Mettler Toledo DL31, DL38 Operating Instructions Manual

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Operating Instructions

KF Titrators

DL31 / DL38

Contents

Page

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

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

2.1 Measures for your protection .......................................................................................... 6

2.2 Measures for operational safety ...................................................................................... 6

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

3.1 Putting into operation .................................................................................................... 8

3.2 The operating concept ................................................................................................... 8

3.2.1 The command keys....................................................................................................... 9

3.2.2 The menu keys ........................................................................................................... 10

3.2.3 The auxiliary function keys ........................................................................................... 10

3.2.4 The key................................................................................................................11

3.2.5 The entry and arrow keys ............................................................................................. 11

3.3 Changing the language ............................................................................................... 12

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

4.1 KF titrants ..................................................................................................................13

4.2 Br No. titrants (DL38 only) .......................................................................................... 15

4.3 KF standards .............................................................................................................. 16

4.4 Main methods (DL38 only).......................................................................................... 17

4.5 Peripherals................................................................................................................. 18

4.5.1 Printer ....................................................................................................................... 18

4.5.2 Balance ..................................................................................................................... 19

4.5.3 Titration stand............................................................................................................. 19

4.5.4 Computer ...................................................................................................................19

4.6 Settings .....................................................................................................................20

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

5.1 The KF standard method .............................................................................................. 23

5.2 KF method parameters ................................................................................................ 24

5.2.1 No. (of the method) .................................................................................................... 24

5.2.2 Title (of the method).................................................................................................... 24

5.2.3 Sample parameters ..................................................................................................... 24

5.2.4 Speed ........................................................................................................................ 24

5.2.5 Mix time .................................................................................................................... 24

5.2.6 Titrant ........................................................................................................................ 24

5.2.7 Volume (for predispensing).......................................................................................... 25

5.2.8 Wait time (after predispensing)..................................................................................... 25

5.2.9 Auto start (DL38 only)................................................................................................. 25

5.2.10 Control parameters...................................................................................................... 25

5.2.11 Termination parameters ............................................................................................... 25

5.2.12 Blank ........................................................................................................................ 26

5.2.13 Drift ........................................................................................................................... 26

METTLER TOLEDO DL31/DL38 1

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

5.2.15 Calculation (DL38 only) .............................................................................................. 26

5.2.16 Standby ..................................................................................................................... 27

5.2.17 Report ....................................................................................................................... 27

5.2.18 Author of the method ................................................................................................... 27

5.3 Storage procedures ..................................................................................................... 28

5.4 User and METTLER methods (DL38 only) ...................................................................... 30

5.4.1 METTLER methods "908 Bromine No." and "909 Blank Br No." (DL38 only)..................... 31

5.4.2 METTLER method "910 Stromboli" (DL38 only) ............................................................. 32

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

6.1 Starting a method ....................................................................................................... 34

6.1.1 Menu sequence up to standby mode (KF methods) ........................................................ 35

6.1.2 Standby mode ............................................................................................................ 36

6.2 Sample determination.................................................................................................. 37

6.2.1 Weight transfer from a balance ..................................................................................... 40

6.2.2 Post consumption ....................................................................................................... 40

6.2.3 Calculations ...............................................................................................................40

6.2.4 Sample series with statistics (DL38 only) ...................................................................... 41

6.3 Concentration determination ......................................................................................... 42

6.4 Blank determination .................................................................................................... 44

6.5 Drift determination....................................................................................................... 44

6.6 Bromine number determination (DL38 only) .................................................................. 45

6.7 Sample determination with the oven sample changer Stromboli (DL38 only) ..................... 46

6.8 KF learn titration ......................................................................................................... 48

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

7.1 <Stirrer> ....................................................................................................................50

7.2 <Burette>................................................................................................................... 50

7.3 <Pump> .................................................................................................................... 51

7.4 <Results> .................................................................................................................. 52

7.4.1 All results ................................................................................................................... 52

7.4.2 Recalculation ............................................................................................................. 53

7.4.3 Report ....................................................................................................................... 54

7.4.4 Calculations (DL38 only) ............................................................................................ 54

7.4.5 Statistics (DL38 only) ................................................................................................. 54

7.4.6 Statistics series (DL38 only) ........................................................................................ 55

8 Information menu ( key) ....................................................................................... 56

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

9.1 Error messages from the titrator .................................................................................... 57

9.2 Other errors and malfunctions ...................................................................................... 59

9.3 Hardware tests ........................................................................................................... 60

9.3.1 User interface .............................................................................................................60

9.3.2 Peripheral interfaces .................................................................................................... 60

9.3.3 Inputs and outputs ...................................................................................................... 61

2 METTLER TOLEDO DL31/DL38

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

10.1 Equipping the titration stand ......................................................................................... 62

10.2 Installing the burette .................................................................................................... 63

10.3 Installing the solvent and waste bottles.......................................................................... 64

10.4 Attaching the magnetic stirrer, electrode and devices ....................................................... 65

10.5 Using TTL inputs and outputs (DL38 only)..................................................................... 66

10.6 Maintenance and servicing .......................................................................................... 66

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

11.1 Standard equipment .................................................................................................... 68

11.2 Optional equipment ..................................................................................................... 70

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

13 Index ........................................................................................................................ 81

METTLER TOLEDO DL31/DL38 3

4 METTLER TOLEDO DL31/DL38

The DL31/DL38 KF titrators

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- or HP-compatible printer to the Centronics interface and, at the DL38's TTLinterface, the METTLER TOLEDO oven sample changer Stromboli. The METTLER TOLEDO LabX titration software allows you to control your titrator via a computer.

The titrators have a tutorial stored which quickly enables you to become acquainted with the operation and method of functioning of the instrument.

The two titrators have the same operation. Differences in the hardware and software are mentioned in the corresponding sections.

These Operating Instructions correspond to software version 2.0 or higher.

Where can you find what information?

These Operating Instructions and the Help texts integrated in the titrator provide a complete description of the method of functioning of the two titrators. Explanations of parameters contained in the Help texts are supplemented here when necessary.

On the Memo card you can find a short overview of menus and methods. The Application brochure explains the theoretical fundamentals of the Karl Fischer titration, the control of

the titration in the DL31/DL38 and documents the METTLER methods stored in the DL38. The Help texts in the titrator provide you with more information or refer you to the Operating Instructions or

the Application brochure. You will find a detailed description of the communication between the titrator and a computer in the

Description of the computer interface.

METTLER TOLEDO DL31/DL38 5

Safety measures

2 Safety measures

The titrators have been tested for the experiments and intended purposes documented in these Operating Instructions. However, this does not absolve you from the responsibility of performing your own tests of the products supplied by us regarding their suitability for the methods and purposes you intend to use them for. You should therefore observe the following safety measures.

2.1 Measures for your protection

– Ensure that you plug the power cable supplied into a receptacle outlet that is grounded! In

the absence of grounding, a technical fault could be lethal.

Risk of

electric shock

– Never work in an environment subject to explosion hazards! The housing of the instru-

ment is not gas tight (explosion hazard due to spark formation, corrosion caused by the ingress of gases).

Risk of

explosion

– When using chemicals and solvents, comply with the instructions of the producer and

the general lab safety rules!

All Karl Fischer reagents are readily flammable and toxic. – In the case of skin contact, immediately wash off with copious amounts of water! – If eye contact occurs, rinse intensively with copious amounts of water and consult a

physician!

2.2 Measures for operational safety

– Have the instrument serviced only by METTLER TOLEDO Service! – Make sure that every connector is in the correct position! Do not damage the connector

pins of the magnetic stirrer cable! Pins damaged by faulty insertion can cause a short circuit at the "Stirrer" output. This renders the titrator non-functional.

– Always wipe off splashed liquids immediately! The instrument is not water-proof.

Caution

– 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!

6 METTLER TOLEDO DL31/DL38

3 The titrator

Burette

The titrator

Titration stand

Titrant bottle

Arrestment knob

Pump knob

Keypad

Rear view

External stand (DV705)

Stirrer output

Electrode input (KF)

Solvent bottle

Waste bottle

Magnetic stirrer

Balance (RS232C)

GA42 printer (RS232C)

Computer (RS232C)

Stromboli, TBox, etc. (TTL I/O)

EPSON- and HP-compatible printers (Centronics)

Pump unit

On/Off switch

Suction fitting

Output fitting

METTLER TOLEDO DL31/DL38 7

Socket for external power pack

The titrator

3.1 Putting into operation

– Plug the supplied external power pack into the titrator’s socket, connect to the power supply and switch

on the titrator: A self-test is performed before the name of the titrator appears (example DL38).

Hello!

Arrow keys

(

) 9

]

[

Del

Shift

Entry keys

<Reset> key

key

Auxiliary function keys

Display

Reset

Burette

Stirrer

Results

Pump

METTLER TOLEDO DL38 Version 2.0

Esc

Setup

Method

Run

Command keys

Menu keys

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

3.2 The operating concept

– Press, e.g. the <Setup> key:

Title line

Selection bar

Resources SETUP

KF titrants Br No. titrants KF standards ▼

Print OK

Name of the key, in other words the displayed list of resources belongs to the Setup menu

Commands

DL31: No "Br No. titrants"!

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

▼ 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). OK Press <F3>: The list of KF titrants appears.

8 METTLER TOLEDO DL31/DL38

The titrator

3.2.1 The command keys

The commands which can be triggered with <F1>...<F3> change according to the selected menu item. The following commands require an explanation:

Hello! When the instrument is delivered, the <F3> command in the initial mask "METTLER TOLEDO..."

is assigned to a Tutorial menu. This is deleted when you have performed the first titration with the Tutorial.

Note You can call up the Tutorial at any time with the key.

OK This command is always a confirmation for what you

• wish to view,

• have viewed or entered,

• wish to adopt from a selection.

Modify When this command appears a

• submenu can appear which can or must be modified,

• a selection menu appears from which you can or must accept values or names,

• an existing parameter value or name can be directly replaced. If a value can be modified or entered only with the keypad, the "Modify" command is missing.

ABC This command always appears when you can select letters or characters, e.g. for a name. In

this case, you can not enter numbers until you have confirmed "ABC" (press <F1>).

Help Information about the selected resource appears.

The <Esc> key

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

Esc

the original values/names remain in force. <Esc> always effects a return to the previous display.

The <Reset> key

The initial mask "METTLER TOLEDO..." reappears: <Reset> is used to terminate analyses or

Reset

other actions. Data that are not stored are lost.

METTLER TOLEDO DL31/DL38 9

The titrator

3.2.2 The menu keys

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

All resources required for the titration such as KF titrants and KF standards are stored in the

Setup

Setup menu and can be changed.

The sample is determined with the aid of a method. All methods necessary for the different

Method

analyses are stored in the Method menu and can be changed. All resources defined in the Setup menu are available for these methods.

DL31: Only one method can be stored. DL38: Fifty user methods can be stored.

The titration is performed in the Analysis menu. The method called up determines the analysis

Run

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 analysis, but can support it, we call them auxiliary functions. They are accessible under the corresponding keys.

You can switch the stirrer on or off and change the stirring speed.

Stirrer

Pump

Burette

You can add or siphon off solvent.

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

Results

10 METTLER TOLEDO DL31/DL38

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

3.2.4 The key

The value of the current solvent capacity, the last drift determination, the last blank value

determination for DL38/Stromboli (METTLER method 910), the "Hello!" Tutorial, the KF learn method and a menu for testing the titrator hardware are accessible with this key.

