubbles "hidden"
in the stopcock are siphoned up and then expelled.

Always place the dispensing tubing in a waste beaker!

50

METTLER TOLEDO DL31/DL38

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

Rinse tip
Start

5% of the burette volume are delivered to eliminate any diffusion of solvent in the dispensing
tubing tip.
Note You should also place the dispensing tubing in a waste beaker during this operation to ensure the
titrated solvent is not "overtitrated".
Dispense
Start
You can dispense the displayed volume immediately. With <F3>, "Stop", you can stop the
dispensing.
<F2>
With <F2> this mask appears in which you can modify the dispensing parameters:
Burette

BURETTE

Volume [mL] 0 . 0 1 0
Burette
5 mL
Fill
rate
[%]100
Start

7.3

<Pump>

With the aid of the pump you can add solvent to the titration vessel and siphon it off.
Pump
PUMP
To empty, press <F3>
To fill, press <F3>
and press and h
blue pump butt
Start

You switch the pump on and off with <F3>.

Pump

PUMP

Emptying/filling...

Stir

Stop

While the pump is running, you can switch on the


stirrer with <F2>, "Stir".

Filling
Push the dispensing tubing up to the 60 mL mark of the titration vessel so that the solvent does not
splash during filling. The solvent starts to flow into the titration vessel as soon as a sufficiently high
vacuum which siphons up the solvent has built up in the titration vessel.
Add approx. 40 mL to the titration vessel (the platinum pins of the electrode must be immersed in the
solvent!), release the pump button and press <F3>.
Pull up the tubing.
Emptying
Push the suction tubing to the base of the titration vessel so that the solvent can be siphoned off.
Pull up the tubing when the pump is running as far as it will go, then press <F3>.

METTLER TOLED O DL31/DL38

51

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

Note
The pump switches off automatically when the pumping time defined in the Setup menu is reached.
Each pumping operation resets the solvent capacity to the value defined in the Setup menu. At the same
time, the value is stored under the <i> key.
In the case of the pump of the attached DV705 Titration Stand, you must press the lower arrow key
during emptying and the upper arrow key during siphoning up.

7.4

<Results>

The following functions are available in this menu:


All
results
Recalculation
Calculations
(DL38
only)
Statistics
(DL38
only)
Report
Statistics
series
(DL38

All results
Statistics
Report
Statistics series

only)

is accessible when one result is available.


are accessible when 2 results of a sample series are available.
is accessible when a drift determination has been performed or a result is available.
is accessible when the first result of a sample series is available.

In order to change, e.g. results of KF determinations in the standby mode,


press the <Results> key, change the result under "Recalculation" and confirm with "OK".
Press the <Run> key to switch back to the Analysis menu.
7.4.1

All results

You can view the results generated in the titration of a sample or sample series. You can also print out the
results. The data in the result memory are deleted when you switch off the titrator.
DL31: The results of the last 20 determinations are stored.
DL38: You can perform a sample series with 99 samples. The results of the last 60 samples remain
stored, in other words the results of sample 1 are eliminated when you start to titrate sample 61.
Statistical data of the last 60 samples are always calculated.
Note
As "Result" the sample whose determination was terminated with the error message "No titration!" is also
stored.
A result is also stored if you terminate a determination with <Reset>. The result is calculated with the
titrant volume consumed up to that time.

52

METTLER TOLEDO DL31/DL38

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

7.4.2

Recalculation

You can recalculate existing results by changing the following values for each sample:
in a KF sample determination: Drift, concentration, blank value and/or amount of sample.
in a KF conc. determination: Drift and/or amount of sample.
in a bromine number determination: Concentration, blank value and/or amount of sample.
R e c a l c u l n RESULTS
Method 11
Sample 1
R1 = 0.77%
Sample 2

M o d i f y OK

DL31:

R = 0.77%

R e c a l c u l n RESULTS
Sample 1
Drift g/min]
[
6
Conc.
[mg/mL]
4.9875
Blank g]
[
0
Undo
OK

If you change one of the values, you can nullify it with <F1>, "Undo". With
<F1>, "Undo", the changed values are always reset to the original values.

R e c a l c u l n RESULTS
Method 11
*Sample 1
R1 = 0.77%
Sample 2

M o d i f y OK

The sample with the changed result is marked by an asterisk (*).

Note
The values obtained in the determination always remain stored so that you can also nullify changes later.
Under "All results" you can print out the recalculated results. Here, the changed values and the original
are reported.
DL38: The changed results are also taken into account for the statistical data.
DL38: In KF conc. determinations the calculated result or its mean value is not entered in the parameter
list of the KF titrant if you change a value, e.g. after three determinations. However, if you perform a conc.
determination after this change, the recalculated result is taken into account in the statistics calculation.

METTLER TOLED O DL31/DL38

53

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

7.4.3

Report

At the end of every determination, you can print out an (additional) data report or send it to the computer.
Report

RESULTS

OutputPrint.+Comp
Type
GLP
Help Modify

OK

Note If you have changed the result of this last determination beforehand, it will be printed out marked
with an asterisk (*).
7.4.4

Calculations (DL38 only)

At the end of every titration you can perform additional calculations for this sample.
C a l c u l a t i oRESULTS
ns
R =
x [mg]*
f =
1.0000
Unit
mg
H e l p M o d i f y OK

7.4.5

With "OK" the result is displayed and can then be printed out.

Statistics (DL38 only)

If you have selected "Statistics: Yes" in the method under calculation 1, 2 or 3, in a series of 2 samples the
mean value will be calculated, in one comprising more that 2 samples the absolute and relative standard
deviation. You can print out these results here and change the statistical evaluation by eliminating outliers.
The DL38 does not incorporate results in the statistics which were obtained after a learn titration, a "Reset",
and the following messages:
No titration!,
End point not reached! Termination through Vmax,
CONC value not stored! Conc. range exceeded,
CONC value not stored! Termination through Vmax.

