Eco Titrator

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Eco Titrator

Product manual
8.1008.8001EN / 2021-08-27
Metrohm AG
Ionenstrasse
CH-9100 Herisau
Switzerland
+41 71 353 85 85
[email protected]
www.metrohm.com

Eco Titrator

Firmware version 57.1008.0011 or higher

Product manual

8.1008.8001EN /
2021-08-27
Technical Communication
Metrohm AG
CH-9100 Herisau

This documentation is protected by copyright. All rights reserved.


This documentation has been prepared with great care. However, errors
can never be entirely ruled out. Please send comments regarding possible
errors to the address above.

Disclaimer
Deficiencies arising from circumstances that are not the responsibility of
Metrohm, such as improper storage or improper use, etc., are expressly
excluded from the warranty. Unauthorized modifications to the product
(e.g. conversions or attachments) exclude any liability on the part of the
manufacturer for resulting damage and its consequences. Instructions and
notes in the Metrohm product documentation must be strictly followed.
Otherwise, Metrohm's liability is excluded.
■■■■■■■■■■■■■■■■■■■■■■ Table of contents

Table of contents
1 Overview 1
1.1 Product description .............................................................. 1
1.2 Product versions ................................................................... 2
1.3 Symbols and conventions .................................................... 3
1.4 Additional information ......................................................... 3
1.5 Accessories ............................................................................ 3

2 Safety 5
2.1 Intended use ......................................................................... 5
2.2 Responsibility of the operator ............................................. 5
2.3 Requirements for operating personnel ............................... 6
2.4 Safety instructions ................................................................ 6
2.4.1 Danger from electrical potential ............................................... 6
2.4.2 Danger from biological and chemical hazardous substances ..... 6
2.4.3 Danger from highly flammable substances ............................... 7
2.4.4 Danger from leaking liquids ..................................................... 7
2.4.5 Danger during transport of the product ................................... 8
2.5 Design of warning messages ............................................... 8
2.6 Meaning of warning signs ................................................... 9

3 Functional description 11
3.1 System overview ................................................................. 11
3.1.1 Signals ................................................................................... 11
3.1.2 Interfaces and connectors ...................................................... 11
3.2 Eco Titrator – Overview ..................................................... 13
3.2.1 Dosing unit ............................................................................ 17
3.2.2 Bottle unit ............................................................................. 20
3.3 Function ............................................................................... 20
3.3.1 Magnetic stirrer ..................................................................... 20
3.3.2 Dosing unit ............................................................................ 20
3.4 Indicators and controls ...................................................... 21
3.5 Interfaces and connectors ................................................. 22
3.6 Remote interface ................................................................ 23
3.7 Remote control ................................................................... 25
3.8 Arithmetic algorithms ........................................................ 27

■■■■■■■■ III
Table of contents ■■■■■■■■■■■■■■■■■■■■■■

4 Delivery and packaging 30


4.1 Delivery ................................................................................ 30
4.2 Packaging ............................................................................ 30

5 Installation 31
5.1 Setup location ..................................................................... 31
5.2 Preparing the assembly ...................................................... 31
5.3 Switching the instrument on and off ................................ 33
5.4 Initial assembly of the cylinder unit .................................. 34
5.5 Mounting the support rod ................................................. 36
5.6 Preparing the bottle unit ................................................... 37
5.7 Mounting the tubing connections .................................... 38
5.8 Mounting the electrode ..................................................... 39

6 Start-up 40
6.1 Switching the instrument on and off ................................ 40
6.2 Setting the language, date and time ................................ 41
6.3 Setting the dialog type ...................................................... 42

7 Operation and control 44


7.1 Display elements and controls .......................................... 44
7.2 Switching the instrument on and off ................................ 45
7.3 User interface ...................................................................... 46
7.3.1 Formula editor ....................................................................... 50
7.4 Manual control ................................................................... 53
7.4.1 Manual control – Dosing ....................................................... 54
7.4.2 Manual control – Measurement ............................................. 56
7.4.3 Exchanging the cylinder unit .................................................. 57
7.4.4 Preparing the buret (PREP) ..................................................... 60
7.4.5 Operating the magnetic stirrer ............................................... 60
7.5 Methods .............................................................................. 62
7.5.1 Using and managing methods ............................................... 63
7.6 Sample data ........................................................................ 69
7.6.1 Sample series ......................................................................... 71
7.7 System – Configuration ...................................................... 75
7.7.1 System – Settings ................................................................... 76
7.7.2 Managing sensors ................................................................. 79
7.7.3 Managing solutions ............................................................... 82
7.7.4 Managing common variables ................................................. 85
7.7.5 Managing external devices .................................................... 87

IV ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Table of contents

7.7.6 System – File management .................................................... 88


7.7.7 Instrument diagnosis ............................................................. 92
7.7.8 Ethernet settings .................................................................... 93
7.7.9 Service – Brief description ...................................................... 93
7.7.10 Changing the password ......................................................... 93
7.7.11 COM port settings ................................................................. 94
7.8 Carrying out a pH calibration ............................................ 96
7.9 Carrying out the determination ........................................ 97
7.10 Results ............................................................................... 100
7.11 Printing reports ................................................................ 103
7.12 Parameters ........................................................................ 105
7.12.1 Dynamic equivalence point titration (DET) ............................ 106
7.12.2 Monotonic equivalence point titrations (MET) ...................... 126
7.12.3 Endpoint titrations (SET) ....................................................... 145
7.12.4 pH calibration (CAL) ............................................................. 161

8 Maintenance 167
8.1 Maintenance ..................................................................... 167
8.2 Cleaning the product surface .......................................... 167
8.2.1 Performing maintenance on the cylinder unit ....................... 168
8.2.2 Mounting the cylinder unit .................................................. 172
8.3 Displaying system data .................................................... 173
8.4 Resetting the system ........................................................ 174

9 Troubleshooting 176
10 Disposal 177
11 Technical specifications 178
11.1 Ambient conditions .......................................................... 178
11.2 Energy supply ................................................................... 178
11.3 Dimensions ........................................................................ 179
11.4 Housing ............................................................................. 179
11.5 Connectors specifications ................................................ 180
11.6 Display specifications ....................................................... 181
11.7 Operation specifications .................................................. 181
11.8 Measurement specifications ............................................ 182
11.9 Stirrer specifications ......................................................... 183
11.10 Liquid handling specifications ......................................... 183

■■■■■■■■ V
■■■■■■■■■■■■■■■■■■■■■■ Overview

1 Overview

1.1 Product description


The Eco Titrator is a titrator for volumetric titrations for universal use that
is equipped with the following functional units:
■ Built-in magnetic stirrer
■ Dosing unit with exchangeable cylinder unit
Methods can be created and saved on the instrument. The methods can
be exported to and imported from a connected USB flash drive. This
allows to copy methods from one instrument to another.

Titration modes
The following titration modes are supported:
■ DET
■ MET
■ SET

Calibration mode
The CAL calibration mode is used to calibrate the electrode.

Connectors
The instrument is equipped with the following connectors:
■ USB 1 and USB 2
■ Ethernet
■ Remote
■ 24 VDC Power OUT
■ 24 VDC Power IN
■ Ind
■ Ref
■ Temp
■ Pol

■■■■■■■■ 1
Product versions ■■■■■■■■■■■■■■■■■■■■■■

1.2 Product versions


The product is available in the following versions:
Table 1 Product versions
Art. no. Designation Version feature
2.1008.0010 Eco Titrator with magnetic stirrer
2.1008.1010 Eco Titrator Acid/Base with magnetic stirrer
2.1008.2010 Eco Titrator Salt with magnetic stirrer
2.1008.3010 Eco Titrator Oil with magnetic stirrer
2.1008.4010 Eco Titrator Redox with magnetic stirrer

The required numbers for the customer service can be found on the type
plate (see example):

Figure 1 Type plate (example)

1 (01) = External article number 2 (21) = Serial number

3 (240) = Metrohm article number

NOTICE

Information on the accessories for the respective product version can


be obtained either on the Internet at http://www.metrohm.com or
from your regional Metrohm representative.

2 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Overview

1.3 Symbols and conventions


The following formatting may appear in the documentation:

Cross-reference to figure legend


The first number refers to the figure number. The
second number refers to the product part in the fig-
ure.
Instruction step
Numbers indicate the order of the instructions steps.
Method Names of parameters, menu items, tabs and dialog
windows
File ▶ New Menu path
[Continue] Button or key

1.4 Additional information


Additional information concerning the topic can be found:
■ in the Metrohm information portal on the Internet
https://guide.metrohm.com

1.5 Accessories
Up-to-date information on the scope of delivery and on optional accesso-
ries can be found on the Metrohm website. Download this information as
follows:

Downloading the accessories list

1 Go to https://www.metrohm.com.

2 Enter the article number of the product (e.g. 2.1001.0010) into the
search field.
The search result is displayed.

3 Click on the product.


Detailed information regarding the product is shown on various tabs.

4 On the Included parts tab, click the link to download the PDF.

■■■■■■■■ 3
Accessories ■■■■■■■■■■■■■■■■■■■■■■

The PDF file with the accessories data is loaded.

NOTICE

Metrohm recommends downloading the accessories list from the


Internet and keeping it for reference purposes.

4 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Safety

2 Safety

2.1 Intended use


Metrohm products are used for the analysis and handling of chemicals.
Usage therefore requires the user to have basic knowledge and experience
in handling chemicals. Knowledge regarding the application of fire preven-
tion measures prescribed for laboratories is also mandatory.
Adherence to this technical documentation and compliance with the
maintenance specifications make up an important part of intended use.
Any utilization in excess of or deviating from the intended use is regarded
as misuse.
Specifications regarding the operating values and limit values of individual
products are contained in the "Technical specifications" section, if relevant.
Exceeding and/or not observing the mentioned limit values during opera-
tion puts people and components at risk. The manufacturer assumes no
liability for damage due to non-observance of these limit values.
The EU declaration of conformity loses its validity as soon as modifications
are carried out on the products and/or the components.

2.2 Responsibility of the operator


The operator must ensure that basic regulations on occupational safety
and accident prevention in chemical laboratories are observed. The opera-
tor has the following responsibilities:
■ Instruct personnel in the safe handling of the product.
■ Train personnel in the use of the product according to the user docu-
mentation (e.g. install, operate, clean, eliminate faults).
■ Train staff on basic occupational safety and accident prevention regula-
tions.
■ Provide personal protective equipment (e.g. protective glasses, gloves).
■ Provide suitable tools and equipment to carry out the work safely.
The product may be used only when it is in perfect condition. The follow-
ing measures are required to ensure the safe operation of the product:
■ Check the condition of the product before use.
■ Remedy defects and malfunctions immediately.
■ Maintain and clean the product regularly.

■■■■■■■■ 5
Requirements for operating personnel ■■■■■■■■■■■■■■■■■■■■■■

2.3 Requirements for operating personnel


Only qualified personnel may operate the product. Qualified personnel are
persons who meet the following requirements:
■ Basic regulations on occupational safety and accident prevention for
chemical laboratories are known and complied with.
■ Knowledge of handling hazardous chemicals is present. Personnel have
the ability to recognize and avoid potential dangers.
■ Knowledge regarding the application of fire prevention measures for
laboratories is available.
■ Safety-relevant information is communicated and understood. The per-
sonnel can operate the product safely.
■ The user documentation has been read and understood. The personnel
operate the product according to the instructions in the user documen-
tation.

2.4 Safety instructions


2.4.1 Danger from electrical potential
Contact with electrical potential can cause serious injuries or death. To
avoid danger from electrical potential, observe the following:
■ Operate the product only if it is in perfect condition. The housing must
also be intact.
■ Only use the product with the covers fitted. If covers are damaged or
missing, disconnect the product from the energy supply and contact
the regional Metrohm service representative.
■ Protect live components (e.g. power supply unit, power cord, connec-
tion sockets) against moisture.
■ Always have maintenance work and repairs on electrical components
carried out by a regional Metrohm service representative.
■ Disconnect the product from the energy supply immediately if at least
one of the following cases occurs:
– The housing is damaged or open.
– Live parts are damaged.
– Moisture penetrates.

2.4.2 Danger from biological and chemical hazardous substances


Contact with biological hazardous substances may cause poisoning from
toxins or infections from microorganisms. Contact with aggressive chemi-
cal substances may cause poisoning or chemical burns. To avoid danger
from biological or chemical hazardous substances, observe the following:

6 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Safety

■ Label the product according to regulations if it is used for substances


that have a potential for chemical hazards and are generally subject to
the Hazardous Substances Ordinance.
■ Wear personal protective equipment (e.g. protective glasses, gloves).
■ Use exhaust equipment when working with vaporizing hazardous sub-
stances.
■ Dispose of hazardous substances in accordance with regulations.
■ Clean and disinfect contaminated surfaces.
■ Only use detergents that do not cause any unwanted side reactions
with the materials to be cleaned.
■ Dispose of chemically contaminated materials (e.g. cleaning material) in
accordance with regulations.
■ Proceed as follows in case of a return shipment to Metrohm AG or a
regional Metrohm representative:
– Decontaminate the product or product component.
– Remove the labeling for hazardous substances.
– Create a declaration of decontamination and enclose it with the
product.

2.4.3 Danger from highly flammable substances


Using highly flammable substances or gases may cause fires or explosions.
To avoid danger from highly flammable substances, observe the following:
■ Avoid ignition sources.
■ Use protective grounding.
■ Use exhaust equipment.

2.4.4 Danger from leaking liquids


Leaking liquids may cause injuries and may damage the product. To avoid
danger from leaking liquids, observe the following:
■ Check the product and its accessories for leakages and loose connec-
tions.
■ Replace leaking parts and connecting elements without delay.
■ Tighten loose connecting elements.
■ Do not loosen tubing connections under pressure.
■ Do not remove aspiration tubing under pressure.
■ Carefully pull the ends of the tubing out of the containers.
■ Carefully let liquids from tubing drain into suitable containers.
■ Insert the buret tips completely into the containers.
■ Remove and dispose of leaked liquids in accordance with regulations.
■ If you suspect that liquid has penetrated the instrument, disconnect the
instrument from the energy supply. Then have the instrument checked
by a regional Metrohm service representative.

■■■■■■■■ 7
Design of warning messages ■■■■■■■■■■■■■■■■■■■■■■

2.4.5 Danger during transport of the product


Chemical or biological substances may be spilled during the transport of
the product. Parts of the product may fall down or may be damaged.
There is a risk of injury from chemical or biological substances and pieces
of broken glass. To ensure safe transport, observe the following:
■ Remove loose parts (e.g. sample racks, sample vessels, bottles) before
transport.
■ Remove liquids.
■ Lift and transport the product with both hands on the base plate.
■ Lift and transport heavy products only according to instructions.

2.5 Design of warning messages


There are 4 hazard levels for warning messages. The following signal
words are used for classifying the hazard levels in warning messages:
■ DANGER indicates a hazardous situation which, if not avoided, will
result in serious injury or death.
■ WARNING indicates a hazardous situation which, if not avoided,
could result in serious injury or death.
■ CAUTION indicates a hazardous situation which, if not avoided, could
result in minor or moderate injury.
■ NOTICE indicates a hazardous situation which, if not avoided, could
result in property damage.
Warning messages differ in design (color and warning sign) depending on
the hazard level:

DANGER

Type and source of danger


Consequences when not observing the notice: An irreversible injury
that may result in death is very probable.
■ Measures to avoid the danger

8 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Safety

WARNING

Type or source of danger


Consequences when not observing the notice: A serious injury that
may result in death is probable.
■ Measures to avoid the danger

CAUTION

Type or source of danger


Consequences when not observing the notice: A minor to moderate
injury is probable.
■ Measures to avoid the danger

2.6 Meaning of warning signs


This documentation uses the following warning signs:
Table 2 Warning sign according to ISO 7010
Warning sign Meaning
General warning sign

Warning of electrical voltage

Warning of hand injuries

Warning of sharp object

Warning of hot surface

Warning of biological hazard

Warning of toxic materials

■■■■■■■■ 9
Meaning of warning signs ■■■■■■■■■■■■■■■■■■■■■■

Warning sign Meaning


Warning of flammable materials

Warning of corrosive substances

Warning of optical radiation

Warning of laser beams

Depending on the intended use of the product, the corresponding warn-


ing sign stickers must be placed on the product.

10 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

3 Functional description

3.1 System overview


3.1.1 Signals
The status display uses flashing patterns to display the operating status of
the instrument.
Table 3 Status display
Signal Flashing pat- Meaning
tern
LED lights up Ready for operation
green
LED flashes In operation / Waiting
green (slowly)
LED flashes Malfunction or error
green (fast)

The status indicator uses colors to display the operating status of the
instrument.
Table 4 Status indicator
Signal Color Meaning
Green Ready for operation

Orange In operation

Yellow Waiting

Red Malfunction or error

3.1.2 Interfaces and connectors


The instrument provides the following interfaces and connectors.
Table 5 Interfaces
Designation Type Use
USB 1 USB Connector for USB devices
USB 2 USB Connector for USB devices

■■■■■■■■ 11
System overview ■■■■■■■■■■■■■■■■■■■■■■

Designation Type Use


Ethernet RJ-45 Connector for RS-232 instrument
server
Remote D-Sub Connector for devices with remote
interface
Power OUT Mini DIN
Power IN Mini DIN Connector for the energy supply
Ind Socket F High-ohm measuring input for pH
electrodes and redox electrodes
Ref Socket B, 4 mm High-ohm measuring input for
separate reference electrodes
Temp Socket B, 2 mm Measuring input for the Pt1000 or
NTC type temperature sensor
Pol Socket F Measuring input for polarizable
electrodes

NOTICE

Both temperature connectors must always be used for temperature


measurement. If a temperature sensor is used with only one banana
plug, the temperature cannot be measured.

