Operating Instructions

DL31/DL38 KF Titrators

Contents
Page

1 The DL31/DL38 KF Titrators ....................................................... 1

2 Safety measures ....................................................................... 2

2.1 Measures for your protection ......................................................... 2
2.2 Measures for operational safety ..................................................... 3
3 The titrator ............................................................................... 4
3.1 Putting into operation .................................................................. 5
3.2 The operating concept ................................................................. 5
3.3 Changing the language ................................................................ 10

4 Setup ....................................................................................... 11
4.1 KF titrants ................................................................................... 12
4.2 Br No. titrants (DL38 only) ........................................................... 14
4.3 KF standards .............................................................................. 15
4.4 Main methods (DL38 only) .......................................................... 17
4.5 Peripherals ................................................................................. 18
4.6 Settings ...................................................................................... 21
5 Methods ................................................................................... 25
5.1 The KF standard method .............................................................. 26
5.2 KF method parameters ................................................................. 29
5.3 Storage procedures ...................................................................... 35
5.4 DL38: User and METTLER methods ............................................... 37
5.5 DL38: Bromine number method No. 908 ....................................... 38

6 Analysis (Run) .......................................................................... 41

6.1 Starting a method ........................................................................ 41
 Page

6.2 Sample determination .................................................................. 45

6.3 Concentration determination ......................................................... 51
6.4 Drift determination ....................................................................... 53
6.5 Bromine number determination (DL38 only) .................................. 54
6.6 KF learn titration .......................................................................... 55

7 Auxiliary functions .................................................................... 58

7.1 Stirrer ......................................................................................... 58
7.2 Burette ....................................................................................... 59
7.3 Pump ........................................................................................ 60
7.4 Results ....................................................................................... 61
8 Information menu .................................................................... 66

9 Error messages and malfunctions .............................................. 67

9.1 Error messages from the titrator ..................................................... 67
9.2 Other errors and malfunctions ....................................................... 70
9.3 Checking hardware ..................................................................... 72
10 Installation and maintenance ..................................................... 75
10.1 Equipping the titration stand ......................................................... 75
10.2 Installing the burette .................................................................... 76
10.3 Installing the solvent and waste bottles ........................................... 77
10.4 Attaching the magnetic stirrer, electrode and devices ........................ 78
10.5 Using TTL inputs and outputs (DL38 only) ..................................... 80
10.6 Maintenance and servicing ........................................................... 81

11 Standard and optional equipment .............................................. 84

11.1 Standard equipment .................................................................... 84
11.2 Optional equipment ..................................................................... 88
12 Technical data .......................................................................... 91
13 Index ...................................................................................... 97
1 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-compatible printer to the Centronics interface.
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 hard-
ware and software are mentioned in the corresponding sections.
These Operating Instructions correspond to software version 1.0.

Where can you find what information?

1. 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.
2. 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 refer to either a section of this
"manual" or the "brochure".
3. You will find a detailed description of the communication between
the titrator and a computer in the manual for the computer inter-
face. This you can order.

DL31/DL38 1
2 Safety measures
The titrators have been tested for the experiments and intended
purposes documented in these Operating Instructions. However, this
does not absolve you from the responsibility of performing your own
tests of the products supplied by us regarding their suitability for the
methods and purposes you intend to use them for. You should there-
fore 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, cor-
Risk of explosion rosion caused by the ingress of gases).

– 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 DL31/DL38
2.2 Measures for operational safety

– Have the instrument serviced only by METTLER

TOLEDO Service!
– Always wipe off splashed liquids immediately! The
Caution
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!

DL31/DL38 3
3 The titrator

Titration stand

Burette

Titrant bottle Solvent bottle

Arrestment knob
Pump knob
Waste bottle

Keypad

Magnetic stirrer

Rear view
RS232C interface
for balance
RS232C
Attachment interface for
DV705 GA42 Printer

RS232C interface
Stirrer output for computer

Electrode TTL-I/O interface

input (KF)
Centronics interface
Attachment for EPSON-compa-
waste bottle tible printers

Pump unit
Connector for On/off switch
power cable

4 DL31/DL38
3.1 Putting into operation
– Plug the power cable supplied into the connector of the titrator,
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 (mask))
,,,,,,,,,,
Arrow keys

,,,,,,,,,,
Reset

i
,,,,,,,,,,
,,,,,,,,,, 7
(
8
)
9

,,,,,,,,,,
METTLER TOLEDO
[ ]

,,,,,,,,,,
4 5 6
DL38
Entry
,,,,,,,,,,
Auxiliary Stirrer Burette

function Version 1.0 1 2 3 keys

,,,,,,,,,,
Hello!
keys *
,,,,,,,,,,
Pump Results * CE
0 . Del
Esc F1 F2 F3
Shift

Setup Method Run

Menu keys Command keys

The command key <F3>, "Hello" (see Section 3.2.1), 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:

Name of the key, in

Title line Resources SETUP other words the
displayed list of
Selection bar KF titrants resources belongs to
the Setup menu
Br No. titrants
DL31: No KF standards ▼
"Br No. titrants"! Print OK Commands

DL31/DL38 5
You can now also activate the arrow key (∇), Reset and Command
keys <F2>, Print and <F3>, 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.
Print: Press <F2>: The list of KF titrants is printed out (if a printer
is selected and defined, see Section 4.5.1).
OK: Press <F3>: The list of KF titrants appears.

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 re-
quire 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.

6 DL31/DL38
 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 let-
ters or characters, e.g. for a name. In this case, you can
not enter numbers until you have confirmed ABC (press
<F1>).

The Esc key

If you have made changes in the current menu or submenu, they are
discarded, in other words 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.

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.
All resources required for the titration such as KF titrants
Setup and KF standards are stored in the Setup menu and can
be changed.

DL31/DL38 7
 The sample is determined with the aid of a method. All
Method 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 meth-
ods.
DL31: Only one method can be stored!
The titration is performed in the Analysis menu. The meth-
Run od called up determines the analysis sequence.
Note
Each menu is subdivided into task areas (submenus)
which are designated menus, lists or masks in these
Operating Instructions.

3.2.3 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 analy-
sis, 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

You can add or siphon off solvent.

Pump

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

8 DL31/DL38
 You can view the result list of analyzed samples, perform
*
Results
recalculations, change the statistical evaluation of a se-
ries (DL38 only!) and print out additional reports.

3.2.4 The i key

The value of the current solvent capacity and the last drift
determination, the “Hello“ Tutorial, the KF learn method
i and a menu for testing the titrator hardware are accessi-
ble with this key.

3.2.5 The entry and arrow keys

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

CE Del: You delete the number/character/letter last entered.

Del CE: You delete all entered numbers/characters/letters.

Shift You can move the cursor to the right or left (only if
+
7 letters/characters are selected), see example:
Shift + User a
4
abcdefghijklm
Cursor nopqrstuvwxyz
ABCDEFGHIJKLM ▼
Help Select OK

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

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

DL31/DL38 9
3.3 Changing the language
All texts in the titrator are stored in English, German, French, Spanish
and Italian. If you have not run the Tutorial and understand one of the
available languages better than the one displayed, you should select
it:

Setup

Resources SETUP

KF titrants
Br No. titrants – Press the Shift and Arrow (∇)
KF standards ▼
once, then press only the Arrow
Print OK key to select "Settings".

Resources SETUP
Peripherals
Settings

OK – Press <F3>.

Settings SETUP

Language English
User list
– Press <F2> repeatedly until,
Date 20-08-1998 ▼
Modify OK e.g. "Español" appears.

Settings SETUP

Lengua Español With OK or Esc the "Resources"

Lista usarios mask reappears.
Fecha 20-08-1998▼ OK: Spanish texts appear.
Modif. OK
Esc: English texts appear.

10 DL31/DL38
4 Setup
In order to perform titrations, the titrator must know the titrants and
their concentration. It must know the settings of the attached instru-
ments 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.

NOTICE All titrants and KF standards needed for the METTLER

methods are stored! If you delete one of these resourc-
es, the error message that it is missing does not appear
until the start of the titration.

Print Depending on your choice of resource, its list with the

corresponding parameters will be printed out.
OK The list of the selected resources appears.

DL31/DL38 11
4.1 KF titrants

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

1-comp 5 ---- 1 component reagent : 5 mg/mL

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

Delete The titrant is deleted.

Print The parameters of the titrant are printed out.
Modify 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 Press <F1>, "ABC" to change the name. The titrant with
its parameters will be stored under this name.
Conc. You can change the concentration or its range. You
should change the concentration only if you know the
correct value!