54

METTLER TOLEDO DL31/DL38

Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>)

Example of a statistical evaluation of 3 samples


Statistics
R ESULTS
Method 11
R1 n = 3
x = 0.77%
s = 0.102194 %
R e s u l tP r i n t OK

Using the result list (press <F1>) you decide what sample result is an
outlier and then delete it.

Statistics
R ESULTS
Method 11
Sample 1
R1 = 0.77%
Sample 2

Delete
OK

Statistics
R ESULTS
Method 11
R1 n = 2
x = 0.70 %
R e s u l tP r i n t

OK

If you delete "Sample 1" with <F1>, "Undo" is superimposed to allow


you nullify the command. At the same time, sample 1 is marked as
"deleted".
Confirm "OK" to show the following:
(Example: Sample 1 is deleted)

The statistical data are calculated with the changed number of samples.
You can delete several sample results and print out the result each time.

As long as the result list of this sample series is stored, you can nullify the deletion operation.
7.4.6

Statistics series (DL38 only)

With the aid of this function you can terminate a sample series. This deletes all data in the result memory,
a subsequent analysis with the same method restarts with "Sample 1".
S t a t . s e r i eRESULTS
s
End
series?
No
Yes
OK

METTLER TOLED O DL31/DL38

55

Information menu (<i> key)

Information menu (<i> key)

The measured values and menus below are stored under the <i> key:
Solv.
capac.[mL]
Drift g/min]
[
Blank g]
[
(DL38/Stromboli
KF
learn
titration
Hello!
(Tutorial)
Hardware
tests

only)

Solv. capac.

The solvent capacity defined in the Setup menu is entered as an initial value. After each
titration, the difference between the initial value and the amount of titrant consumed is
displayed. If "0" is reached or exceeded, an error message appears. As soon as you
switch on the pump, the value defined in the Setup menu is reentered.
In bromine number determinations, the solvent capacity is set to "0".
Drift
Here, the value of the drift determination last performed is stored and automatically adopted
for the drift compensation if you have defined "Drift: Determination" as a method parameter.
Blank
The value of the last blank determination perfomed is stored here and automatically adopted
for calculations (only for method with Stromboli).
KF learn titr.
The course of this titration is described in Section 6.
Hello!
As you get to know the titrator step by step, the procedure is not described.
Hardware tests The functions of this menu which you can use to test the hardware of the titrator are
described in Section 9.

56

METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

Error messages, malfunctions and hardware tests

9.1

Error messages from the titrator

Here, the error messages which refer to this section or are not self-explanatory are explained.
A
After the titrator has been switched on, the following errors can be displayed:
ERROR
RAM x test ERROR(Q) "x" represents a number
ERROR > HW version
ERROR > DCB
ERROR > application
No application found
The messages refer to a faulty hardware component.
Press any key: The titrator attempts to continue the start process; this may be successful, but does not
guarantee 100% functioning.
Measures
1. Note the displayed text.
2. Note the instrument number and software version of the titrator (shown on every report).
3. Please then inform METTLER TOLEDO service of these points and the attached peripheral units with the
defined configuration.
B.

If the following three displays appear, parts of the hardware may be faulty.

Internal
error:
xxxxxxxxxxxxxxxxxxxx
xxxxxxxxxxxxxxxxxxxx
xxxxxxxxxxxxxxxxxxxx
SYSTEM IS BLOCKED!
See
manual:
Error

OS ERROR: x
P1: xx
P2: xx
D1: xx
D2: xx
SYSTEM IS BLOCKED!
Please
call
METTL
TOLEDO
service

ERROR:

SYSTEM IS BLOCKED
Please call METTLER
TOLEDO service

"x": represents letters and/


or numbers.

Measures
1. Note the text or error (e.g. "ERROR: 1000") and the operation that triggered it.
2. Note the instrument number and software version of the titrator (shown on every report).
3. Then switch off the titrator.
4. Please inform METTLER TOLEDO service of these points and the attached peripheral units with the
defined configuration.

METTLER TOLEDO DL31/DL38

57

Error messages, malfunctions and hardware tests

C.

If the following warning appears, you should regard the executed action as failed and repeat it.

Warning:

"x": represents a numberl

Press any key


to continue

Measures
1. Press any key: The titrator can continue to function.
2. On no account consider the result of a determination terminated in this manner!
3. If the warning appears frequently, you should take the measures described under point B.
D. Faulty data deleted!
The titrator has stored only part of a method if, e.g. the power fails when the method is being stored. It
deletes this method completely. It is also possible that it has deleted several methods.
Measures
1. Confirm the message.
2. Check whether your methods have been deleted, if so reenter them.
The titrator has stored only parts of parameters of a resource if, e.g. the power failed during storage of the
parameters. All data stored in the Setup menu are deleted.
Measures
1. Confirm the message. The titrator now loads the default parameters of the Setup menu, in other words all
data stored on delivery of the titrator.
2. Switch the titrator off and on.
3. Check whether the default parameters are again available and reenter the names and values stored
before the failure.
If you receive this error message frequently, the battery is discharged! This must be changed by
METTLER TOLEDO service.
E.
Method not stored!
The titrator can no longer store a method if the user data memory is full.
Measure
1. Confirm the message.
2. Delete one or more methods from the memory or transfer to the computer.
3. Reenter the new method and save it.