12 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

3.2 Eco Titrator – Overview

Figure 2 Eco Titrator – Front

1 Bottle holder 2 Space for cylinder unit

3 Flat stopcock 4 Stand attachment

5 Magnetic stirrer 6 Status display, touch screen and con-


trol bar

■■■■■■■■ 13
Eco Titrator – Overview ■■■■■■■■■■■■■■■■■■■■■■

Figure 3 Eco Titrator – Rear

1 Type plate 2 USB connector (USB 1 and USB 2)

3 Ethernet connector (RJ-45) 4 Remote connector

5 "Power OUT" connector 6 "Power IN" connector

7 Pol connector 8 Temp connectors

9 Ref connector 10 Ind connector

14 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

Figure 4 Eco Titrator – Accessories

1 Cylinder unit 2 Tubing connections

3 Electrode cable 4 Electrode

5 Electrode holder 6 Guide sleeve

7 Clamping ring 8 Support rod

9 Buret tip 10 Amber glass bottle with GL 45 thread

11 Clip for SGJ 14/15 12 Bottle cap

13 Threaded stopper 14 Adsorber tube

■■■■■■■■ 15
Eco Titrator – Overview ■■■■■■■■■■■■■■■■■■■■■■

Figure 5 Eco Titrator – Peripherals

1 Printer Q3X (opt. accessory) 2 USB flash drive

3 Ethernet cable (opt. accessory) 4 Power supply unit

16 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

3.2.1 Dosing unit

Figure 6 Dosing unit – Overview

1 Cylinder unit 2 Push rod (dosing drive)

3 Flat stopcock

■■■■■■■■ 17
Eco Titrator – Overview ■■■■■■■■■■■■■■■■■■■■■■

3.2.1.1 Cylinder unit

Figure 7 Cylinder unit – Overview

1 Light protection 2 Dosing cylinder

3 Piston with sealing lips and piston rod 4 Mounting ring

18 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

3.2.1.2 Flat stopcock

Figure 8 Flat stopcock – Overview

1 Connector for the tubing connection to 2 Connector for the tubing connection to
the bottle the cylinder unit

3 Connector for the tubing connection to 4 Switching lever


the buret tip

■■■■■■■■ 19
Function ■■■■■■■■■■■■■■■■■■■■■■

3.2.2 Bottle unit

Figure 9 Bottle unit – Overview

1 Cannula 2 Threaded stopper

3 Bottle cap 4 Amber glass bottle with GL 45 thread

5 Clip for SGJ 14/15 6 Adsorber tube

3.3 Function
3.3.1 Magnetic stirrer
The magnetic stirrer ensures that the sample is well mixed. The stirring
rate can be adjusted depending on the amount and viscosity of the sam-
ple.
A clamping ring and an electrode holder can be fastened to the support
rod of the magnetic stirrer.

3.3.2 Dosing unit


Liquid volumes can be accurately dosed with the dosing unit.
The dosing unit is comprised of the following units:
■ Cylinder unit
■ Dosing drive
■ Flat stopcock
The dosing drive is permanently installed in the housing of the instrument.
The drive moves the push rod to raise and lower the piston in the dosing

20 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

cylinder of the cylinder unit and is responsible for accurate dosing of the
solution.
The flat stopcock switches between filling and emptying the dosing cylin-
der of the cylinder unit.
Once the cylinder unit is put into place, the dosing drive and the flat stop-
cock handle the following functions:
■ Raising and lowering the piston:
Solution is aspirated while the piston is being lowered. The dosing cyl-
inder fills up.
Solution is dosed while the piston is being raised. The dosing cylinder
empties.
■ Rotating the flat stopcock:
The position of the flat stopcock determines which connectors the sol-
ution flows through.

3.4 Indicators and controls


Indicators – Status display and status indicator

Figure 10 Indicators

1 Status display 2 Status indicator

The status indicator is only displayed on the touch screen.

Controls – Control bar

Figure 11 Control bar keys

1 On/Off 2 Increase stirring rate

3 Reduce stirring rate 4 Stop

5 Start

■■■■■■■■ 21
Interfaces and connectors ■■■■■■■■■■■■■■■■■■■■■■

3.5 Interfaces and connectors

Figure 12 Eco Titrator – Interfaces and connectors

1 USB 2 Ethernet
Connect USB flash drive, printer, balance, Remote control via local network
etc.

3 Remote 4 Power IN
Connect analog remote control / Eco Dosi- Connect power supply unit
mat

5 Pol 6 Temp
Connect a polarizable electrode Connect a temperature sensor (Pt1000 or
NTC) or an electrode with integrated tem-
perature sensor

7 Ref 8 Ind
Connect a reference electrode Connect a non-polarizable electrode (e.g.
ion-selective, pH, redox or other electrode)

NOTICE

Both temperature connectors must always be used for temperature


measurement. If a temperature sensor is used with only one banana
plug, the temperature cannot be measured.

22 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

3.6 Remote interface


Pin assignment of the remote interface
5 1
1 5

9 6
6 9
Figure 13 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies to all Metrohm instru-
ments with 9-pin D-Sub remote connector.
Table 6 Inputs and outputs of the remote interface
Pin no. Assignment Function
1 Output 0 Ready/EOD
2 Output 1 Activate/Dosimat
3 Output 2 Titration/Determination
4 Output 3 Cond. OK
5 Output 4 Error
6 0 volt (GND)
7 +5 Volt
8 Input 0 Start
9 Input 1 Stop

Inputs
+5 V approx. 5 kΩ Pull-up
tp
tP > 100 ms
active = low, inactive = high

Outputs

■■■■■■■■ 23
Remote interface ■■■■■■■■■■■■■■■■■■■■■■

Open Collector
tp
tp > 200 ms
active = low, inactive = high
IC = 20 mA, VCEO = 40 V
+5 V: maximum load = 20 mA

Status diagrams of the remote interface


EOD = End of Determination
Titration modes MET, DET, SET
EOD
Ready/EOD OUTPUT 0

Activ./Dos. OUTPUT 1

Titr./Determ. OUTPUT 2

Cond. OK OUTPUT 3

Error OUTPUT 4

Start INPUT 0

Stop INPUT 1

Figure 14 Remote status diagram titration mode, without error event

Ready/EOD OUTPUT 0

Activ./Dos. OUTPUT 1

Titr./Determ. OUTPUT 2

Cond. OK OUTPUT 3

Error OUTPUT 4

Start INPUT 0

Stop INPUT 1

Figure 15 Remote status diagram titration mode, with error event


CAL calibration mode

24 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

EOD EOD
Ready/EOD OUTPUT 0

Activ./Dos. OUTPUT 1

Titr./Determ. OUTPUT 2

Cond. OK OUTPUT 3

Error OUTPUT 4

Start INPUT 0

Stop INPUT 1

Figure 16 Remote status diagram CAL, without error event


EOD
Ready/EOD OUTPUT 0

Activ./Dos. OUTPUT 1

Titr./Determ. OUTPUT 2

Cond. OK OUTPUT 3

Error OUTPUT 4

Start INPUT 0

Stop INPUT 1

Figure 17 Remote status diagram CAL, with error event

3.7 Remote control


The instrument can be remote controlled via an Ethernet connection. An
RJ-45 plug with Local Area Network (LAN) is required for this. Connect the
Ethernet cable to the Ethernet connector on the rear of the instrument.
The connection can only be established if the instrument and the com-
puter are part of the same local network (LAN) and communicate via the
port 8005. The IP address of the instrument is defined under: Sys-
tem ▶ Ethernet settings

Transfer protocol
The data communication is synchronous. On each command there is an
acknowledgement by the instrument.
A command must be sent to the instrument with the control characters
CRLF as terminator. The acknowledgements of the instrument will also be
transferred with CRLF as terminator.
The instrument does not send spontaneous messages.

Commands and variables

■■■■■■■■ 25
Remote control ■■■■■■■■■■■■■■■■■■■■■■

Command Function Comment


$G Start/Continue Corresponds to the [START]
or [Continue] key.
$S Stop Corresponds to the [STOP]
key.
$H Hold Hold the method run.
$D Scan instrument Acknowledgements: Ready;0,
status Busy;0 or Hold;0 (0 = no mes-
sage).
If a message on the instrument
requires the interaction of the
user, the acknowledgement of
the status scan displays the
corresponding message num-
ber. Example:
Busy;010-119
= "Check buret unit"
The message can be acknowl-
edged with [OK] or [Cancel],
see below.
$A Confirm mes- Confirm the message on the
sage instrument with [OK].
A mandatory status scan pro-
viding the message number
must take place immediately
before confirming the mes-
sage, see above.
$A(CONTINUE), Confirm mes- Confirm the message with
$A(CANCEL) sage [CONTINUE] or [CANCEL].
$A(DELETE), Confirm mes- Confirm the message with
$A(CANCEL) sage [DELETE] or [CANCEL].
$A(YES), Confirm mes- Confirm the message with
$A(CANCEL) sage [YES] or [CANCEL].
$A(RECONNECT) Confirm mes- Confirm the message with
sage [RECONNECT].
$L(method Loading the The method name has to be
name) method known and unique.

26 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

Command Function Comment


$Q(variable) Request varia- Examples for variables: EP1,
ble value R1, C00.
Complete list of the variables:
see chapter Formula editor.

The values of the variables are only available after the end of a determina-
tion (in the status 'ready').

Acknowledge- Comment
ment of the
instrument
OK Command executed
E1 Method not found
E2 Invalid variable
E3 Invalid command

3.8 Arithmetic algorithms


Numerical format
The software of the instrument calculates in accordance with the wide-
spread standard IEEE 754 (IEEE Standard for Binary Floating-Point Arith-
metic for Microprocessor Systems). This means that the numbers are used
in calculations in "double precision" (64 bit). Decimal numbers are conver-
ted into binary numbers in the computer and used in this form for calcula-
tions. The output on the display and in reports once again contains deci-
mal numbers; the binary numbers are thus converted back into decimal
numbers. In order to be able to check the internal calculations performed
by the computer yourself in accordance with IEEE 754, the numbers are
reproduced in the calculation report in complete accuracy. A minimal dif-
ference may arise between an originally entered decimal number and the
internal computer representation in complete accuracy in the range of the
rear decimal places. This difference results from the fact that an exact
binary equivalent does not exist for every decimal number. If, for example,
you enter the sample size 50.3 mg, this will be depicted in the calculation
report in "double precision" with 5.02999999999999E+01.

Rounding-off process
Measured values and results are rounded to the defined number of deci-
mal places (commercial rounding, in accordance with the US Pharmaco-
peia USP). If the digit at the first dropped decimal place is 1, 2, 3 or 4,
then it will be rounded off; if this digit is 5, 6, 7, 8 or 9, then it will be

■■■■■■■■ 27
Arithmetic algorithms ■■■■■■■■■■■■■■■■■■■■■■

rounded up. Negative digits will be rounded in accordance with their


amount, i.e. away from zero.
Examples:
2.33 yields 2.3
2.35 yields 2.4
2.47 yields 2.5
–2.38 yields –2.4
–2.45 yields –2.5

Statistics
The arithmetic mean value and the absolute and relative standard devia-
tions of results are calculated:
You can statistically evaluate a maximum of five results (1 ≤ k ≤ 5) calcula-
ted in a determination. A statistical series can contain a maximum of 20
determinations (1 ≤ n ≤ 20).
The following convention applies to the subsequent formulas:
1 ≤ n ≤ 20 and 1 ≤ k ≤ 5.

Mean value:

Absolute standard deviation:

Relative standard deviation (in %):

Explanations
The individual values are incorporated in the statistics with full accuracy.
15 significant places are yielded when the 64 bit numerical format is
applied for the floating-point number in decimal presentation.
The accuracy can be controlled by the selection of the prefix of the unit
(milli, micro) and the number of decimal places.
Example
The result displayed, 1234.56789158763 mg/L , has 15 significant pla-
ces. It should be rounded off to three decimal places according to the
above rounding-off process:
■ 1234.568 mg/L.

28 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Functional description

If the same result is expressed in "g/L" (1.23456789158763 g/L), and is


also rounded off to three decimal places, this yields
■ 1.235 g/L.
I.e. you obtain the lowest losses in accuracy with rounding when you
select the application and the numerical format in such a way that the
numbers displayed have as many places before the decimal point as possi-
ble.
A complete recalculation of the statistics using a pocket calculator or PC
calculation programs may exhibit deviations. This can be explained by the
different binary numerical formats used by these computers.

NOTICE

The above losses of accuracy by rounding off in the range of signifi-


cant places are only relevant theoretically. They are generally several
orders of magnitude less than measurement technique uncertainties
(balance errors, dosing errors, measuring errors).

■■■■■■■■ 29
Delivery ■■■■■■■■■■■■■■■■■■■■■■

4 Delivery and packaging

4.1 Delivery
Inspect the delivery immediately upon receipt:
■ Check the delivery against the delivery note to ensure completeness.
■ Check the product for damage.
■ If the delivery is incomplete or damaged, contact your regional Met-
rohm representative.

4.2 Packaging
The product and accessories are supplied in protective special packaging.
Keep this packaging to ensure safe transportation of the product. If a
transport locking device is present, keep this as well for future reuse.

30 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Installation

5 Installation

5.1 Setup location


The product is only suitable for operation indoors and may not be used in
explosive environments.
The following requirements apply to the setup location:
■ The room is well ventilated, protected against direct sunlight and
excessive temperature fluctuations.
■ The setup space is stable and free of vibrations. The setup space must
be suitable for the dimensions and weight of the components (see
Technical specifications).
■ All cables and connectors are accessible during operation. The cables
are safely installed (no tripping hazards).
■ The workplace is ergonomically designed and ensures trouble-free
operation of the product.

5.2 Preparing the assembly

WARNING

Electric shock from electrical potential


Risk of injury by touching live components or through moisture on
live parts.
■ Never open the housing of the product.
■ Protect live parts (e.g. power supply unit, power cord, connection
sockets) against moisture.
■ If you suspect that moisture has gotten into the product, discon-
nect the product from the energy supply. Then notify Metrohm
Service.
■ Only personnel who have been issued Metrohm qualification may
perform service and repair work on electrical and electronic com-
ponents.

■■■■■■■■ 31
Preparing the assembly ■■■■■■■■■■■■■■■■■■■■■■

Connecting the power cord

Figure 18 Rear of the instrument – Connecting the power cord

NOTICE

The flat side of the plug of the power supply unit must face
downwards.

Connect the power supply unit to the Power IN connector. Note the
orientation (see figure).
The instrument can now be switched on and off.

32 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Installation

5.3 Switching the instrument on and off


Switching on the instrument

Prerequisite
The power cord is connected.

1 Press the key.


The instrument is initialized and a system test is performed.
If the Beep parameter is activated in the system settings of the
parameters, then a beep will be heard after switch-on.

2 If the PREP warning is activated in the system settings, a message


to execute the Prepare buret (PREP) function will appear.
Make sure that the buret tip points into a vessel. [Continue].
All tubing and the cylinder are rinsed and filled with Prepare buret
(PREP).

The instrument is switched on and the start page is displayed.

Switching off the instrument

The instrument is switched off with the key. In order to prevent acci-
dental switch-off, the key must be held for an extended time.

1 Press and hold the key for at least 4 s.


A progress bar appears. If the key is released during this time, the
instrument will remain switched on.

NOTICE

To power down the product, you must unplug the power cord
from the energy supply.

■■■■■■■■ 33
Initial assembly of the cylinder unit ■■■■■■■■■■■■■■■■■■■■■■

5.4 Initial assembly of the cylinder unit


The initial assembly of the cylinder unit is carried out with an installation
wizard.
The installation wizard not only supports the assembly of the cylinder unit
but also the assembly of the remaining accessories:
■ Support rod and clamping ring
■ Electrode holder
■ Bottle unit
■ Tubing connections
■ Beaker and stirring bar
■ Link stopper and buret tip
■ Electrode

NOTICE

If the instrument has already been set up, the cylinder unit is disas-
sembled and assembled with the Manual control ▶ Exchange cyl-
inder unit function.

Executing the installation wizard

Prerequisite
The instrument is switched on. The push rod is in the lowest position.
Procedure

1 If the instrument is switched on for the first time, the installation wiz-
ard is started automatically.
The installation wizard can be opened manually with the Manual
control ▶ Installation wizard function.

34 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Installation

Figure 19 Opening the installation wizard manually

2 Mount the cylinder unit according to the instructions on the screen.


After having executed a step, move to the next step with .
The cylinder unit has been mounted.

3 Continue with the installation wizard to mount the remaining


accessories.
The last picture shows the instrument with all the accessories moun-

ted. Click on to end the installation wizard.

NOTICE

Further accessories can also be mounted without the installation wiz-


ard.

■■■■■■■■ 35
Mounting the support rod ■■■■■■■■■■■■■■■■■■■■■■

5.5 Mounting the support rod


Mounting the support rod

Procedure

1 Screw the support rod onto the stand attachment.


The clamping ring and the electrode holder can now be mounted to
the support rod.

NOTICE

The clamping ring is used as the lower stop for the electrode
holder. The clamping ring prevents the electrode holder with the
mounted electrode from being lowered too far.

Mounting the electrode holder and the clamping ring

Procedure

1 Push the clamping ring over the support rod with the indent facing
upward as far as it will go.

2 Press the locking lever on the electrode holder.

3 Push the electrode holder over the support rod.

4 To fix the electrode holder in place, release the locking lever at the
desired height.

5 Push the clamping ring under the electrode holder.


Rotate the clamping ring in such a way that the wedge on the elec-
trode holder fits in the indent in the clamping ring.
Tighten the knurled screw.
The clamping ring is used as the lower stop for the electrode holder.

The electrode holder can now be equipped with the accessories.

36 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Installation

5.6 Preparing the bottle unit

Preparing the bottle cap with adsorber tube

1 Insert the cannula.

2 Insert the threaded stopper.

3 Fill the adsorber tube with a suitable sorbent:


■ Molecular sieve for water sensitive samples.
■ Soda lime for CO2 sensitive samples.
If no special sorbent is required, then the adsorber tube can be filled
with cotton and used as a dust filter.

4 Place the filled adsorber tube on the bottle cap.

5 Secure the adsorber tube in place with the clip for SGJ 14/15.

■■■■■■■■ 37
Mounting the tubing connections ■■■■■■■■■■■■■■■■■■■■■■

Assembling and setting up the bottle

1 Set the bottle in the bottle holder.

2 Screw the prepared bottle cap onto the bottle and tighten it by
hand.

5.7 Mounting the tubing connections


The tubing connections connect the bottle cap with the flat stopcock, the
cylinder unit and the buret tip.

Figure 20 Tubing connections

NOTICE

Tighten all the tubing connections by hand. Use no other aids. The
thread of the screw nipples and the tubing openings must not be
deformed.

38 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Installation

Mounting the tubing connections and the buret tip

Prerequisite:
■ The cylinder unit, electrode holder and bottle unit are set up.