12 DL31/DL38
Type 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).
Burette Select the burette (volume) which is used to dispense the
titrant.
Batch 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 listed on page 12 always appear, only the
name of the titrant is missing.
– Change the parameters as described above.

NOTICE The name of the new titrant must differ from those
already stored, otherwise an existing titrant will be over-
written!
Note
In the DL31 you can store 10 titrants, in the DL38 20.

DL31/DL38 13
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 The titrant is deleted.

Print The parameters of the titrant are printed out.
Modify The parameters of the titrant appear:

Name Br-/BrO3-
Conc. [mol/L] 0.05
Burette 5 mL
Fill rate [%] 100
Batch

Name Press <F1>, "ABC" to change the name. The titrant and
its parameters will be stored under this name.
Burette Select the burette (volume) which is used to dispense the
titrant.
Batch 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.

14 DL31/DL38
New Br No. titrant
You add a new titrant to the titrant list when you confirm the free line
with <F3>, OK. The parameters listed on page 14 always appear,
only the name of the titrant is missing.
– Change the parameters as described above.

NOTICE The name of the new titrant must differ from the one
already stored, otherwise an existing titrant will be over-
written!
Note
You can store 5 titrants for the bromine number.

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 ----- di-sodium tartrate . 2 H2O

H2O standard 10 ----- Water standard : 10 mg/g
H2O standard 1 ----- Water standard: 1 mg/g
H2O standard 5 ----- Water standard: 5 mg/mL
H2O ISO 3696 ----- pure water following ISO standard
... ----- free line for a new standard

Delete The standard is deleted.

Print The parameters of the standard are printed out.
Modify The parameters of the standard appear:

DL31/DL38 15
 Name di-Na tartrate
H2O content 15.660
Unit %
Batch
Type Mass
Weight [g] 0.0500

Name Press <F1>, "ABC" to change the name. The standard

and its parameters will be stored under this name.
Batch Press <F1>, "ABC" to enter the batch number specified
on the bottle.
Type You can select mass, volume or pieces. "Weight" chang-
es accordingly to "Volume" or Number".
Weight 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,
Volume • 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.

16 DL31/DL38
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 listed on page 16 always
appear, only the name of the standard is missing.
– Change the parameters as described above.

NOTICE The name of the new standard must differ from those
already stored, otherwise an existing standard will be
overwritten!
Notes
1. In the DL31 you can store 10 standards, in the DL38 20.
2. The Application brochure offers tips on sample preparation, sam-
pling and the optimum amount of sample (see Section 5.4).

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 immedi-
ately. 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):

F1: Free

You can select a method from the METTLER methods (or from the
user methods if available), e.g. "900 Standard 10":

F1: Method 900

Title Standard 10

DL31/DL38 17
With <F3>, "OK" the following appears:

F2: Free

You can select a different method to configure the <F2> command. If

you confirm this display with OK , the following appears:

F3: Hello!

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

method (press <F2>).

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 None
Balance None
Titrn stand Internal
Computer Not def.

4.5.1 Printer

GA42 – Select the attached printer.

EPSON – With an EPSON printer change the type and
None possibly the settings with <F2>.

18 DL31/DL38
Standard settings for the EPSON printer

Type LX/SX
Paper Fanfold
Format A4
Automatic feed No

Type Select LX/SX or LQ/Stylus.

Paper Select Fanfold or Single sheet (see "Feed")
Format • DIN 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.

Set a nonproportional character font, e.g. "Courier" for

NOTICE
the EPSON printer!

4.5.2 Balance

Select Unidirect., Bidirect. or None.

Unidirectional: On request for the weight, the balance continuously
transfers the current weight value.

Data to titrator
Titrator Balance Configuration: "Send Cont."

DL31/DL38 19
Bidirectional: On request for the weight, the balance transfers the
current weight value when ordered by the titrator.
Command from titrator

Titrator Balance Configuration: "Send Stable"

("Send on Transfer")
Data to titrator

4.5.3 Titration stand

Select Internal or 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.

4.5.4 Computer
– If you attach a computer, you must
Defined
select "Defined" and possibly change
Not defined
the settings.

Default settings for the computer

Baud rate 4800

Parity Even
Number data bits 8
Number stop bits 1
Character set ASCII
Start/end '{'/CR

20 DL31/DL38
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 Select ASCII or DL.
set Notice: If you select DL, you must specify 8 for the
number of data bits!
Start/end Select '{'/CR or STX/ETX.
Note
You will find additional information on the communication between
titrator and computer in the Operating !nstructions for the computer
interface.

4.6 Settings

You can or must select or define the following settings for the titrator:

Language English
User list
Date 26-08-1998
Time 10:20
Titrator ID
Access for Expert
Beep Yes
Solv. capac.[mL] 80
Pumping time [s] 60

Language Select one of the available languages.

DL31/DL38 21
User free line for the first or
list ... a new name

Press <F1>, "ABC" and enter your name.

With <F2> the list of the defined names with the command
for deletion appears.
You can (must) then select your name for both the devel-
opment of a method and the performance of the analysis.

Date Day 26
Month 8
Year 1998
Format 31-08-1998

Format: Select 31/08/1998, 08-31-1998, 31-Aug-1998

or Aug/31/1998.

Time Hour 10
Minute 20
Format 24 h

Format: Select 24 h or am/pm.

Titrator ID To enter an identification for your titrator, press <F1>,

"ABC". The ID is always reported.

Access for 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".

22 DL31/DL38
 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.
Reaccess for experts is described on the last page of
these Instructions.

Beep Select Yes, Minimum or No.

• 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.

Solvent You can perform several titrations in the same solvent in

capacity 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.

DL31/DL38 23
Pumping The defined time is a safety criterion: The pump should
time shut off if you, e.g. leave the lab while it is running.

24 DL31/DL38
5 Methods
The titrator automatically performs analyses with the help of
predefined methods. On delivery of the instrument
in the DL31 the KF standard in the DL38 the KF standard
method specified by us is method specified by us and 10
stored. You can modify this METTLER methods are stored.
method and save it under a You can modify these methods
number. and save them as user meth-
ods.
Methods METHOD
Methods METHOD
KF standard method
User methods
METTLER methods
Help Modify KF standard method
Help Print OK
Method METHOD
Print: The list of methods you
No. 0 have developed is printed out.
of the method OK: The user methods with their
defined numbers and titles ap-
Help OK pear (example):

When you have modified and Methods METHOD

saved the method, the following
appears (example): 22 Coffee
33 Tea
Methods METHOD 113 Powdered milk
Delete Print Modify
123 Cellulose
KF standard method

Print Modify

DL31/DL38 25
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.

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 param-
eters, which are shown as a group in a mask. In the DL38 case, 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 ap-
pears in its own mask (see Section 5.3).
Note
The method is always shown with the following default parameters.
The parameters which you can modify and those which are faded in or
out are listed in Section 5.2.

26 DL31/DL38
DL31 / DL38

No. 0
of the method
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] 0.0000
for predispensing
Auto start No ....... DL38 only
Control parameters
Current [µA] 20
End point[mV] 100
∆Vmin [µL] 0.5
∆Vmax [µL] 8.0
∆Vmax factor [%] 30
Start Cautious
Termination param.
Max. time [s] 600
Drift stop Rel.
Drift [µg/min] 15
Vmax [mL] 10.000
Blank [µg] 0

DL31/DL38 27
 Drift Online
Result % ....... DL31 only
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 DL38 only
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Calculation 3
R3 = No calculation
f3 = 1.0000
Unit
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Standby Ja
Report
Output Print.+Comp.
Type GLP
Author
of the method

28 DL31/DL38
5.2 KF method parameters

No. (of the method)

The method is stored under the number: The numbers 900-999 are
reserved for METTLER methods.

Title (of the method)

You can give the method a specific name.

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 appears when "Mass", "Volume" or "Pieces" is selected.
Maximum 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"
(see next page), on storage "Before" is automatically set
to "During".

DL31/DL38 29
Speed
You should not set the stirring speed higher than 60% to prevent the
magnetic stirring bar "jumping".

Mix time
The time is an empirical value and can be entered specific to the
sample ("Request")..

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

Volume (for predispensing)

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

Wait time
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.)

Auto start (DL38 only)

You should select "Yes" for determinations in which, e.g. side-reac-
tions could occur during the titration. As the titrator starts to titrate
immediately following sample addition when it detects water, the time
for possible side-reactions becomes shorter.