58

METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

9.2

Other errors and malfunctions

The following collection of errors and malfunctions which are not reported by the titrator will help you to
rectify the fault yourself in many cases so that you do not have to rely on the METTLER TOLEDO service
(specified in the Table as "Service").
You can also first check some malfunctions with the hardware test (see Section 9.3) before you contact the
service.
Error

Possible cause

Rectification

No display on titrator

Instrument not attached


to power supply.

Attach to power supply, otherwise contact service.

Several points of the


display are missing

Contact service, see also Section 9.3.1.

The display and the


key do not match

Contact service, see also Section 9.3.1.

Transmission error to
attached peripheral device

Peripheral device faulty


or switched off.

Check attached devices for correct functioning,


see also Section 9.3.2.

Device (printer, balance,


computer) does not react

Instrument not switched on;


wrong settings and/or configuration
(switch settings wrong);
wrong cable.

Switch on instrument;
settings and configuration must match,
see Sections 4.5 and 9.3.2;
cable see Section 11.2.

Pump does not function

Suction tubing not connected,


titration stand leaks;
pump faulty.

Connect suction tubing and check connections,


see Section 10.3;
check pump, see Section 9.3.3.

TTL inputs or outputs


do not function

Inputs and/or outputs faulty.

Check inputs/outputs, see Section 9.3.3.

Burette and stopcock


do not move to zero
position on switching on

Burette drive faulty.

Contact service.

Magnetic stirring bar


does not rotate

Cable of magnetic stirrer not


plugged in properly;
wrong magnetic stirring bar.

Check magnetic stirrer, see also 9.3.3;


change magnetic stirrer;
use bar supplied, see Section 11.

Wrong potential values

Electrode faulty or contaminated.

Check electrode (see electrode specifications bulletin);


use new electrode.

No dispensing,
titrant expelled from
stopcock or piston

Burette tip blocked.

Clean burette tip.

METTLER TOLEDO DL31/DL38

59

Error messages, malfunctions and hardware tests

9.3

Hardware tests

The menu "Hardware tests" is stored under the <i> key and you can use to check whether, e.g. the stirrer
and pump of the titrator are functioning correctly. If you order the connector set for the interface check, you
can also test the interface and the TTL inputs and outputs (DL38 only) of the titrator.
9.3.1

User interface

Display test
5 displays appear in succession, 4 with different patterns, the last without a pattern. This allows you to
detect faulty pixels of the display. The test mode automatically switches off after approx. 20 seconds.
Keypad test
When you press a key, a numeric code assigned to this key appears which allows you to recognize a faulty key
(see following Table).
Press the <Esc> key to quit the test mode.
Key codes
Key ............ Code

Key ............. Code

Key ............. Code

Reset .......... 23

F1 ............... 17

3 ................. 3

i ................. 30

F2 ............... 18

4 ................. 4

Stirrer .......... 28

F3 ............... 19

5 ................. 5

Pump ......... 27

............... 11

6 ................. 6

Burette ........ 29

................ 12

7 ................. 7

Results ....... 26

Shift ............ 10

8 ................. 8

Setup .......... 25

0 ................ 0

9 ................. 9

Method ....... 24

1 ................ 1

Del .............. 31

Run ............ 21

2 ................ 2

. .................. 33

Beep tests
You test the internal beeper.
9.3.2

Peripheral interfaces

Interface test
Before the test
plug the test socket 51107288 into the balance, computer or GA42 interface.
plug the Centronics cable into the Centronics interface and the test plug 51107287 into the Centronics
socket of the cable.
After the test phase, either "Test successful" or "Test failed" appears.

60

METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

Balance test
The menu option is faded out if no balance is defined in the Setup menu.
The weight displayed on the balance must appear in the titrator display.
Printer test (GA42, EPSON or HP)
The appropriate printer must be attached. If the error message "Printer: No connection" appears, you can
quit this error message with <Esc>: With "OK", the titrator attempts to set up the connection to the printer
again.
The letters and characters available in the titrator must be printed out.
9.3.3

Inputs and outputs

TTL-I/O (DL38 only)


Before the test, plug test plug 51107723 into the TTL-I/O interface.
After the test phase, either "Test successful" or "Test failed" appears.
Internal stirrer
You test the rotational movement and change in the speed of the magnetic stirring bar.
External stirrer
You test the rotational movement and change in the speed of the magnetic stirring bar with the attached
DV705 Titration Stand.
Internal pump
You check whether the pump functions:
A "noise" must be heard.
It must be able to dispense and siphon off when solvent and waste bottle are correctly attached.
External pump
You check whether the pump of the attached DV705 Titration Stand functions (see "Internal pump").
Note For dispensing, you must always press the lower button ( arrow), for siphoning off the upper
button ( arrow).

METTLER TOLEDO DL31/DL38

61

Installation and maintenance

10

Installation and maintenance

10.1

Equipping the titration stand

On delivery, the titration vessel comprises O-ring, cover and threaded ring. The seal is fastened in the
titration stand. If you have to change the cover or replace the O-ring, the illustration will serve as an aid. The
titration arm can be turned in both directions.

Silicon tubing (133 mm)

Threaded ring with lug


Connector
Stopper ST 7.5
3-hole adapter
O-ring

1. Carefully slide the magnetic stirring bar supplied into


the titration vessel.
2. Insert the titration vessel with the lug of the threaded
ring into the middle groove of the titration arm and
push downward towards the stirrer. Fasten the screw.
3. Place the three-hole adapter, the ST stopper and the
connector in the cover openings.
4. Fill a drying tube with molecular sieves, close with
the cover and "push" into the titration stand to ensure tightness. Connect the cover and the connector
by silicon tubing.