1 Screw the 6.1805.090 tubing securely to the cylinder unit and to the
flat stopcock.

2 Screw the 6.1805.090 tubing securely to the bottle unit and to the
flat stopcock.

3 Screw the 6.1805.100 tubing securely to the flat stopcock.

4 Screw the buret tip securely to the 6.1805.100 tubing.

5 Insert the buret tip into the guide sleeve on the electrode holder.

5.8 Mounting the electrode


During the titration, it is important that the solution is mixed well. The stir-
ring rate should be high enough to form a small vortex. If the stirring rate
is too high, then air bubbles will be stirred into the measuring solution.
This results in incorrect measured values. If the stirring rate is too low,
then the solution at the electrode will not be mixed correctly. In order for
the measurement to be taken in a well-mixed solution after the addition
of the titrant, the buret tip should be positioned where turbulence is high.
Furthermore, the distance between the addition of the titrant and the
electrode should be as large as possible. Therefore, take into account the
stirring direction when positioning the electrode and buret tip.

Figure 21 Schematic arrangement during a titration

1 Stirring bar 2 Electrode

3 Buret tip

■■■■■■■■ 39
Switching the instrument on and off ■■■■■■■■■■■■■■■■■■■■■■

6 Start-up

6.1 Switching the instrument on and off


Switching on the instrument

Prerequisite
The power cord is connected.

1 Press the key.


The instrument is initialized and a system test is performed.
If the Beep parameter is activated in the system settings of the
parameters, then a beep will be heard after switch-on.

2 If the PREP warning is activated in the system settings, a message


to execute the Prepare buret (PREP) function will appear.
Make sure that the buret tip points into a vessel. [Continue].
All tubing and the cylinder are rinsed and filled with Prepare buret
(PREP).

The instrument is switched on and the start page is displayed.

Switching off the instrument

The instrument is switched off with the key. In order to prevent acci-
dental switch-off, the key must be held for an extended time.

1 Press and hold the key for at least 4 s.


A progress bar appears. If the key is released during this time, the
instrument will remain switched on.

NOTICE

To power down the product, you must unplug the power cord
from the energy supply.

40 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Start-up

6.2 Setting the language, date and time


Date, time, language and dialog type can be set once the instrument has
been correctly installed.

Setting the language

Prerequisite:
■ The instrument is switched on.

1 On the Start page, open the System ▶ Settings menu.

2 Click on the Language button.

3 Select the desired dialog language.


The user interface is now displayed in the selected language.

Setting the date and time

1 On the Start page, open the System ▶ Settings menu.

2 Click in the Date input field.

3 Enter the current date. Format: YYYY-MM-DD.

4 Confirm the entry with OK.

5 Click in the Time input field.

6 Enter the current time. Format: hh:mm:ss.

7 Confirm the entry with OK.

■■■■■■■■ 41
Setting the dialog type ■■■■■■■■■■■■■■■■■■■■■■

6.3 Setting the dialog type


The user rights can be restricted with the [Dialog type] input field:
■ Dialog type Expert (default value)
In the dialog type Expert, all the user settings are available.
■ Dialog type Routine
In the dialog type Routine, the availability of the settings is restricted.
The System and Methods menus as well as the Parameters work
area can only be opened with a password. Methods can be loaded,
however, on the start page.

NOTICE

If the instrument is switched off, the dialog type that was set remains
activated.

Setting the Routine dialog type

1 On the Start page, open the System ▶ Settings menu.


The [Dialog type] input field is on page 2/2:

2 Expand the [Dialog type] input field. Select the Routine dialog
type.

3 Exit the System menu.


The instrument is now in Routine mode. The availability of the set-
tings is restricted.

Setting the Expert dialog type

1 On the Start page, click on the System button.


The Enter password message appears:

42 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Start-up

2 Click in the input field.


A keyboard appears.

3 Enter the password:


■ Password for firmware version 57.1008.0010 or higher:
METROHM9100
■ Password for firmware version 57.1008.0009 or lower:
MSH9101
Confirm with [OK].

4 Confirm the entry with OK.


The System menu opens. The menu is now ready for use.
If you exit the System menu at this point, the instrument will return
to Routine mode.

5 Click on the [Settings] button.

6 Expand the [Dialog type] input field. Select the Expert dialog type.
All the user settings are available.

■■■■■■■■ 43
Display elements and controls ■■■■■■■■■■■■■■■■■■■■■■

7 Operation and control

7.1 Display elements and controls


All displays, controls and commands for operating the Eco Titrator can be
found in the user guidance (status display, touch screen and control bar).

Figure 22 User guidance – Status display, touch screen and control bar

1 Status display 2 Touch screen

3 Control bar

The status display uses flashing patterns to display the operating status
of the instrument.
The touch screen is used to enter data and to control runs. Results and
evaluations are also displayed on the touch screen.
The control bar is used to switch the instrument on and off, to control
the stirring rate during a determination and to start and stop determina-
tions.

44 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

NOTICE

Commercially available glass cleaner can be used for cleaning the


touch screen.

7.2 Switching the instrument on and off


Switching on the instrument

Prerequisite
The power cord is connected.

1 Press the key.


The instrument is initialized and a system test is performed.
If the Beep parameter is activated in the system settings of the
parameters, then a beep will be heard after switch-on.

2 If the PREP warning is activated in the system settings, a message


to execute the Prepare buret (PREP) function will appear.
Make sure that the buret tip points into a vessel. [Continue].
All tubing and the cylinder are rinsed and filled with Prepare buret
(PREP).

The instrument is switched on and the start page is displayed.

Switching off the instrument

The instrument is switched off with the key. In order to prevent acci-
dental switch-off, the key must be held for an extended time.

1 Press and hold the key for at least 4 s.


A progress bar appears. If the key is released during this time, the
instrument will remain switched on.

■■■■■■■■ 45
User interface ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

To power down the product, you must unplug the power cord
from the energy supply.

7.3 User interface

Figure 23 Start page with access to the functions

1 Work areas 2 Menu path

3 Button 4 Status indicator

5 Icon 6 Method selection bar

Work areas
Once the instrument is ready for operation, the work areas can be selec-
ted. Work areas that cannot be selected are grayed out.

NOTICE

If necessary, click the button so that the piston moves to the basic
position, the status display lights up and the status indicator is green.

The following work areas can be selected:

46 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

Eco Titrator start page


The start page with access to the functions:
■ Methods
■ Manual control
■ System
■ Print reports

Sample data
Access to the sample data: sample size, unit, ID1 and ID2

Parameters
Access to the parameters, grouped into the following categories:
■ Start conditions
■ Titration parameters
■ Stop conditions
■ Evaluation
■ Calculation
■ Statistics
■ Reports

Results
Access to the calculated results and the stop criterion.

Live status
Access to the graphic display of the ongoing determination.

Menu path
In the menu path, clicking one of the elements of the menu path can be
used to call up the respective menu.

Buttons, input fields, keyboards and help texts


The menu provides the following possible inputs and information:
■ Buttons
The respective menu is called up by clicking the button.
■ On/off switch
The corresponding function is activated or deactivated by clicking on
[ON] or [OFF].

■■■■■■■■ 47
User interface ■■■■■■■■■■■■■■■■■■■■■■

■ Input fields
The respective keyboard is called up by clicking the button of the input
field.
■ Keyboards
Input of text, numbers or characters. An appropriate keyboard is called
up, depending on the type of input.

NOTICE

Help texts
Help texts (in English) are available for the input fields. The respective
help text is called up by long pressing (for at least 3 seconds) on an
input field. Default values and possible inputs are displayed.

Status indicator
The status indicator on the touch screen uses colors to display the operat-
ing status of the instrument.

Icon
The following functions can be called up with the different icons -
depending on the context:
■ Save
■ Delete
■ Export
■ etc.

Method selection bar


The list of saved methods opens by clicking on the method selection bar.
The list can be searched with the scroll bar and the requested method can
be loaded by clicking on it.

Brightness of the display


The brightness of the display can be adjusted on the start page in the Sys-
tem ▶ Diagnosis ▶ Display test menu.

NOTICE

The most recently set brightness appears when the instrument is


switched on.

48 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

Brightness
Input range 1 to 10
Default value = 7

Figure 24 Display – Controls

1 Menu path 2 Reduce brightness

3 Increase brightness

Keyboards
Different keyboard types are available.

Figure 25 Keyboard (example: lower-case characters)

1 Input field 2 Delete entry

3 Backspace 4 Cancel input (close window)

5 Apply entry 6 Forwards in the input field

■■■■■■■■ 49
User interface ■■■■■■■■■■■■■■■■■■■■■■

7 Backwards in the input field 8 Space

9 Switch keyboard

Figure 26 Keyboard (example: numbers)

1 Input field 2 Delete entry

3 Backspace 4 Cancel input (close window)

5 Apply entry 6 Forwards in the input field

7 Backwards in the input field 8 Specifications

9 Algebraic sign change

7.3.1 Formula editor

Figure 27 Formula editor

1 Input field 2 Delete entry

3 Backspace 4 Cancel input (close window)

50 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

5 Apply entry 6 Forwards in the input field

7 Backwards in the input field

The formula editor allows for the entry of formulas. The formula editor is
equipped with an automatic syntax check. This is triggered as soon as a
formula is applied. The generally valid rules of priority apply for the calcu-
lation operations.

Variable Description
C00 Sample size
EP# Volume of endpoint EP# (# = 1–9)
CI# Sample identification (# = 1–2)
R# Result (# = 1–5)
FP# Volume of fixed point FP# (# = 1–2)
CV0# Common variable (# = 1–5)
SMN# Mean value of result R# (# = 1–5)
TITER Titer of selected solution
CONC Concentration of selected solution
Var List of additional variables
Templates List of predefined calculation formulas

"#" stands for a sequential number that you must enter manually. Exam-
ple: If you apply the variable EP# in the formula, only EP is entered. In
order to define the EP to be used, the corresponding number has to be
added manually after "EP". Example: EP5

Variables
Clicking on [Var] displays a list with additional variables. You can enter
these variables either directly into the formula or also by selecting them
from the list and applying them with [OK].

Variable Description
MIM Initial measured value, i.e. measured value prior to the
processing of the start conditions
MSM Start measured value, i.e. measured value after the pro-
cessing of the start conditions
MCV End volume, i.e. total dosed volume at the end of the
titration
ET# Temperature at endpoint EP# (# = 1–9)

■■■■■■■■ 51
User interface ■■■■■■■■■■■■■■■■■■■■■■

Variable Description
EM# Measured value of endpoint EP# (# = 1–9)
ED# Time at endpoint EP# (# = 1–9)
MSV Start volume
MEN Electrode zero point pH(0)
MSL Electrode slope
DD Duration of the entire determination
MST Start temperature
MCT End temperature
FT# Temperature at fixed point FP# (# = 1–2)
FM# Measured value of fixed point FP# (# = 1–2)
FD# Time at fixed point FP# (# = 1–2)

For information on the meaning of the placeholder Molw, see the follow-
ing note.

Calculation templates
Pressing [Templates] displays a list with calculation templates. You can
apply these templates directly with .

NOTICE

Some templates contain the placeholder Molw, which stands for the
molar mass of the sample. You must replace this placeholder with the
correct value in the calculation formula.

Template Description
Content % Content in %
Unit of the sample size = g
Content Content in mmol/L
mmol/L
Unit of the sample size = mL
Content Content in mol/L
mol/L
Unit of the sample size = mL
Content g/L Content in g/L
Unit of the sample size = mL

52 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

Template Description
Content Content in ppm
ppm
Unit of the sample size = g
Titer Titer calculation
Unit of the sample size = g
Blank mean Blank value as mean value of single results
value
Blank single Blank value as single value
value

7.4 Manual control


The [Manual control] button on the start page offers the following func-
tions:

Figure 28 Manual control – Functions


■ Dosing – Dose a specified volume or dose continuously.
■ Measurement – pH measurement or potentiometric potential measure-
ment.
■ Exchange cylinder unit – Empty and safely exchange the cylinder unit.
■ Prepare buret – The cylinder and the tubing of the buret unit are rinsed
and filled.
■ Stirrer – Switch the stirrer on and off and set the stirring rate.
■ Installation wizard – Initial installation of the cylinder unit.

■■■■■■■■ 53
Manual control ■■■■■■■■■■■■■■■■■■■■■■

7.4.1 Manual control – Dosing


The following manual dosing functions are available with the Eco Titrator:
■ Dosing a fixed volume (ADD) – Dosing a specified volume.
■ Continuous dosing (DOS) – Dosing as long as the key is being
pressed.

Dosing a specified volume (ADD)

1 Selecting the dosing function


Click on Start page ▶ Manual control ▶ Dosing ▶ ADD.

2 Configuring the dosing function

NOTICE

■ The dosing and filling rates should be decreased for viscous


and highly volatile liquids.
■ The maximum dosing rate and maximum filling rate depend
on the cylinder volume.
■ In manual control, the instrument doses in steps of 1/20,000
of the cylinder volume. The entered dosing volume is rounded
accordingly.

■ Enter the dosing rate.


■ Enter the filling rate (filling the cylinder).
■ Enter the required dosing volume.

54 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

3 Starting the dosing

Press the key.


The dosed volume is shown on the screen.
After the volume of one cylinder has been dosed, the dosing cylinder
will be refilled automatically.

Dosing continuously (DOS)

1 Selecting the dosing function


Click on Start page ▶ Manual control ▶ Dosing ▶ DOS.

2 Configuring the dosing function

NOTICE

■ The dosing and filling rates should be decreased for viscous


and highly volatile liquids.
■ The maximum dosing rate and maximum filling rate depend
on the cylinder volume.

■ Enter the dosing rate.


■ Enter the filling rate (filling the cylinder).

■■■■■■■■ 55
Manual control ■■■■■■■■■■■■■■■■■■■■■■

3 Starting the dosing

■ Press the key for as long as dosing should take place.


Pausing the dosing: Release the key.
Continuing the dosing: Press the key again for as long as dos-
ing should take place.
The dosed volume is shown on the touch screen.

4 Use the button to stop the process and fill the cylinder.

7.4.2 Manual control – Measurement


The following measuring functions are available in the manual control:
■ pH – pH measurement
■ U – potentiometric potential measurement

Measuring manually

1 Selecting the measuring function


Click on Start page ▶ Manual control ▶ Measurement.

2 Selecting the measured quantity


Click on [pH] or [U].

3 Configuring the measuring mode


■ Select the required electrode from the sensor list. The selection
depends on the measuring mode.
The sensor list can be managed under System ▶ Sensors on the
Start page.
■ Enter the measuring temperature if no temperature sensor is
connected.
If a temperature sensor is connected, then the temperature will be
measured automatically.
The measuring temperature is used for automatic temperature
compensation with pH measurements.

4 Starting the measurement

Press the key.


The current measured value and the measuring temperature are
shown on the screen.

56 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

5 Stopping the measurement

Press the key.

7.4.3 Exchanging the cylinder unit


In the Exchange cylinder unit function, the drive moves the push rod
into the exchange position.

CAUTION

Property damage caused by jammed cylinder unit


Damage caused by disassembling of a jammed cylinder unit. The
damaged cylinder unit must be replaced.
■ Do not use force to rotate the cylinder top piece.
■ Follow the instructions for disassembling the cylinder unit.

CAUTION

Instrument damage from aggressive chemical hazardous sub-


stances
Damage of the instrument or malfunction through contact with
aggressive chemical substances.
■ Clean up spilled liquids and solids immediately.
■ Use protective grounding when working with highly flammable
chemical substances and gases.
■ If you suspect that chemical substances have gotten into the
instrument, disconnect the instrument from the energy supply.
Then, notify Metrohm Service.

Emptying, disassembling and mounting

1 On the start page, open the Manual control menu.


Click on the [Exchange cylinder unit] button.
A splash warning appears:

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Manual control ■■■■■■■■■■■■■■■■■■■■■■

2 ■ Make sure that the buret tip points into a vessel.


■ [Continue]
The piston rises and the dosing cylinder empties as much as possible.
The message Exchanging cylinder unit... appears.
Once the push rod has reached the top position, the following warn-
ing appears:

3 ■ Make sure that the tubing from the bottle cap is removed.
■ [Continue]
The message Exchanging cylinder unit... appears and the piston is
lowered down to the height at which the cylinder unit can be disas-
sembled.

4 ■ Remove the tubing of the cylinder unit.


■ [Continue]

5 Disassembling the cylinder unit and mounting a new cylinder


unit
■ Rotate the cylinder unit counterclockwise until it detaches from its
thread. Pull the cylinder unit upwards until the piston rod is visible.
Carefully slide the cylinder unit to the side to remove it.

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■■■■■■■■■■■■■■■■■■■■■■ Operation and control

NOTICE

The disassembled cylinder unit can be cleaned and reused or


replaced with a new cylinder unit.

■ To mount the new cylinder unit, the piston rod should protrude by
approx. 6 mm from the dosing cylinder. If necessary, pull the pis-
ton carefully out of the dosing cylinder with the 6.1546.040 pis-
ton tool.
While doing so, make sure that the sealing lips and the piston in
the dosing cylinder are not damaged.
■ Couple the piston rod with the push rod.
When doing so, the hook profile of the piston rod must be care-
fully aligned in the hook profile of the push rod.
■ Carefully push the cylinder unit downwards. The piston is pushed
into the dosing cylinder.
Screw the light protection of the cylinder unit securely into the
thread of the housing.

6 Click on the [Continue] button.


The push rod moves the piston into the basic position.

7 ■ Make sure that the cylinder unit has been mounted correctly.
■ [Continue]

8 [Continue]

NOTICE

Make sure that the value for the cylinder volume in the System
menu is the same as the volume of the mounted cylinder unit.

9
NOTICE

Carry out the Prepare buret (PREP) command.

The cylinder unit has been replaced and is ready for use.

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Manual control ■■■■■■■■■■■■■■■■■■■■■■

7.4.4 Preparing the buret (PREP)


The PREP function is used to rinse the cylinder and tubings of the buret
unit and fill them air bubble-free. You should carry out this function daily
before the first determination.

Preparing the buret (PREP)

1 On the Start page, click on the [Manual control] button.

2 Click on the [Prepare buret (PREP)] button.


A splash warning appears:

3 Make sure that the buret tip points into a vessel.


[Continue]
The piston rises and sinks and the cylinder empties and fills in 2
cycles.
Then, the buret is prepared.

7.4.5 Operating the magnetic stirrer

Switching the stirrer on and off

1 Add the stirring bar to the titration vessel.

2 On the Start page, click on the [Manual control] button.

3 Click on the [Stirrer] button.


The controls for the magnetic stirrer appear:

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4 Switching on the stirrer

Click on the button. This button is only visible if the stirrer is


switched off.
The stirrer begins stirring with the most recently set stirring rate.

5 Switching off the stirrer

Click on the button. This button is only visible if the stirrer is


switched on.
The stirrer stops.

Stirring rate
The stirring rate can be adjusted in 15 steps. The default value is 8.