3.2.5 The entry and arrow keys

The titrator

Shift

CE Del

Shift

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

CE You delete all entered numbers/characters/letters. Del You delete the number/character/letter last entered.

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

User a

Cursor

abcdefghijklm nopqrstuvwxyz ABCDEFGHIJKLM ▼ Help Select OK

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

▲▼ The arrow appears in the display when there are more lines to the list than are visible.

When you press the arrow keys (∇∆) next to the display, the lines are scrolled downwards or upwards. The selection bar is fixed. By pressing <Shift>, ∇ or <Shift>, ∆ the lines are moved a page at a time. The commands that can be executed always refer to the line highlighted by the selection bar.

METTLER TOLEDO DL31/DL38 11

The titrator

3.3 Changing the language

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

Setup

Resources SETUP

KF titrants Br No. titrants KF standards ▼

Print OK

▼

Resources SETUP Peripherals Settings

▼

Settings SETUP

Language English User list Date 20-08-1998▼

Modify OK

–Press the <Setup> key.

– Press the <Shift> and Arrow (∇) once, then press only the Arrow key

to select "Settings".

– Press <F3>, "OK".

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

▼

Settings SETUP

Lengua Español Lista usarios Fecha 20-08-1998 ▼

Modif. OK

12 METTLER TOLEDO DL31/DL38

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

OK Spanish texts appear. Esc English texts appear.

Setup (<Setup> key)

4 Setup (<Setup> key)

In order to perform titrations, the titrator must know the titrants and their concentration. It must know the settings of the attached instruments to transfer the data. In this menu you define and store these resources: You set up your titrator.

When you press the <Setup> key, the list of resources appears:

KF titrants Br No. titrants (DL38 only) KF standards Main methods (DL38 only) Peripherals Settings

The most commonly used titrants and KF standards are already stored in the titrator. You can not only delete these or change their parameters, but also define new ones.

All titrants and KF standards needed for the METTLER methods are stored! If you delete one of these resources, the error message that it is missing does not appear until the start of the titration.

Print Depending on your choice of resource, its list with the corresponding parameters will be printed

out.

OK The list of the selected resources appears.

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

METTLER TOLEDO DL31/DL38 13

Setup (<Setup> key)

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!

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 always appear, only the name of the titrant is missing.

– Change the parameters as described above.

The name of the new titrant must differ from those already stored, otherwise an existing titrant will be overwritten!

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

14 METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

4.2 Br No. titrants (DL38 only)

With <F3>, "OK" the stored titrants for determination of the bromine number appear:

Br-/BrO ... free line for a new titrant

Bromide/bromate solution

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

Name Br-/BrO 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.

New Br No. titrant

You add a new titrant to the titrant list when you confirm the free line with <F3>, "OK". The parameters always appear, only the name of the titrant is missing.

– Change the parameters as described above.

The name of the new titrant must differ from the one already stored, otherwise an existing titrant will be overwritten!

Note You can store 5 titrants for the bromine number.

METTLER TOLEDO DL31/DL38 15

Setup (<Setup> key)

4.3 KF standards

With <F3>, "OK" the stored Karl Fischer standards appear which you can use to determine the concentration of the KF titrants.

di-Na tartrate 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:

Name di-Na tartrate H2O content 15.660 Unit % Batch Type Mass Weight [g]0 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 or volume. "Weight" changes accordingly to "Volume". 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.

New KF standard

You can add a standard to the list of KF standards if you confirm the free line with <F3>, "OK". The parameters always appear, only the name of the standard is missing.

– Change the parameters as described above.

The name of the new standard must differ from those already stored, otherwise an existing standard will be overwritten!

16 METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

Note

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

• The Application brochure offers tips on sample preparation, sampling and the optimum amount of sample.

4.4 Main methods (DL38 only)

When the titrator is delivered, the <F3> command is assigned to the Tutorial "Hello!", in other words you can select its sequence immediately. In this menu you can assign methods to command keys <F1>...<F3> or delete "Hello!".

With <F3>, "OK", the following appears (example on delivery of the titrator):

Main methods SETUP

F1: Free

Modify OK

Main methods SETUP

User methods METTLER methods

Main methods SETUP

F1: Method 910 Title Stromboli

Delete Modify OK

Main methods SETUP

F2: Free

Modify OK

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

You can select a method from the METTLER methods (or from the user methods if available), e.g. "910 Stromboli":

With <F3>, "OK", the following appears:

You can select a different method to configure the <F2> command (press <F2>, "Modify").

If you confirm this display with <F3>, "OK", the following appears:

Main methods SETUP

F3: Hello!

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

Delete Modify OK

METTLER TOLEDO DL31/DL38 17

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

Setup (<Setup> key)

4.5 Peripherals

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

Printer Balance Titrn stand Computer

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

4.5.1 Printer

With <F3>, "OK" the names of the printers which you can attach to the titrator appear.

HP GA42 EPSON None

– Select the attached printer. – With an EPSON or HP printer change the type and possibly the settings with <F2>.

Type Select "PCL3+", "PCL3", "LQ/Stylus" or "LX/SX" Paper Select "Single sheet" or "Fanfold" (see "Feed") Format A4 width = 21 cm, length = 29.7 cm

81/2 * 11" width = 81/2 inches, length = 11 inches 81/2 * 12" width = 81/2 inches, length = 12 inches

Feed Select "Yes" or "No".

Yes Each report starts on a new page; with "Paper: Single sheet" a footer is printed out

on each page.

No The individual reports are separated by a distance of 2 lines.

– If you select an EPSON- or HP-compatible printer, you must enter the following settings:

Standard settings for the printer are printed in bold HP-compatible EPSON-compatible

Type PCL3+ or PCL3 LQ/Stylus or LX/SX Paper Single sheet Single sheet or Fanfold Format A4 or 81/2 * 11" A4, 81/2 * 11" or 81/2 * 12" Automatic feed Yes Yes or No

18 METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

4.5.2 Balance

Unidirectional Bidirectional None

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

Bidirect.

Titrator Balance

Data to titrator

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

Titrator Balance

Command from titrator

Data to titrator

Configuration: "Send Cont."

Configuration: "Send Stable"

("Send on Transfer")

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

4.5.3 Titration stand

Internal External

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

4.5.4 Computer

Defined Not defined

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

Baud rate Select 1200, 2400, 4800 or 9600. Parity Select "Even", "Odd" or "None". Data bits Select 7 or 8 bits. Stop bits Select 1 or 2 bit(s). Character set Select "ASCII" or "DL".

Note If you select "DL", you must specify 8 for the number of data bits!

Start/end Select "'{'/CR" or "STX/ETX".

METTLER TOLEDO DL31/DL38 19

Setup (<Setup> key)

Default settings for the computer

Baud rate 4800 Parity Even Number data bits 8 Number stop bits 1 Character set ASCII Start/end '{'/CR

Note

• The METTLER TOLEDO LabX titration software allows you to control your titrator via a computer.

•

You will find additional information on the communication between titrator and computer in the Description of the computer interface.

4.6 Settings

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

Language User list Date Time Titrator ID Access for Beep Solv. capac.[mL] Pumping time [s]

Language Select English, German, French, Spanish, Italian or Russian. User list Press <F2>, "Modify", and a list of defined names and an empty line ("…") appears

where you can enter a new name. Press "ABC" and you can enter your name. Erase a selected name with "Delete".

You can then select your name for both the development of a method and the performance of the analysis.

Date You can set the date and select the format.

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 You can set the time and select the format.

Hour 10 Minute 20 Format 24 h

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

20 METTLER TOLEDO DL31/DL38

Setup (<Setup> key)

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".

Routine You can

• in the Setup menu only print out the defined resources and view the list of

• in the Method menu only print out the list of methods (DL38 only) and

• in the Results menu not perform any recalculation and not change any

• under the key, select neither the Tutorial, the KF learn titration nor the

Renewed access for experts is described on the last page of these Operating Instructions.

Beep You can select:

Yes Minimum No

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

results and in the case of error messages.

settings.

each method.

statistical data.

Hardware tests menu.

Yes A beep also sounds after each keystroke.

Solv. capac. You can perform several titrations in the same solvent in succession, but its capacity is

limited. In the vicinity of the capacity limit, the reaction rate decreases. You should enter a value for the maximum titrant volume which is suitable for your

sample determinations. If this value is exceeded, the error message "Solvent capacity exhausted" appears.

Only the titrant volume which is consumed during the analysis is summed. The volume which is added, e.g. using the auxiliary function "Dispense" is not taken into account. The difference between the defined value and the titrant consumption is shown under the key.

Pumping time The defined time is a safety criterion: the pump will shut off after this time if you, e.g.

leave the titrator while the pump is running.

METTLER TOLEDO DL31/DL38 21

Methods (<Method> key)

5 Methods (<Method> key)

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

in the DL31 the KF standard method specified by us is stored. You can modify this method and save it under a number.

Methods METHOD

KF standard method

Help Modify

▼

Method METHOD

No. 0 of the method

Help OK

When you have modified and saved the method, the following appears (example):

Methods METHOD

in the DL38 the KF standard method specified by us and 11 METTLER methods are stored. You can modify these methods and save them as user methods.

Methods METHOD

User methods METTLER methods KF standard method Help Print OK

Print The list of methods you have developed is

printed out.

OK The user methods with their defined numbers

and titles appear (example):

Methods METHOD

22 Coffee 33 Tea 113 Powdered milk Delete Print Modify

123 Cellulose KF standard method

Print Modify

A complete titration method comprises sample preparation, mixing and wait times, the actual titration, result calculation and a report. These partial steps are defined in the titrator as parameters which determine the progress of an analysis.

You modify a method

by changing its parameters.

22 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

5.1 The KF standard method

You can use the KF standard method to develop your own method. In this you are guided from one parameter to another in the specified order. Exceptions are sample, control, termination and report parameters, which are shown as a group in a mask. In the case of the DL38, this also applies to the calculation parameters.

With the user and METTLER methods, all parameters appear as a list in a mask. Exceptions are again the above-mentioned groups. The last parameter of a method "Author of the method" always appears in its own mask.

The method is always shown with the following default parameters. The parameters which you can modify are listed in Section 5.2.

No. of the method 0 Title of the method Sample parameters

ID Type Mass Minimum [g] 0.0000 Maximum [g] 5.0000 Entry Before

Speed [%] 35 Mix time [s] 10 Titrant 2-comp 5 Volume [mL] for predisp. 0.0000 (Wait time [s] after predisp. 0)

Auto start No → 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 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 Yes Report

Output Print.+Comp. Type GLP

Author of the method

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

METTLER TOLEDO DL31/DL38 23

Methods (<Method> key)

5.2 KF method parameters

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

5.2.1 No. (of the method)

The method is stored under this number. The numbers 900 – 999 are reserved for METTLER methods.

5.2.2 Title (of the method)

You can give the method a specific name.

5.2.3 Sample parameters ID You can enter an identification for the sample(s) now or just before the titration for every sample

("Request").