Titration vessel

Cover and drying tube


Seal

Groove of
titration arm

Screw

Titration
stand

62

METTLER TOLEDO DL31/DL38

Installation and maintenance

10.2

Installing the burette

1. Screw the burette with holder onto the titrant bottle (see DV100x Operating Instructions).
Never inhale the vapors of Karl Fischer reagents and avoid skin contact. The reagents are
toxic.

2. Place the drying tube holder in the opening of the burette holder, fill a drying tube with molecular sieves
and position in the holder.
3. Push the burette onto the titrator: The slot of the driver cam and piston rod must be parallel to the insert.
(If this is not the case, press the <Reset> key.)
4. Turn arrestment knob in the opposite direction to the arrow and when pushing in check whether the
piston rod of the burette is correctly positioned in the push rod.
5. Turn the arresting knob in the direction of the arrow to fasten the burette.
6. Place the dispensing tubing in the cover opening.
When you rinse burette and tubing, place the dispensing tubing in a waste beaker;
do not dispense in the titration vessel!

Driver cam

Hole for dispensing tubing

Arrestment knob

Push rod of
the burette drive

METTLER TOLEDO DL31/DL38

63

Installation and maintenance

10.3

Installing the solvent and waste bottles


Screw sleeve
Socket
Screw cap
Gasket

Dispensing or
suction tubing

Adjusting sleeve
Teflon seal

Output
fitting

64

1. Open the solvent bottle, lay in the gasket and screw


on the screw cap (you may need an adapter, see
DV100x Operating Instructions).
2. Loosen the screw sleeve and slide over one of the
pump tubing. Push this dispensing tubing to the base
of the bottle and screw fasten the sleeve. (There is
an O-ring in the socket which ensures tightness.)
3. Push the other end of the dispensing tubing into the
opening on the left of the three-hole adapter and fasten with the adjusting sleeve.
4. Perform steps 1 and 2 with the waste bottle supplied. Push the suction tubing to just shortly beneath
the screw cap and fasten the sleeve.
5. Push the other end of the suction tubing into the
opening on the right of the three-hole adapter and
fasten with the adjustment sleeve so that you can
easily push the tubing to the base of the titration
vessel and pull it up again.
6. Fill two drying tubes with molecular sieve and place
them in the screw cap of the bottles.
7. Push the silicon tubing (450 mm) over the drying
tube cover of the waste bottle and connect to the
suction fitting of the pump.
8. You can connect the output fitting to tubing to lead
off the solvent vapor to a suitable place.

Suction
fitting

Check all drying tubes and screw fittings once again for
firm seating to assure the tightness of the system!

METTLER TOLEDO DL31/DL38

Installation and maintenance

10.4

Attaching the magnetic stirrer, electrode and devices

Balance (RS232C)
External stand (DV705)
GA42 printer (RS232C)

Computer (RS232C)
Stirrer output
Stromboli, TBox, etc. (TTL I/O)
Electrode input (KF)
EPSON- and HP-compatible printers
(Centronics)
Pump unit
On/Off switch
Suction fitting
Output fitting

Socket for
external power pack

Magnetic stirrer
On delivery, the magnetic stirrer is pushed into the slot for the
burette drive. Attach its cable to the stirrer output. The arrow on
the Mini-DIN connector must point towards the screw.

Magnetic stirrer

Make sure that every connector is in the correct position! Do not damage the connector
pins of the magnetic stirrer cable! Pins damaged by faulty insertion can cause a short
circuit at the "Stirrer" output. This renders the titrator non-functional.
Electrode
Unscrew the protective cover of the DM143-SC and connect the electrode to the triaxial cable. Plug the cable
into the KF input and insert the electrode in the corresponding cover opening of the titration vessel.
Balance, printer, computer, TBox DR42
Attach all peripheral devices to the same plug connector (phase) to which the titrator is connected!
Otherwise, equalizing currents could flow across the cables.
Attach the devices used to the corresponding connectors/sockets on the rear side of the titrator.
METTLER TOLEDO and SARTORIUS balances are compatible with these titrators.

METTLER TOLEDO DL31/DL38

65

Installation and maintenance

10.5

Using TTL inputs and outputs (DL38 only)

The TTL-I/O socket has two inputs and four outputs (In 1, In 2 and Out 1...Out 4). The outputs are occupied
by the titrator for commands.
If you have the METTLER TOLEDO oven sample changer Stromboli connected to the TTL I/O interface, no
further entries are necessary.
Inputs
A level change from "high" to "low" is detected at the inputs.
In 1
In the Run menu
the pretitration in KF titrations or the titration in bromine determinations is started,
the sample determination in KF titrations is started (always corresponds to the <F3> key),
the actual analysis is started (corresponds to confirming the sample addition),
the result display is confirmed.
In 2
corresponds to the <Reset> command on the keypad.
Outputs
At output 1 a pulse is given with a length of 100 200 ms. The other outputs assume either an active
("low") or inactive ("high") condition.
Out 1
outputs a pulse before the display of "Add sample" and before display of the result list.
Out 2
is inactive when an analysis can be started.
Out 3
is active in the case of an error message; the condition does not change until the message has
been confirmed with "OK".
Out 4
is active only during the mix time defined in the method.
For this condition, the connection of the TBox DR42 is suitable, it can be used to control an
homogenizer (see TBox Operating Instructions).

10.6

Maintenance and servicing

Cleaning
You can clean the titrator with a cloth moistened with alcohol.
To clean the titration vessel, turn the titration arm to the right and unscrew the vessel from the cover.
To clean the cover, loosen the fastener screw, take the titration vessel with cover up and out and unscrew
cover.
You should clean the electrode when their response time deteriorates owing to certain Karl Fischer
reagents and samples (the end point drifts!): Either place in an ultrasound bath with deionized water for
a few minutes or for 60 seconds in a chromic acid bath and then rinse with water or ethanol.