Setting the stirring rate

Prerequisite:
■ The magnetic stirrer controls are opened: Start page ▶ Manual con-
trol ▶ Stirrer
■ The stirrer is switched on.

1 Reducing the stirring rate in steps

Click on the button repeatedly until the desired stirring rate has
been reached.
Each click reduces the stirring rate by one step. The current stirring
rate is displayed.

2 Increasing the stirring rate in steps

Click on the button repeatedly until the desired stirring rate has
been reached.
Each click increases the stirring rate by one step. The current stirring
rate is displayed.

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Methods ■■■■■■■■■■■■■■■■■■■■■■

7.5 Methods
Definition
A method determines how determinations are carried out. The titration
mode, measured quantity and further parameters are defined in a
method.
Methods are saved under a freely selectable method name. A method
name consists of a maximum of 12 characters.

Method selection bar


The method selection bar on the start page shows the method that has
been loaded. If needed, another method can be loaded in the method
selection bar. Determinations can be executed with the method that has
been loaded.

Figure 29 Method selection bar

Display in the Example Meaning


method selection
bar
Method name MET_pH The method is saved in the
method list.
Method name MET_pH The method has just been created.
[New] [New] It has not been saved.
Method name MET_pH The method has been modified.
[Modified] [Modified] The modifications have not been
saved.

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A new or modified method is available for determinations until it is


changed or until another method is loaded. To use the method at a later
point, it can be saved in the method list.

Method list
The [Method] button on the start page shows a list of all the saved meth-
ods. Methods can be created, exported and deleted here.

Figure 30 Method list (example)


A scroll bar appears if the list is longer.

Titration mode
Each method is based on a titration mode. The following titration modes
are available:
■ MET – Monotonic equivalence point titration
3 measured quantities are available: pH, U or Ipol
■ DET – Dynamic equivalence point titration
3 measured quantities are available: pH, U or Ipol
■ SET – Endpoint titration
3 measured quantities are available: pH, U or Ipol
■ CAL – Calibration of pH electrodes
Measured quantity: pH

7.5.1 Using and managing methods


Methods are used as follows:
■ Load method – Allows for the execution of determinations with the
method that has been loaded. Allows for changes of the method that
has been loaded.
■ Change method parameters – Changes the parameters of the
method that has been loaded.
■ Store method – The method that has been loaded can be added to
the method list.

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Methods ■■■■■■■■■■■■■■■■■■■■■■

The following options are available to create and manage methods:


■ Create new method
■ Delete method – Remove the method from the method list.
■ Export method – Print out the method or save it to a USB flash drive.
■ Import method – Add a method from a USB flash drive to the
method list.

Loading the method

Procedure

1 Open the method selection bar on the Start page:


Click on .
A list with the saved methods appears. The list can be searched with
the scroll bar.

2 Select the desired method.


The desired method appears in the method selection bar and is loa-
ded.

3 Change the method parameters if necessary.


The method is available for determinations.

Changing the method parameters

Procedure

1 Load the method that you want to change in the method selection
bar on the Start page.

2
Open the Parameters work area:

3 Set the parameters if necessary.

4 Continue with one of the following steps:


■ Carry out determinations with the modified method.
■ Go to the Start page and save the method for later use.

Saving the method

If you modify method parameters, then you can save these as your own
method. A maximum of 120 methods can be saved.

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Procedure
The method that you want to save is loaded in the method selection
bar. The method is marked [New] or [Modified].

1 Save the method:

An input field for the name appears.

2 Click on the input field.


A keyboard appears.

3 Enter the desired name with the keyboard. Finish with [OK].
The name that was entered appears in the method selection bar. The
method is now saved in the method list.

Creating a new method

Procedure

1 On the Start page, click on the [Methods] button.


The method list opens.

2 Create a new method:

A selection of titration modes and measured quantities appears.

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Methods ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

If modifications on the method that was loaded before have not


been saved, the following warning appears:
Store method: The modifications of the current method
have not been saved. Do you want to load the method
anyway?
■ [Yes] – a new method is created. The changes on the method
that is currently loaded are discarded.
■ [Cancel] – creation of the new method is canceled.

3 ■ Select the desired titration mode by clicking on it. Example: MET


■ Click to select the desired measured quantity. Example: pH

■ Click on .
The new method appears in the method selection bar. The method is
marked with [New]. Example: MET_pH [New]

4 Set the method parameters.

5 Continue with one of the following steps:


■ Carry out determinations with the new method.
■ Save the method for later use.

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Deleting a method

Procedure

1 On the Start page, click on the [Methods] button.


The method list appears.

2 Select the method that you want to delete by clicking on it.


The selected method is highlighted in green.

3 Delete the highlighted method:

The warning Delete method appears.

4 Confirm deleting: [Delete]


The deleted method is no longer available in the method list.

Exporting a method

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [Methods] button.


The method list appears.

3 Select the method that you want to export by clicking on it.


The selected method is highlighted in green.

4 Export the marked method:

The message Exporting method to USB flash drive... appears.


Once the message has disappeared, the method is saved to the USB
flash drive that is connected.

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Methods ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

If a method with the same name already exists on the USB flash
drive, then the following warning appears: Store method:
Method name already exists. Do you want to overwrite
the name?.
■ [Yes]: The method on the USB flash drive will be overwritten.
■ [No]: The method will not be exported.

Importing a method

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [System] button. Move to page 2


and click on [File management].
A list with the methods saved on the USB flash drive appears.

3 Select the method that you want to import by clicking on it.


The selected method is highlighted in green.

4 Import the highlighted method:

The message Importing method from USB flash drive...


appears.
Once the message has disappeared, the method is saved to the
instrument.

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NOTICE

If a method with the same name already exists on the instru-


ment, then the following warning appears: Store method:
Method name already exists. Do you want to overwrite
the name?.
■ [Yes]: The method on the instrument will be overwritten.
■ [No]: The method will not be imported.

7.6 Sample data


Definition
A sample is the substance to be analyzed. With the sample data, the
samples can be identified.

Input options
There are 2 options for entering sample data:
■ Directly in the Sample data work area.
■ Automatic request immediately after the start of the determination.

Entering the sample data in the Sample data work area

Clicking on the button displays the Sample data work area.

The data for the sample can be entered in the Sample data work area,
even if the determination is ongoing.

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Sample data ■■■■■■■■■■■■■■■■■■■■■■

ID1
The sample identification ID1 can be used in calculations as the variable
CI1.
Input: max. 10 characters
Default value: empty

ID2
The sample identification ID2 can be used in calculations as the variable
CI2.
Input: max. 10 characters
Default value: empty

Sample size
The value of the sample size can be used in calculations as the variable
C00.
Input range –999,999,999 to 9999999999
Default value 1.0

Unit
Unit of the sample size.
Selection:
■ g
■ mg
■ µg
■ mL
■ µL
■ Pieces
■ User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.
Default value: g

Requesting sample data at the start of the determination


The sample data can be requested immediately after the start of the deter-
mination in order to ensure that the sample data entry is not forgotten.
This automatic request is indispensable if the samples are weighed by dif-
ference.

70 ■■■■■■■■
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The automatic sample data request can be controlled for each method
separately. The following parameters are available under [Start condi-
tions] in the Parameters work area:
■ Request sample ID
■ Request sample size
■ Request sample unit
■ If the Hold at request parameter is activated, the run will be paused
and must be continued with after the sample data has been
entered.
■ If Hold at request is deactivated, then the titration will be started in
the background. This dialog will be displayed until the entering of the
sample data is confirmed with or until the sample data is transfer-
red from the balance, even if the titration is already completed. This
ensures that the sample data is available for calculations.

7.6.1 Sample series


The following options are available to create and manage sample data:
■ Activate sample series
■ Create new samples
■ Edit samples
■ Delete individual samples – Delete samples from the sample table.
■ Delete sample table – Delete all samples from the sample table.
■ Reset sample table – All samples are reset to not executed.

Activating the sample series

1 On the Start page, click on the [Sample series] button.

2 Click on [ON].

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Sample data ■■■■■■■■■■■■■■■■■■■■■■

3
Go to the Sample data work area:
The sample table appears.

Creating new samples

1
Go to the Sample data work area:

2 Insert a new sample:


The message Inserting a new sample... appears.
The new sample is inserted in the sample table as soon as the mes-
sage disappears.

72 ■■■■■■■■
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Editing samples

1
Go to the Sample data work area:

2 Select the sample that you want to edit by clicking on it.

3 Edit sample:

4 Make the desired changes.

Deleting individual samples

1
Go to the Sample data work area:

2 Select the sample that you want to delete by clicking on it.


The selected line is highlighted in green.

3 Delete sample:

The message Do you really want to delete the selected line?


appears.

4 Confirm deleting: [Delete]


The deleted line is no longer available in the sample table.

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Sample data ■■■■■■■■■■■■■■■■■■■■■■

Deleting the sample table

1
Go to the Sample data work area:

2 Delete sample table:

The message The whole sample table will be deleted. Do you


want to continue anyway? appears.

3 Confirm deleting: [Yes]


The whole sample table is now deleted.

Resetting the sample table

1
Go to the Sample data work area:

2 Reset sample table:

The sample table is reset. All samples can be processed again.

74 ■■■■■■■■
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7.7 System – Configuration


The system configuration of the Eco Titrator defines the basic, method-
independent configuration of the instrument.
The following submenus can be found under the [System] button on the
Start page:

Figure 31 System menu page 1

Figure 32 System menu page 2


■ Settings – Basic instrument settings.
■ Sensors – Manage the sensor list and define the sensor data.
■ Solutions
■ Common variables
■ External devices (peripherals)
■ Diagnosis
■ File management

■■■■■■■■ 75
System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

■ Ethernet settings
■ Service
■ About
■ Change password
■ COM port settings

7.7.1 System – Settings


System ▶ Settings

Figure 33 System – Settings page 1

Figure 34 System – Settings page 2

User name
A user name can be entered here for the report. This parameter will only
be printed if a user has been defined.
Input: max. 12 characters
Default value: empty

76 ■■■■■■■■
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Instrument name
An instrument name can be entered here for the report. This parameter
will only be printed if a designation has been defined.
Input: max. 10 characters
Default value: empty

Language
Set the dialog language.

Dialog type
The user dialog can be limited for routine operations. The resetting of the
dialog will take effect as soon as you exit the start page.
■ Dialog type Expert (default value)
In the dialog type Expert, all the user settings are available.
■ Dialog type Routine
In the dialog type Routine, the availability of the settings is restricted.
The [System] and [Methods] menus as well as the Parameters work
area can only be opened with a password. Methods can be loaded,
however, on the start page.

NOTICE

The Routine setting will only take effect once the [System] menu
has been exited.
To switch back to expert mode, open the [System] menu and enter
the password:
■ Password for firmware version 57.1008.0010 or higher:
METROHM9100
■ Password for firmware version 57.1008.0009 or lower: MSH9101
Then activate the Expert dialog type.

Selection:
■ Expert
■ Routine
Default value: Expert

Time
Current time. Only numbers that make sense can be entered.
Format: hh:mm:ss

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System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

Date
Current date. Only numbers that make sense can be entered.
Format: YYYY:MM:DD

PREP warning
If the PREP warning is activated, the recommendation to execute the
Prepare buret (PREP) function appears:
■ After the instrument is switched on.
■ Each time a buret unit is attached.
All tubing and the cylinder are rinsed with this function.

Switch:
■ OFF
■ ON
Default value: ON

Beep
If Beep is activated, a short acoustic signal sounds in the following cases:
■ When a key is pressed.
■ At the end of the determination.
■ When the system remains conditioned without interruption for 10 sec-
onds.

Switch:
■ OFF
■ ON
Default value: ON

Cylinder volume (mL)


Cylinder volume of the buret unit in mL.
Selection:
■ 5
■ 10
■ 20
■ 50
Default value: 20

Temperature sensor
The instrument supports the use of two different temperature measure-
ment techniques:

78 ■■■■■■■■
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■ NTC (Negative Temperature Coefficient)


■ Pt1000 (platinum resistance)
Select the type here that has been connected to the instrument. If you use
an NTC sensor, it is required that two characteristics for the sensor are
entered in addition. These characteristics are listed in the specifications of
the sensor.
Selection:
■ NTC
■ Pt1000
Default value: Pt1000

R (25 °C)
This parameter is visible only when Temperature sensor = NTC.
Nominal resistance of the NTC sensor at 25 °C.
Input range 1,000 to 99,999 Ω
Default value 30,000 Ω

B value
This parameter is visible only when Temperature sensor = NTC.
Material constant of the NTC sensor. B values of NTC sensors are fre-
quently based on different reference temperatures (usually 25 °C and 50–
100 °C).
Input range 1,000 to 9,999 K
Default value 4,100 K

7.7.2 Managing sensors


System ▶ Sensors

■■■■■■■■ 79
System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

Figure 35 Sensor list (example)


3 standard sensors are defined in the sensor list: pH electrode, Metal
electrode and Temperature sensor. These sensors cannot be deleted
or renamed. The sensor list can contain a maximum of 10 sensors.
Every sensor is identified with a unique name. This means that it is not
possible to use the same name twice, e.g. for a pH electrode and for a
metal electrode.
Table 7 Managing the sensor list
Add a new sensor to the list. Sensor data see below.
The following sensor types can be selected:
■ pH electrode
■ Metal electrode
■ Temperature sensor
■ Other sensor, e.g. Spectrosense
Edit the data of the selected sensor. Sensor data see
below.
Delete the selected sensor from the list.

Sensor data

Name
The designation of the sensor is used for unambiguous identification.
Input: max. 24 characters
Default value: empty

Type
The sensor type is displayed.

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■■■■■■■■■■■■■■■■■■■■■■ Operation and control

Selection:
■ pH electrode
■ Metal electrode
■ Temperature sensor
■ Other sensor

Slope
This parameter is only visible with pH electrodes.
Slope of the pH electrode. With a 1-point calibration, only pH(0) can be
calculated, 100.0% is used as the slope.
Input range –999.9 to 999.9 %
Default value 100 %

pH(0)
This parameter is only visible with pH electrodes.
pH value of the pH electrode at 0 mV. Apart from the slope, pH(0) is the
second characteristic of the calibration curve.
Input range –20.000 to 20.000
Default value 7.000

Calibration temperature
This parameter is only visible with pH electrodes.
Temperature at which the last calibration was carried out.
Input range –20.0 to 150.0 °C
Default value 25.0 °C

Calibration date
This parameter is only visible with pH electrodes.
Date of the last calibration.

Monitoring
This parameter is only visible with pH electrodes.
Activate and deactivate the calibration monitoring.

Switch:
■ OFF
■ ON
Default value: OFF

Time interval
This parameter is visible only when Monitoring = ON.

■■■■■■■■ 81
System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

When you start a method, you will be notified if this time interval (in days)
has already elapsed. You can then select whether or not you would still
like to start the method.
Input range 1 to 999 d
Default value 999 d

7.7.3 Managing solutions


System ▶ Solutions

Figure 36 Solution list (example)


A maximum of 20 solutions can be saved.
Table 8 Managing the solution list
Add a new solution to the list. Solution data see below.

Edit the data of the selected solution. Solution data see


below.
Delete the selected solution from the list.

Solution data

The solution data for New ( ) and Edit ( ) are the same, therefore
only pictures for System ▶ Solutions ▶ New are shown:

82 ■■■■■■■■
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Figure 37 Solutions – Solution data page 1

Figure 38 Solutions – Solution data page 2

Name
The designation of the solution is used for unique identification.
Input: max. 24 characters
Default value: empty

Titer
Titer of the solution.
Input range –999,999,999 to 9999999999
Default value 1.000

Titer unit
Unit of the titer.

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System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ µmol/mL
■ mmol/L
■ mol/L
■ g/L
■ mg/L
■ mg/mL
■ µg/L
■ ppm
■ %
■ mEq/L
■ empty
■ User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. An empty entry can be generated this way as well.
Default value: empty

Concentration
Concentration of the solution.
Input range –999,999,999 to 9999999999
Default value 1.000

Concentration unit
Unit of the concentration.
Selection:
■ mol/L
■ %
■ g/L
■ mEq/L
■ mg/L
■ mg/mL
■ mmol/L
■ ppm
■ µg/L
■ µmol/mL
■ User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. An empty entry can be generated this way as well.
Default value: mol/L

84 ■■■■■■■■
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Cylinder volume (mL)


Cylinder volume of the buret unit in mL.
Selection:
■ 5
■ 10
■ 20
■ 50
Default value: 20

Date titer det.


Date of the last titer determination.

Monitoring
Activate and deactivate titer monitoring.

Switch:
■ OFF
■ ON
Default value: OFF

Time interval
This parameter is visible only when Monitoring = On.
When you start a method, you will be notified if this time interval (in days)
has already elapsed. You can then select whether or not you would still
like to start the method.
Input range 1 to 999 d
Default value 999 d

7.7.4 Managing common variables


System ▶ Common variables

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System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

Figure 39 Common variables


The instrument offers the possibility of saving 5 method-independent
variables, so-called common variables. These variables remain saved in
the instrument and can be used in future calculations. Common variables
are useful, e.g. for the following applications:
■ Determination of a blank value which will be taken into account during
the content determination of the sample.
■ Determination of the content of a standard solution, which will be
taken into account during the content determination of the sample.
The common variables have the designations CV01–CV05 that cannot be
changed. The value for every variable is displayed. No unit can be assigned
to the common variables.

Editing common variables


The common variables can be modified as follows:
■ Manually in this dialog.
■ Automatic assignment from the determination run. A calculation result
must be configured accordingly for this purpose (see below).

Assigning a result automatically to a common variable

1 Loading the method


■ Load the method that contains the result to be used in the
method selection bar on the Start page.

2 Opening the editing dialog of the result


■ Open the Parameters work area.
■ Click on the [Calculation] button.

86 ■■■■■■■■
■■■■■■■■■■■■■■■■■■■■■■ Operation and control

■ Select the result whose value is to be assigned to a common vari-


able.
■ Edit the highlighted result:

3 Adjusting the result properties

■ Activate the Save as CV button:

The assignment of the result to a common variable occurs automatically


according to the following scheme:
■ Result R1⇨ Common variable CV01
■ Result R2⇨ Common variable CV02
■ etc.

NOTICE

If the parameter Statistics is set to [ON], then the mean value of the
results will be assigned to the respective common variable.