30 DL31/DL38
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,
Section 4).

1 component 2 components Pyridine

Pol. current 20 µA 20 µA 20 µA
End point 100 mV 100 mV 100 mV
∆Vmin 0.5 µL 0.5 µL 0.5 µL
∆Vmax 4.0 µL 8.0 µL 3.0 µL
∆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.
Pol. current A Karl Fischer titration can be indicated by a positive or
negative polarization current. Both determinations result
in equivalent measured values. With the DL31/DL38 the
entry possibility is thus limited to positive values for polar-
ization current and end point.

Termination parameters
To terminate the titration you must define "Drift stop" (or "Delay") and
"Vmax" as a condition; the maximum time is an additional termination
condition. The titration is terminated when the first of the selected
conditions is met.

DL31/DL38 31
Drift stop Select Rel.(ative), Abs.(olute) or No.
No: Drift [µg/min] is faded out and Delay [s] superim-
posed.
Delay If you enter "0" for the delay time, the titration is terminat-
ed as soon as the end point is reached.
Vmax The maximum volume is intended as a safety precaution:
It avoids dispensing an unnecessarily large amount of
titrant if the titration is faulty.

Blank
For the entry of a correct value, you should perform a determination.
You can enter the value specific to the sample ("Request").

Drift
The drift value is needed for calculation of the result (see Section
6.2.3). You can enter a value in the method ("µg/min") or just before
every titration ("Request") or have it entered:
"Online": The moisture which enters the titration vessel is always
measured, evaluated and displayed in the standby mode.
"Determination": Some standard operating procedures require inser-
tion 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 (see Sections 6.2.3 and 8).

Result (DL31 only)

The water content is calculated with the appropriate formula by selec-
tion of the unit: mg, µg, %, ppm, mg/pcs., mg or µg and % or ppm
(see Section 6.2.3).

32 DL31/DL38
"mg or µg" / "% or ppm": With the following limit values, the result is
automatically set from one unit to the other:
mg µg % ppm
less than 0.1 99... less than 0.1 999...
0.1.. greater than 100 0.1.. greater than 1000

Calculation 1 (DL38 only)

R1 Result of the first calculation. The water content is calcu-
lated with the appropriate formula by selection of the unit:
mg, µg, %, ppm, mg/pcs or g/kg (see Section 6.2.3).
mL: Titrant consumption up to the end point.
min: Duration of the titration (see Section 6.2.3).
ppm (ext.extr), % (ext. extr.) and ppm (ext. soln),
% (ext. soln): Special calculation for samples which are
used after an external extraction or external dissolution.
The 2nd and 3rd calculations are needed. See Sections
7.2 and 7.3 of the 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" (see Section
7.4.5).
Max. srel If the entered value for the max. relative standard devia-
tion is exceeded, an error message appears.

DL31/DL38 33
Calculation 2/Calculation 3 (DL38 only)
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 dissolu-
tion 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 (see Section 4.6: Access for).

Standby
"Yes": 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.
"No": After a titration the start mask of the Analysis menu reappears
(see Section 6.1).
"[min]": After the sample determination, a switch is made to the
standby mode and the subsequent rate of consumption is displayed
and printed out during the defined time (see Section 6.2.2).

Report
Output Select printer, computer or Print .+Comp. as output
device.
Type 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-compati-
ble printer.
(GLP report: All data which are required by the rules of
Good Laboratory Practice)

34 DL31/DL38
Author of the method
The selection of your name documents that you are responsible for
the development of the method (see Section 4.6: User list).

5.3 Storage procedures

DL31 / DL38
The following always appears as the last parameter of a method:
Method METHOD

Author
of the method The modified method is stored when
you confirm OK (examples):
Help Modify OK

DL31 DL38
Methods METHOD Methods METHOD

123 CaCl2 4 H3PO4

KF standard method 31 Oil

Help Print Modify Delete Print Modify

If you have not entered any or a wrong method No., the following
appears:
Error METHOD Method METHOD

No/invalid value No. 0

Min: 1.00000 of the method
Max: 899.000
OK Help OK

– Enter the number and confirm OK: The method is stored.

DL31/DL38 35
DL38
If you have entered a method No. which already exists, the following
appears:

Method 22 METHOD Change number: "No. of the

Method No. exists method" reappears (see page 35).
Change number Overwrite method:: The new or
Overwrite method modified method is stored, that with
the same number deleted.
OK

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 (see Section 6.1).
b. If you have already modified a parameter of the method, the mask
"Author of the method" appears (see page 35). The method is
stored with OK and the start mask of the Analysis menu is dis-
played.

36 DL31/DL38
5.4 DL38: User and METTLER methods

You can print out the selected method with <F2>. You can delete user
methods, but not METTLER methods.
Methods METHOD Methods METHOD

22 Coffee 900 Standard 10

33 Tea 901 Na tartrate
113 Powdered milk 902 Toluene dry ▼
Delete Print Modify Print Modify

If you press <F1>, the follow- You can modify METTLER

ing appears: methods, but in this case you
must always give them a
Delete? METHOD
number (1-899) so that they are
Yes
stored as user methods.
No

OK

5.4.1 METTLER methods

The following methods have been developed by us and can be

performed immediately (see Application brochure).

900 Standard 10 905 Ext. Extr.

901 Na tartrate 906 KF Oven
902 Toluene dry 907 Gas
903 Ketone 908 Bromine No.
904 Homogenizer 909 Blank Br No.

DL31/DL38 37
5.5 DL38: Bromine number method No. 908

If you wish to develop a bromine number determination to meet your

requirements, you can modify METTLER method 908 or 909 and store
as a user method (see Sections 5.3 and 5.4).

No. 908 ...... see Section 5.2

Title Bromine No. ...... see Section 5.2
Sample parameters
ID Request ...... see Section 5.2
Type Mass
Minimum [g] 0.2000
Maximum [g] 0.4000
Entry Before
Speed [%] 30
Mix time [s] 120
Titrant Br-/BrO3- see Sectn 5.2 and Help texts
Predisp. [mL] 0.0000
Wait time [s] 0
Control parameters
Current [µA] 1
End point [mV] 150
∆Vmin [µL] 1.0
∆Vmax [µL] 20.0 see Help texts and method
∆Vmax factor [%] 100 No. 908 in the Application
Start Normal brochure
Termination param.
Max. time [s] 6000
Delay [s] 15
Vmax [mL] 20.000
Blank Request ...... see Method 909 and Section
5.2

38 DL31/DL38
 Calculation 1
R1 = x[Br No.]*f1
f1 = 1.0000
Unit
Decimal places 2
Statistic Yes ....... see Section 5.2
Max. srel [%] 0.00 ....... see Section 5.2
Calculation 2 mL
R2 = x[mL]*f2
f2 = 1.0000
Unit mL
Decimal places 3
Statistics No
Max. srel [%] 0.00
Calculation 3 see Section 5.2
R3 = No calculation
f3 = 1.0000
Unit
Decimal places 2
Statistics Yes
Max. srel [%] 0.00
Report
Output Print.+Comp. see Section 5.2
Type GLP
Author
of the method ........see Section 5.2

Note
"Author of the method" only appears if you change the method.

DL31/DL38 39
Sample parameters
Type Select Mass, Fixed mass, Volume or Fixed volume
Weight appears when "Fixed mass" is selected.
Volume appears when "Fixed volume" is selected.
Density appears when "Volume" of "Fixed volume" is selected.
Minimum appear when "Mass" or "Volume" is selected. The unit
Maximum depends on the type of sample: g or mL.
Entry of the amount of sample before or during the actual
titration. "Entry" is faded out when "Fixed mass" or "Fixed
volume" is selected.

Calculation 1
R1 Result of the first calculation. The bromine number or
bromine index is calculated using the appropriate formu-
la by selection of "Br No." or Br index" (see Section 6.5).
mL: titrant consumption up to the end point .
min: duration of the titration
Unit Bromine number and bromine index are characteristics
without dimension: The bromine number is the calculated
number of grams of bromine which react with 100 g
sample, the bromine index is the calculated number of
milligrams of bromine which react with 100 g sample.

40 DL31/DL38
6 Analysis (Run)
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
1. Press the Burette key. Rinse the burette and fill ensuring that
there are no air bubbles in the burette and tubing (see Section
7.2).
2. Press the Pump key and fill the titration vessel with approx. 40 mL
solvent (see Section 7.3).
When you press the "Run" key, the start mask appears:
DL31 DL38
Start RUN Start RUN

Method No. 22 Method No. 22

Title Title
User User
Help OK Help Modify 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.

DL31/DL38 41
• in the DL38 case the number which you enter directly or accept it
with <F2> from the METTLER or user methods is entered.