66

METTLER TOLEDO DL31/DL38

Installation and maintenance

O-rings
You should replace the O-rings of the screw caps when the system is no longer tight:
Loosen the screw sleeve, take out the pump tubing and remove the O-ring using tweezers (see also
illustration in Section 10.3).
You should replace the O-ring of the threaded ring for the same reason:
Loosen the fastener screw of the titration vessel, take titration vessel with cover up and out and unscrew
(see illustration in Section 10.1).
Dispensing and suction tubing
You should replace the pump tubing when the Teflon seal is no longer properly tight (wear and tear).
Molecular sieve
If the drift of the KF solution remains too high, you should fill the drying tubes with fresh molecular sieve.
You can regenerate molecular sieve in a drying oven at 160 300 C for at least 24 hours. As the molecular
sieve used on the waste bottle also contains SO2, you should rinse it with deionized water before regeneration.
Pump unit
If the diaphragm pump no longer functions, you can replace it:
Pull out the pump unit and insert a new one.
Pump button
If the pump button becomes too brittle, you should replace it:
Remove the button and place a new one over the ring.
Magnetic stirrer
If the magnetic stirrer is faulty, you can replace it:
Swing out the titration arm and push the motor out of the burette slot.
Push in the new magnetic stirrer and attach its cable to the stirrer output.
Battery
The battery installed in the titrator has a service life of approx. 5 years. The battery may be changed only by
METTLER TOLEDO service.
Disposal
Contact your METTLER TOLEDO dealer if you have to dispose of the titrator.

METTLER TOLEDO DL31/DL38

67

Standard and optional equipment

11

Standard and optional equipment

11.1

Standard equipment

1 KF titrator
1 Set Operating Instructions (DL31/DL38)
1 Application brochure
1 Memo card
1 CD Software LabX light
1 Set Operating Instructions (LabX light)
1 Keypad cover

according to order
according to order
according to order
according to order
according to order
according to order

You can order each part listed with an order number from METTLER TOLEDO.
Note

The standard and optional equipment for the 5 mL burette are listed in the Operating Instructions
for the interchangeable burrettes enlosed in the burette package.

4 drying tubes with cover

1 dispensing tubing with Teflon seal


1 suction tubing with Teflon seal
1 silicon tubing
1 connector

1 drying tube holder


1 seal
A 5 mL interchangeable burette
incl. 1 L brown glass bottle
1 titration vessel with cover incl.
one 3-hole adapter with stoppers
1 pump button

1 stopper ST 7.5

2 screw caps with flat seal


1 siphoning tubing

One 1 L brown glass bottle


1 magnetic stirring bar
1 magnetic stirrer

68

1 double platinum pin electrode DM143-SC


incl. 1 electrode cable (SC-LEMO-60)

METTLER TOLEDO DL31/DL38

Standard and optional equipment

Threaded ring
51107459
Cover
51107462
with:
3-hole adapter
23982
(with 1 ST 10, ST 7.5 and 1 needle
hole stopper)
Stopper ST 7.5
23452
(set of 5)
Connector
23957
O-Ring
51190366
Titration vessel
51107463
(nominal volume: 250 mL)

1-L brown glass bottle


71296

Gasket
(min. order quantity: set of 5)
23981

Screw cap
23937

Fastener screw
(for titration vessel)
51107474

Pump tubing
(suction/dispensing tubing)
51107481

Magnetic stirring rod


51191159

Silicon tubing 450 mm


(suction tubing)
51107490

Magnetic stirrer
51108750

Pump unit
51107479

Silicon tubing 133 mm


51107480

Pump button
51107600

Drying tube holder


23915

Double platinum pin electrode


DM143-SC
51107699

Drying tube with cover


23961

Triaxial cable SC-LEMO-60


(length: 60 cm)
89601

Seal
(drying tube of titration stand)
51107492

Molecular sieve
1 Bottle
71478

METTLER TOLEDO DL31/DL38

69

Standard and optional equipment

External power pack


51107777

11.2

Connection cable for computers


DTE 9-pin, female
51190362

Optional equipment
Drying oven
DO307

Oven sample changer Stromboli


with DL38 only
Stromboli

O-ring (for screw caps)


(set of 4)
51107496

connection cable for Stromboli


(DL38 only)
51190589

Thermostatable beaker
51107497

Gas inlet for operation of a DL38


with a Stromboli
105091

Stoppers for three-hole adapter


(1 set) (1 ST 10, 1 ST 7.5,
6 needle hole stoppers)
25883

Weighing boat (set of 5)


Glass, 20 x 60
Glass, 30 x 80
PE, 25 x 65
PE, 38 x 100

Connector set
(for interface check)
51107790

Homogenizer adapter set 12


(for Kinematica)
51107534

Septum stoppers (set of 10)


ST 10
23949
ST 24
23950

Homogenizer adapter set 18


(for IKA)
51107409

External stand
DV705

Visco Spoon
51107668

POWER

TEMPERAT
URE

C
HEATING

120 140 160


180
100
200
80
220
60
240
40
260
OFF

70

280
300

23951
23952
23953
23954

METTLER TOLEDO DL31/DL38

Standard and optional equipment

Connection cable for


METTLER TOLEDO balances
AB, AX, PB, PG-S (RS9 interface)
11101051

Triaxial cable SC-LEMO-100


(length: 100 cm)
89602

Connection cable for


METTLER TOLEDO balances
AE with the Option 011
59759

Connection cable for


METTLER TOLEDO balances
AM, PM, AT
229029

Connection cable for


SARTORIUS balances
51190363

Connection cable for


METTLER TOLEDO balances
AG, AB, PB, PG (LC interface)
229065

Connection cable for


GA42 printer
51190362

17.3
19.3 75 g
8.00 19 g
7.77 3 g
6.55 3
10.5 4 g g
8.09 06 g
5.87 7 g
3.20 6 g
1.09 5 g
8g