7.7.5 Managing external devices


System ▶ External devices

PC/LIMS report
Specification of the storage location for the PC/LIMS report. The PC/LIMS
report is a machine-readable report with all of the important data for a
determination. It can be saved as follows:
■ as a TXT file on a USB flash drive.
■ to a LIMS via the Ethernet interface and an RS-232 instrument server.
Selection:
■ USB flash drive
■ Ethernet/RS-232
Default value: USB flash drive

USB flash The report will be saved as a TXT file on the USB flash
drive drive in the folder pc_lims_report.
Ethernet/ The report is sent via an RS-232 instrument server. The
RS-232 interface parameters are set on the RS-232 instrument
server (see Application Bulletin AB-435).

Printer
If a printer is connected, then the printer type needs to be defined here in
order for the reports to be printed out correctly.

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System – Configuration ■■■■■■■■■■■■■■■■■■■■■■

The printers that have the designation ESC-POS are so-called POS printers
(point-of-sale printers), i.e. they print on continuous paper.
Selection:
■ PDF (Save on USB flash drive)
■ Custom (ESC-POS)
■ PostScript
Default value: Custom (ESC-POS)
Commercially available A4 printers that communicate via PostScript can be
connected directly via USB.

Keyboard layout
Layout of the on-screen keyboard.
Selection:
■ English US

Balance
Selection:
■ Sartorius
For balances with RS-232 interface: Use the 6.2148.050 USB/RS-232 Con-
verter.
Configure the serial interface: System ▶ COM port settings
The parameters set for the RS-232 interface on the balance must match
those on the Eco Titrator.

7.7.6 System – File management


Start page ▶ System ▶ File management
This dialog offers the following functions:
■ Importing a method from a USB flash drive to the instrument.
■ Deleting the method on the USB flash drive.
■ Writing a system backup to a USB flash drive. The backup contains all
the data and settings of the instrument.
■ Restoring the system of the instrument with an existing backup.
We recommend to create a backup of the current system status before
restoring the system.

Folder structure on the USB flash drive


A folder with the instrument number will be created on the USB flash
drive. The structure within this folder appears as follows:

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Backup All of the files of the backup are stored in this


folder. The folder is created as soon as a
backup is created for the first time.
The file names of the backups are structured
as follows: SF_YYYY-MM-DD_hhmmss.ods
Files Exported methods are stored in this folder.
The folder is created as soon as a method is
exported for the first time.
Only methods located in this folder can be
imported.
pc_lims_report PC/LIMS reports are stored in this folder as
TXT files. The folder is created as soon as a
PC/LIMS report is printed for the first time.

Importing a method

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [System] button. Move to page 2


and click on [File management].
A list with the methods saved on the USB flash drive appears.

3 Select the method that you want to import by clicking on it.


The selected method is highlighted in green.

4 Import the highlighted method:

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The message Importing method from USB flash drive...


appears.
Once the message has disappeared, the method is saved to the
instrument.

NOTICE

If a method with the same name already exists on the instru-


ment, then the following warning appears: Store method:
Method name already exists. Do you want to overwrite
the name?.
■ [Yes]: The method on the instrument will be overwritten.
■ [No]: The method will not be imported.

Deleting the method on the USB flash drive

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [System] button. Move to page 2


and click on [File management].
A list with the methods saved on the USB flash drive appears.

3 Select the method that you want to delete by clicking on it.


The selected method is highlighted in green.

4 Delete the highlighted method:

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The message Method deleted successfully from USB flash


drive. confirms the deletion process.

Creating a backup

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [System] button. Move to page 2


and click on [File management].

3 Start the backup:


The message Backing up data and settings to USB flash
drive... appears.
Once the message has disappeared, the backup is saved to the USB
flash drive.

Restoring

Procedure

1 Connect the USB flash drive to the instrument.

2 On the Start page, click on the [System] button. Move to page 2


and click on [File management].

3 Restore the system:


A list with the backups saved on the USB flash drive appears.
The file names of the backups are structured as follows: SF_YYYY-
MM-DD_hhmmss.ods

4 Click on the desired backup.


The warning System restore appears.

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5 Confirm the system restore: [Yes]


The following message appears before the instrument is restarted:
System files are restored. Press [Next] to restart the instru-
ment.

6 Restart the instrument: [Continue]


The instrument restarts. The system is restored.

7.7.7 Instrument diagnosis


System ▶ Diagnosis

Figure 40 System menu – Diagnosis

Display test
The [Display test] button offers settings for brightness, various test
images and a calibration program for the screen:

Brightness Set the screen brightness: and buttons


Shows a number of test images to check image quality.

Starts the calibration program.


■ Look at the screen in such a way that your line of
sight is vertical to the screen.
■ A crosshair appears in succession at various places on
the screen. Each time, click in the center of the cross-
hair.
Once the calibration has been completed, the instrument
is restarted automatically.

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Keyboard test
■ Start the test: [Keyboard test]
■ Press the five keys of the control bar one after the other:

■ The instrument confirms each successful press of a key with a tick:

Logs
■ Show error log: [Logs]
■ Save error log to a USB flash drive:

7.7.8 Ethernet settings


System ▶ Ethernet settings
Example of usage: Reports can be sent to a LIMS directly via an RS-232/
Ethernet Box.

Mode
This network configuration can be done manually or automatically.
Selection:
■ Static
The network configuration is done manually. The input fields IP
address, Subnet mask and Gateway are used for this.
■ DHCP
The network configuration is assigned automatically via a server.
Default value: DHCP

7.7.9 Service – Brief description


The [Service] button leads to a protected area to which only Metrohm
Service has access.

7.7.10 Changing the password


With the password for the Expert dialog type you can control access to
the menus System and Methods as well as the Parameters work area.
Changing the password for the Expert dialog type:

1 On the Start page, open the System ▶ Change password menu.

2 Enter the current password and then the new password twice.

3 Perform the change:

The password is changed.

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NOTICE

Make a note of the password and store it in a safe place.


If you lose the password, the system must be reset to factory settings
with a system initialization. The default password is:
■ Password for firmware version 57.1008.0010 or higher:
METROHM9100
■ Password for firmware version 57.1008.0009 or lower: MSH9101
The system can then be restored with a backup.

7.7.11 COM port settings


System ▶ COM port settings
When using a balance with serial interface, adjust the corresponding set-
tings. The parameters set for the RS-232 interface on the balance must
match those on the instrument.

NOTICE

Use the 6.2148.050 USB/RS-232 Converter. This converter provides


the serial connector.

Baud rate
Transfer rate in characters per second.
Selection:
■ 1,200
■ 2,400
■ 4,800
■ 9,600
■ 19,200
■ 38,400
■ 57,600
■ 115,200
Default value: 9,600

Data bits
Number of data bits.

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Selection:
■ 7
■ 8
Default value: 8

Stop bits
Number of stop bits.
Selection:
■ 1
■ 2
Default value: 1

Parity
Type of parity testing.
Selection:
■ Even
■ None
■ Odd
Default value: None

Handshake
Type of the data transfer protocol.
Selection:
■ Hardware
■ Software
■ none
Default value: Hardware

NOTICE

If communication problems occur, set the parameter Handshake to


Software, and make another attempt.

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7.8 Carrying out a pH calibration


Procedure

1 Loading the method


Load a calibration method (CAL).

2 Setting the parameters


■ Open Parameters ▶ Calibration parameters. Select the pH
electrode used in the [Sensor] input field.
■ Open Parameters ▶ Buffers. Enter the type and number of buf-
fers that need to be used. The pH values of the buffers to be used
must be entered manually for the Special buffer type.
We recommend to measure at least 3 buffers (3-point calibration).

3 Measuring buffer 1
■ Immerse the pH electrode in the buffer 1.
■ Press the key.
■ Enter the current temperature. If a temperature sensor is connec-
ted, then the temperature will be measured automatically.
The measurement is started. The on-screen display changes to the
Live status work area:

Figure 41 Live status – Calibration mode CAL

Pauses the measurement.

Continues the measurement.


This button appears as soon as the measurement is paused.

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After the measurement has been completed successfully, the warning


message New buffer appears.

4 Measuring further buffers


Follow these steps for the remaining buffers:
■ Rinse the electrode.
■ Change to the next buffer.
■ Immerse the pH electrode in the new buffer.
■ Click on the OK button.
■ Once the warning message New buffer appears, repeat step 4.

5 Calibration completed successfully


Once the last buffer has been measured, the new calibration data is
saved for the corresponding pH electrode.
You can view the calibration data if needed:
■ System ▶ Sensors ▶
■ Select the calibrated pH electrode.
■ Click on .

7.9 Carrying out the determination

1 Loading the method


Load the method

2 Preparing the sample

NOTICE

Calculate the amount of the sample so that it results in titrant


consumption of 10 to 90% of the cylinder volume.

■ Weigh in or measure the sample in a sample vessel.


■ Add solvent if necessary.
■ Add the stirring bar to the sample vessel.
■ Place the sample vessel on the stirrer.
■ Immerse the electrode and buret tip in the solution.

3 Entering the sample size


Enter the sample size.

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4 Starting the titration

Press the key.


The titration is started. The on-screen display changes to the Live
status work area:

Figure 42 Live status – Titration modes DET, MET, SET


The axes are scaled automatically.

Pauses the determination.

Continues the determination.


This button appears as soon as the determination is paused.

5 Live modifications
Make live modifications if necessary:
■ Editing the sample data of the running determination
■ Editing the method parameters of the running determination
■ Modifying the stirring rate

6 Cancelling the determination manually (if necessary)

A determination can be canceled at any time with the key.


The determination data is saved up to the point of cancellation.

7 Determination completed successfully


The on-screen display changes to the Results work area.

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Editing the sample data of the running determination

The sample data can be entered or modified in the Samples work area
while a determination is running. The sample data entered at the end of
the titration in the Samples work area is always used in calculations.

1 Opening the Samples work area

Click on .
The Samples work area appears. The determination continues to
run in the background.

2 Editing sample data


Edit the sample data.

3 Open the Live status work area

Click on .
The Live status work area appears again.

NOTICE

If the determination is finished while an editing dialog is opened (e.g.


of the sample size), then this will be closed automatically and the
results dialog will be displayed. The value entered must be entered
once more and the determination must be recalculated.
Make sure that the editing dialogs are closed before the determina-
tion is finished.

Editing the method parameters of the running determina-


tion

Certain method parameters can be edited while a determination is being


carried out. Only parameters that are not grayed out can be edited. The
modified parameters are taken into account at once. However, if you
modify, for instance, the start conditions after the start volume has been

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Results ■■■■■■■■■■■■■■■■■■■■■■

dosed, then these modifications will not be taken into account until the
next determination.

1 Open the Parameters work area

Click on .
The Parameters work area appears. The determination continues to
run in the background.

2 Editing the method parameters


Edit the method parameters.

3 Open the Live status work area

Click on .
The Live status work area appears again.

Modifying the stirring rate

1 The stirring rate of the magnetic stirrer can be changed with the con-
trol bar while a determination is carried out.

■ Increase the stirring rate in steps:


■ Reduce the stirring rate in steps:

7.10 Results

shows the Results work area.


After a titration has been completed, the Results work area opens auto-
matically.

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Figure 43 Results overview


The results overview shows the calculated results and the stop criterion:
■ Click on the desired result row or stop criterion row.

Curve

By clicking on the key, the curve of the current determination is dis-


played.

Recalculating

By clicking on the key, the current determination is recalculated. The


procedure will be executed immediately.

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Results ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

Recalculation cannot be undone.

All the results of the determination that was carried out last are recalcula-
ted with the Recalc function. This is necessary if, for example, the calcula-
tion, the titer or the sample size has been modified.

Statistics
By clicking on the key, the statistical overview of a determination ser-
ies is displayed.

NOTICE

This function is only visible, if the Statistics parameter is set to [ON].

The mean value Mean, the absolute standard deviation s abs and the rel-
ative standard deviation s rel are displayed in the overview. For the mean
value, the number of individual results from which it has been calculated is
displayed in parentheses. In this example, it is 3.
The Statistics row shows how many determinations have already been car-
ried out and how many determinations are to be carried out in total. 3 out
of 4 determinations were carried out in this example.

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Details
Shows further data of the determination series.
The result and the sample size of each determination are shown.
A determination can be removed from the Statistics in the col-
umn On/Off. That row is then marked with . All the results
from the highlighted determination are removed from the statis-
tics. The statistics are automatically recalculated.
Reset
Deletes all statistics data.
The statistics data is deleted automatically in the following
cases:
■ Once all the determinations of the determination series have
been carried out and a new determination is started.
■ Once a new method is being loaded.
Increase
Adds an additional sample to a determination series, e.g.
because a determination was faulty and had to be removed
from the statistics. The second number in the Statistics line will
be increased automatically by one.

7.11 Printing reports


The following reports can be printed out:
■ Result
Result report with determination properties, sample data, calculated
results, etc.
■ Curve
Curve report.
■ Measuring point list
Measuring point list report.
■ Parameters
Report with all method parameters of the loaded method.
■ System
System report with system settings, solution list, external devices, etc.
■ Calculations/statistics
Calculation report. The statistics are also printed out in the case of mul-
tiple determinations. The individual determinations with the respective
sample size, the mean value, the absolute and the relative standard
deviation are printed out for each result.

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Printing reports ■■■■■■■■■■■■■■■■■■■■■■

■ Report as in method
The reports that are defined in the method will be printed out.
■ PC/LIMS
Machine-readable report with all of the data for a determination. This
report can be saved as a TXT file to a connected USB flash drive.

Preparing to print

1 On the System ▶ External devices start page, click on the Printer


button.
A list of output options opens:
■ PDF
■ Custom (ESC-POS)

2 Select the desired output.


If the command Print reports is executed, then the reports will be
printed out on the Custom printer or saved in PDF form on the con-
nected USB flash drive.

Printing reports manually

1 On the start page, click on the Print reports button.


A list with the following options opens:
■ Result
■ Curve
■ Measuring point list
■ Parameters
■ System
■ Calculation/statistics
■ Report as in method
■ PC/LIMS

2 Select the desired report.


The report data is recorded and output.

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7.12 Parameters
Titrations
Dynamic equivalence Dynamic equivalence point titration is a titration mode for all standard
point titration (DET) titrations. The reagent is added in variable volume steps. The volume steps
vary as a function of the slope of the curve. An attempt is made to reach
constant measured value changes with each dosing. The optimal volume
for dosing is determined from the measured value changes of the previous
dosings. Measured value acceptance is drift-controlled (equilibrium titra-
tion) or after a waiting time. Equivalence points are evaluated automati-
cally.
U/mV

V/mL
Figure 44 Reagent dosing for DET

Monotonic equiva- Monotonic equivalence point titration is a titration mode for titrations
lence point titration with relatively high signal fluctuations or suddenly occurring potential
(MET) jumps and for slow titrations or slow-response electrodes. The reagent is
added in constant volume steps. Measured value acceptance is drift-con-
trolled (equilibrium titration) or after a waiting time. Equivalence points are
evaluated automatically.
U/mV

V/mL
Figure 45 Reagent dosing for MET

Endpoint titration Endpoint titration is a titration mode for rapid routine determinations to a
(SET) preset endpoint (e.g. titrations in accordance with special standards) and
titrations for which reagent overflow must be avoided. The titration termi-
nation at the endpoint takes place either drift-controlled or after a waiting

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

time. The volume dosed until the endpoint is used for calculating the con-
tent of the sample.
U/mV
Endpoint

Control range

V/mL
t/s

Initial Continuous V/mL


dosing dosing

Figure 46 Reagent dosing for SET

7.12.1 Dynamic equivalence point titration (DET)

Figure 47 DET parameters – Menu page 1

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Figure 48 DET parameters – Menu page 2

7.12.1.1 Start conditions


Parameters ▶ Start conditions
The parameters that are carried out before the start of titration are
defined under [Start conditions].

Request sample ID
Selection of the sample identification that is queried at the start of the
determination.
Selection:
■ ID1
■ ID2
■ ID1&ID2
■ Off
Default value: Off

Start delay time


Waiting time after the start of the determination, before the titration is
started.
During this period, substances such as auxiliary solution can be added
with a Dosimat (parameterization on the Dosimat, the Activation pulse
switch must be switched on for this).
Input range 0 to 999,999 s
Default value 0s

Start volume
Volume that is dosed prior to the start of the titration.

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Input range 0.00000 to 9,999.99 mL


Default value 0.00000 mL

Dosing rate
Rate at which the start volume is dosed.
Input range 0.02 to Max. mL/min
Additional selection: Max. = maximum dosing rate.
Default value: Max.

NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 9 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

Pause
Waiting time, e.g. for the stabilization of the measured value after the
start, for dissolving solid substances or a reaction time after the dosing of
a start volume.
Input range 0 to 999,999 s
Default value 0s

Activation pulse
If it is activated, an activation pulse is sent to a remote line that starts a
connected Dosimat. We recommend to define a Start delay time for
this.

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Switch:
■ OFF
■ ON
Default value: OFF

Request sample size


If this parameter is activated, then the value for the sample size will be
requested at the start of the determination.

Switch:
■ OFF
■ ON
Default value: OFF

Request sample unit


If this parameter is activated, then the unit for the sample size will be
requested at the start of the determination.

Switch:
■ OFF
■ ON
Default value: OFF

Hold at request
If this parameter is activated, then the run will be paused during the
request. If the parameter is switched off, the titration will be started in the
background.

Switch:
■ OFF
■ ON
Default value: ON

7.12.1.2 Titration parameters


Parameters ▶ Titration parameters
The parameters that are carried out at the start of titration are defined
under [Titration parameters].

Stirrer
If this parameter is activated, then the stirrer is switched on at the start of
the determination.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Switch:
■ OFF
■ ON
Default value: ON

Stirring rate
Setting the stirring rate. The stirring direction is always clockwise.
Conversion: Value x 120 ± 5 rpm = stirring rate in rpm
e.g.: 8 × 120 ± 5 rpm = 960 ± 40 rpm
Input range 1 to 15
Default value 8

Temperature
Manually entered titration temperature. If a temperature sensor is connec-
ted, then the temperature will be measured continuously. For determina-
tions in pH mode, the value is used for temperature compensation (elec-
trode slope is adjusted accordingly).
Input range –20.0 to 150.0 °C
Default value 25.0 °C

Sensor
Open the selection list and select a sensor.
The selection depends on the measuring mode. Sensors are defined and
listed under System ▶ Sensors, e.g.:

Solution
Open the selection list and select a solution.
Solutions are defined and listed under System ▶ Solutions, e.g.:

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We, at Metrohm, always recommend selecting the solution.


This ensures that accurate data (titer, concentration, etc.) is always used
for the calculation and that the volume of the selected solution is com-
pared to the volume defined under System ▶ Settings.