Notes
1. You can select the user name. The name which was selected in
the analysis last performed remains stored.
2. 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 determina-
tion (see Section 6.3).
3. 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 (see next point).
4. 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
Operating Instructions of the com- Start RUN
puter interface). If it is available, the
pretitration is started immediately Data transfer...
following transfer; if it is not avail-
able, "Method not available" ap-
pears.

42 DL31/DL38
6.1.1 Menu sequence up to standby mode (KF methods)

DL31/DL38 (example)
Start RUN

Method No. 22
Title Coffee
Benutzer C. De Caro
Help Modify OK DL31: <F2>, Modify is missing.
The pretitration starts with OK: It is
PRETITRATION RUN always executed with the control pa-
rameters of the selected method.
The length of the solid bar reflects
the addition of the titrant. The verti-
cal bar represents the threshold for
Help
the transition to the standby mode.
STANDBY RUN
→: This arrow indicates that you can
Active method: 22 start a determination.
→ :Wait, drift still decreasing!
Drift [µg/min] 2→
DRIFT CONC. SAMPLE →:Wait, drift increasing again!

Press <F1> to start the drift determination (see Section 6.4),

<F2> to start the concentration determination (see Section 6.3),
<F3> to start the sample determination (see Section 6.2).

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.

DL31/DL38 43
6.1.2 Standby mode

During standby, the following menus are blocked or selectable:

Blocked Setup menu, auxiliary functions Burette and Pump, the
Tutorial, the KF learn titration and the Hardware tests
menu (under the i key)
Select- Method menu, auxiliary functions Stirrer and Results. You
able can view the values for the solvent capacity and drift under
the i key.
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: You can change the speed. This is reported for the subse-
quent sample determination.

Results: The menu is not shown until you have performed the first
measurement or a result is available (see Section 7.4).

Method: 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 docu-
mentation conforming with GLP, you should print out the method
before you switch back to the Analysis menu.

DL38: If you modify the parameters of the active method, a sample

series will be terminated (see Section 6.2.4).

44 DL31/DL38
6.2 Sample determination

With <F3> or <Run> the following can appear, depending on the

method:
1. in succession the sample-specif- ANALYSIS RUN
ic parameters if they are defined
with "Request" (e.g. mixing Mix time [s] 10
time), then one of the masks
mentioned under points 2 and 3
appears. OK

ANALYSIS RUN
2. the masks for the sample entry if H2O exp. [%] 2.00
a variable amount of sample is Weight [g] 0
defined with "Entry: Before". Minimum [g] 0.3750
Maximum [g] 0.8750
Help Bal.* OK
3. the mask for the sample addition
ANALYSIS RUN
if a variable amount of sample is
defined with "Entry: During" (ex- Please add sample
ample: mass). 0.3750 g -
0.8750 g
Help OK
Notes
1. If you take longer than 5 minutes for the entry of samples or
sample-specific parameters, the titrator switches back to the
standby mode.
2. If you add a sample while the titrator is in the standby mode
without first pressing the Run key, the titrator will begin a pretitra-
tion to titrate all the water in the sample. Immediately pressing the
Reset key and thereafter pressing the Shift and Run keys simul-
taneously 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”.
DL31/DL38 45
Sequence of the sample determination (with point 2)

ANALYSIS RUN The values for the expected water

H2O exp. [%] 2.00 content and the limits for the weight
Weight [g] 0 are adopted from the defined sample
Minimum [g] 0.3750 parameters of the method. The limits
Maximum [g] 0.8750 are recalculated if you change the
Help Bal.* OK
value for "H2O exp.".
ANALYSIS RUN
If you now enter the weight value or
Add sample or have it transferred from the balance,
confirm addition: the mask shown appears, otherwise
0.3750 g - that under point 3 is displayed (see
0.8750 g page 45).
Help OK * Appears only if a balance is defined (see
Sections 4.5.2 and 6.2.1).
ANALYSIS RUN
During the titration you can switch
between four different displays.
In the graph, the bar fills and empties
in accordance with the drift. The ver-
Sample**Drift tical bar represents the end point of
the titration.
ANALYSIS RUN ** Appears only if you have not yet entered the
Drift: amount of sample. With <F1> the parameter
"Weight [g]" is displayed to enter the value.
9500 µg/min
Sample** Cont. Graph

ANALYSIS RUN
The titration is ended in accordance
Content: with the defined termination param-
eters. In the background the titrator
42.0012 mg switches to the standby mode or the
Sample**Consum Graph start mask .

46 DL31/DL38
ANALYSIS RUN

Consumpn: 1.2010 mL
Duration: 0:31 min
If you have not yet entered the
Sample** Drift Graph amount of sample, the parameter
"Weight [g]" appears.
Report RUN
Otherwise, the result is reported be-
Printing... fore it is displayed.

DL31: R = 1.98 %

Result RUN
Method 22
Sample 1
R1 = 1.98 %

OK

If you confirm OK, either

• the standby mask (method parameter "Standby: Yes" appears or
• the start mask ("Standby: No"), see page 41, or
• the post consumption mask (method parameter "Standby: [min]"),
see Section 6.2.2.
The result is now stored under the auxiliary function "Results" so that
you can, e.g. recalculate it (see Section 7.4.2).

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> "Sam-
ple" to enter the amount of sample (see titration masks).

DL31/DL38 47
6.2.1 Weight transfer from a balance

ANALYSIS RUN If you press <F2> "Balance" in the

corresponding mask, the value dis-
> 1.3245 g played on the balance appears. It is
transferred with OK.
OK

6.2.2 Post consumption

STANDBY RUN If you have selected "Standby [min]"

Post consumption: in the method, the subsequent meas-
Duration: 0:34 min urement of the drift is performed di-
Drift: 6 µg/min rectly after the sample determination
and a drift value automatically printed
Stop
out every minute.

6.2.3 Calculations

DL31/DL38 (manual start)

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

Confirm
SAMPLE Requests Mix time Predisp.. Wait time Titration
Measured value acquisition
Sample
addition

Standby Time measurement (duration)

48 DL31/DL38
DL38 (Auto start)
In the case of an automatic start of the titration, the titrator does not
start the time measurement until you have entered the sample.

Confirm
SAMPLE Requests Mix time Predisp.. Wait time Titration

Meas. value acquisition

Sample
addition

Standby Time measurement (duration)

Calculation formulae

1 mg H2 O = (consumption ⋅ conc.) – (drift ⋅ duration) – blank

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

(consumption ⋅ conc.) – (drift ⋅ duration) – blank

2 % H2 O =
mass

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

for the H2O content in g/kg by 10.

(consumption ⋅ conc.) – (drift ⋅ duration) – blank

3 mg H2 O/pcs =
number

These parameters are listed on every GLP report to allow you to

check the result using the formula.

DL31/DL38 49
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" (see
Section 7.4.1).
The series is terminated if you
• enter the appropriate command (see Section 7.4.6),
• switch off the titrator,
• 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. See Sections
7.4.1 and 7.4.5.

50 DL31/DL38
After, e.g. the third sample determination, the following appears:
Result RUN
Method 22
Sample 3
R1 = 1.91 % <F1>: You can switch between the
result and statistics displays.
x OK
Note
Statistics RUN The mean value is calculated after
Method 22 two samples, the absolute and rela-
R1 n = 3 tive standard deviation after three
x = 1.95 %
samples.
s = 0.021095 % ▼
Result OK

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 also Section 5.2 in the Application brochure).
The concentration is always determined with the control and termina-
tion 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

H2 O content ⋅ mass
CONC in mg/mL =
 drift ⋅ duration 
consumption –  
 conc. (old) 

DL31/DL38 51
With <F2>, CONC appears:
CONC RUN You can select one of the standards
KF standard: stored in the Setup menu with <F2>
di-Na tartrate (see Section 4.3).

Help Modify OK

CONC RUN A batch number defined in the Setup

di-Na tartrate: menu is entered here. If you change
Batch or enter this for the first time, it will be
H2O content 15.660 adopted for the current concentra-
% tion determination.
ABC OK
Irrespective of the mixing time you
CONC RUN
have defined in the method, you can
Mix time [s] 10 enter this according to the standard.

OK
This mask appears when "Entry: Be-
CONC RUN fore" is defined in the method. If "En-
di-Na tartrate: try: During" is defined, the sample
Weight [g] 0 addition mask appears immedi-
Proposal [g] 0.0500 ately..
* Appears only if a balance is defined (see
Help Bal.* OK Sections 4.5.2 and 6.2.1).

ANALYSIS RUN The amount of sample suggested in

the previous mask is displayed.
Please add sample The further progress corresponds to
0.0500 g (approx.) that of the sample determination
(see Section 6.2).
Help OK

52 DL31/DL38
DL31
Each result is entered in the parameter list of the titrant, in other words
the second overwrites the first etc.