GA42

Prin

METTLER
TOLEDO

Printer
GA42

ter

Olivetti Artjet printer


EU version
US version

Connection cable for computers


DTE 9-pin, female
51190362
DTE 25-pin, female
51107781

TBox DR42 (control of


external devices via TTL I/O)
DR42

OU
T
OU 1
T
OU 2
T
OU 3
T
IN 4
1
IN
2
ON

Connection cable for


EPSON-/HP-compatible printers
(i.e. Olivetti Artjet)
51107780

OUT 1

OUT 2

24 VDC 1.2 A

OUT 3
100-240 V
50/60 Hz
unfused
max. 9 A

51190985
51190986

OUT 4

TBox DR42

Syringes (package of 100)


1 mL
71492
10 mL
71482

Connection cable for TBox DR42


51190589

Injection needles (package of 12)


80 x 1.2 mm
71483
80 x 0.8 mm
71484

Keypad cover
(3 pieces)
51107666

1 mL

80 x

1.2

Software LabX professional


incl. Operating Instructions
German
51106302
English
51106300

METTLER TOLEDO DL31/DL38

Software LabX multi


incl. Operating Instructions
German
51106312
English
51106310

71

Standard and optional equipment

Bedienungsanleitung

KF-Titratoren

DL31 / DL38

Die 4 wichtigsten Schritte


Setup

Das Coulometer mit den entsprechenden Hilfsmitteln einrichten.

Method

Eine Methode whlen und nach Bedarf


ndern.

Hauptmethoden (nur DL39)


Peripherie
Einstellungen

Die KF-Standardmethode
Nr. der Methode

Drehzahl [%]

40

Mischzeit [s]

10

Autostart

Regelparameter
Pol.-Strom [A]
2
Endpunkt [mV]
100
Erz.-rate
Normal

911
912
913
914
915

Standard 1.0
Stromboli
Ext.Extr.
Br Index
Br Blank

KF-Standardmethode

Nein

Blindwert [g]

Online

Autor
Analyse mit der gewhlten Methode
star-der Methode
Resultat
ten, indem Sie <Run> oder <F3>, ProBerechnung 1
ppm
be, drcken.
R1 =
x [ppm]*f1
f1 =
1.0000
Abfragen beantworten.
Einheit
ppm
Probe zugeben. (DL39: Falls Autostart:
Dezimalstellen
2
Statistik
Ja
Ja gewhlt wurde, beginnt die Titration
Max. srel [%]
0.00
automatisch bereits nach Zugabe der
Berechnung 2
Probe.)
R2 =
Keine Berech.
<Run> oder <F3>, Start, drcken, um
f2 =
1.0000
die Analyse zu starten. (DL39: Falls
Einheit
Autostart: Ja gewhlt wurde, entfllt
Dezimalstellen
2
Statistik
Ja
dieser Schritt.)
Max. srel [%]

Results

Resultatliste von analysierten Proben


anschauen, Nachberechnungen durchfhren, die statistische Auswertung einer Serie ndern (nur DL39!) sowie zustzliche Protokolle ausdrucken.

0.00

Berechnung 3
R3 =
Keine Berech.
f3 =
1.0000
Einheit
Dezimalstellen
2
Statistik
Ja
Max. srel [%]
0.00
Standby

Ja

Protokoll
Ausgabe Druck.+Comp.
Typ
GLP

72

nur DL39

Abbruchparameter
Max. Zeit [s]
600
Driftstopp
Rel.
Drift [g/min]
5
Drift

Run

Titel der Methode


Probenparameter
ID
Art
Masse
Minimum [g]
0.0000
Maximum [g]
5.0000
Eingabe
Vorher

Benutzermethoden (nur DL39)


METTLER-Methoden (nur DL39)

nur DL32

nur DL39

Operating Instructions
German
English
French
Spanish
Italian

51709849
51709850
51709851
51709852
51709853

Memo card
German
English
French
Spanish
Italian

51710187
51710188
51710189
51710190
51710191

Application brochure DL31/DL38


German
51709854
English
51709855
French
51709856
Spanish
51709857
Italian
51709858
Operating Instructions

METTLER TOLEDO

DL31/DL38: Description of the Computer Interface

Description of the computer interface


German
51709875
English
51709876

METTLER TOLEDO DL31/DL38

Technical data

12

Technical data

Power supply
Voltages
Frequency
Power consumption
Voltage

100 240 VAC 10%


50/60 Hz
45 VA
24 VDC 0.8 A / 5 VDC 1.2 A

Dimensions
Width
Depth
Height
Weight

240 mm
305 mm
370 mm
Approx. 5 kg

Materials
Titrator housing
Titration stand
Keypad housing
Membrane keypad
Dispensing/suction tubing
Siphoning/connection tubing
Three-hole adapter
O-ring (screw cap)
O-ring (threaded ring)
Ring seal (bottle)
Seal (dispensing/suction tubing)
Connector

Polypropylene
Polypropylene
Polyester
Polyester
FEP
Silicon
Polypropylene
EPDM
FEP/silicon
PTFE/silicon
PTFE
Polypropylene

Ambient conditions
Ambient temperature
Atmospheric humidity
Use
Overvoltage category
Pollution degree