Titration rate
3 predefined sets of parameters and 1 set of parameters that can be
defined manually are available for setting the titration rate.
Selection:
■ Slow: For titrations in which the finest details are to be visible. This
can, however, also lead to an increase in noise, which may result in
unwanted equivalence points.
■ Optimal: For all standard titrations. The parameters have been opti-
mized for the most frequent applications.
■ Fast: For fast and less critical titrations.
■ User: The individual titration parameters can be modified.
Default value: Optimal

Table 10 Default values of the predefined sets of parameters for DET


Slow Optimal Fast
Meas. point 2 4 6
density
Min. incre- 10.00 µL 10.00 µL 30.00 µL
ment
Max. incre- Off Off Off
ment
Dosing rate Max. Max. Max.
Signal drift 20.0 mV/min 50.0 mV/min 80.0 mV/min
Min. waiting 0s 0s 0s
time
Max. waiting 38 s 26 s 21 s
time

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NOTICE

Select Optimal as titration rate if you are developing a new titration


method. This parameter is suitable for virtually all titrations and only
needs adaptation in special cases.

Meas. point density


This parameter is only active if the titration rate is set to User.
A lower value means there are more measuring points per unit:
■ Low value: High measuring point density
All the finest details are shown in the curve. This may cause noise and
unwanted equivalence points.
■ High value: Low measuring point density
Allows for faster titrations. It is an advantage if you work with low cyl-
inder volumes (you should also set a smaller signal drift and a higher EP
criterion at the same time).
Input range 0 to 9
Default value 4

Min. Increment
This parameter is only active if the titration rate is set to User.
This smallest permitted volume increment is added at the start of the titra-
tion and with steep curves in the region of the equivalence point. Very
small values should only be used if a low titrant consumption is expected.
Otherwise unwanted equivalence points may be evaluated.
Input range 0.05 to 999.90 µL
Default value 10.0 µL

Max. Increment
This parameter is only active if the titration rate is set to User.
A maximum volume increment should be selected in the following cases:
■ If titrant consumption is very low until the equivalence point is reached.
■ If a start volume is dosed until shortly before the equivalence point is
reached.
■ If the change of direction in the jumping range is very abrupt, because
otherwise it is easily possible for an excessively large volume to be
dosed in the region of the equivalence point.
The value should not be set to less than 1/100 of the cylinder volume.

112 ■■■■■■■■
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Input range 0.1 to 9,999.9 µL


Additional selection: Off
Default value: Off

NOTICE

It is not advisable to select similar volumes for the minimum and the
maximum increment. Monotonic equivalence point titration (MET) is
appropriate for these applications.

Min. waiting time


This parameter is only active if the titration rate is set to User.
The measured value is not accepted until the minimum waiting time has
elapsed, even if the signal drift has already been reached. The minimum
waiting time is only important for drift-controlled measurements.
Input range 0 to 999,999 s
Default value 0s

Max. Waiting time


This parameter is only active if the titration rate is set to User.
If the signal drift has been switched off or has not yet been reached, then
the measured value will be accepted once the maximum waiting time has
elapsed.
Input range 0 to 999,999 s
Default value 26 s

Signal drift
This parameter is only active if the titration rate is set to User.
Maximum permissible drift for the measured value acceptance, i.e. maxi-
mum change of the measured value per minute. This type of titration is
often referred to as equilibrium titration.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

A constant measured value is often only reached after a certain time,


as mixing and the reaction itself require a certain time. The response
time of an electrode can also increase with time, i.e., reaching a con-
stant measured value takes longer and longer. Drift-controlled meas-
ured value acceptance is particularly advisable in such cases, as the
measured values are only accepted when equilibrium has almost been
reached.

Input range 0.1 to 999.0 mV/min


Default value 50.0 mV/min
Additional selection: Off: Measured value acceptance will take place after
the maximum waiting time has elapsed. This can be useful when the titra-
tion reaction proceeds slowly or the electrode is slow to respond.

Dosing rate
This parameter is only active if the titration rate is set to User.
Rate at which the volume increments are dosed.
Input range 0.01 to Max. mL/min
Additional selection: Max. = maximum dosing rate.
Default value: Max.

NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 11 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min

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Cylinder volume maximum dosing rate / filling


rate
50 mL 150.00 mL/min

Ipol
This parameter is only active with Ipol determinations.
The polarization current is the current that is applied to a polarizable elec-
trode during voltametric measurement.
Selection:
■ 1 µA
■ 20 µA
■ 50 µA
■ 100 µA
Default value: 1 µA

Electrode test
This parameter is only active with Ipol determinations.
In the case of polarizable electrodes, an electrode test can be carried out.
A check is made that the electrode is properly connected and that no
short-circuit is present. The electrode test is carried out when the determi-
nation is started.

Switch:
■ OFF
■ ON
Default value: OFF

7.12.1.3 Stop conditions


Parameters ▶ Stop conditions
The conditions for canceling the titration are defined under [Stop condi-
tions].

Stop volume
The titration is canceled when the specified volume has been dosed since
the start of the titration.
Adjust this volume to the size of the titration vessel in order to prevent the
contents from overflowing.
Input range 0.00000 to 9,999.99 mL
Default value 100.000 mL
Additional selection: Off

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Stop measured value (measured quantity pH)


The titration is canceled when the specified measured value has been
reached since the start of the titration.
Input range –20.000 to 20.000
Default value Off
Additional selection: Off

Stop measured value (measured quantities U and Ipol)


The titration is canceled when the specified measured value has been
reached since the start of the titration.
Input range –2,000.0 to 2,000.0 mV
Additional selection: Off
Default value: Off

Stop EP
The titration is canceled when the specified number of equivalence points
has been found.
Input range 1 to 9
Default value 9
Additional selection: Off

Volume after EP
The entered volume will be dosed when the number of equivalence points
defined under Stop EP has been found. The curve shape after the equiva-
lence point can also be seen this way.
Input range 0.01000 to 9,999.99 mL
Additional selection: Off
Default value: Off

Stop time
The titration is canceled when the specified time has elapsed since the
start of the titration.
Input range 0 to 999,999 s
Additional selection: Off
Default value: Off

Filling rate
Rate at which the dosing cylinder is filled after the titration.

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Input range 0.01 to Max. mL/min


Additional selection: Max. = maximum filling rate.
Default value: Max.

NOTICE

The maximum filling rate depends on the cylinder volume (see table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the filling rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 12 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

7.12.1.4 Evaluation
Parameters ▶ Evaluation
The parameters for the evaluation of the titration curve are defined under
[Evaluation].

Window
If ON is selected, a measured value range (window) can be defined. Only
equivalence points that are within this window are recognized.
Only one window can be defined.

Switch:
■ OFF
■ ON
Default value: OFF

EP recognition (Window = OFF)


Filters for the sought equivalence points:

■■■■■■■■ 117
Parameters ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ All: All equivalence points will be recognized.
■ Greatest: Only the equivalence point with the greatest ERC value, i.e.
the steepest jump, will be recognized.
■ Last: Only the last equivalence point will be recognized.
■ Off: No evaluation takes place.
Default value: All

EP recognition (Window = ON)


Filters for the sought equivalence points:
Selection:
■ First: Only the first equivalence point will be recognized.
■ Greatest: Only the equivalence point with the greatest ERC value, i.e.
the steepest jump, will be recognized.
■ Last: Only the last equivalence point will be recognized.
Default value: First

Fixed EP1 (measured quantity pH)


The associated volume will be interpolated from the measuring point list
for the measured value entered. The fixed point must lie between the first
and the final entry in the measuring point list.
Input range –20 to 20
Additional selection: Off
Default value: Off

Fixed P1 (measured quantities U and Ipol)


The associated volume will be interpolated from the measuring point list
for the measured value entered. The fixed point must lie between the first
and the final entry in the measuring point list.
Input range –2,000.0 to 2,000.0 mV
Additional selection: Off
Default value: Off

Fixed EP2 (measured quantity pH)


see fixed EP1

Fixed P2 (measured quantities U and Ipol)


see fixed EP1

Lower limit (measured quantity pH)


This parameter is only active if Window = ON.

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Measured value for the lower limit.


Input range –20.000 to 20.000
Default value –20.000

Upper limit (measured quantity pH)


This parameter is only active if Window = ON.
Measured value for the upper limit.
Input range –20.000 to 20.0000
Default value 20.000

Lower limit (measured quantities U and Ipol)


This parameter is only active if Window = ON.
Measured value for the lower limit.
Input range –2,000.0 to 2,000.0 mV
Default value –2,000.0 mV

Upper limit (measured quantities U and Ipol)


This parameter is only active if Window = ON.
Measured value for the upper limit.
Input range –2,000.0 to 2,000.0 mV
Default value 2,000.0 mV

EP criterion
The equivalence point criterion found (ERC = Equivalence point Recogni-
tion Criterion) is compared with this value. Equivalence points whose ERC
is less than the value defined here will be ignored.
Input range 0 to 200
Default value 5

Evaluation and equivalence point criterion with DET


The equivalence points (EP) are localized in a way similar to the Tubbs
method [1][2]. The volume value of the equivalence point (VE) is shifted
from the inflection point (see arrow) towards the smaller circle of curva-
ture for real asymmetric titration curves.
[1] C. F. Tubbs, Anal. Chem.1954, 26, 1670–1671.
[2] E. Bartholomé, E. Biekert, H. Hellmann, H. Ley, M. Weigert, E. Weise,
Ullmanns Encyklopädie der technischen Chemie, Vol. 5, Verlag Chemie,
Weinheim, 1980, p. 659.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

pH

VE V/mL
Figure 49 Tubbs method for determining the equivalence point
The figure shows that the evaluation still requires measured values from
the measuring point list even after the equivalence point.
For the recognition of the EPs found, the set EP criterion is compared to
the ERC (Equivalence point Recognition Criterion) found. The ERC is the
first derivative of the titration curve combined with a mathematical func-
tion that is more sensitive for flat jumps than for steeper ones. EPs whose
ERC is smaller than the defined EP criterion will not be recognized.
The ERC is displayed under Results for each discovered and recognized
EP.
If you adjust the EP criterion retroactively in order to recognize more or
fewer EPs, then you can initiate the reevaluation under Results.

7.12.1.5 Calculation
Parameters ▶ Calculation
A maximum of five calculations can be defined in one method. A series of
variables (raw data from the determination, previously calculated results) is
available for the calculations.
For each calculation, you can define whether the result is to be saved as a
titer or as a common variable.
The five possible calculations are shown in a list:

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Figure 50 Parameters calculation – Result list


The result name is specified in the list for each calculation.
Scroll down for result R5.

Editing a calculation

1 Select a calculation in the result list.

2 Click on .

■■■■■■■■ 121
Parameters ■■■■■■■■■■■■■■■■■■■■■■

3 Make the desired changes.

Result name
The result name is the text that will be shown in the result view and in the
report.
Input: max. 12 characters
Default value: empty

Decimal places
Number of decimal places used to display the result.
Input range 0 to 5
Default value 2

Save as CV
The calculated result can be saved as a method-independent variable,
called a common variable. The result is then also available in other meth-
ods for calculations. If statistics has been switched on, then the current
mean value of the determination series will be saved.

Switch:
■ OFF
■ ON
Default value: OFF

Save as titer
The result can be saved as titer for the selected solution (the solution must
be selected). If statistics has been switched on, then the current mean
value of the determination series will be saved.

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Switch:
■ OFF
■ ON
Default value: OFF

R1=… – R5=…
Shows the calculation formula. The formula editor is opened for the defi-
nition.

Result unit
The result unit is displayed and saved along with the result.
Selection:
■ %
■ mol/L
■ mmol/L
■ g/L
■ mg/L
■ mg/mL
■ ppm
■ g
■ mg
■ mL
■ mg/piece
■ °C
■ µL
■ mL/min
■ User-defined
Default value: %

7.12.1.6 Statistics
Parameters ▶ Statistics
The statistics calculation of a multiple determination is activated under
[Statistics] and definition is made as to how many determinations the
series contains.

Statistics
If it is set to ON, statistics calculations will be carried out for all of the
defined results.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Switch:
■ OFF
■ ON
Default value: OFF

Number of samples
The number of determinations that are carried out for the statistics calcu-
lations.
Input range 2 to 20
Default value 3

7.12.1.7 Reports
Parameters ▶ Reports
The reports that will be printed out automatically or saved as a PDF report
after a determination are defined under [Reports].

Results
The result report contains the calculated results, equivalence points, end-
points, sample data, etc.

Switch:
■ OFF
■ ON
Default value: OFF

Curve
The report is shown as a curve.

Switch:
■ OFF
■ ON
Default value: OFF

Calculation/statistics
Output of the calculation formulas for the individual results. Results are
specified with full accuracy. This makes checking with an external program
possible.
If the switch under Parameters ▶ Statistics is set to ON, the following
data will be printed out as well:
■ Result and sample size of the individual determinations
■ Mean value as well as absolute and relative standard deviation

124 ■■■■■■■■
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Switch:
■ OFF
■ ON
Default value: OFF

Measuring point list


Output of the measuring point list.

Switch:
■ OFF
■ ON
Default value: OFF

Parameters
All of the parameters of the current method are shown in the parameter
report.

Switch:
■ OFF
■ ON
Default value: OFF

NOTICE

The printer for the report data above is defined under Start
page ▶ System ▶ External devices ▶ Printer.
■ If a connected printer is selected, then the report contains the
data defined by the switches above.
■ If [PDF] is selected as printer and at least one switch is set to ON,
then the report contains the complete data except for the measur-
ing point list. The measuring points are only printed if the switch
measuring point list is set to ON.

PC/LIMS
The PC/LIMS report is a machine-readable report with all of the important
data for a determination. This report can be saved as a TXT file on a USB
flash drive or sent to a LIMS via an RS-232 interface. The output location is
defined under Start page ▶ System ▶ External devices ▶ PC/LIMS
report.
The file name of the TXT file has the following structure:

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

PC_LIMS_Report_ID1_YYYYMMDD-hhmmss.txt

Switch:
■ OFF
■ ON
Default value: OFF

7.12.2 Monotonic equivalence point titrations (MET)

Figure 51 MET parameters – Menu page 1

Figure 52 MET parameters – Menu page 2

7.12.2.1 Start conditions


Parameters ▶ Start conditions
The parameters that are carried out before the start of titration are
defined under [Start conditions].

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Request sample ID
Selection of the sample identification that is queried at the start of the
determination.
Selection:
■ ID1
■ ID2
■ ID1&ID2
■ Off
Default value: Off

Start delay time


Waiting time after the start of the determination, before titration takes
place.
During this period, substances such as auxiliary solution can be added
with a Dosimat (parameterization on the Dosimat, the Activation pulse
switch must be switched on for this).
Input range 0 to 999,999 s
Default value 0s

Start volume
Volume that is dosed prior to the start of the titration.
Input range 0.00000 to 9,999.99 mL
Default value 0.00000 mL

Dosing rate
Rate at which the start volume is dosed.
Input range 0.02 to Max. mL/min
Additional selection: Max. = maximum dosing rate.
Default value: Max.

NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 13 Maximum dosing rate / filling rate

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Cylinder volume maximum dosing rate / filling


rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

Pause
Waiting time, e.g. for the stabilization of the measured value after the
start, for dissolving solid substances or a reaction time after the dosing of
a start volume.
Input range 0 to 999,999 s
Default value 0s

Activation pulse
If it is activated, an activation pulse is sent to a remote line that starts a
connected Dosimat. We recommend to define a Start delay time for
this.

Switch:
■ OFF
■ ON
Default value: OFF

Request sample size


If this parameter is activated, then the value for the sample size will be
requested at the start of the determination.

Switch:
■ OFF
■ ON
Default value: OFF

Request sample unit


If this parameter is activated, then the unit for the sample size will be
requested at the start of the determination.

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Switch:
■ OFF
■ ON
Default value: OFF

Hold at request
If this parameter is activated, then the run will be paused during the
request. If the parameter is switched off, the titration will be started in the
background.

Switch:
■ OFF
■ ON
Default value: ON

7.12.2.2 Titration parameters


Parameters ▶ Titration parameters
The parameters that are carried out at the start of titration are defined
under [Titration parameters].

Titration rate
3 predefined sets of parameters and 1 set of parameters that can be
defined manually are available for setting the titration rate.
Selection:
■ Slow: For titrations in which the finest details are to be visible. This
can, however, also lead to an increase in noise, which may result in
unwanted equivalence points.
■ Optimal: For all standard titrations. The parameters have been opti-
mized for the most frequent applications.
■ Fast: For fast and less critical titrations.
■ User: The individual titration parameters can be modified.
Default value: Optimal

Table 14 Default values of the predefined sets of parameters for MET


Slow Optimal Fast
Volume incre- 2 4 6
ment
Dosing rate Max. Max. Max.
Signal drift 20.0 mV/min 50.0 mV/min 80.0 mV/min

■■■■■■■■ 129
Parameters ■■■■■■■■■■■■■■■■■■■■■■

Min. waiting 0s 0s 0s
time
Max. waiting 38 s 26 s 21 s
time

NOTICE

Select Optimal as titration rate if you are developing a new titration


method. This parameter is suitable for virtually all titrations and only
needs adaptation in special cases.

Volume increment
This parameter is only active if the titration rate is set to User.
Volume dosed at each dosing step.
High accuracy requires using the correct volume increment. A good guide-
line is 1/20 of the expected endpoint volume. The volume increment
should be closer to 1/100 of the endpoint volume for steep jumps and
closer to 1/10 for flat jumps.
Small volume increments are used for determining blank values or with
very asymmetrical curves. The accuracy of the evaluation cannot be
increased by using smaller increments as the measured value changes
between two measuring points are then of the same order of magnitude
as the noise.
Input range 0.00005 to 999.900 mL
Default value 0.10000 mL

Dosing rate
This parameter is only active if the titration rate is set to User.
Rate at which the volume increments are dosed.
Input range 0.01 to Max. mL/min
Additional selection: Max. = maximum dosing rate.
Default value: Max.

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NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 15 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

Signal drift
This parameter is only active if the titration rate is set to User.
Maximum permissible drift for the measured value acceptance, i.e. maxi-
mum change of the measured value per minute. This type of titration is
often referred to as equilibrium titration.

NOTICE

A constant measured value is often only reached after a certain time,


as mixing and the reaction itself require a certain time. The response
time of an electrode can also increase with time, i.e., reaching a con-
stant measured value takes longer and longer. Drift-controlled meas-
ured value acceptance is particularly advisable in such cases, as the
measured values are only accepted when equilibrium has almost been
reached.