Type Select "Mass", "Fixed mass", "Volume", "Fixed volume", "Pieces" or "Fixed pieces". Weight appears when "Fixed mass" is selected. Volume appears when "Fixed volume" is selected. Number appears when "Fixed pieces" is selected. Density appears when "Volume" or "Fixed volume" is selected. Minimum/Maximum

appears when "Mass", "Volume" or "Pieces" is selected. The unit depends on the type of sample: g, mL or pcs. <F1>, "Help" For a fixed or variable amount of sample you can have the titrator calculate

and enter values if you know the approximate water content of your sample.

Entry of the amount of sample before or during the actual titration. "Entry" is faded out when "Fixed

mass", "Fixed volume" or "Fixed pieces" is selected. DL38:

If you select "Yes" for the parameter "Auto start", on storage "Before" is automatically set to "During".

5.2.4 Speed

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

5.2.5 Mix time

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

5.2.6 Titrant

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

24 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

5.2.7 Volume (for predispensing)

A predispensing shortens the titration time and can be entered specific to the sample ("Request").

Note In the user and METTLER methods the parameter is called "Predis.".

5.2.8 Wait time (after predispensing)

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

5.2.9 Auto start (DL38 only) Yes The DL38 begins analysis as soon as a sample has been added. The time for adding a sample

may not exceed 30 seconds or the instrument will revert to its "Standby" mode. You should select "Yes" for determinations in which, e.g. side-reactions could occur during the titration.

5.2.10 Control parameters

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

1 component 2 components Pyridine

Current 20 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.

Current Select 1, 2, 5, 10, 15, 20, 30 or 40 µA for polarization current.

5.2.11 Termination parameters

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

METTLER TOLEDO DL31/DL38 25

Methods (<Method> key)

Vmax

The maximum volume is intended as a safety precaution: It avoids dispensing an unnecessarily large amount of titrant if the titration is faulty.

Drift stop Select "Relative", "Absolute" or "No".

Relative Termination when actual drift is less than the drift measured before the titration (D0)

plus the entered value (Di): D < D0 + Di.

Absolute Termination when the drift is less than the entered value (Di): D < Di. No "Drift [µg/min]" disappears and "Delay [s]" appears.

Delay If you enter "0" for the delay time, the titration is terminated as soon as the end point is reached.

5.2.12 Blank

For the entry of a correct value, you should perform a determination.

[µg] You can enter a value in the method. Request Before each titration, the value is requested individually for each sample.

5.2.13 Drift

The drift value is needed for calculation of the result.

[µg/min] You can enter a value in the method. Request Before each titration, the value is requested individually for each sample. Online The moisture which enters the titration vessel is always measured, evaluated and displayed in

the standby mode.

Determin. Some standard operating procedures require insertion of the value of a drift determination. If

you have performed a drift determination, the result is stored under the key and used in the calculation.

5.2.14 Result (DL31 only)

The water content is calculated with the appropriate formula by selection of the unit: [mg], [µg], [%], [ppm], [mg/pc], [mg or µg] and [% or ppm].

[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

5.2.15 Calculation (DL38 only) Calculation 1

R1 Result of the first calculation. The water content is calculated with the appropriate formula by

selection of the unit: [mg], [µg], [%], [ppm], [mg/pc], [g/kg], [mL], [min], [ppm]ext.extr., [ppm]ext.soln., [%]ext.extr., [%]ext.soln..

26 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

[mL] Titrant consumption up to the end point. [min] Duration of the titration. [ppm]ext.extr., [ppm]ext.soln., [%]ext.extr., [%]ext.soln.

Special calculation for samples which are used after an external extraction or external dissolution. The second and third calculation are needed (see Application brochure).

Unit You can enter a nonselectable unit, e.g. "g" if you define a factor of 0.001 for the calculation of

the H2O content in "mg".

Statistics

To obtain the mean value "x", the standard deviation "s" and the relative standard deviation "srel" of a sample series, you must select "Yes". You can terminate a sample series using the auxiliary function "Results" (<Results> key).

Max. srel If the entered value for the max. relative standard deviation is exceeded, a message appears.

Calculation 2 / Calculation 3

The available parameters are the same as for Calculation 1. Instead of a formula, you can select "No calculation". The following units are missing: [ppm]ext.extr, [%]ext.extr., [ppm]ext.soln, [%]ext.soln.

Note You can not determine samples from an external extraction or dissolution in the routine mode

as you must enter the amount of sample for the extraction/dissolution and the amount of solvent under calculation 2 and 3.

5.2.16 Standby Yes 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. [min] After the sample determination, a switch is made to the "Standby" mode. The subsequent rate

of consumption is displayed and printed out during the defined time.

5.2.17 Report Output 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 or HP-compatible printer.

(GLP report: All data which are required by the rules of Good Laboratory Practice.)

5.2.18 Author of the method

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

METTLER TOLEDO DL31/DL38 27

Methods (<Method> key)

5.3 Storage procedures

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

Method METHOD

Author of the method

Help Modify OK

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

DL31 DL38

Methods METHOD

123 CaCl KF standard method

Help Print Modify

Methods METHOD

4 H3PO 31 Oil

Delete Print Modify

If you have not entered any or a wrong method no., the following appears:

Error

No/invalid value Min: 1.00000 Max: 899.000

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

Method METHOD

No. 0 of the Method

Help OK

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

28 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

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

DL38

Method 22 METHOD Method No. exists Change number Overwrite method

Change number "No. of the method" reappears. Overwrite method The new or modified method is stored, that with

the same number deleted.

While you are modifying a user or a METTLER method, you can press the <Run> key (the <Setup> and Auxiliary functions keys are blocked).

a. If you have not yet modified any parameter of the method, the start mask of the Analysis menu appears. b. If you have already modified a parameter of the method, the mask "Author of the method" appears. The

method is stored with "OK" and the start mask of the Analysis menu is displayed.

METTLER TOLEDO DL31/DL38 29

Methods (<Method> key)

5.4 User and METTLER methods (DL38 only)

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

900 Standard 10 901 Na tartrate 902 Toluene dry 903 Ketone

904 Homogenizer 905 Ext. Extr. 906 KF Oven 907 Gas

908 Bromine No. 909 Blank Br No. 910 Stromboli

You can modify METTLER methods, but in this case you must always give them a number (1-899) so that they are stored as user methods.

You can print out the selected methods by pressing <F2>, "Print".

User methods can be deleted (only in expert mode).

Methods METHOD

22 Coffee 33 Tea 113 Powdered milk Delete Print Modify

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

Delete? METHOD

Yes No

Yes Pressing <F3>, "OK", will delete the method. No Pressing <F3>, "OK", will bring up the list of methods.

The method is not deleted.

METTLER methods cannot be deleted.

Methods METHOD

900 Standard 10 901 Na tartrate 902 Toluene dry ▼

Print Modify

30 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

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

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

No. 908 Title Bromine No. Sample parameters

ID Request Type Mass Minimum [g] 0.2000 Maximum [g] 0.4000 Entry Before

Speed [%] 30 Mix time [s] 120 Titrant Br-/BrO3Predisp. [mL] 0.0000 Wait time [s] 0 Control parameters

Current [µA] 2 End point [mV] 150

∆Vmin [µL] 1.0 ∆Vmax [µL] 20.0 ∆Vmax factor [%] 100

Start Normal

Termination param.

Max. time [s] 6000 Delay [s] 15 Vmax [mL] 20.000

Blank Request

Calculation 1

R1 = x[Br No.]*f1 f1 = 1.0000 Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00

Calculation 2 mL

R2 = x [mL]*f2 f2 = 1.0000 Unit mL Decimal places 3 Statistics No Max. srel [%] 0.00

Calculation 3

R3 = No calculation f3 = 1.0000 Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00

Report

Output Print.+Comp. Type GLP

Author of the method

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. Min./Max. appear when "Mass" or "Volume" is selected. The unit 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.

No. 909 Title Blank Br No. Sample parameters

ID Request Type Fixed volume Density [g/mL] 1.000 Volume [mL] 50

Speed [%] 30 Mix time [s] 120 Titrant Br-/BrO Predisp. [mL] 0.0000 Wait time [s] 0 Control parameters

Current [µA] 2 End point [mV] 150

∆Vmin [µL] 1.0 ∆Vmax [µL] 5.0 ∆Vmax factor [%] 100

Start Cautious

Termination param.

Max. time [s] 6000 Delay [s] 15 Vmax [mL] 10.000

Calculation 1 mmol

R1 = x [mL]*f1 f1 = 0.0500 Unit mmol Decimal places 4 Statistics Yes Max. srel [%] 0.00

Calculation 2

R2 = No calculation f2 = 1.0000 Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00

Calculation 3 Report

Output Print.+Comp. Type GLP

Author of the method

METTLER TOLEDO DL31/DL38 31

Methods (<Method> key)

R1 Result of the first calculation. The bromine number or bromine index is calculated using the

appropriate formula by selection of [Br No.] or [Br index].

[mL] Titrant consumption up to the end point. [min] Duration of the titration.

Unit Bromine number and bromine index are quantities without dimension.

The bromine number is the amount of bromine in [g] reacting with 100 g of sample. The bromine index is the amount of bromine in [mg] reacting with 100 g of sample.

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

5.4.2 METTLER method "910 Stromboli" (DL38 only)

If, according to your needs, you wish to develop an automated determination of water content of thermally stable liquids or solids, then you can modify the METTLER method "910 Stromboli" and store it as a user method.

No. 910 Title Stromboli Sample parameters

Type Mass Minimum [g] 0.0000 Maximum [g] 5.0000

Speed [%] 40 Mix time [s] 300 Set temperature 150 Titrant 1-comp 5 Control parameters

Current [µA] 5 End point [mV] 100

∆Vmin [µL] 0.5 ∆Vmax [µL] 4.0 ∆Vmax factor [%] 100

Start Cautious

Sample parameter The sample parameters "ID" and "Enter" are not applicable,

Termination param.

Max. time [s] 600 Driftstop Rel. Drift [µg/min] 10 Vmax [mL] 10.000

Blank Auto Drift Auto Calculation 1 ppm

R1 = x [ppm]*f1 f1 = 1.0000 Unit ppm Decimal places 3 Statistics Yes Max. srel [%] 0.00

Calculation 2 Calculation 3 Report

Output Print.+Comp. Type GLP

Author of the method

because the sequence

of the sample series is controlled automatically.

Mix time The time (in seconds) during which the water in the sample evaporates completely

and dissolves into the solvent in the titration vessel.

Auto start

This parameter does not apply because the sequence of the sample series is controlled automatically.

Set temperature Enter in °C at the desired temperature at which the water determinations are to be

performed. The set temperature can be selected between 50 °C to 300 °C. This setting cannot be changed during a series. The set temperature is noted in the titration protocol.

32 METTLER TOLEDO DL31/DL38

Methods (<Method> key)

Blank

Drift

The blank [µg] is made up of the water content of the purge gas (time-dependent) and the water content of the sample vessel (independent of time). The determination is performed as a "normal" sample determination with the defined method parameters and, therefore, can be integrated into the series’ sequence. The product of drift and duration (Drift * Duration) is subtracted from the result, so that the blank is an absolute value independent of time. The blank for the Stromboli can be viewed at any time by pressing the key.

Request The value is retrieved prior to the series. Auto The value is determined automatically prior to the sample series ("Blank"

position on the sample rack). The result is stored under the key and automatically integrated into the calculations.

Determination Note

The most recently stored value is used.

A one-time blank determination can be used for various sample series. In order to do this, a method with the method parameter "Blank: Auto" is developed. In the request for the sample parameters enter "0" for the number of samples. The resulting blank value is stored and can be viewed at any time by pressing the key, i.e., it is available for all ensuing sample series.