Result RUN If you calculate the mean value of

Method 22 the results and then enter this in the
Sample 2 list, date and time are deleted (see
Conc. = 4.9892 mg/mL Section 4.1); this means the shelf
life date can not be checked.
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 RUN As in the sample determination, you

Method 22 can switch between the statistics
Sample 2 and result displays (see Section
Conc. = 4.9892 mg/mL 6.2.4).
x OK

6.4 Drift determination

You must determine the drift when a value is required for the calcula-
tion of the water content which has been obtained by a titration (see
Section 5.2: Drift). With <F1> "DRIFT" appears:

DRIFT RUN The length of the solid bar repre-

sents the elapsed time.
After 5 minutes, the result is report-
ed and displayed. At the same time,
Duration: 4:24 min the value is stored under the i key
Help (see Section 8).

DL31/DL38 53
6.5 Bromine number determination (DL38 only)

The course of the determinations corresponds to the sample determi-

nation of a KF titration (see Section 6.2). This also applies to the
performance of a sample series (see Section 6.2.4).

Start RUN

Method No. 123

Title Bromine No.
User R. Huber
Help Modify OK If method parameters are defined
with "Request", they are displayed
before the sample entry mask ap-
ANALYSIS RUN pears (example "Mass" and "Entry:
Before")..
Weight [g] 0
Minimum [g] 0.2000
Maximum [g] 0.4000 * Appears only if a balance is defined (see
Help Bal.* OK Sections 4.5.2 and 6.2.1).

ANALYSIS RUN When you have confirmed the sam-

Verbrauch: ple addition, the titration starts.
** Appears only if you have not yet entered the
2.3450 mL amount of sample. With <F1> the parameter
"Weight [g]“ is displayed to enter the value.
Sample**

After the end of the titration, the re-

Result RUN
sult is reported before it is displayed.
Method 123
Sample 2
If you confirm OK, the start mask
Bromine No.= 4 reappears.

OK

54 DL31/DL38
Calculation formula

(consumption ⋅ conc. – blank) ⋅ 15.98

Bromine number =
mass

6.6 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.
If you confirm "KF learn titration" with OK, the following appears:

Method KF-L If you enter a number under which a

method is already stored, an appro-
No. 55 priate message appears:
of the method
DL31: Although the method is
Help OK overwritten, you should enter a dif-
ferent number (documentation of the
method!).
DL38: The method is stored as a
Method 55 KF-L new user method with a different
number.
Type Mass
of the sample

Modify OK

DL31/DL38 55
Method 55 KF-L

Calculation 1 % DL31: Instead of "Calculation 1",

"Result" appears.
Modify OK

Start KF-L Correct selection of the titrant used

KF learn titration is important: The control depends on
Titrant 1-comp 5 the titrant type!
Type 1-component
User V. Müller
Help Modify OK The pretitration starts with OK.

STANDBY KF-L

Active method 55 – Wait until the drift is completely

stable before you confirm SAM-
Drift [µg/min] 2→ PLE!
Help SAMPLE
The masks for the entry of mixing
time and sample ID appear before
the amount of sample is request-
Analysis KF-L ed.

Weight [g] 0

Help Bal.* OK
* Appears only if a balance is defined (see
Sections 4.5.2 and 6.2.1).
ANALYSIS KF-L
Add sample or
Appears if you have already entered
confirm addition:
1.2345 g the amount of sample. Otherwise,
"Please add sample" appears.
Help OK

56 DL31/DL38
Result KF-L After the end of the titration, the re-
sult and the "learned" parameters
R1 = 0.61% ! are printed out before the result is
Calculated parame- displayed. The result is always
ters are stored marked with an exclamation mark.
OK
The standby mask of the Analysis
STANDBY RUN menu with the active method
number appears so that you can de-
Active method: 55 termine the next sample with the
"learned" method.
Drift [µg/min] 2→

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).

DL31/DL38 57
7 Auxiliary functions
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.
Stirrer STIRRER Start and stop the stirring with <F3>.
Start: The stirrer stirs at the defined
Speed [%] 35 rate.

Start

Stirrer STIRRER To change the speed in the standby

mode in KF titrations,
Speed [%] 35
– press the Stirrer key, change the
speed and confirm with OK: the
OK stirrer stirs at the new rate.

– Press the Run key to switch back to the Analysis menu.

58 DL31/DL38
7.2 Burette

The following functions are possible under this menu:

Burette BURETTE Rinse
Start and stop the rinsing process
Rinse (rate: 100%) with <F3>.
Rinse tip
Dispense: 0.010 mL Notice: Always place the dispensing
Help Modify Start tubing in a waste beaker!

Rate: 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.
Start: 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.
Rinse tip
Start: 5% of the burette volume are delivered to eliminate any diffusion
of solvent in the dispensing tubing tip.
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.

Burette BURETTE With <F2> this mask appears in

which you can modify the dispensing
Volume [mL] 0.010 parameters.
Burette 5 mL
With <F3> you can stop the dispens-
Fill rate [%] 100
Start ing.

DL31/DL38 59
7.3 Pump

Pump PUMP With the aid of the pump you can

To empty, press <F3>
To fill, press <F3>
and press and hold
blue pump button
Start
add solvent to the titration vessel
and siphon it off. You switch the
pump on and off with <F3>. While
the pump is running, you can switch
on the stirrer with <F2>.

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>.
Notes
1. The pump switches off automatically when the pumping time
defined in the Setup menu is reached (see Section 4.6).
2. Each pumping operation resets the solvent capacity to the value
defined in the Setup menu (see Sections 4.6 and 8).
3. 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.

60 DL31/DL38
7.4 Results

The following functions are available in this menu:

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

"All results" is accessible when one result is available.

"Statistics" are accessible when 2 results of a sample series are
available (see Section 6.2.4).
"Report" is accessible when a drift determination has been performed
or a result is available.
"Statistics series" 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 (see Section 7.4.2).
– 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.

DL31/DL38 61
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.
Notes
1. As "Result" the sample whose determination was terminated with
the error message "No titration!" is also stored.
2. 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.

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.
Recalculn RESULTS
Method 11
Sample 1
R1 = 0.77 % DL31: R = 0.77 %
Sample 2 ▼
Modify OK

62 DL31/DL38
Recalculn RESULTS If you change one of the values, you
Probe 1 can nullify it with "Undo". With <F1>
Drift [µg/min] 6 the changed values are always reset
Conc. [mg/mL] 4.9875 to the original values.
Blank [µg] 0▼
Undo OK

Recalculn RESULTS The sample with the changed result

Method 11 is marked by an asterisk.
*Sample 1
R1 = 0.77 %
Sample 2
Modify OK

Notes
1. The values obtained in the determination always remain stored so
that you can also nullify changes later.
2. Under "All results" you can print out the recalculated results. Here,
the changed values and the original are reported.
3. DL38: The changed results are also taken into account for the
statistical data (see Section 7.4.5).
4. 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.

DL31/DL38 63
7.4.3 Report

Report RESULTS At the end of every determination,

you can print out an (additional) data
Output Print.+Comp. report or send it to the computer. If
Type GLP you change the result of this last
determination beforehand, it will be
Help Modify OK printed out marked by an asterisk.

7.4.4 Calculations (DL38 only)

Calculations RESULTS At the end of every titration you can

perform additional calculations for
R = x [mg]*f this sample.
f = 1.0000
With OK the result is displayed and
Unit mg▼
Help Modify OK can then be printed out.

7.4.5 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 stand-
ard 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.

64 DL31/DL38
Example of a statistical evaluation of 3 samples:
Statistics RESULTS Using the result list (press <F1>) you
Method 11 decide what sample result is an
R1 n = 3 outlier and then delete it.
x = 0.77 %
▼
If you delete "Sample 1" with <F1> ,
s = 0.102194 %
Result Print OK "Undo" is superimposed to allow you
nullify the command. At the same
time, sample 1 is marked as "delet-
Statistics RESULTS
Method 11 ed".
Sample 1
R1 = 0.77 %
Sample 2 ▼ Confirm OK to show the following:
Delete OK (Example: Sample 1 is deleted)

Statistics The statistical data are calculated

RESULTS with the changed number of sam-
Method 11
R1 n = 2
ples. You can delete several sample
x = 0.70 % results and print out the result each
Result Print OK time.

As long as the result list of this sample series is stored, you can nullify
the deletion operation (see also Note in Section 7.4.2).