+5 C to +40 C
Max. 80% at 40 C
Indoors
II
2

METTLER TOLEDO DL31/DL38

73

Technical data

Measurement principle
Volumetric water content determination following Karl Fischer
End point indication
Voltametric: voltage measurement at a polarized
double platinum pin electrode
Measurement range
Several ppm to 100% water
Measurement system
KF input
Current source
Pol. current
Resolution
Max. permissible errors
Voltage range
Range
Resolution
Max. permissible errors
Outputs
Output
Magnetic stirrer
Speed
Power
Max. speed
Output (External stand DV705)
Magnetic stirrer
Speed
Voltage range
Pump
Voltage

74

Triaxial socket
1, 2, 5, 10, 15, 20, 30 or 40 A
1 A
2%
-2000 mV to +2000 mV
1 mV
0.5%

8-pin socket (mini DIN)


Stepper motor
Software-controlled (1-100%)
2W
1050 rpm (40% 600 rpm, 70% 1050 rpm)
5-pin socket (mini DIN)
DC motor
Software-controlled (1-100%)
0 to 18 VDC (max. 300 mA)
24 VDC (max. 400 mA)

METTLER TOLEDO DL31/DL38

Technical data

Burette drive module


Drive
Resolution
Max. permissible errors
Fill time
Delivery time

Stepper motor
1/10000 of the burette volume
0.3% relative to the respective burette volume of 5, 10 or 20 mL
Minimal 20 s (rate can be set between 10 and 100%)
Minimal 20 s

Interchangeable burettes
Volume
Materials which come
into contact with the titrant

Fluoroplastic, borosilicate glass, ceramic

Magnetic stirrer
Type
Max. speed
Power consumption

Stepper motor
1050 rpm
2W

Diaphragm pump
Voltage
Pressure buildup

24 VAC (4 W)
Approx. 150 mbar

Display
Liquid crystal display
Languages

6 lines, 20 characters per line, backlit


English, German, French, Spanish, Italian and Russian

Memories
Database
KF standard method
Tutorial method
KF learn method
METTLER methods
User data memory
User methods
KF titrants
KF standards
Br number titrants

METTLER TOLEDO DL31/DL38

1, 5, 10 and 20 mL

1
1
1
10 (DL38 only)
DL38: max. 50 / DL31: max. 1
DL38: max. 20 / DL31: max. 10
DL38: max. 20 / DL31: max. 10
DL38: max. 5 /

75

Technical data

Attachment possibilities for peripheral devices


Balance
Attachment via RS232C interface (9-pin, D-sub-connector)
for METTLER TOLEDO and SARTORIUS balances
Printer

Attachment via RS232C interface (9-pin, D-sub-connector)


for the GA42 Printer
Attachment via Centronics interface (25-pin, D-sub-connector)
for commercial EPSON- and HP-compatible printers with
parallel interface

Computer

Attachment via RS232C interface (9-pin D-sub-connector):


full-duplex, short-circuit-proof, handshake: X on/off,
no hardware handshake

Stromboli, TBox DR42, etc.

Attachment via TTL I/O socket (9-pin, D-sub)

76

METTLER TOLEDO DL31/DL38

Technical data

RS232C connector (balance/GA42/computer)


5
9
4
8
3
7
2
6
1

RxD (In)

TxD (Out)

DTR

+12 V

470

GND

4
5

Titrator

Data to titrator
Data from titrator
Handshake from titrator fixed to operational readiness
Signal ground, galvanically connected to titrator electronics

TTL I/O socket


IN1
IN2
OUT1
OUT2
OUT3
OUT4

1
6
2
7
3
8
4
9
5

GND

Titrator

1
2
3
4
5
6
7
8

In

TTL; short-circuit-proof; Pulse 150 ms


(the input signal for the titrator must be at least 150 ms)

Out

Open collector
Vce max. = 24 V
Ic max. = 20 mA
Signal ground, galvanically connected to titrator electronics

GND

Centronics socket

13
25
12
24
11
23
10
22
9
21
8
20
7
19
6
18
5

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25

\Strobe
PD0
PD1
PD2
PD3
PD4
PD5
PD6
PD7
\ACK
\BUSY
PE
SLCT
\AUTOFDXT
\ERROR
\INIT
\SLCTIN

17
4
16
3
15
2
14
1

Data ready

Data accepted
Printer busy
End of paper
Printer active
Automatic line feed
Printer error
Printer initialized
Printed selected

Signal ground, galvanically connected to titrator


electronics

Titrator

METTLER TOLEDO DL31/DL38

77

Technical data

Declaration of System Validation


We herewith inform you that the products/systems
DL31, DL38
including software and accessories were developed, tested and successfully validated according to the
international ISO9001:1994 based Life cycle rules of Mettler-Toledo GmbH, Analytical.
Life cycle checkpoint details were reviewed and approved by the Project Supervisory Group (PSG). The
products/systems 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 GmbH, 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.
Schwerzenbach,
August 1998

Dr. Bernhard Grob


General Manager
Business Unit Analytical

Dr. Rolf Rohner


Marketing Manager
Titration

ISO 9001 certificate for METTLER TOLEDO


The Mettler-Toledo GmbH company, Greifensee, was examined and evaluated in 1991 by the Swiss
Association for Quality and Management Systems (SQS), and was awarded the ISO 9001 certificate.
This certifies that Mettler-Toledo GmbH, Greifensee, has a quality management system that conforms
with the international standards of the ISO 9000 series.
Repeat audits are carried out by the SQS at intervals to check that the quality management system is
operated in the proper manner and is continuously updated in relation to changes brought about.