The drift [µg/min] can be determined at any time in the STANDBY mode (press <F1>, "Drift") or automatically prior to a sample series.

Request The value is retrieved prior to the series. Auto The value is determined automatically prior to the sample series ("Drift"

position on the sample rack). The result is stored under the key and automatically integrated into the calculations.

Determination

The most recently stored value is used.

Standby This parameter does not apply as no post consumption measurements are performed. Protocol The results are printed out at the end of a series. Author "Author of the method" only appears if you change the method.

At the beginning of a sample series, the following parameters need to be entered, provided you chose "Request" in the method:

Mix time [s] Blank [µg] Drift [µg/min] ID [Text] No. of samples [max. 13] Sample parameters (mass, volume, amount, etc.)

METTLER TOLEDO DL31/DL38 33

Analysis (<Run> key)

6 Analysis (<Run> key)

You perform titrations with a selected method. The required data are stored in the Method and Setup menu. You prepare your sample, titrate and obtain the result.

While an analysis is running, all menus and auxiliary functions are blocked.

6.1 Starting a method Preparations

–Press the <Burette> key. Rinse the burette and fill ensuring that there are no air bubbles in the burette and

tubing.

– Press the <Pump> key and fill the titration vessel with approx. 40 mL solvent.

When you press the <Run> key, the start mask appears:

DL31 DL38

Start RUN

Method No. 22 Title User

Help OK

Start RUN

Method No. 22 Title User

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.

• in the DL38 case the number which you enter directly or accept it with <F2> from the METTLER or user

methods is entered.

Note

•You can select the user name. The name which was selected in the analysis last performed remains stored.

• If you have defined an expiry date for the titrant and this has been passed, an appropriate message appears before the pretitration starts. You should then first perform a concentration determination.

• DL38: The start mask always shows the number of the method with which an analysis was last performed, e.g. Method No. 22. If you delete this, "Method not available" appears when you confirm the mask with "OK".

34 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

Start RUN

• The titrator also accepts methods which are stored in the attached computer: When you enter a number whose method is not stored in

Data transfer..

the titrator, the method is requested from the computer (see Description of the computer interface). If it is available, the pretitration is started immediately following transfer; if it is not available, "Method not available" appears.

6.1.1 Menu sequence up to standby mode (KF methods)

Example:

Start RUN

Method No. 22 Title Coffe User C. De Ca

Help Modify OK

▼

DL31: "Modify", is missing. The pretitration starts with <F3>, "OK": It is always executed with the

control parameters of the selected method. The length of the solid bar reflects the addition of the titrant. The vertical bar represents the thresh-

PRETITRATION RUN

old for the transition to the standby mode.

Help

STANDBY RUN

Active method:22 Potential [mV]74 Drift [µg/min] 2→

DRIFT CONZ Sample

➞ This arrow indicates that you can start a determination. ➘ Wait, drift still decreasing! ➚ Wait, drift increasing again!

Press <F1> to start the drift determination, <F2> to start the concentration determination, <F3> to start the sample determination.

Note If the pretitration lasts longer that 10 minutes, a message appears. After confirmation with "OK", a

pretitration again starts. In such a case, you should check whether, e.g. all connections of the titration stand are tight.

METTLER TOLEDO DL31/DL38 35

Analysis (<Run> key)

6.1.2 Standby mode

During standby, the following menus are blocked or selectable:

Blocked

<Setup>, <Burette>, <Pump> and under the key: "Hello!", "KF learn titration" and "Hardware tests".

Selectable <Stirrer>, <Results>, <Method>, <Run> and key (except

"Hardware tests"

"Hello!", "KF learn titration" and

Note If you press the <Run> key, the sample determination is started!

–To switch to the Analysis menu from the selected menu/selected auxiliary function, press the <Run> key.

Stirrer (<Stirrer> key)

You can change the speed. This is reported for the subsequent sample determination.

Results (<Results> key)

The menu is not shown until you have performed the first measurement or a result is available.

Method (<Method> key)

You can modify all methods. With the active method you can not modify the following parameters:

•Titrant

• Polarization current

• End point The modified parameters are adopted for the next sample. For documentation conforming with GLP, you

should print out the method before you switch back to the Analysis menu. Note (DL38 only) If you modify the parameters of the active method, a sample series will be terminated.

If you restart a method, the results of the current series are deleted.

36 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

6.2 Sample determination

With <F3>, "OK", or <Run> you start a sample determination. According to th selected method, the following masks may appear.

In succession, specific parameters are requested if defined in the method as "Request". Example:

ANALYSIS RUN

Mix time [s] 10

Then one of the follwing mask appears:

ANALYSIS RUN H2O exp. [%] 2.00 Weight [g] 0 Minimum [g] 0.3750 Maximum [g] 0.8750

Help Bal.* OK

The mask for the sample entry appears if a variable amount of sample is defined with "Entry: Before".

ANALYSIS RUN

Please add sample

0.3750 g -

0.8750

Help OK

The mask for sample addition appears if a variable amount of sample is defined with "Entry: During" (example: mass).

Note

• If you take longer than 5 minutes for the entry of samples or sample-specific parameters, the titrator switches back to the standby mode.

• If you add a sample while the titrator is in the standby mode without first pressing the <Run> key, the titrator will begin a pretitration to titrate all the water in the sample. Immediately pressing the <Reset> key and thereafter pressing the <Shift> and <Run> keys simultaneously can prevent this. By doing this, the pretitration and standby mode is skipped and one of the above masks appears. In this manner your sample is not "lost".

METTLER TOLEDO DL31/DL38 37

Analysis (<Run> key)

Sequence of the sample determination Example (with "Entry: Before"):

ANALYSIS RUN H2O exp. [%] 2.00 Weight [g] 0 Minimum [g] 0.3750 Maximum [g] 0.8750

Help Bal.* OK

▼

ANALYSIS RUN Add sample or confirm additio

0.3750 g -

0.8750

Help OK

▼

ANALYSIS RUN

Sample**

Drift

▼

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

* Appears only if a balance is defined.

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

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

In the graph, the bar fills and empties in accordance with the drift. The vertical bar represents the end point of the titration.

** Appears only if you have not yet entered the amount of sample. With <F1>, "Sample", the parameter

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

During the titration you can switch between three different displays:

ANALYSIS RUN

Drift: 9500 µg/min

Sample Cont. Graph

ANALYSIS RUN

Content:

42.0012 mg

SampleConsum Graph

ANALYSIS RUN

Consumpn: 1.2010 m Duration: 0:31 m

Sample DriftGraph

38 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

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

Report RUN

Printing...

Result RUN Method 22 Sample 1 R1 = 1.98%

The result is reported before it is displayed.

DL31: R = 1.98%

If you confirm "OK", either

• the standby mask (method parameter "Standby: Yes") appears or

• the start mask (method parameter "Standby: No"), or

• the post consumption mask (method parameter "Standby: [min]").

The result is now stored under the auxiliary function "Results" (<Results> key) so that you can, e.g. recalculate it.

Note If, after the sample addition, the elapsing mixing time is shown and no amount of sample has been

entered, you can also press <F1>, "Sample", to enter the amount of sample.

METTLER TOLEDO DL31/DL38 39

Analysis (<Run> key)

6.2.1 Weight transfer from a balance

ANALYSIS RUN

If you press <F2>, "Balance", in the corresponding mask, the value displayed on the balance appears. It is transferred with <F3>, "OK".

> 1.3245 g

6.2.2 Post consumption

STANDBY RUN Post consumption Duration:0:34 mi Drift: 6 µg/mi

Stop

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

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

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

Sample

addition

Mix time TitrationConfirm Sample Requests Predisp. Wait time

Measured value acquisition

Standby Time measuremnet (duration)

DL38 ("Auto start: Yes")

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

Sample

addition

Mix time TitrationConfirm Sample Requests Predisp. Wait time

Measured value acquisition

Standby Time measuremnet (duration)

40 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

Calculation formulae

H2O [mg] = (consumption [mL] * CONC [mg/mL]) – ((drift [µg/min] * duration [min]) + blank [µg]) * 10-3 [mg/µg]

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

H2O [%] =

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

weight [g]

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

for the H2O content in g/kg by 10.

H2O [mg/pc.] =

H2O [mg]

number [pc.]

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

6.2.4 Sample series with statistics (DL38 only)

If you have selected "Statistics: Yes" in the method under Calculation 1, 2 or 3, results and statistical data of the sample or concentration determinations are stored under the auxiliary function <Results>.

The series is terminated if you

• enter the appropriate command,

• switch off the titrator or an attached Stromboli,

• modify the method parameters of the active method,

• select another method.

A sample series is also terminated if you

• select the concentration determination in the standby mode,

• change the current titrant in the Setup menu after a Reset.

A conc. series is also terminated if you

• select the sample determination in the standby mode,

• change the KF standard during the determinations,

• change the current standard in the Setup menu after a Reset.

The series is not terminated if you stop a determination with <Reset> and perform the next determination with the same method.

Note You can perform a series with maximum 99 samples. The last 60 results are stored. (This is not the

case if operating a Stromboli!)

METTLER TOLEDO DL31/DL38 41

Analysis (<Run> key)

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

Result RUN Method 22 Sample 3 R1 = 1.91 %

x OK

▲

<F1> You can switch between the result and statistics displays.

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

Result OK

▼

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

three samples.

6.3 Concentration determination

For the correct determination of the water content of a sample, you should determine the concentration of the titrant with Karl Fischer standards (see Application brochure).

The concentration is always determined with the control and termination parameters of the active method. A predispensing and wait time defined in the method are not performed, a defined blank value is not incorporated in the calculation and the selection of "Standby: No" is not taken into account. After a concentration determination, a switch to the standby mode is always made to allow duplicate or multiple determinations.

Calculation formula

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

CONC [mg/mL] =

42 METTLER TOLEDO DL31/DL38

consumption [mL] –

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

CONC "old" [mg/mL]

With <F2>, "CONC" appears:

Analysis (<Run> key)

CONC RUN KF standard: di-Na tartrate

Help Modify OK

▼

CONC RUN di-Na tartrate: Batch H2O content 15.660 Unit %

ABC OK

▼

CONC RUN

Mix time [s] 10

▼

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

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

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

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

This mask appears when "Entry: Before" is defined in the method. If "Entry: During" is defined, the sample addition mask appears immediately.

Help Bal.* OK

▼

ANALYSIS RUN

Please add sample

0.0500 g (approx

Help OK

* Appears only if a balance is defined.

The amount of sample suggested in the previous mask is displayed. The further progress corresponds to that of the sample determination.

METTLER TOLEDO DL31/DL38 43

Analysis (<Run> key)

DL31

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

Result RUN Method 22 Sample 2 Conc.= 4.9892 mg/m

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

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 Method 22 Sample 2 Conc.= 4.9892 mg/m

x OK

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

6.4 Blank determination

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

The blank value of the METTLER method "910 Stromboli" is stored under the key.

6.5 Drift determination

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

DRIFT RUN

The length of the solid bar represents the elapsed time.