7.4.6 Statistics series (DL38 only)

Stat. series RESULTS With the aid of this function you can
End series? terminate a sample series. This de-
No letes all data in the result memory, a
Yes subsequent analysis with the same
method restarts with "Sample 1".
OK

DL31/DL38 65
8 Information menu
The measured values and menus below are stored under the i key:

Solv. capac.[mL] 80
Drift [µg/min] 0
KF learn titration
Hello! (Tutorial)
Hardware tests

Solv. capac. The solvent capacity defined in the Setup menu is en-
tered as an initial value (see Section 4.6). 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 compen-
sation if you have defined "Drift: Determination" as a
method parameter (see Section 5.2).
KF learn t. The course of this titration is described in Section 6.6..
Tutorial As you get to know the titrator step by step, the proce-
dure is not described.
Hardware The functions of this menu which you can use to test the
tests hardware of the titrator are described in Section 9.3.

66 DL31/DL38
9 Error messages and malfunctions
9.1 Error messages from the titrator

Here, the error messages which refer to this section or are not self-
explanatory are explained.

1. 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 proc-
ess; 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.

DL31/DL38 67
2. If the following three displays appear, parts of the hardware may
be faulty.

Internal error: x OS ERROR: x

P1: xx
xxxxxxxxxxxxxxxxxxxx P2: xx
xxxxxxxxxxxxxxxxxxxx D1: xx
xxxxxxxxxxxxxxxxxxxx D2: xx
SYSTEM IS BLOCKED! SYSTEM IS BLOCKED!
See manual: Errors Please call METTLER
TOLEDO service

ERROR: x

SYSTEM IS BLOCKED!
Please call METTLER "x": represents letters and/or
TOLEDO service 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).
4. Then switch off the titrator.
3. Please inform METTLER TOLEDO service of these points and
the attached peripheral units with the defined configuration.

3. If the following warning appears, you must press any key: The
titrator can continue to function.
You should regard the executed action as failed and repeat it.On
no account consider the result of a determination terminated in
this manner!

68 DL31/DL38
Warning: x
"x": represents a numberl
Press any key
to continue
If the warning appears frequently,
you should take the measures de-
scribed under point 2.

4. Faulty data deleted!

a. 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 complete-
ly. 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.
b. 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 param-
eters 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.

DL31/DL38 69
5. 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
compute .

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
before you contact the service. See Section 9.3.

Error Possible cause Rectification

No display on Instrument not attached Attach to power supply,
titrator to power supply otherwise contact
service

Several points of the Contact service

display are missing See also Section 9.3.1

The display and the Contact service

key do not match See also Section 9.3.1

Transmission error Peripheral device faulty Check attached devices

to attached or switched off for correct functioning
peripheral device See also Section 9.3.2

70 DL31/DL38
 Error Possible cause Rectification

Device (printer, Instrument not switched Switch on instrument;

balance, computer) on; wrong settings settings and
does not react and/or confi- configuration must
guration (switch match, see Sections
settings wrong) 4.5 & 9.3.2; Cable
Wrong cable see Section 11.2

Pump does not Suction tubing not Connect suction

function connected, tubing and check
Titration stand leaks connections,
see Section 10.3;
Pump faulty Check pump, see
Section 9.3.3

TTL inputs or outputs Inputs and/or outputs Check inputs/outputs,

do not function faulty see Section 9.3.3

Burette and stopcock Burette drive faulty Contact service

do not move to zero
position on switching on

Magnetic stirring bar Cable of magnetic Check magnetic

does not rotate stirrer not plugged in stirrer, see also 9.3.3;
properly Change mag. stirrer
Wrong magnetic Use bar supplied,
stirring bar see Section 11.1

Wrong potential Electrode faulty or Check electrode (see

values contaminated electrode specifica-
tions bulletin)
Use new electrode

No dispensing, titrant Burette tip blocked Clean burette tip

expelled from
stopcock or piston

DL31/DL38 71
9.3 Checking hardware

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 function-
ing correctly. If you order the connector set for the interface check, you
can also test the interface and the TTL inputs and outputs 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

72 DL31/DL38
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.

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 or EPSON)

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.

DL31/DL38 73
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" ap-
pears.

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:
1. A "noise" must be heard.
2. 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").
3. For dispensing, you must always press the lower button (⇓ arrow),
for siphoning off the upper button (⇑ arrow).

74 DL31/DL38
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) 1. Carefully slide the magnetic stir-
ring bar supplied into the titration
vessel.
2. Insert the titration vessel with the
lug of the threaded ring into the
Threaded ring middle groove of the titration arm
with lug
and push downward towards the
Connector stirrer. Fasten the screw.
Stopper ST 7.5
3. Place the three-hole adapter, the
3-hole adapter
ST stopper and the connector in
O-ring
the cover openings.
4. Fill a drying tube with molecular
Titration vessel sieves, close with the cover and
"push" into the titration stand to
Cover ensure tightness. Connect the
and dry- cover and the connector by sili-
ing tube
Seal
con tubing.

Screw

Groove of
titration arm

Titration stand

DL31/DL38 75
10.2 Installing the burette
1. Screw the burette with holder onto the titrant bottle, see Section 2
in the DV100x operating instructions.
WARNING 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.
Hole for 3. Push the burette onto the titrator:
dispensing
Driver cam tubing 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 oppo-
site direction to the arrow and when
pushing in check whether the piston
rod of the burette is correctly posi-
tioned in the push rod.
5. Turn the arresting knob in the direc-
Push rod of the Arrestment
burette drive knob tion of the arrow to fasten the bu-
rette.
6. Place the dispensing tubing in the
cover opening.

NOTICE When you rinse burette and tubing, place the dispensing
tubing in a waste beaker; do not dispense in the titration
vessel!

76 DL31/DL38
10.3 Installing the solvent and waste bottles

Screw sleeve 1. Open the solvent bottle, lay in the

gasket and screw on the screw cap
Socket
(you may need an adapter, see
Screw cap
DV100x Operating Instructions )
Gasket 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
Dispensing or bottle supplied. Push the suction tub-
suction tubing
ing 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
Adjusting
sleeve up again.
Teflon seal 6. Fill two drying tubes with molecular
sieves and place them in the screw
cap of the bottles.

DL31/DL38 77
 7. Push the silicon tubing (450 mm)
over the drying tube cover of the
waste bottle and connect to the suc-
tion fitting of the pump.
8. You can connect the output fitting to
tubing to lead off the solvent vapor to
a suitable place.
Output Suction
fitting fitting

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

10.4 Attaching the magnetic stirrer, electrode and devices

RS232C interface
for balance

RS232C
DV705 interface for
connection GA42 printer

RS232C interface
Stirrer output for computer

TTL-I/O interface
Electrode
input (KF) Centronics interface
for EPSON-com-
patible printers
Pump unit

Connector for On/off switch

power cable

78 DL31/DL38
1. Magnetic stirrer
On delivery, the magnetic stirrer
is pushed into the slot for the
Magnetic
burette drive. Attach its cable to stirrer
the stirrer output.

2. 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.

3. 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
(the required cables are listed in Section 11.2).

DL31/DL38 79
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.

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 (al-
ways 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).

80 DL31/DL38
10.6 Maintenance and servicing
10.6.1 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 deterio-
rates 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.

10.6.2 O-rings
You should replace the O-rings of the screw caps when the system is
no longer tight (see Section 11.2):
– 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).

10.6.3 Dispensing and suction tubing

You should replace the pump tubing when the Teflon seal is no longer
properly tight (wear and tear).

DL31/DL38 81
10.6.4 Molecular sieves
If the drift of the KF solution remains too high, you should fill the drying
tubes with fresh molecular sieves.
You can regenerate molecular sieves in a drying oven at 160 - 300 °C
for at least 24 hours. As the molecular sieves used on the waste bottle
also contain SO2 , you should rinse them with deionized water before
regeneration.

10.6.5 Pump unit

If the diaphragm pump no longer functions, you
can replace it (see Section 11.1):
– Pull out the pump unit and insert a new one.

10.6.6 Pump button

If the pump button becomes too brittle, you should replace it (see
Section 11.1):
– Remove the button and place a new one over the ring.

10.6.7 Magnetic stirrer

If the magnetic stirrer is faulty, you can replace it (see Section 11.1):
– Swing out the titration arm and push the mo-
tor out of the burette slot.
– Push in the new magnetic stirrer and attach
its cable to the stirrer output.

10.6.8 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. (See
also Section 9.1, point 4.)