78

METTLER TOLEDO DL31/DL38

Technical data

Product Life Cycle Model


Ideas

Project Study

Project Start

Project Release

Phase:
Basic Know how

Product Guidelines
Performance Specifications
Quality Plan
Documentation Plan
Project Plan
Review Report

Phase:
Feasibility

Software Specifications
Test Plan
Review Report

Phase:
Confirmation

Review Report

Project End

Phase:
Readiness

Review Report

Usage

Customer Complaints (CRIS)


Customer Requirements

Phase out

METTLER TOLEDO DL31/DL38

79

80

METTLER TOLEDO DL31/DL38

Index

13

Index

Symbole
<F1>...<F3> 9

Access for expert/routine 21


All results 52
Amount of sample (calculating) 24
Analyse (Run) 34
Arrow keys 11
Author 27
Auto start 25
Auxiliary function keys 10
Auxiliary functions 50

Database 75
Date 20
Delay (time) 26
Dispense 51
Drift 26
Drift compensation 40
Drift determination 44
Drift stop 26
Drift value (i key) 56
Duration (KF titration) 40

B
Balance (attaching) 65
Balance (defining) 19
Balance (weight transfer) 40
Beep 21
Blank 26
Br No. titrants 15
Bromine number determination 45
Burette (auxiliary fct.) 50
Burette (installing) 63

Calculation 1 (KF) 26
Calculation 2/3 (KF) 27
Calculation formula (KF conc.) 42
Calculation formulae (KF) 41
Calculations (auxiliary fct.) 54
Centronics socket 77
Cleaning 66
Command keys 9
Computer (attaching) 65
Computer (defining) 19
Computer method 35
Concentration (KF) 14
Concentration determination (KF) 42
Control parameters (Br No.) 31, 32
Control parameters (KF) 25

Fill rate 50
Filling (titration vessel) 51

METTLER TOLEDO DL31/DL38

Electrode (attaching) 65
Emptying (titration vessel) 51
End point (KF) 25
Entry keys 11
Error messages 57
Esc key 9
Expert 21
Expiry date 34

G
GLP 27

H
Hardware tests 60
Hello! 56
Help texts 5

I
i key 11
Information menu 56
Inputs and outputs (ckecking) 61
Installation 62

81

Index

Keypad 8
KF learn titration 48
KF standard method 23
KF standards 16
KF titrants 13

Safety measures 6
Sample determination (Br No.) 45
Sample determination (KF, Br No.) 37
Sample determination (KF) 38
Sample parameters (KF) 24
Sample series 41
Series (terminating) 55
Settings 20
Setup 13
Solvent bottle (installing) 64
Solvent capacity 21, 56
Speed (stirrer) 24
Standard equipment 68
Standby (method parameter) 27
Standby mode 36
Starting a method 34
Statistics (changing) 54
Statistics (method parameter) 27
Statistics (printout) 54
Statistics series 55
Stirrer (auxiliary fct.) 50
Stirrer speed 24
Storage procedure 14, 15, 16, 28

L
Language (changing) 12

M
Magnetic stirrer (attaching) 65
Main methods 17
Maintenance 66
Malfunctions 59
Max. srel 27
Menu keys 10
Method parameters (Br No.) 31
Method parameters (KF) 24
Methods 22
METTLER methods 30
Mix time 24

O
Operating concept 8
Optional equipment 70

P
Peripheral interfaces (checking) 60
Peripherals 18
Post consumption 40
Predispensing 25
Printer (attaching) 65
Printer (defining) 18
Pump (auxiliary fct.) 51
Pump unit (replacing) 67
Pumping time 21
Putting into operation 8

R
Recalculation 53
Report (auxiliary fct.) 54
Report (method parameter) 27
Reset key 9
Resources 13
Result (DL31) 26
Rinse tip 51
RS232C connector 77
Run (analysis menu) 34

82

T
TBox DR42 (attaching) 65
Technical data 73
Termination parameters (Br No.) 31, 32
Termination parameters (KF) 25
Time 20
Titrant (method parameter) 24
Titration stand 19
Titration stand (equipping) 62
Titrator (overview) 7
Titrator ID 21
TTL I/O socket 77
TTL inputs & outputs 66
Tubing (replacing) 67
Tutorial 9, 56
Type (sample) 24

U
User interface (checking) 60
User list 20

W
Wait time 25
Waste bottle (installing) 64
Weight transfer 40

METTLER TOLEDO DL31/DL38

METTLER TOLEDO DL31/DL38 KF titrators


Switching from routine to expert mode

Settings
SETUP
Titrator ID

Acces for
Routine
Beep
Yes
Solv. capac.[mL]
8 0
Help
OK

"Modify" is assigned to <F2> allowing you to select "Expert".


Confirm <F3>, "OK", to save the change.

Settings
SETUP
Titrator ID

Acces for
Routine
Beep
Yes
Solv. capac.[mL]
8 0
Help M o d i f y O K

Select this line in the Setup menu.


While holding down the <Shift> key, press key <1> three times:

METTLER TOLEDO DL31/DL38

83

84

METTLER TOLEDO DL31/DL38

To protect your METTLER TOLEDO products future:


METTLER TOLEDO Service assures the quality, measuring accuracy and preservation of value of
all METTLER TOLEDO products for years to come. Please send for full details about our attractive
terms of service.
Thank you.

Printed on 100% chlorine-free paper, for the sake of our environment.


Subject to technical changes and to the availability of
the accessories supplied with the instruments.
*P51709850*

Mettler-Toledo GmbH 1998, 1999, 2002

ME-51709850C

Printed in Switzerland 0210/2.12

Mettler-Toledo GmbH, Analytical, Sonnenbergstrasse 74, CH-8603 Schwerzenbach,


Tel. ++41 1 806 77 11, Fax ++41 1 806 73 50, Internet: http://www.mt.com