Duration:4:24 mi

Help

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

44 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

6.6 Bromine number determination (DL38 only)

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

Start RUN

Methode No. 123 Title Bromine N User R. Hube

Help Modify OK

ANALYSIS RUN

Weight [g] 0 Minimum [g] 0.2000 Maximum [g] 0.4000

Help Bal.* OK

ANALYSIS RUN

Consump:

2.3450 mL

Sample**

Result RUN Method 123 Sample 2 Bromine No.= 4

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

* Appears only if a balance is defined.

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

** Appears only if you have not yet entered the amount of sample. With <F1>, "Sample", the parameter

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

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

Calculation formula

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

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

weight [g]

Note Molar mass Br2: 159.8 [g/mol] = 0.1598 [g/mmol]

METTLER TOLEDO DL31/DL38 45

Analysis (<Run> key)

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

The oven sample changer Stromboli is used in combination with the DL38 titrator to automatically determine the water content of thermally stable liquids and solids. For this purpose, the sample is heated in the oven and the evaporated water is transported into the titration vessel by means of a dry inert gas stream. The DL38 controls all of Stromboli’s functions via the METTLER Method "910 Stromboli". Using this method as point of departure, user methods can be developed allowing automatic determination of sample series with up to 13 samples as well as drift and blank determinations. Prior to determination, Stromboli automatically inserts the sample vials on the sample rack into the oven.

The result of a sample determination with Stromboli is made up of the sample’s water content, blank value (water content of an empty sample vial) and drift (sum of the water content of the rinsing vessel over the measuring time "Duration").

The drift determination is automatically performed if "Drift: Auto" was selected in the method. Drift can be determined manually at any time in the standby mode (press <F1>, "Drift"). In both cases the determination is performed with the sample vial in the "Drift" position. The vial is inserted into the oven and the determination is performed for three minutes after the set temperature entered in the method has been reached. The result is stored (i.e., it is available for subsequent sample series) and can be viewed by pressing the key (including date and time of determination).

The blank determination is automatically performed if "Blank: Auto" was selected in the method. The determination is performed with the sample vial in the "Blank" position (empty sample vial). The determination is performed as a "normal" sample determination with the defined method parameters and, therefore, can be integrated into the series’ sequence. The blank value is defined as sample "0" without any content parameters and the default parameter "ID: Blank". The result of the blank determination is stored and can be seen under sample number "0" in the titration report or viewed by pressing the key (including date and time of determination).

Sequence of a sample series

When starting a method from the idle state, the entered, desired temperature is conveyed to the oven. The sample vial in position "Drift" is inserted into the oven and the oven heats to the set temperature during pretitration, i.e., in the standby mode. The temperature display flashes on the Stromboli and the display alternates between current temperature and set temperature. After reaching a constant drift at the set temperature, the sample series can be started from the standby mode by pressing <Run> or <F3>, "Sample".

ANALYSIS #01 RUN ID Weight [g] 0 Minimum [g] 0.0000 Maximum [g] 5.0000

Bal.*Start OK

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

46 METTLER TOLEDO DL31/DL38

Analysis (<Run> key)

No.ID Statu 0 Blank Done 1 Activ 2 Ready 3 Ready

Modify OK

▼

Sample 1 RUN ID Weight [g] 0 Minimum [g] 0.0000 Maximum [g] 5.0000

Help Bal.* OK

* Appears only if a balance is defined.

By pressing <F1>, "Sample" during a series, the current status (ready, active or done) of the samples is displayed. Pressing <F2> "Modify" allows you to alter or complete your entry. After each sample the result is calculated and reported, and the sample series is continued without displaying the results. If a printer is installed, the result is printed out after each sample.

At the end of a sample series the results of the final sample and the series’ statistics (press <F1>, "x") are displayed. In standby mode, the results and statistics can be viewed by pressing the <Results> key.

Note

• If the input of the sample specific parameters takes longer than 5 minutes, the titrator will return to Standby mode. The inputs to this point will then be lost. With a sample series and a Stromboli method, the sample data for the first sample can be entered and the analysis started. The sample data for the remaining samples can be entered while sample 1 is being analyzed by pressing <F1>, "Sample".

• If an analysis is terminated by the termination parameter "Max. time" even though the entire amount of water has not been titrated yet, then the Stromboli’s sample rack returns to its basic position ("Drift" position below the oven) and remains there even during pretitration of the next sample. The Stromboli only moves on to the next sample after the DL38 has gone into standby mode.

• In the following cases the sample series will be interrupted:

•

When one of the following messages appears: "Weight [g] 0", "No titration!", "Capacity exhausted!", "No drift determination performed!", "Blank determination not yet performed!", "CONC determination due!".

•When the calculated value for "srel" is above the value entered in the method. In order to continue the series, the message on the display has to be confirmed by pressing <F3>, "OK",

on the titrator.

• At the beginning of the next series, results and statistics of a series are automatically erased as soon as the message "Series aborted!" is confirmed by pressing <F3>, "OK".

• As soon as a Stromboli is attached to a DL38 and switched on, each titration is started automatically, regardless of whether "Auto start" has been set to "Yes" or "No". The Stromboli must be switched off for

a KF method without Stromboli!

METTLER TOLEDO DL31/DL38 47

Analysis (<Run> key)

t 5

6.8 KF learn titration

If you are unsure what parameters should be entered for your sample, select the learn titration stored under the key. The titrator calculates the range for the amount of sample you need to enter as well as control and termination parameters, stores these and prints them out after the titration.

The learn titration is blocked when an analysis or auxiliary function is running. The learn titration cannot be used with a Stromboli.

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

Method KF-L

No. 55 of the method

Help OK

▼

Method 55 KF-L

Type mass of the sample

Modify OK

▼

Method 55 KF-L

Calculation 1 %

Modify OK

▼

Start KF-L KF learn titra Titrant 1-comp Type 1 componen User V. Müll

Help Modify OK

If you enter a number under which a method is already stored, an appropriate message appears:

DL31:

Although the method is overwritten, you should enter a different number (documentation of the method!).

DL38:

The method is stored as a new user method with a different number.

DL31: Instead of "Calculation 1", "Result" appears.

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

The pretitration starts with <F3>, "OK".

▼

STANDBY KF-L

Active method 55 Potential [mV]87 Drift [µg/min] 2→

Help SAMPLE

48 METTLER TOLEDO DL31/DL38

–

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

Analysis (<Run> key)

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

Analysis KF-L

Weight [g] 0

Help Bal.* OK

▼

ANALYSIS KF-L Add sample or confirm additio

1.2345 g

Help OK

▼

Result KF-L

R1 = 0.61% ! Calculated param ters are stored

▼

STANDBY RUN

Active method:55 Potential [mV]87 Drift [µg/min] 2→

DRIFT CONC. SAMPLE

* Appears only if a balance is defined.

Appears if you have already entered the amount of sample. Otherwise, "Please add sample" appears.

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

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

The following parameters are calculated:

• Minimum and maximum for the amount of sample to be entered,

• ∆Vmin, ∆Vmax, and ∆Vmax factor (control parameters),

• Drift value (termination parameter).

METTLER TOLEDO DL31/DL38 49

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

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

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

7.1 <Stirrer>

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

Stirrer STIRRE

Speed [%] 35

Star

Stirrer STIRRE

Speed [%] 35

Start The stirrer stirs at the defined rate.

To change the speed in the standby mode in KF titrations, –press the <Stirrer> key, change the speed and confirm with "OK": The

stirrer stirs at the new speed.

– Press the <Run> key to return to the Analysis menu.

7.2 <Burette>

The following functions are possible under this menu.

Rinse Rinse tip Dispense

Rinse

Start and stop the rinsing process with <F3>.

Burette BURETTE

Rate

With <F2> you can change the rate at which the burette should be filled. For the two-component reagents we advise always set-

Rinse (rate: 100 Rinse tip Dispense: 0.010

Help Modify Star

Start

ting 60%. They outgas easier than the one-component reagents. The titrator delivers 1 burette volume. The piston of the burette

moves below the zero position to ensure that air bubbles "hidden" in the stopcock are siphoned up and then expelled.

– Always place the dispensing tubing in a waste beaker!

50 METTLER TOLEDO DL31/DL38

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

t t

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

tubing tip.

Note You should also place the dispensing tubing in a waste beaker during this operation to ensure the

titrated solvent is not "overtitrated".

Dispense Start You can dispense the displayed volume immediately. With <F3>, "Stop", you can stop the

dispensing.

<F2> With <F2> this mask appears in which you can modify the dispensing parameters:

Burette BURETTE

Volume [mL] 0.010 Burette 5 mL Fill rate [%]100

Star

7.3 <Pump>

With the aid of the pump you can add solvent to the titration vessel and siphon it off.

Pump PUMP To empty, press <F3> To fill, press <F3>

and press and

blue pump but

Star

Pump PUMP

Emptying/filling...

Stir Stop

You switch the pump on and off with <F3>. While the pump is running, you can switch on the

stirrer with <F2>, "Stir".

Filling

– Push the dispensing tubing up to the 60 mL mark of the titration vessel so that the solvent does not

splash during filling. The solvent starts to flow into the titration vessel as soon as a sufficiently high vacuum which siphons up the solvent has built up in the titration vessel.

– Add approx. 40 mL to the titration vessel (the platinum pins of the electrode must be immersed in the

solvent!), release the pump button and press <F3>.

– Pull up the tubing.

Emptying

– Push the suction tubing to the base of the titration vessel so that the solvent can be siphoned off. – Pull up the tubing when the pump is running as far as it will go, then press <F3>.

METTLER TOLED O DL31/DL38 51

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

Note

• The pump switches off automatically when the pumping time defined in the Setup menu is reached.

• Each pumping operation resets the solvent capacity to the value defined in the Setup menu. At the same time, the value is stored under the key.

• In the case of the pump of the attached DV705 Titration Stand, you must press the lower arrow key during emptying and the upper arrow key during siphoning up.

7.4 <Results>

The following functions are available in this menu:

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

All results is accessible when one result is available. Statistics are accessible when 2 results of a sample series are available. 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". – Press the <Run> key to switch back to the Analysis menu.

7.4.1 All results

You can view the results generated in the titration of a sample or sample series. You can also print out the results. The data in the result memory are deleted when you switch off the titrator.

DL31: The results of the last 20 determinations are stored. DL38: You can perform a sample series with 99 samples. The results of the last 60 samples remain

stored, in other words the results of sample 1 are eliminated when you start to titrate sample 61. Statistical data of the last 60 samples are always calculated.

Note

• As "Result" the sample whose determination was terminated with the error message "No titration!" is also stored.

•A result is also stored if you terminate a determination with <Reset>. The result is calculated with the titrant volume consumed up to that time.

52 METTLER TOLEDO DL31/DL38

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

7.4.2 Recalculation

You can recalculate existing results by changing the following values for each sample:

• in a KF sample determination: Drift, concentration, blank value and/or amount of sample.

• in a KF conc. determination: Drift and/or amount of sample.

• in a bromine number determination: Concentration, blank value and/or amount of sample.

Recalculn RESULTS Method 11 Sample 1 R1 = 0.77% Sample 2 ▼

Modify OK

▼

Recalculn RESULTS Sample 1 Drift [µg/min] 6 Conc. [mg/mL]4.9875 Blank [µg] 0▼

Undo OK

DL31: R = 0.77%

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

▼

Recalculn RESULTS Method 11 *Sample 1 R1 = 0.77% Sample 2 ▼

Modify OK

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

Note

•

The values obtained in the determination always remain stored so that you can also nullify changes later.