Input range 0.1 to 999.0 mV/min


Default value 50.0 mV/min
Additional selection: Off: Measured value acceptance will take place after
the maximum waiting time has elapsed. This can be useful when the titra-
tion reaction proceeds slowly or the electrode is slow to respond.

■■■■■■■■ 131
Parameters ■■■■■■■■■■■■■■■■■■■■■■

Min. waiting time


This parameter is only active if the titration rate is set to User.
The measured value is not accepted until the minimum waiting time has
elapsed, even if the signal drift has already been reached. The minimum
waiting time is only important for drift-controlled measurements.
Input range 0 to 999,999 s
Default value 0s

Max. Waiting time


This parameter is only active if the titration rate is set to User.
If the signal drift has been switched off or has not yet been reached, then
the measured value will be accepted once the maximum waiting time has
elapsed.
Input range 0 to 999,999 s
Default value 26 s

Stirrer
If this parameter is activated, then the stirrer is switched on at the start of
the determination.

Switch:
■ OFF
■ ON
Default value: ON

Stirring rate
Setting the stirring rate. The stirring direction is always clockwise.
Conversion: Value x 120 ± 5 rpm = stirring rate in rpm
e.g.: 8 × 120 ± 5 rpm = 960 ± 40 rpm
Input range 1 to 15
Default value 8

Temperature
Manually entered titration temperature. If a temperature sensor is connec-
ted, then the temperature will be measured continuously. For determina-
tions in pH mode, the value is used for temperature compensation (elec-
trode slope is adjusted accordingly).
Input range –20.0 to 150.0 °C
Default value 25.0 °C

132 ■■■■■■■■
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Sensor
Open the selection list and select a sensor.
The selection depends on the measuring mode. Sensors are defined and
listed under System ▶ Sensors, e.g.:

Solution
Open the selection list and select a solution.
Solutions are defined and listed under System ▶ Solutions, e.g.:

We, at Metrohm, always recommend selecting the solution.


This ensures that accurate data (titer, concentration, etc.) is always used
for the calculation and that the volume of the selected solution is com-
pared to the volume defined under System ▶ Settings.

Ipol
This parameter is only active with Ipol determinations.
The polarization current is the current that is applied to a polarizable elec-
trode during voltametric measurement.
Selection:
■ 1 µA
■ 20 µA
■ 50 µA
■ 100 µA
Default value: 1 µA

■■■■■■■■ 133
Parameters ■■■■■■■■■■■■■■■■■■■■■■

Electrode test
This parameter is only active with Ipol determinations.
In the case of polarizable electrodes, an electrode test can be carried out.
A check is made that the electrode is properly connected and that no
short-circuit is present. The electrode test is carried out when the determi-
nation is started.

Switch:
■ OFF
■ ON
Default value: OFF

7.12.2.3 Stop conditions


Parameters ▶ Stop conditions
The conditions for canceling the titration are defined under [Stop condi-
tions].

Stop volume
The titration is canceled when the specified volume has been dosed since
the start of the titration.
Adjust this volume to the size of the titration vessel in order to prevent the
contents from overflowing.
Input range 0.00000 to 9,999.99 mL
Default value 100.000 mL
Additional selection: Off

Stop measured value (measured quantity pH)


The titration is canceled when the specified measured value has been
reached since the start of the titration.
Input range –20.000 to 20.000
Default value Off
Additional selection: Off

Stop measured value (measured quantities U and Ipol)


The titration is canceled when the specified measured value has been
reached since the start of the titration.
Input range –2,000.0 to 2,000.0 mV
Additional selection: Off
Default value: Off

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Stop EP
The titration is canceled when the specified number of equivalence points
has been found.
Input range 1 to 9
Default value 9
Additional selection: Off

Volume after EP
The entered volume will be dosed when the number of equivalence points
defined under Stop EP has been found. The curve shape after the equiva-
lence point can also be seen this way.
Input range 0.01000 to 9,999.99 mL
Additional selection: Off
Default value: Off

Stop time
The titration is canceled when the specified time has elapsed since the
start of the titration.
Input range 0 to 999,999 s
Additional selection: Off
Default value: Off

Filling rate
Rate at which the dosing cylinder is filled after the titration.
Input range 0.01 to Max. mL/min
Additional selection: Max. = maximum filling rate.
Default value: Max.

NOTICE

The maximum filling rate depends on the cylinder volume (see table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the filling rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 16 Maximum dosing rate / filling rate

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Cylinder volume maximum dosing rate / filling


rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

7.12.2.4 Evaluation
Parameters ▶ Evaluation
The parameters for the evaluation of the titration curve are defined under
[Evaluation].

Window
If ON is selected, a measured value range (window) can be defined. Only
equivalence points that are within this window are recognized.
Only one window can be defined.

Switch:
■ OFF
■ ON
Default value: OFF

EP recognition (Window = OFF)


Filters for the sought equivalence points:
Selection:
■ All: All equivalence points will be recognized.
■ Greatest: Only the equivalence point with the greatest ERC value, i.e.
the steepest jump, will be recognized.
■ Last: Only the last equivalence point will be recognized.
■ Off: No evaluation takes place.
Default value: All

EP recognition (Window = ON)


Filters for the sought equivalence points:

136 ■■■■■■■■
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Selection:
■ First: Only the first equivalence point will be recognized.
■ Greatest: Only the equivalence point with the greatest ERC value, i.e.
the steepest jump, will be recognized.
■ Last: Only the last equivalence point will be recognized.
Default value: First

Fixed EP1 (measured quantity pH)


The associated volume will be interpolated from the measuring point list
for the measured value entered. The fixed point must lie between the first
and the final entry in the measuring point list.
Input range –20 to 20
Additional selection: Off
Default value: Off

Fixed P1 (measured quantities U and Ipol)


The associated volume will be interpolated from the measuring point list
for the measured value entered. The fixed point must lie between the first
and the final entry in the measuring point list.
Input range –2,000.0 to 2,000.0 mV
Additional selection: Off
Default value: Off

Fixed EP2 (measured quantity pH)


see fixed EP1

Fixed P2 (measured quantities U and Ipol)


see fixed EP1

Lower limit (measured quantity pH)


This parameter is only active if Window = ON.
Measured value for the lower limit.
Input range –20.000 to 20.000
Default value –20.000

Upper limit (measured quantity pH)


This parameter is only active if Window = ON.
Measured value for the upper limit.
Input range –20.000 to 20.0000
Default value 20.000

■■■■■■■■ 137
Parameters ■■■■■■■■■■■■■■■■■■■■■■

Lower limit (measured quantities U and Ipol)


This parameter is only active if Window = ON.
Measured value for the lower limit.
Input range –2,000.0 to 2,000.0 mV
Default value –2,000.0 mV

Upper limit (measured quantities U and Ipol)


This parameter is only active if Window = ON.
Measured value for the upper limit.
Input range –2,000.0 to 2,000.0 mV
Default value 2,000.0 mV

EP criterion (measured quantity pH)


The equivalence point criterion found (ERC = Equivalence point Recogni-
tion Criterion) is compared with this value. Equivalence points whose ERC
is less than the value defined here will be ignored.
Input range 0.10 to 9.99
Default value 0.50

EP criterion (measured quantities U and Ipol)


The equivalence point criterion found (ERC = Equivalence point Recogni-
tion Criterion) is compared with this value. Equivalence points whose ERC
is less than the value defined here will be ignored.
Input range 1 to 999 mV
Default value 30 mV

Evaluation and equivalence point criterion with MET


The equivalence points (EP) are localized by a method based on the For-
tuin method, which has been adapted by Metrohm for numerical meth-
ods. A search is made for the largest measured value change ( ). The
exact EP is determined by using an interpolation factor that depends on
the Δ values before and after :

: EP volume

: Dosed total volume before


: Volume increment
: Interpolation factor according to
Fortuin

138 ■■■■■■■■
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For the recognition of the EPs found, the set EP criterion is compared to
the ERC (Equivalence point Recognition Criterion) found. The ERC is the
sum of the measured value changes before and after the jump:

In certain cases, only 3 or only 1 summand is taken into account.


For the recognition of the EPs found, the set EP criterion is compared to
the ERC (Equivalence point Recognition Criterion) found. The ERC is the
first derivative of the titration curve combined with a mathematical func-
tion that is more sensitive for flat jumps than for steeper ones. EPs whose
ERC is smaller than the defined EP criterion will not be recognized.
The ERC is displayed under Results for each discovered and recognized
EP.
If you adjust the EP criterion retroactively in order to recognize more or
fewer EPs, then you can initiate the reevaluation under Results.

7.12.2.5 Calculation
Parameters ▶ Calculation
A maximum of five calculations can be defined in one method. A series of
variables (raw data from the determination, previously calculated results) is
available for the calculations.
For each calculation, you can define whether the result is to be saved as a
titer or as a common variable.
The five possible calculations are shown in a list:

Figure 53 Parameters calculation – Result list


The result name is specified in the list for each calculation.
Scroll down for result R5.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Editing a calculation

1 Select a calculation in the result list.

2 Click on .

3 Make the desired changes.

Result name
The result name is the text that will be shown in the result view and in the
report.
Input: max. 12 characters
Default value: empty

Decimal places
Number of decimal places used to display the result.

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Input range 0 to 5
Default value 2

Save as CV
The calculated result can be saved as a method-independent variable,
called a common variable. The result is then also available in other meth-
ods for calculations. If statistics has been switched on, then the current
mean value of the determination series will be saved.

Switch:
■ OFF
■ ON
Default value: OFF

Save as titer
The result can be saved as titer for the selected solution (the solution must
be selected). If statistics has been switched on, then the current mean
value of the determination series will be saved.

Switch:
■ OFF
■ ON
Default value: OFF

R1=… - R5=…
Shows the calculation formula. The formula editor is opened for the defi-
nition.

Result unit
The result unit is displayed and saved along with the result.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ %
■ mol/L
■ mmol/L
■ g/L
■ mg/L
■ mg/mL
■ ppm
■ g
■ mg
■ mL
■ mg/piece
■ °C
■ µL
■ mL/min
■ User-defined
Default value: %

7.12.2.6 Statistics
Parameters ▶ Statistics
The statistics calculation of a multiple determination is activated under
[Statistics] and definition is made as to how many determinations the
series contains.

Statistics
If it is set to ON, statistics calculations will be carried out for all of the
defined results.

Switch:
■ OFF
■ ON
Default value: OFF

Number of samples
The number of determinations that are carried out for the statistics calcu-
lations.
Input range 2 to 20
Default value 3

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7.12.2.7 Reports
Parameters ▶ Reports
The reports that will be printed out automatically or saved as a PDF report
after a determination are defined under [Reports].

Results
The result report contains the calculated results, equivalence points, end-
points, sample data, etc.

Switch:
■ OFF
■ ON
Default value: OFF

Curve
The report is shown as a curve.

Switch:
■ OFF
■ ON
Default value: OFF

Calculation/statistics
Output of the calculation formulas for the individual results. Results are
specified with full accuracy. This makes checking with an external program
possible.
If the switch under Parameters ▶ Statistics is set to ON, the following
data will be printed out as well:
■ Result and sample size of the individual determinations
■ Mean value as well as absolute and relative standard deviation

Switch:
■ OFF
■ ON
Default value: OFF

Measuring point list


Output of the measuring point list.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Switch:
■ OFF
■ ON
Default value: OFF

Parameters
All of the parameters of the current method are shown in the parameter
report.

Switch:
■ OFF
■ ON
Default value: OFF

NOTICE

The printer for the report data above is defined under Start
page ▶ System ▶ External devices ▶ Printer.
■ If a connected printer is selected, then the report contains the
data defined by the switches above.
■ If [PDF] is selected as printer and at least one switch is set to ON,
then the report contains the complete data except for the measur-
ing point list. The measuring points are only printed if the switch
measuring point list is set to ON.

PC/LIMS
The PC/LIMS report is a machine-readable report with all of the important
data for a determination. This report can be saved as a TXT file on a USB
flash drive or sent to a LIMS via an RS-232 interface. The output location is
defined under Start page ▶ System ▶ External devices ▶ PC/LIMS
report.
The file name of the TXT file has the following structure:
PC_LIMS_Report_ID1_YYYYMMDD-hhmmss.txt

Switch:
■ OFF
■ ON
Default value: OFF

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7.12.3 Endpoint titrations (SET)

Figure 54 SET parameters – Menu page 1

Figure 55 SET parameters – Menu page 2

7.12.3.1 Start conditions


Parameters ▶ Start conditions
The parameters that are carried out before the start of titration are
defined under [Start conditions].

Request sample ID
Selection of the sample identification that is queried at the start of the
determination.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ ID1
■ ID2
■ ID1&ID2
■ Off
Default value: Off

Start delay time


Waiting time after the start of the determination, before titration takes
place.
During this period, substances such as auxiliary solution can be added
with a Dosimat (parameterization on the Dosimat, the Activation pulse
switch must be switched on for this).
Input range 0 to 999,999 s
Default value 0s

Start volume
Volume that is dosed prior to the start of the titration.
Input range 0.00000 to 9,999.99 mL
Default value 0.00000 mL

Dosing rate
Rate at which the start volume is dosed.
Input range 0.02 to Max. mL/min
Additional selection: Max. = maximum dosing rate.
Default value: Max.

NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 17 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min

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Cylinder volume maximum dosing rate / filling


rate
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

Pause
Waiting time, e.g. for the stabilization of the measured value after the
start, for dissolving solid substances or a reaction time after the dosing of
a start volume.
Input range 0 to 999,999 s
Default value 0s

Activation pulse
If it is activated, an activation pulse is sent to a remote line that starts a
connected Dosimat. We recommend to define a Start delay time for
this.

Switch:
■ OFF
■ ON
Default value: OFF

Request sample size


If this parameter is activated, then the value for the sample size will be
requested at the start of the determination.

Switch:
■ OFF
■ ON
Default value: OFF

Request sample unit


If this parameter is activated, then the unit for the sample size will be
requested at the start of the determination.

Switch:
■ OFF
■ ON
Default value: OFF

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Hold at request
If this parameter is activated, then the run will be paused during the
request. If the parameter is switched off, the titration will be started in the
background.

Switch:
■ OFF
■ ON
Default value: ON

7.12.3.2 Titration parameters


Parameters ▶ Titration parameters
The parameters that are carried out at the start of titration are defined
under [Titration parameters].

Stirrer
If this parameter is activated, then the stirrer is switched on at the start of
the determination.

Switch:
■ OFF
■ ON
Default value: ON

Stirring rate
Setting the stirring rate. The stirring direction is always clockwise.
Conversion: Value x 120 ± 5 rpm = stirring rate in rpm
e.g.: 8 × 120 ± 5 rpm = 960 ± 40 rpm
Input range 1 to 15
Default value 8

Temperature
Manually entered titration temperature. If a temperature sensor is connec-
ted, then the temperature will be measured as follows:
■ For measured quantity Ipol: Temperature measurement in the begin-
ning and at the end of the titration.
■ For measured quantities U and pH: Continuous temperature measure-
ment.
For determinations in pH mode, the value is used for temperature com-
pensation (electrode slope is adjusted accordingly).

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Input range –20.0 to 150.0 °C


Default value 25.0 °C

Sensor
Open the selection list and select a sensor.
The selection depends on the measuring mode. Sensors are defined and
listed under System ▶ Sensors, e.g.:

Solution
Open the selection list and select a solution.
Solutions are defined and listed under System ▶ Solutions, e.g.:

We, at Metrohm, always recommend selecting the solution.


This ensures that accurate data (titer, concentration, etc.) is always used
for the calculation and that the volume of the selected solution is com-
pared to the volume defined under System ▶ Settings.

Titration direction
We, at Metrohm, recommend that you specify whenever possible whether
the change of the measured value is positive or negative.
If two endpoints have been set, then the titration direction will be defined
automatically. In this case, the setting will be ignored.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ +: Positive measured value change, i.e. in the direction of a higher pH
value, greater voltage or greater current.
■ -: Negative measured value change, i.e. in the direction of a lower pH
value, lesser voltage or lesser current.
■ Auto: The titration direction is determined automatically from the ini-
tial measured value and the set endpoint.
Default value: Auto

Extraction time
Minimum duration of the titration. The titration will not be canceled dur-
ing the extraction time, even if the endpoint has already been reached.
The titration is, however, canceled if a stop condition is fulfilled in this
time. The entry of an extraction time may be advisable, for instance, for
the titration of sparingly soluble samples.
Input range 0 to 999,999 s
Default value 0s

Time interval MP
Time interval for entering a measuring point in the measuring point list.
The measuring point list is limited to 1000 measuring points.
Input range 0.1 to 999,999.0 s
Default value 2.0 s

Ipol
This parameter is only active with Ipol determinations.
The polarization current is the current that is applied to a polarizable elec-
trode during voltametric measurement.
Selection:
■ 1 µA
■ 20 µA
■ 50 µA
■ 100 µA
Default value: 1 µA

Electrode test
This parameter is only active with Ipol determinations.
In the case of polarizable electrodes, an electrode test can be carried out.
A check is made that the electrode is properly connected and that no
short-circuit is present. The electrode test is carried out when the determi-
nation is started.

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Switch:
■ OFF
■ ON
Default value: OFF

7.12.3.3 Control parameters EP1


Parameters ▶ Control parameters EP1
The control parameters for the first endpoint are defined under [Control
parameters EP1].

Endpoint 1 at (measured quantity pH)


Measured value for the first endpoint.
Input range –20.000 to 20.000
Additional selection: Off
Default value: Off

End point1 at (measured quantities U and Ipol)


Measured value for the first endpoint.
Input range –2,000.0 to 2,000.0 mV
Additional selection: Off
Default value: Off

Titration rate
3 predefined sets of parameters and 1 set of parameters that can be
defined manually are available for setting the titration rate.
Selection:
■ Slow: For titrations with a long reaction time or a steep increase/
decrease at the endpoint. The titration time can be very long.
■ Optimal: For all standard titrations. The parameters have been opti-
mized for the most frequent applications.
■ Fast: For titrations that show a flat curve progression at the endpoint.
The titration is carried out very fast.
■ User: The individual titration parameters can be modified.
Default value: Optimal

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

NOTICE

Select Optimal as titration rate if you are developing a new titration


method. This parameter is suitable for virtually all titrations and only
needs adaptation in special cases.