82 DL31/DL38
10.6.9 Disposal
Contact your METTLER TOLEDO dealer if you have to dispose of the
titrator.

DL31/DL38 83
11 Standard and optional equipment
11.1 Standard equipment

1 KF titrator according to order

1 Power cable according to order
1 Set Operating Instructions according to order
1 Application brochure 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 burettes enclosed
in the burette package.

84 DL31/DL38
 4 drying tubes 1 dispensing tubing
with cover with Teflon seal

1 suction tubing
with Teflon seal

1 drying 1 silicon
tube holder tubing
1 connector

A 5 mL
interchangeable 1 seal
burette incl. 1 L 1 stopper ST
brown glass 7.5
bottle
1 siphoning
1 titration tubing
vessel with
cover incl. 3- 2 screw caps
hole adapter with flat seal
with stoppers
1 pump button

One 1 L brown glass bottle

1 magnetic 1 magnetic 1 double platinum pin electrode DM143-SC

stirring bar stirrer incl. 1 electrode cable (SC-LEMO-60)

DL31/DL38 85
 Order No.
Threaded ring 51107459
Cover with 51107462
• three-hole adapter each with 1 ST 10
ST 7.5 and needle hole stopper 23982
• Stopper ST 7.5 (set of 5) 23452
• Connector 23957
O-Ring 51190366
Titration vessel (nominal volume: 250 mL) 51107463

Fastener screw 51107474

(for titration vessel)

Magnetic stirring bar 51107607

Magnetic stirrer 51107564

Silicon tubing 133 mm 51107480

Drying tube holder 23915

Drying tube with cover 23961

Seal 51107492
(drying tube of titration stand)

86 DL31/DL38
 Order No.
1-L brown glass bottle 71296

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

Screw cap 23937

Pump tubing 51107481

(suction/dispensing tubing)

Silicon tubing 450 mm 51107490

(suction tubing)

Pump unit 51107479

Pump button 51107600

Double platinum pin electrode DM143-SC

Triaxial cable SC-LEMO-60 89601

(length: 60 cm)

1 Bottle molecular sieves 71478

DL31/DL38 87
 Order No.
Operating Instructions
- German 51709849
- English 51709850
- French 51709851
- Spanish 51709852
- Italian 51709853
Application brochure
- German 51709854
- English 51709855
- French 51709856
- Spanish 51709857
- Italian 51709858

11.2 Optional equipment

Drying oven DO305

POWER

TEMPERATURE

°C

HEATING

140 160
100120 180200

80
220
60
240
40
260
OFF
280
300

O-ring: set of 4 51107496

(for screw caps)

Thermostatable beaker 51107497

1 Set stoppers for three-hole adapter 25883

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

Connector set 51107790

(for interface check)

88 DL31/DL38
 Order No.
Septum stoppers
- ST 10: set of 10. 23949
- ST 24: set of 10. 23950
Weighing boat
- glass, ø 20 x 60: set of 5 23951
- glass, ø 30 x 80: set of 5 23952
- PE, ø 25 x 65: set of 5 23953
- PE, ø 38 x 100: set of 5 23954
Syringes
- 1 mL: package of 100 71492
- 10 mL: package of 100 71482
Injection needles
- 80 x 1.2 mm: package of 12 71483
- 80 x 0.8 mm: package of 100 71484

Triaxial cable SC-LEMO-100 89602

(length: 100 cm)

Connection cable for

METTLER TOLEDO balances
- AM, PM, AT 229029

- AG, AB, PB, PG with LC interface 229065

- AB, PB, PG-S with RS9 interface 11101051

DL31/DL38 89
 Order No.
- with the Options 03, 011, 040 59759

Connection cable for

SARTORIUS balances 51190363

Connection cable for GA42 Printer 51190362

Connection cable for EPSON-

compatible printers 51107780

Connection cable for computers

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

Installation disk
Software DLWin or DLWin+ 51106120
DLWin V.xx

for IBM-compatible computers (+) 51106121

1 Installation disk
DLWin V.xx
2 ME-51106120

© Mettler-Toledo AG 1995

(MS-Windows version: ≥ 3.1)

© Mettler-Toledo AG 1995

(MS-Windows NT) incl.

Operating Instructions

TBox DR42 (control of DR42

OUT 1
OUT 2
OUT 3
IN 4
OUT

1
2
ON
IN

OUT 1 OUT 2

24 VDC 1.2 A

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

OUT 4

TBox DR42
external devices via TTLIO)

Connection cable for TBox DR42 51190589

Description of the computer interface

- English 51709876
- German 51709875

90 DL31/DL38
12 Technical data
Power supply
• Voltages 100 – 240 VAC ±10%
• Frequency 50/60 Hz
• Power consumption 45 VA
• Fuse T3,15H250V (not interchangea-
ble)

Dimensions Width: 240 mm, depth:

305 mm, height: 370 mm
Weight approx. 5 kg

Ambient conditions
• Ambient temperature +5 °C to +40 °C
• Atmospheric humidity max. 80% at 40 °C
• Use indoors
• Overvoltage category II
• Pollution degree 2

Materials
• Titrator housing Polypropylene
• Titration stand Polypropylene
• Keypad housing Polyester
• Membrane keypad Polyester
• Dispensing/suction tubing FEP
• Siphoning/connection tubing Silicon
• Three-hole adapter Polypropylene
• O-ring (screw cap) EPDM
• O-ring (threaded ring) FEP/silicon
• Ring seal (bottle) PTFE/silicon
• Seal (dispensing/suction tubing) PTFE
• Connector Polypropylene

DL31/DL38 91
Measurement principle
End point indication
Control
Measurement range
Volumetric water content determina-
tion following Karl Fischer
Voltametric: voltage measurement at a
polarized double platinum pin electrode
Fuzzy logic control (parameters
changeable)
Several ppm to 100% water

Measurement system
KF input Triaxial socket
• Current source
- Range -110 µA to +110 µA
- Resolution 1 µA
- Max. permissible errors 2%
• Voltage range
- Range -2000 mV to +2000 mV
- Resolution 1 mV
- Max. permissible errors 0.5%

Outputs
Magnetic stirrer Type: solid state
• Output 8-pin socket (mini DIN)
• Speed software-controlled (1-100%)
• Power 2 W (24 V)
External titration stand Type: DV705
• Output 5-pin socket (mini DIN)
- Magnetic stirrer DC motor
Speed software-controlled (1-100%)
Voltage range 0 to 18 VDC (max. 300 mA)
- Pump
Voltage 24 VDC (max. 400 mA)

92 DL31/DL38
 Burette drive module
Drive Stepper motor
Resolution 1/10000 of the burette volume
Max. permissible errors 0.3% relative to the respective
burette volume of 5, 10 and 20 mL
Fill time minimal 20 s (rate can be set
between 10 and 100%)
Delivery time minimal 20 s

Interchangeable burettes
Volume 1, 5, 10 and 20 mL
Materials which come
into contact with the Fluoroplastic, borosilicate glass,
titrant ceramic

Magnetic stirrer (solid state)

Max. speed 1500 rpm
Power consumption 2W

Diaphragm pump
Voltage 24 VAC (4 W)
Pressure buildup approx. 180 mbar

Display
Liquid crystal display 6 lines. 20 characters per line,
backlit
Languages English, German, French, Spanish
and Italian

DL31/DL38 93
Memories
Database
• KF standard method 1
• Tutorial method 1
• KF learn method 1
• METTLER methods 10 (DL38 only)
User data memory
• User methods DL38: max. 50 / DL31: max. 1
• KF titrants DL38: max. 20 / DL31: max. 10
• KF standards DL38: max. 20 / DL31: max. 10
• Br number titrants DL38: max. 5 / –

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; baud rate: 2400, data bits: 8
Attachment via Centronics interface
(25-pin, D-sub-connector) for commercial
EPSON-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
TBox DR42 or Attachment via TTLIO socket
third-party devices (9-pin, D-sub)

94 DL31/DL38
RS232C connector (balance/GA42/computer)
Pin
assignment
5
9 RxD (In) 2 Data to titrator
4 Data from titrator
8 TxD (Out) 3
3 470 Ω Handshake from titrator
7 DTR +12 V 4 fixed to operational
2 readiness
6 GND 5
1 Signal ground, galva-
Titrator nically connected to
titrator electronics

TTL-I/O socket (TTL: transistor transistor logic)

Pin
assignment
In: TTL; short-circuit-
IN1 1 proof; Pulse ≥150 ms
1 (the input signal for the
6 IN2 2 titrator must be at least
2 OUT1 3
7 150 ms)
3 OUT2 4
Out: Open collector
8 OUT3 5 • Vce max. = 24 V
4 OUT4 6
9 • Ic max. = 20 mA
5 7
GND: Signal ground,
GND 8 galvanically connected
Titrator to titrator electronics