• Under "All results" you can print out the recalculated results. Here, the changed values and the original

are reported.

• DL38: The changed results are also taken into account for the statistical data.

• DL38: In KF conc. determinations the calculated result or its mean value is not entered in the parameter

list of the KF titrant if you change a value, e.g. after three determinations. However, if you perform a conc. determination after this change, the recalculated result is taken into account in the statistics calculation.

METTLER TOLED O DL31/DL38 53

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

7.4.3 Report

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

Report RESULTS

OutputPrint.+Com Type GLP

Help Modify OK

Note If you have changed the result of this last determination beforehand, it will be printed out marked

with an asterisk (*).

7.4.4 Calculations (DL38 only)

At the end of every titration you can perform additional calculations for this sample.

CalculationsRESULTS

R = x [mg]* f = 1.0000 Unit mg▼

Help Modify OK

With "OK" the result is displayed and 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 standard deviation. You can print out these results here and change the statistical evaluation by eliminating outliers.

The DL38 does not incorporate results in the statistics which were obtained after a learn titration, a "Reset", and the following messages:

• No titration!,

• End point not reached! Termination through Vmax,

• CONC value not stored! Conc. range exceeded,

• CONC value not stored! Termination through Vmax.

54 METTLER TOLEDO DL31/DL38

Example of a statistical evaluation of 3 samples

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

StatisticsRESULTS Method 11 R1 n = 3 x = 0.77%

s =

0.102194 % ▼

ResultPrint OK

▼

StatisticsRESULTS Method 11 Sample 1 R1 = 0.77% Sample 2 ▼

Delete OK

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

If you delete "Sample 1" with <F1>, "Undo" is superimposed to allow you nullify the command. At the same time, sample 1 is marked as "deleted".

Confirm "OK" to show the following:

▼

StatisticsRESULTS Method 11 R1

n =

x = 0.70 %

ResultPrint OK

(Example: Sample 1 is deleted)

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

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

7.4.6 Statistics series (DL38 only)

With the aid of this function you can terminate a sample series. This deletes all data in the result memory, a subsequent analysis with the same method restarts with "Sample 1".

Stat.seriesRESULTS End series? No Yes

METTLER TOLED O DL31/DL38 55

Information menu ( key)

8 Information menu ( key)

The measured values and menus below are stored under the key:

Solv. capac.[mL] Drift [µg/min] Blank [µg] (DL38/Stromboli only) KF learn titration Hello! (Tutorial) Hardware tests

Solv. capac. The solvent capacity defined in the Setup menu is entered as an initial value. After each

titration, the difference between the initial value and the amount of titrant consumed is displayed. If "0" is reached or exceeded, an error message appears. As soon as you switch on the pump, the value defined in the Setup menu is reentered.

In bromine number determinations, the solvent capacity is set to "0".

Drift

Here, the value of the drift determination last performed is stored and automatically adopted for the drift compensation if you have defined "Drift: Determination" as a method parameter.

Blank The value of the last blank determination perfomed is stored here and automatically adopted

for calculations (only for method with Stromboli).

KF learn titr. The course of this titration is described in Section 6. Hello! As you get to know the titrator step by step, the procedure is not described. Hardware tests The functions of this menu which you can use to test the hardware of the titrator are

described in Section 9.

56 METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

x x x

9 Error messages, malfunctions and hardware tests

9.1 Error messages from the titrator

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

A After the titrator has been switched on, the following errors can be displayed:

• ERROR

• RAM x test ERROR(Q)"x" represents a number

• ERROR –> HW version

• ERROR –> DCB

• ERROR –> application

• No application found The messages refer to a faulty hardware component. – Press any key: The titrator attempts to continue the start process; this may be successful, but does not

guarantee 100% functioning.

Measures

1. Note the displayed text.

2. Note the instrument number and software version of the titrator (shown on every report).

3. Please then inform METTLER TOLEDO service of these points and the attached peripheral units with the

defined configuration.

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

Internal error: xxxxxxxxxxxxxxxxxxx xxxxxxxxxxxxxxxxxxx xxxxxxxxxxxxxxxxxxx SYSTEM IS BLOCKED! See manual: Erro

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

ERROR: x

SYSTEM IS BLOCKE

Please call METTLER

TOLEDO service

"x": represents letters and/

or numbers.

Measures

1. Note the text or error (e.g. "ERROR: 1000") and the operation that triggered it.

2. Note the instrument number and software version of the titrator (shown on every report).

3. Then switch off the titrator.

4. Please inform METTLER TOLEDO service of these points and the attached peripheral units with the

defined configuration.

METTLER TOLEDO DL31/DL38 57

Error messages, malfunctions and hardware tests

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

Warning: x

Press any key to continue

"x": represents a numberl

Measures

1. Press any key: The titrator can continue to function.

2. On no account consider the result of a determination terminated in this manner!

3. If the warning appears frequently, you should take the measures described under point B.

D. Faulty data deleted!

The titrator has stored only part of a method if, e.g. the power fails when the method is being stored. It deletes this method completely. It is also possible that it has deleted several methods.

Measures

1. Confirm the message.

2. Check whether your methods have been deleted, if so reenter them.

The titrator has stored only parts of parameters of a resource if, e.g. the power failed during storage of the parameters. All data stored in the Setup menu are deleted.

Measures

1. Confirm the message. The titrator now loads the default parameters of the Setup menu, in other words all data stored on delivery of the titrator.

2. Switch the titrator off and on.

3. Check whether the default parameters are again available and reenter the names and values stored before the failure.

If you receive this error message frequently, the battery is discharged! This must be changed by METTLER TOLEDO service.

E. Method not stored!

The titrator can no longer store a method if the user data memory is full.

Measure

1. Confirm the message.

2. Delete one or more methods from the memory or transfer to the computer.

3. Reenter the new method and save it.

58 METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

9.2 Other errors and malfunctions

The following collection of errors and malfunctions which are not reported by the titrator will help you to rectify the fault yourself in many cases so that you do not have to rely on the METTLER TOLEDO service (specified in the Table as "Service").

You can also first check some malfunctions with the hardware test (see Section 9.3) before you contact the service.

Error Possible cause Rectification

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

to power supply.

Several points of the Contact service, see also Section 9.3.1. display are missing

The display and the Contact service, see also Section 9.3.1. key do not match

Transmission error to Peripheral device faulty Check attached devices for correct functioning, attached peripheral device or switched off. see also Section 9.3.2.

Device (printer, balance, Instrument not switched on; Switch on instrument; computer) does not react wrong settings and/or configuration settings and configuration must match,

(switch settings wrong); see Sections 4.5 and 9.3.2; wrong cable. cable see Section 11.2.

Pump does not function Suction tubing not connected, Connect suction tubing and check connections,

titration stand leaks; see Section 10.3; pump faulty. check pump, see Section 9.3.3.

TTL inputs or outputs Inputs and/or outputs faulty. Check inputs/outputs, see Section 9.3.3. do not function

Burette and stopcock Burette drive faulty. Contact service. do not move to zero position on switching on

Magnetic stirring bar Cable of magnetic stirrer not Check magnetic stirrer, see also 9.3.3; does not rotate plugged in properly; change magnetic stirrer;

wrong magnetic stirring bar. use bar supplied, see Section 11.

Wrong potential values Electrode faulty or contaminated. Check electrode (see electrode specifications bulletin);

use new electrode.

No dispensing, Burette tip blocked. Clean burette tip. titrant expelled from stopcock or piston

METTLER TOLEDO DL31/DL38 59

Error messages, malfunctions and hardware tests

9.3 Hardware tests

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

9.3.1 User interface

Display test

5 displays appear in succession, 4 with different patterns, the last without a pattern. This allows you to detect faulty pixels of the display. The test mode automatically switches off after approx. 20 seconds.

Keypad test

When you press a key, a numeric code assigned to this key appears which allows you to recognize a faulty key (see following Table).

– Press the <Esc> key to quit the test mode.

Key codes

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

Reset ..........23 F1 ............... 17 3................. 3

i ................. 30 F2 ............... 18 4................. 4

Stirrer..........28 F3............... 19 5................. 5

Pump .........27 —............... 11 6................. 6

Burette ........29 ∆ ................ 12 7................. 7

Results ....... 26 Shift ............ 10 8................. 8

Setup .......... 25 0 ................ 0 9................. 9

Method .......24 1 ................ 1 Del .............. 31

Run ............21 2 ................ 2 ................... 33

Beep tests

You test the internal beeper.

9.3.2 Peripheral interfaces

Interface test

– Before the test

– plug the test socket 51107288 into the balance, computer or GA42 interface. – plug the Centronics cable into the Centronics interface and the test plug 51107287 into the Centronics

socket of the cable.

After the test phase, either "Test successful" or "Test failed" appears.

60 METTLER TOLEDO DL31/DL38

Error messages, malfunctions and hardware tests

Balance test

The menu option is faded out if no balance is defined in the Setup menu.

• The weight displayed on the balance must appear in the titrator display.

Printer test (GA42, EPSON or HP)

The appropriate printer must be attached. If the error message "Printer: No connection" appears, you can quit this error message with <Esc>: With "OK", the titrator attempts to set up the connection to the printer again.

• The letters and characters available in the titrator must be printed out.

9.3.3 Inputs and outputs TTL-I/O (DL38 only)

– Before the test, plug test plug 51107723 into the TTL-I/O interface. After the test phase, either "Test successful" or "Test failed" appears.

Internal stirrer

You test the rotational movement and change in the speed of the magnetic stirring bar.

External stirrer

You test the rotational movement and change in the speed of the magnetic stirring bar with the attached DV705 Titration Stand.

Internal pump

You check whether the pump functions:

•A "noise" must be heard.

• It must be able to dispense and siphon off when solvent and waste bottle are correctly attached.

External pump

You check whether the pump of the attached DV705 Titration Stand functions (see "Internal pump"). Note For dispensing, you must always press the lower button (⇓ arrow), for siphoning off the upper

button (⇑ arrow).

METTLER TOLEDO DL31/DL38 61

Installation and maintenance

10 Installation and maintenance

10.1 Equipping the titration stand

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

Silicon tubing (133 mm)

Threaded ring with lug

Connector Stopper ST 7.5 3-hole adapter O-ring

Titration vessel

titration arm

1. Carefully slide the magnetic stirring bar supplied into the titration vessel.

2. Insert the titration vessel with the lug of the threaded ring into the middle groove of the titration arm and push downward towards the stirrer. Fasten the screw.

3. Place the three-hole adapter, the ST stopper and the connector in the cover openings.

4. Fill a drying tube with molecular sieves, close with the cover and "push" into the titration stand to ensure tightness. Connect the cover and the connector by silicon tubing.

Cover and drying tube Seal

ScrewGroove of

Titration

stand

62 METTLER TOLEDO DL31/DL38

Installation and maintenance

10.2 Installing the burette

1. Screw the burette with holder onto the titrant bottle (see DV100x Operating Instructions).

– Never inhale the vapors of Karl Fischer reagents and avoid skin contact. The reagents are

toxic.

2. Place the drying tube holder in the opening of the burette holder, fill a drying tube with molecular sieves and position in the holder.

3. Push the burette onto the titrator: The slot of the driver cam and piston rod must be parallel to the insert. (If this is not the case, press the <Reset> key.)

4. Turn arrestment knob in the opposite direction to the arrow and when pushing in check whether the piston rod of the burette is correctly positioned in the push rod.

5. Turn the arresting knob in the direction of the arrow to fasten the burette.

6. Place the dispensing tubing in the cover opening.

– When you rinse burette and tubing, place the dispensing tubing in a waste beaker;

do not dispense in the titration vessel!

Driver cam

Push rod of

the burette drive

Hole for dispensing tubing

Arrestment knob

METTLER TOLEDO DL31/DL38 63

Installation and maintenance

10.3 Installing the solvent and waste bottles

Screw sleeve Socket

Screw cap Gasket

Dispensing or suction tubing

Adjusting sleeve

1. Open the solvent bottle, lay in the gasket and screw on the screw cap (you may need an adapter, see DV100x Operating Instructions).

2. Loosen the screw sleeve and slide over one of the pump tubing. Push this dispensing tubing to the base of the bottle and screw fasten the sleeve. (There is an O-ring in the socket which ensures tightness.)

3. Push the other end of the dispensing tubing into the opening on the left of the three-hole adapter and fasten with the adjusting sleeve.

4. Perform steps 1 and 2 with the waste bottle supplied. Push the suction tubing to just shortly beneath the screw cap and fasten the sleeve.

5. Push the other end of the suction tubing into the opening on the right of the three-hole adapter and fasten with the adjustment sleeve so that you can easily push the tubing to the base of the titration vessel and pull it up again.

Teflon seal

Output

fitting

Suction fitting

6. Fill two drying tubes with molecular sieve and place them in the screw cap of the bottles.

7. Push the silicon tubing (450 mm) over the drying tube cover of the waste bottle and connect to the suction fitting of the pump.

8. You can connect the output fitting to tubing to lead off the solvent vapor to a suitable place.

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

64 METTLER TOLEDO DL31/DL38

10.4 Attaching the magnetic stirrer, electrode and devices

Installation and maintenance

Balance (RS232C)

External stand (DV705)

Stirrer output

Electrode input (KF)

Pump unit

Suction fitting

Output fitting

Socket for external power pack

Magnetic stirrer

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

GA42 printer (RS232C)

Computer (RS232C)

Stromboli, TBox, etc. (TTL I/O)

EPSON- and HP-compatible printers (Centronics)

On/Off switch

Magnetic stirrer

– Make sure that every connector is in the correct position! Do not damage the connector

pins of the magnetic stirrer cable! Pins damaged by faulty insertion can cause a short circuit at the "Stirrer" output. This renders the titrator non-functional.

Electrode

Unscrew the protective cover of the DM143-SC and connect the electrode to the triaxial cable. Plug the cable into the KF input and insert the electrode in the corresponding cover opening of the titration vessel.

Balance, printer, computer, TBox DR42

Attach all peripheral devices to the same plug connector (phase) to which the titrator is connected! Otherwise, equalizing currents could flow across the cables.

Attach the devices used to the corresponding connectors/sockets on the rear side of the titrator. METTLER TOLEDO and SARTORIUS balances are compatible with these titrators.

METTLER TOLEDO DL31/DL38 65

Installation and maintenance

10.5 Using TTL inputs and outputs (DL38 only)

The TTL-I/O socket has two inputs and four outputs (In 1, In 2 and Out 1...Out 4). The outputs are occupied by the titrator for commands.

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

Inputs

A level change from "high" to "low" is detected at the inputs. In 1 In the Run menu

• the pretitration in KF titrations or the titration in bromine determinations is started,

• the sample determination in KF titrations is started (always corresponds to the <F3> key),

• the actual analysis is started (corresponds to confirming the sample addition),

• the result display is confirmed.

In 2 corresponds to the <Reset> command on the keypad.

Outputs

At output 1 a pulse is given with a length of 100 – 200 ms. The other outputs assume either an active ("low") or inactive ("high") condition.

Out 1 outputs a pulse before the display of "Add sample" and before display of the result list. Out 2 is inactive when an analysis can be started. Out 3 is active in the case of an error message; the condition does not change until the message has

been confirmed with "OK".

Out 4 is active only during the mix time defined in the method.

For this condition, the connection of the TBox DR42 is suitable, it can be used to control an homogenizer (see TBox Operating Instructions).

10.6 Maintenance and servicing Cleaning

–You can clean the titrator with a cloth moistened with alcohol. –To clean the titration vessel, turn the titration arm to the right and unscrew the vessel from the cover. –To clean the cover, loosen the fastener screw, take the titration vessel with cover up and out and unscrew

cover.

–You should clean the electrode when their response time deteriorates owing to certain Karl Fischer

reagents and samples (the end point drifts!): Either place in an ultrasound bath with deionized water for a few minutes or for 60 seconds in a chromic acid bath and then rinse with water or ethanol.

66 METTLER TOLEDO DL31/DL38

Installation and maintenance

O-rings

You should replace the O-rings of the screw caps when the system is no longer tight: – Loosen the screw sleeve, take out the pump tubing and remove the O-ring using tweezers (see also

illustration in Section 10.3). You should replace the O-ring of the threaded ring for the same reason: – Loosen the fastener screw of the titration vessel, take titration vessel with cover up and out and unscrew

(see illustration in Section 10.1).

Dispensing and suction tubing

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

Molecular sieve

If the drift of the KF solution remains too high, you should fill the drying tubes with fresh molecular sieve. You can regenerate molecular sieve in a drying oven at 160 – 300 °C for at least 24 hours. As the molecular

sieve used on the waste bottle also contains SO2, you should rinse it with deionized water before regeneration.

Pump unit

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

Pump button

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

Magnetic stirrer

If the magnetic stirrer is faulty, you can replace it: – Swing out the titration arm and push the motor out of the burette slot. – Push in the new magnetic stirrer and attach its cable to the stirrer output.

Battery

The battery installed in the titrator has a service life of approx. 5 years. The battery may be changed only by METTLER TOLEDO service.

Disposal

Contact your METTLER TOLEDO dealer if you have to dispose of the titrator.

METTLER TOLEDO DL31/DL38 67

Standard and optional equipment

11 Standard and optional equipment

11.1 Standard equipment

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

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

Note

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

1 drying tube holder

A 5 mL interchangeable burette

incl. 1 L brown glass bottle

1 titration vessel with cover incl.

one 3-hole adapter with stoppers

1 pump button

4 drying tubes with cover

1 dispensing tubing with Teflon seal

1 suction tubing with Teflon seal

1 silicon tubing

1 connector

1 seal

1 stopper ST 7.5

2 screw caps with flat seal

1 siphoning tubing

One 1 L brown glass bottle

1 magnetic stirring bar

1 magnetic stirrer

68 METTLER TOLEDO DL31/DL38

1 double platinum pin electrode DM143-SC incl. 1 electrode cable (SC-LEMO-60)

Standard and optional equipment

Threaded ring 51107459 Cover 51107462 with:

• 3-hole adapter 23982 (with 1 ST 10, ST 7.5 and 1 needle hole stopper)

• Stopper ST 7.5 23452 (set of 5)

• Connector 23957 O-Ring 51190366

Titration vessel 51107463 (nominal volume: 250 mL)

Fastener screw (for titration vessel)

51107474

Magnetic stirring rod

51191159

1-L brown glass bottle

71296

Gasket (min. order quantity: set of 5)

23981

Screw cap

23937

Pump tubing (suction/dispensing tubing)

51107481

Silicon tubing 450 mm (suction tubing)

51107490

Magnetic stirrer

51108750

Silicon tubing 133 mm

51107480

Drying tube holder

23915

Drying tube with cover

23961

Seal (drying tube of titration stand)

51107492

Pump unit

51107479

Pump button

51107600

Double platinum pin electrode DM143-SC

51107699

Triaxial cable SC-LEMO-60 (length: 60 cm)

89601

Molecular sieve 1 Bottle

71478

METTLER TOLEDO DL31/DL38 69

Standard and optional equipment

External power pack

51107777

11.2 Optional equipment

Drying oven

DO307

P O W E

T E M P

E R A T U R E

H E A T I

N G

1 1 4 6 0

0 2 0

0 1 0 0

0 8 0

0 4 0

2 6

0 O F F

2 8

3 0

O-ring (for screw caps) (set of 4)

51107496

Thermostatable beaker

51107497

Connection cable for computers DTE 9-pin, female

51190362

Oven sample changer Stromboli with DL38 only

Stromboli

connection cable for Stromboli (DL38 only)

51190589

Gas inlet for operation of a DL38 with a Stromboli

105091

Stoppers for three-hole adapter (1 set) (1 ST 10, 1 ST 7.5, 6 needle hole stoppers)

25883

Connector set (for interface check)

51107790

Septum stoppers (set of 10) ST 10 23949 ST 24 23950

External stand

DV705

Weighing boat (set of 5) Glass, ø 20 x 60 23951 Glass, ø 30 x 80 23952 PE, ø 25 x 65 23953 PE, ø 38 x 100 23954

Homogenizer adapter set 12 (for Kinematica)

51107534

Homogenizer adapter set 18 (for IKA)

51107409

Visco Spoon™

51107668

70 METTLER TOLEDO DL31/DL38

Standard and optional equipment

Connection cable for METTLER TOLEDO balances AB, AX, PB, PG-S (RS9 interface)

11101051

Connection cable for METTLER TOLEDO balances AE with the Option 011

59759

Connection cable for SARTORIUS balances

51190363

Connection cable for GA42 printer

51190362

Connection cable for EPSON-/HP-compatible printers (i.e. Olivetti Artjet)

51107780

Triaxial cable SC-LEMO-100 (length: 100 cm)

89602

Connection cable for METTLER TOLEDO balances AM, PM, AT

229029

Connection cable for METTLER TOLEDO balances AG, AB, PB, PG (LC interface)

229065

1 7

. 3 7

g . 3

1 9

0 0

7 3

5 5

5 0

g . 0

MET

9 7

. 8

ER TO

2 0

g . 0

8 g

Printer

GA42

Olivetti Artjet printer EU version 51190985 US version 51190986



Connection cable for computers DTE 9-pin, female 51190362 DTE 25-pin, female 51107781

Syringes (package of 100) 1 mL 71492

24 VDC 1.2 A

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

TBox DR42

TBox DR42 (control of external devices via TTL I/O)

DR42

Connection cable for TBox DR42

51190589

10 mL 71482

1 mL

Injection needles (package of 12) 80 x 1.2 mm 71483

80 x 0.8 mm 71484

Software LabX professional incl. Operating Instructions German 51106302 English 51106300



Keypad cover (3 pieces)

51107666

Software LabX multi incl. Operating Instructions German 51106312 English 51106310

METTLER TOLEDO DL31/DL38 71

Standard and optional equipment

Operating

Instructions

METTLER

TOLEDO

DL31/DL38:

Description

the

Computer

Interface

Die 4 wichtigsten Schritte

Method

Setup

Run

Results

–Das Coulometer mit den entsprechen-

den Hilfsmitteln einrichten.

Hauptmethoden (nur DL39) Peripherie Einstellungen

–Eine Methode wählen und nach Bedarf

ändern.