DL31/DL38 95
Centronics socket
Pin
assignment

\Strobe 1 Data ready

PD0 2
PD1 3
13 PD2 4
25 PD3 5
12 PD4 6
24
11 PD5 7
23 PD6 8
10 PD7 9
22 \ACK 10 Data accepted
9 \BUSY 11 Printer busy
21
8 PE 12 End of paper
20 SLCT 13 Printer active
Automatic
7 \AUTOFDXT 14 line feed
19 \ERROR 15 Printer error
6 \INIT 16 Printer initialized
18
5 \SLCTIN 17 Printed selected
17 18
4 19
16 20 Signal ground,
3 21 galvanically
15 connected to
2 22 titrator elec-
14 23 tronics
1 24
25

Titrator

96 DL31/DL38
13 Index
<F1>...<F3> 6
Access for expert/routine 22
All results 61
Amount of sample
(calculating) 29
Analyse (Run) 41
Arrow keys 9
Author 35
Auto start 30
Auxiliary function keys 8
Auxiliary functions 58
Balance (attaching) 79
Balance (defining) 19
Balance (weight transfer) 48
Battery (replacing) 82
Beep 23
Blank 32
Br No. titrants 14
Bromine number deter-
mination 54
Bromine number method 38
Burette (auxiliary fct.) 59
Burette (installing) 76
Calculation 1 (Br No.) 40
Calculation 1 (KF) 33
Calculation 2/3 (KF) 34
Calculation formula (Br No.) 55
Calculation formula
(KF conc.) 51
Calculation formulae (KF) 49
DL31/DL38
Calculations (auxiliary fct.) 64
Centronics socket 96
Cleaning 81
Command keys 6
Computer (attaching) 79
Computer (defining) 20
Computer method 42
Concentration (KF) 12
Concentration determination
(KF) 51
Control parameters (Br No.) 38
Control parameters (KF) 31
Database 94
Date 22
Delay (time) 32
Dispense 59
Disposal (of titrator) 83
Drift 32
Drift compensation 48
Drift determination 53
Drift stop 32
Drift value (i key) 66
Duration (KF titration) 48
Electrode (attaching) 78
Emptying (titration vessel) 60
End point (KF) 31
Entry (amount of sample) 29
Entry keys 9
Error messages 67
Esc key 7
Expert 22
97
Expiry date 42 METTLER methods 37
Mix time 30
Fill rate 59 Molecular sieves (replacing) 82
Filling (titration vessel) 60
O-rings (replacing) 81
GLP 34 Operating concept 5
Optional equipment 88
Hardware tests 72
Help texts 1 Peripheral interfaces
(checking) 73
Peripherals 18
i key 9
Polarization current 31
Information menu 66
Post consumption 48
Inputs and outputs
(ckecking) 74 Predispensing 30
Installation 75 Pretitration 43
Printer (attaching) 79
Printer (defining) 18
Keypad 5
Pump (auxiliary fct.) 60
KF learn titration 55
Pump button (replacing) 82
KF standard method 26
Pump unit (replacing) 82
KF standards 15
Pumping time 24
KF titrants 12
Putting into operation 5

Language (changing) 10
Recalculation 62
Report (auxiliary fct.) 64
Magnetic stirrer (attaching) 78 Report (method parameter) 34
Magnetic stirrer (replacing) 82 Reset key 7
Main methods 17 Resources 11
Maintenance 81 Result (DL31) 32
Malfunctions 70 Results (auxiliary fct.) 61
Max. srel 33 Rinse tip 59
Menu keys 7 Routine 23
Method parameters (Br No.) 38 RS232C connector 95
Method parameters (KF) 29 Run (analysis menu) 41
Methods 25

98 DL31/DL38
Safety measures 2 Titrant (method parameter) 30
Sample determination Titration stand 20
(Br No.) 54 Titration stand (equipping) 75
Sample determination Titrator (overview) 4
(KF, Br No.) 45 Titrator ID 22
Sample determination (KF) 46 TTL inputs & outputs 80
Sample parameters (Br No.) 40 TTL-I/O socket 95
Sample parameters (KF) 29 Tubing (replacing) 81
Sample series 50 Tutorial 6, 66
Series (terminating) 65 Type (sample) 29
Settings 21
Setup 11 User data memory 94
Solvent bottle (installing) 77 User interface (checking) 72
Solvent capacity 23,66 User list 22
Speed (stirrer) 30 User methods 37
Standard equipment 84
Standby (method parameter) 34
Wait time 30
Standby mode 44
Waste bottle (installing) 77
Starting a method 41
Weight transfer 48
Statistics (changing) 64
Statistics (method
parameter) 33
Statistics (printout) 64
Statistics series 65
Stirrer (auxiliary fct.) 58
Stirrer speed 30
Storage procedure
13, 14, 16, 35

TBox DR42 (attaching) 79

Technical data 91
Termination parameters
(Br No.) 38
Termination parameters (KF) 31
Time 22

DL31/DL38 99
 Declaration of conformity
We, Mettler-Toledo GmbH, Analytical, Sonnenbergstrasse 74, CH-8603
Schwerzenbach, Switzerland, declare under our sole responsibility that the
products listed below – marked with “CE” – are in conformity with the
directives mentioned.

98

Product Directive

73/23/EEC
DL31 Low voltage
DL38
89/336/EEC
Electromagnetic compatibility

Schwerzenbach,
August 1998

Dr. Bernhard Grob Dr. Rolf Rohner

General Manager Marketing Manager
Business Unit Analytical Titration

The following standards have been applied for the declaration of conformity:

EN61010-1: 1993 + A2: 1995 Safety regulations

EN55011 Kl. B: 1991 Emissions

EN50082-2: 1995 Immunity

DL31/DL38 101
 Safety testing of our products
These products have passed the required safety tests for electrical prod-
ucts for the approvals and marks mentioned.

Switzerland Canada
Standard
CAN/CSA-C22.2 No. 1010.1-92
UL Std. No. 3101-1
MG8 NRTL/C FCC, Part 15, class A

ISO 9001 certificate for METTLER TOLEDO

The Mettler-Toledo GmbH company, Greifensee, was examined and eval-
uated 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.

FCC rules
This equipment has been tested and found to comply with the limits for a
Class A digital device, pursuant to both Part 15 of the FCC Rules and the
radio interference regulations of the Canadian Department of Communica-
tions. These limits are designed to provide reasonable protection against
harmful interference when the equipment is operated in a commercial
environment. This equipment generates, uses and can radiate radio fre-
quency energy and, if not installed and used in accordance with the
instruction manual, may cause harmful interference to radio communica-
tions. Operation of this equipment in a residential area is like to cause
harmful interference in which case the user will be required to correct the
interference at his own expense.

102 DL31/DL38
 Declaration of System Validation

We herewith inform you that the products/systems:

DL31, DL38

including software and accessories were developed, tested and suc-

cessfully 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 require-
ments, we will make the following documents available to an autho-
rized, 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 docu-
ments and their reproductions and may require a non-disclosure
agreement to be provided by those requiring access to these docu-
ments.

Schwerzenbach, Wolfgang Machill Dr. Rolf Rohner

August 1998 Quality Manager Marketing Manager
Titration

DL31/DL38 103
Product Life Cycle Model

Ideas

Project Study Project release

Project Start Phase: Product Guidelines

Basic Know how Performance Specifications

Quality Plan

Documentation Plan

Project Plan

Review Report

Phase: Software Specifications

Feasibility Test Plan

Review Report

Phase:
Confirmation Review Report

Phase:
Project End Readiness Review Report

Usage Customer Complaints (CRIS)

Customer Requirements

Phase out

104 DL31/DL38
 DL31/DL38
Switching from routine to expert mode

Settings SETUP Select this line in the Setup

Titrator ID
▼
menu.
Acces for Routine – While holding down the
Beep Yes Shift key, press key 1 three
Solv. capac.[mL] 80▼
times:
Help OK

Settings SETUP “Modify” is assigned to <F2>

Titrator ID
▼
allowing you to select “Ex-
Acces for Routine pert”.
Beep Yes – Confirm OK to save the
Solv. capac.[mL] 80▼
change.
Help Modify OK
✃

DL31/DL38 105
To protect your METTLER TOLEDO product’s 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 ME-51709850

Printed in Switzerland 9808/2.11

Mettler-ToledoGmbH,Analytical,Sonnenbergstrasse74,
CH-8603Schwerzenbach,
Tel. (01) 806 77 11, Fax (01) 806 73 50, Internet:http://www.mt.com