Benutzermethoden (nur DL39) METTLER-Methoden (nur DL39) 911Standard 1.0 912Stromboli 913Ext.Extr. 914Br Index 915Br Blank KF-Standardmethode

–Analyse mit der gewählten Methode star-

ten, indem Sie <Run> oder <F3>, „Pro-

be“, drücken. –Abfragen beantworten. –Probe zugeben. (DL39: Falls „Autostart:

Ja“ gewählt wurde, beginnt die Titration

automatisch bereits nach Zugabe der

Probe.) –<Run> oder <F3>, „Start“, drücken, um

die Analyse zu starten. (DL39: Falls

„Autostart: Ja“ gewählt wurde, entfällt

dieser Schritt.)

–Resultatliste von analysierten Proben

anschauen, Nachberechnungen durch-

führen, die statistische Auswertung ei-

ner Serie ändern (nur DL39!) sowie zu-

sätzliche Protokolle ausdrucken.

Bedienungsanleitung

Operating Instructions German 51709849 English 51709850

KF-Titratoren

DL31 / DL38

French 51709851 Spanish 51709852 Italian 51709853

Die KF-Standardmethode

Nr. der Methode 0 Titel der Methode Probenparameter

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

Drehzahl [%] 40 Mischzeit [s] 10

→→ → nur DL39

Autostart Nein

→→

Regelparameter

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

Abbruchparameter

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

∝

g] 0

Blindwert [ Drift Online

Autor der Methode

→→

Resultat

→ nur DL32 →→

Berechnung 1 ppm

R1 = x [ppm]*f1 f1 = 1.0000 Einheit ppm Dezimalstellen 2 Statistik Ja Max. srel [%] 0.00

Berechnung 2

R2 = Keine Berech. f2 = 1.0000

→→

Einheit

→ nur DL39 →→

Dezimalstellen 2 Statistik Ja Max. srel [%] 0.00

Berechnung 3

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

Standby Ja Protokoll

AusgabeDruck.+Comp. Typ GLP

Memo card German 51710187 English 51710188 French 51710189

Operating

Instructions

METTLER

TOLEDO

DL31/DL38:

Description

the

Computer

Interface

Application brochure DL31/DL38 German 51709854 English 51709855 French 51709856 Spanish 51709857 Italian 51709858

Description of the computer interface German 51709875 English 51709876

Spanish 51710190 Italian 51710191

72 METTLER TOLEDO DL31/DL38

12 Technical data

Power supply

Voltages 100 – 240 VAC ±10% Frequency 50/60 Hz Power consumption 45 VA Voltage 24 VDC 0.8 A / 5 VDC 1.2 A

Dimensions

Width 240 mm Depth 305 mm Height 370 mm Weight Approx. 5 kg

Materials

Technical data

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

Ambient conditions

Ambient temperature +5 °C to +40 °C Atmospheric humidity Max. 80% at 40 °C Use Indoors Overvoltage category II Pollution degree 2

METTLER TOLEDO DL31/DL38 73

Technical data

Measurement principle

Volumetric water content determination following Karl Fischer End point indication Voltametric: voltage measurement at a polarized

double platinum pin electrode

Measurement range Several ppm to 100% water

Measurement system

• KF input Triaxial socket Current source

Pol. current 1, 2, 5, 10, 15, 20, 30 or 40 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

• Output 8-pin socket (mini DIN) Magnetic stirrer Stepper motor

Speed Software-controlled (1-100%) Power 2 W Max. speed 1050 rpm (40% ≈ 600 rpm, 70% ≈ 1050 rpm)

• Output (External stand DV705) 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)

74 METTLER TOLEDO DL31/DL38

Burette drive module

Drive Stepper motor

Resolution 1/10000 of the burette volume

Technical data

Max. permissible errors

0.3% relative to the respective burette volume of 5, 10 or 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 titrant Fluoroplastic, borosilicate glass, ceramic

Magnetic stirrer

Type Stepper motor Max. speed 1050 rpm Power consumption 2 W

Diaphragm pump

Voltage 24 VAC (4 W) Pressure buildup Approx. 150 mbar

Display

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

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 / –

METTLER TOLEDO DL31/DL38 75

Technical data

Attachment possibilities for peripheral devices Balance Attachment via RS232C interface (9-pin, D-sub-connector)

for METTLER TOLEDO and SARTORIUS balances

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

for the GA42 Printer Attachment via Centronics interface (25-pin, D-sub-connector)

for commercial EPSON- and HP-compatible printers with parallel interface

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

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

Stromboli, TBox DR42, etc. Attachment via TTL I/O socket (9-pin, D-sub)

76 METTLER TOLEDO DL31/DL38

RS232C connector (balance/GA42/computer)

RxD (In)

TxD (Out)

DTR GND

+12 V

470 Ω

Titrator

Data to titrator

Data from titrator

Handshake from titrator fixed to operational readiness

Signal ground, galvanically connected to titrator electronics

TTL I/O socket

Technical data

IN1 IN2 OUT1 OUT2 OUT3 OUT4

GND

Centronics socket

\Strobe PD0 PD1

25 24 23 22 21 20 19 18 17 16 15 14

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

13 12 11 10 9 8 7 6 5 4 3 2 1

Titrator

In TTL; short-circuit-proof; Pulse ≥150 ms

2 3 4 5 6 7 8

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

Out Open collector

• Vce max. = 24 V

• Ic max. = 20 mA

GND Signal ground, galvanically connected to titrator electronics

Data ready

2 3 4 5 6 7 8 9

Data accepted

Printer busy

End of paper

Printer active

Automatic line feed

Printer error

Printer initialized

Printed selected

17 18 19 20 21 22

Signal ground, galvanically connected to titrator electronics

23 24 25

Titrator

METTLER TOLEDO DL31/DL38 77

Technical data

Declaration of System Validation

We herewith inform you that the products/systems

DL31, DL38

including software and accessories were developed, tested and successfully validated according to the international ISO9001:1994 based Life cycle rules of Mettler-Toledo GmbH, Analytical.

Life cycle checkpoint details were reviewed and approved by the Project Supervisory Group (PSG). The products/systems were tested to meet functional and performance specifications and release criteria at release to shipment. In order to support GLP and validation requirements, we will make the following documents available to an authorized, governmental or regulatory agency for inspection.

• Performance Specifications

• Software Specifications

• Quality Plan

• Project Management System

• Test Plan

• Customer Requirements

• Review Reports

• Source Code

Mettler-Toledo GmbH, Analytical will maintain possession of all documents and their reproductions and may require a non-disclosure agreement to be provided by those requiring access to these documents.

Schwerzenbach, Dr. Bernhard Grob Dr. Rolf Rohner August 1998 General Manager Marketing Manager

Business Unit Analytical Titration

ISO 9001 certificate for METTLER TOLEDO

The Mettler-Toledo GmbH company, Greifensee, was examined and evaluated in 1991 by the Swiss Association for Quality and Management Systems (SQS), and was awarded the ISO 9001 certificate. This certifies that Mettler-Toledo GmbH, Greifensee, has a quality management system that conforms with the international standards of the ISO 9000 series.

Repeat audits are carried out by the SQS at intervals to check that the quality management system is operated in the proper manner and is continuously updated in relation to changes brought about.

78 METTLER TOLEDO DL31/DL38

Product Life Cycle Model

Ideas

Technical data

Project Study

Project Start

Phase: Basic Know how

Phase: Feasibility

Phase:

Project Release

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

Software Specifications Test Plan Review Report

Confirmation

Review Report

Phase:

Project End

Usage

Readiness

Review Report

Customer Complaints (CRIS) Customer Requirements

Phase out

METTLER TOLEDO DL31/DL38 79

80 METTLER TOLEDO DL31/DL38

13 Index

Symbole

<F1>...<F3> 9

Index

Access for expert/routine 21 All results 52 Amount of sample (calculating) 24 Analyse (Run) 34 Arrow keys 11 Author 27 Auto start 25 Auxiliary function keys 10 Auxiliary functions 50

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

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

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

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

Fill rate 50 Filling (titration vessel) 51

GLP 27

Hardware tests 60 Hello! 56 Help texts 5

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

METTLER TOLEDO DL31/DL38 81

Index

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

Language (changing) 12

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

Operating concept 8 Optional equipment 70

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

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

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

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

User interface (checking) 60 User list 20

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

82 METTLER TOLEDO DL31/DL38

METTLER TOLEDO DL31/DL38 KF titrators Switching from routine to expert mode

Settings SETUP Titrator ID ▲ Acces for Routin Beep Y es Solv. capac.[mL]80▼

Help O K

Settings SETUP Titrator ID ▲ Acces for Routin Beep Y es Solv. capac.[mL]80▼

Help Modify O K

Select this line in the Setup menu. –While holding down the <Shift> key, press key <1> three times:

"Modify" is assigned to <F2> allowing you to select "Expert". – Confirm <F3>, "OK", to save the change.

✃

METTLER TOLEDO DL31/DL38 83

84 METTLER TOLEDO DL31/DL38

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, Analytical, Sonnenbergstrasse 74, CH-8603 Schwerzenbach,

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

Mettler Toledo DL31, DL38 Operating Instructions Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

1 The DL31/DL38 KF titrators

2 Safety measures

2.1 Measures for your protection

2.2 Measures for operational safety

3 The titrator

3.1 Putting into operation

3.2 The operating concept

3.2.1 The command keys

3.2.2 The menu keys

3.2.3 The auxiliary function keys

3.2.4 The <i> key

3.2.5 The entry and arrow keys

3.3 Changing the language

4 Setup (<Setup> key)

4.1 KF titrants

4.2 Br No. titrants (DL38 only)

4.3 KF standards

4.4 Main methods (DL38 only)

4.5 Peripherals

4.5.1 Printer

4.5.2 Balance

4.5.3 Titration stand

4.5.4 Computer

4.6 Settings

5 Methods (<Method> key)

5.1 The KF standard method

5.2 KF method parameters

5.2.1 No. (of the method)

5.2.2 Title (of the method)

5.2.3 Sample parameters ID You can enter an identification for the sample(s) now or just before the titration for every sample

5.2.4 Speed

5.2.5 Mix time

5.2.6 Titrant

5.2.7 Volume (for predispensing)

5.2.8 Wait time (after predispensing)

5.2.9 Auto start (DL38 only) Yes The DL38 begins analysis as soon as a sample has been added. The time for adding a sample

5.2.10 Control parameters

5.2.11 Termination parameters

5.2.12 Blank

5.2.13 Drift

5.2.14 Result (DL31 only)

5.2.15 Calculation (DL38 only) Calculation 1

5.2.16 Standby Yes After a titration, the titration vessel is kept anhydrous. We recommend allowing the standby

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

5.2.18 Author of the method

5.3 Storage procedures

5.4 User and METTLER methods (DL38 only)

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

5.4.2 METTLER method "910 Stromboli" (DL38 only)

6 Analysis (<Run> key)

6.1 Starting a method Preparations

6.1.1 Menu sequence up to standby mode (KF methods)

6.1.2 Standby mode

6.2 Sample determination

6.2.1 Weight transfer from a balance

6.2.2 Post consumption

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

6.2.4 Sample series with statistics (DL38 only)

6.3 Concentration determination

6.4 Blank determination

6.5 Drift determination

6.6 Bromine number determination (DL38 only)

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

6.8 KF learn titration

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

7.1 <Stirrer>

7.2 <Burette>

7.3 <Pump>

7.4 <Results>

7.4.1 All results

7.4.2 Recalculation

7.4.3 Report

7.4.4 Calculations (DL38 only)

7.4.5 Statistics (DL38 only)

7.4.6 Statistics series (DL38 only)

8 Information menu (<i> key)