Table 18 Default values of the predefined sets of parameters for MET


Slow Optimal Fast
Control range 5.000 2.000 0.500
pH
Control range 300.0 mV 100.0 mV 30.0 mV
U and Ipol
Min. rate 5.00 µL/min 25.00 µL/min 50.00 µL/min
Max. rate 1.00 mL/min 10.00 mL/min Maximum dos-
ing rate

Minimum rate
This parameter is only active if the titration rate is set to User.
Rate at which dosing is carried out at the very beginning of the titration
and in the control range at the end of the titration.
This parameter has a vital influence on the titration rate and thus also on
the accuracy. The smaller the selected minimum rate, the slower the titra-
tion.
Input range 0.01 to 9,999.00 µL/min
Default value 25.00 µL/min

Maximum rate
This parameter is only active if the titration rate is set to User.
Rate at which dosing is carried out outside of the control range.
Input range 0.01 to Max. mL/min
Default value 10.00 mL/min
Additional selection: Max. = maximum dosing rate.

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NOTICE

The maximum dosing rate depends on the cylinder volume (see


table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the dosing rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 19 Maximum dosing rate / filling rate


Cylinder volume maximum dosing rate / filling
rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

Control range (measured quantity pH)


This parameter is only active if the titration rate is set to User.
This parameter defines the control range before the specified endpoint.
Individual volume steps are dosed in the control range; the dosing is finely
controlled. Within the control range, dosing is done with the rate defined
under Minimum rate.
The larger the control range, the slower the titration. Outside of the con-
trol range, dosing is carried out continuously; the dosing rate is defined
under Maximum rate.
Input range 0.001 to 20.000
Default value 2.000
Additional selection: Off

Control range (measured quantities U and Ipol)


This parameter is only active if the titration rate is set to User.
This parameter defines the control range before the specified endpoint.
Individual volume steps are dosed in the control range; the dosing is finely
controlled. The closer the endpoint, the slower the dosing until the dosing
rate defined under Minimum rate has been reached.
The larger the control range, the slower the titration. Outside of the con-
trol range, dosing is carried out continuously; the dosing rate is defined
under Maximum rate.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Input range 0.1 to 1,250.0 mV


Default value 100.0 mV
Additional selection: Off

Stop criterion
The titration is canceled when the endpoint has been reached and this
stop criterion has been fulfilled. If no stop criterion was defined, the titra-
tion is completed according to the stop conditions.
Selection:
■ Drift: The titration is canceled once the stop drift has been reached.
■ Time: The titration is canceled once the Delay time has been
reached.
■ Off: The titration will not be canceled until the stop conditions are
fulfilled.
Default value: All

Stop drift
This parameter is only active if the stop criterion is set to Drift.
The titration is canceled as soon as the endpoint and the stop drift have
been reached.
Input range 1 to 999 µL/min
Default value 20 µL/min

Delay time
This parameter is only active if the stop criterion is set to Time.
When the endpoint has been reached, the Delay time is allowed to
elapse after the last dosing and the titration is then stopped.
Input range 0 to 999 s
Default value 10 s

7.12.3.4 Control parameters EP2


Parameters ▶ Control parameters EP2
The control parameters for the second endpoint are defined under [Con-
trol parameters EP2].

NOTICE

The parameters and their selection and input ranges are identical to
the Control parameters EP1.

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7.12.3.5 Stop conditions


Parameters ▶ Stop conditions
The conditions for canceling the titration are defined under [Stop condi-
tions], if this does not occur automatically. This is the case if the set end-
point was not reached or if the stop criterion was not fulfilled.

Stop volume
The titration is canceled when the specified volume has been dosed since
the start of the titration.
Adjust this volume to the size of the titration vessel in order to prevent the
contents from overflowing.
Input range 0.00000 to 9,999.99 mL
Default value 100.000 mL
Additional selection: Off

Stop time
The titration is canceled when the specified time has elapsed since the
start of the titration.
Input range 0 to 999,999 s
Additional selection: Off
Default value: Off

Filling rate
Rate at which the dosing cylinder is filled after the titration.
Input range 0.01 to Max. mL/min
Additional selection: Max. = maximum filling rate.
Default value: Max.

NOTICE

The maximum filling rate depends on the cylinder volume (see table).
If volatile solvents/solutions or solutions with a high viscosity are
used, the filling rate must be reduced accordingly so that the dosing
unit is not overloaded.

Table 20 Maximum dosing rate / filling rate

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Cylinder volume maximum dosing rate / filling


rate
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min

7.12.3.6 Calculation
Parameters ▶ Calculation
A maximum of five calculations can be defined in one method. A series of
variables (raw data from the determination, previously calculated results) is
available for the calculations.
For each calculation, you can define whether the result is to be saved as a
titer or as a common variable.
The five possible calculations are shown in a list:

Figure 56 Parameters calculation – Result list


The result name is specified in the list for each calculation.
Scroll down for result R5.

Editing a calculation

1 Select a calculation in the result list.

2 Click on .

156 ■■■■■■■■
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3 Make the desired changes.

Result name
The result name is the text that will be shown in the result view and in the
report.
Input: max. 12 characters
Default value: empty

Decimal places
Number of decimal places used to display the result.
Input range 0 to 5
Default value 2

Save as CV
The calculated result can be saved as a method-independent variable,
called a common variable. The result is then also available in other meth-

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

ods for calculations. If statistics has been switched on, then the current
mean value of the determination series will be saved.

Switch:
■ OFF
■ ON
Default value: OFF

Save as titer
The result can be saved as titer for the selected solution (the solution must
be selected). If statistics has been switched on, then the current mean
value of the determination series will be saved.

Switch:
■ OFF
■ ON
Default value: OFF

R1=… - R5=…
Shows the calculation formula. The formula editor is opened for the defi-
nition.

Result unit
The result unit is displayed and saved along with the result.
Selection:
■ %
■ mol/L
■ mmol/L
■ g/L
■ mg/L
■ mg/mL
■ ppm
■ g
■ mg
■ mL
■ mg/piece
■ °C
■ µL
■ mL/min
■ User-defined
Default value: %

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7.12.3.7 Statistics
Parameters ▶ Statistics
The statistics calculation of a multiple determination is activated under
[Statistics] and definition is made as to how many determinations the
series contains.

Statistics
If the switch is set to ON, statistics calculations will be carried out for all of
the defined results.

Switch:
■ OFF
■ ON
Default value: OFF

Number of samples
The number of determinations that are carried out for the statistics calcu-
lations.
Input range 2 to 20
Default value 3

7.12.3.8 Reports
Parameters ▶ Reports
The reports that will be printed out automatically or saved as a PDF report
after a determination are defined under [Reports].

Results
The result report contains the calculated results, equivalence points, end-
points, sample data, etc.

Switch:
■ OFF
■ ON
Default value: OFF

Curve
The report is shown as a curve.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Switch:
■ OFF
■ ON
Default value: OFF

Calculation/statistics
Output of the calculation formulas for the individual results. Results are
specified with full accuracy. This makes checking with an external program
possible.
If the switch under Parameters ▶ Statistics is set to ON, the following
data will be printed out as well:
■ Result and sample size of the individual determinations
■ Mean value as well as absolute and relative standard deviation

Switch:
■ OFF
■ ON
Default value: OFF

Measuring point list


Output of the measuring point list.

Switch:
■ OFF
■ ON
Default value: OFF

Parameters
All of the parameters of the current method are shown in the parameter
report.

Switch:
■ OFF
■ ON
Default value: OFF

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NOTICE

The printer for the report data above is defined under Start
page ▶ System ▶ External devices ▶ Printer.
■ If a connected printer is selected, then the report contains the
data defined by the switches above.
■ If [PDF] is selected as printer and at least one switch is set to ON,
then the report contains the complete data except for the measur-
ing point list. The measuring points are only printed if the switch
measuring point list is set to ON.

PC/LIMS
The PC/LIMS report is a machine-readable report with all of the important
data for a determination. This report can be saved as a TXT file on a USB
flash drive or sent to a LIMS via an RS-232 interface. The output location is
defined under Start page ▶ System ▶ External devices ▶ PC/LIMS
report.
The file name of the TXT file has the following structure:
PC_LIMS_Report_ID1_YYYYMMDD-hhmmss.txt

Switch:
■ OFF
■ ON
Default value: OFF

7.12.4 pH calibration (CAL)

Figure 57 CAL parameters – Menu

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

7.12.4.1 Calibration parameters


Parameters ▶ Calibration parameters
The parameters that are carried out at the start of calibration are defined
under [Calibration parameters].

Signal drift
Maximum permissible drift for the measured value acceptance, i.e. maxi-
mum change of the measured value per minute.
Input range 0.1 to 999.0 mV/min
Default value 2.0 mV/min
Additional selection: Off: Measured value acceptance will take place after
the maximum waiting time has elapsed. This can be useful when the elec-
trode is slow to respond.

Temperature
Calibration temperature. If a temperature sensor is connected, the calibra-
tion temperature is automatically applied. The calibration temperature can
also be entered manually.
The calibration temperature allows for the temperature compensation dur-
ing a determination. If a temperature sensor is connected, this happens
automatically. If there is no temperature sensor, the temperature can be
entered manually as a method parameter. The calibration temperature is
necessary for selecting the corresponding pH value of the buffer.
Input range –20.0 to 150.0 °C
Default value 25.0 °C

Min. waiting time


The measured value is not accepted until the minimum waiting time has
elapsed, even if the signal drift has already been reached. The minimum
waiting time is only important for drift-controlled measurements.
Input range 0 to 999,999 s
Default value 10 s

Max. Waiting time


If the signal drift has been switched off or has not yet been reached, then
the measured value will be accepted once the maximum waiting time has
elapsed.
Input range 0 to 999,999 s
Default value 110 s

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Sensor
Open the selection list and select a sensor.
Only sensors of the pH electrode type can be selected.

Stirrer
If this parameter is activated, then the stirrer is switched on at the start of
the determination.

Switch:
■ OFF
■ ON
Default value: ON

Stirring rate
Setting the stirring rate. The stirring direction is always clockwise.
Conversion: Value × 120±5 rpm = stirring rate in rpm
e.g.: 8 × 120±5 rpm = 960±40 rpm
Input range 1 to 15
Default value 8

7.12.4.2 Buffers
Parameters ▶ Buffers
The statistics calculation of a multiple determination is activated under
[Buffers] and definition is made as to how many determinations the ser-
ies contains.

Buffer type
Selection of a predefined buffer series or definition of special buffers. In
the case of predefined buffer series, the instrument automatically recogni-
zes which buffer is involved.

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Selection:
■ Baker
■ Beckmann
■ DIN
■ Fisher
■ Fluka Basel
■ Hamilton
■ Merck CertiPUR
■ Merck Titrisol
■ Metrohm
■ Mettler
■ NIST
■ Precisa
■ Radiometer
■ Special
Default value: Metrohm

NOTICE

Merck CertiPUR:
Reference temperature = 25 °C.
When using Merck CertiPUR buffers with a reference temperature of
20 °C, the buffer type Merck Titrisol must be selected.

NOTICE

Special:
Up to 5 calibration buffers can be defined in the method. The buffers
are not recognized automatically here. Enter the buffers exactly in the
specified sequence.

Number of buffers
Number of buffers that are used for calibration.
If calibration is accomplished with more than two buffers, then certain
buffers can be used repeatedly in order to give them more statistical
weight. The first two buffers must, however, always be different from one
another.

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Selection:
■ 1
■ 2
■ 3
■ 4
■ 5
Default value: 2

Buffer 1 pH
This parameter is only available if the buffer type is set to Special.
Input range –20.000 to 20.000
Default value 7.000

Buffer 2 pH
This parameter is only available if the buffer type is set to Special.
Input range –20.000 to 20.000
Additional selection: Off
Default value: 4.000

Buffer 3 pH
This parameter is only available if the buffer type is set to Special.
Input range –20.000 to 20.000
Additional selection: Off
Default value: Off

Buffer 4 pH
See buffer 3 pH

Buffer 5 pH
See buffer 3 pH

7.12.4.3 Reports
Parameters ▶ Reports
The reports that will be printed out automatically or saved as a PDF report
after a determination are defined under [Reports].

Results
The result report contains the specifications for the calibration (slope,
pH(0), etc.).

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Parameters ■■■■■■■■■■■■■■■■■■■■■■

Switch:
■ OFF
■ ON
Default value: OFF

Parameters
All of the parameters of the current method are shown in the parameter
report.

Switch:
■ OFF
■ ON
Default value: OFF

PC/LIMS
The PC/LIMS report is a machine-readable report with all of the important
data for a determination. This report can be saved as a TXT file on a USB
flash drive or sent to a LIMS via an RS-232 interface. The output location is
defined under System ▶ External devices.
The file name of the TXT file has the following structure:
PC_LIMS_Report_ID1_YYYYMMDD-hhmmss.txt

Switch:
■ OFF
■ ON
Default value: OFF

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8 Maintenance

8.1 Maintenance
Regularly perform maintenance work on the product to prevent malfunc-
tions and to ensure a long service life.
■ Metrohm recommends having the products maintained by specialist
personnel of Metrohm AG as part of an annual service. Shorter mainte-
nance intervals may be necessary if you frequently work with caustic
and corrosive chemicals.
■ Only perform maintenance work that is described in this instruction.
Contact your regional Metrohm service representative for further main-
tenance work and repairs. The regional Metrohm service representative
offers every form of technical advice for maintenance and service of all
Metrohm products.
■ Only use spare parts that meet the technical requirements of the man-
ufacturer. Original spare parts always meet these requirements.

8.2 Cleaning the product surface


Regularly clean the product to prevent malfunctions and to ensure a long
service life.
■ Remove spilled chemicals immediately.
■ Protect plug connections against contamination.

WARNING

Chemical hazardous substances


Contact with aggressive chemical substances may cause poisoning or
chemical burns.
■ Wear personal protective equipment (e.g. protective glasses,
gloves).
■ Use exhaust equipment when working with vaporizing hazardous
substances.
■ Clean contaminated surfaces.
■ Only use detergents that do not cause any unwanted side reac-
tions with the materials to be cleaned.
■ Dispose of chemically contaminated materials (e.g. cleaning mate-
rial) in accordance with regulations.

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Cleaning the product surface ■■■■■■■■■■■■■■■■■■■■■■

WARNING

Electrical potential
Contact with electrical potential can cause serious injuries or death.
■ Operate the product only if it is in perfect condition. The housing
must also be intact.
■ Only use the product with the covers fitted.
■ Protect live components (e.g. power supply unit, power cord, con-
nection sockets) against moisture.
■ Always have maintenance work and repairs on electrical compo-
nents carried out by a regional Metrohm service representative.

Prerequisite:
■ The product is switched off and disconnected from the energy supply.
Required accessories:
■ Cleaning cloth (soft, lint-free)
■ Water or ethanol

1 Clean the surface with a damp cloth. Remove persistent contamina-


tion with ethanol.

2 Wipe the surface with a dry cloth.

3 Clean the connectors with a dry cloth.

8.2.1 Performing maintenance on the cylinder unit


In the Manual control ▶ Exchange cylinder unit function, the drive
moves the push rod into the exchange position.

CAUTION

Property damage caused by jammed cylinder unit


Damage caused by disassembling of a jammed cylinder unit. The
damaged cylinder unit must be replaced.
■ Do not use force to rotate the cylinder top piece.
■ Follow the instructions for disassembling the cylinder unit.

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CAUTION

Instrument damage from aggressive chemical hazardous sub-


stances
Damage of the instrument or malfunction through contact with
aggressive chemical substances.
■ Clean up spilled liquids and solids immediately.
■ Use protective grounding when working with highly flammable
chemical substances and gases.
■ If you suspect that chemical substances have gotten into the
instrument, disconnect the instrument from the energy supply.
Then, notify Metrohm Service.

Maintenance steps
■ Emptying the cylinder unit as far as possible and removing it
■ Taking the cylinder unit apart
■ Cleaning the cylinder unit
■ Assembling the cylinder unit
Once the maintenance steps have been carried out professionally, the cyl-
inder unit can be mounted again.

Emptying and removing the cylinder unit


For emptying and removing the cylinder unit see Exchanging the cylinder
unit (see chapter 7.4.3, page 57)
The disassembled cylinder unit can now be taken apart and cleaned or
replaced.

Taking the cylinder unit apart

The cylinder unit has been disassembled.


Required accessories:
■ 6.1546.040 piston tool

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NOTICE

It is normally not necessary to remove the mounting ring out of the


light protection or the screw nipple on the dosing cylinder for clean-
ing. The parts can be cleaned while still in their pre-mounted state.

Push the dosing cylinder out of the light protection from above.

Remaining fluid can be emptied out of the dosing cylinder through


the dosing cylinder tip.

Lift the piston carefully out of the dosing cylinder. Use the
6.1546.040 piston tool to accomplish this.
The individual parts can now be cleaned and checked.

Cleaning the disassembled cylinder unit

1 Clean the individual parts of the cylinder unit with deionized water.

2 In the event of severe contamination, place the individual parts in


warm water with a little dishwashing detergent and then rinse off
with deionized water.

3 Check the individual parts of the cylinder unit (dosing cylinder, piston,
sealing lips and piston rod) for the following defects:
■ Are rough areas or scratches visible on the dosing cylinder?

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■ Are scratches visible on the piston surface?


■ Is any unevenness visible on the sealing lips of the piston?
If any of these defects is visible, replace the entire cylinder unit.

Assembling the cylinder unit

Required accessories:
■ 6.2803.010 paraffin grease

1 Greasing the piston


■ Grease the piston.

NOTICE

Grease only the edge of the piston.


The tip of the piston must not be greased.

Figure 58 Greasing the piston


■ Using your finger, carefully apply a trace of paraffin grease
(6.2803.010) to the exterior of the sealing lips of the piston.
■ Wipe off excess grease with a soft, lint-free cloth.

2 Carefully slide the piston far enough into the dosing cylinder that the
piston rod still protrudes out of it by approximately 6 mm.

3 Push the dosing cylinder far enough into the light protection so that
its flange is securely up against the mounting ring (gray plastic ring).
The cylinder unit can now be mounted.

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8.2.2 Mounting the cylinder unit

Mounting the cylinder unit

Prerequisite
The instrument is switched on.
The [Exchange cylinder unit] process was executed up to the point
when the cylinder unit can be removed from the instrument.
The maintenance has been carried out professionally or a new cylinder
unit is ready to be mounted.
The instrument is carrying out the [Exchange cylinder unit] procedure
and the push rod of the dosing drive is at the height at which the cylinder
unit can be mounted. The following message is displayed:

Procedure

1 To mount the cylinder unit, the piston rod must be pulled out of the
dosing cylinder by approx. 6 mm. If necessary, pull the piston care-
fully out of the dosing cylinder with the 6.1546.040 piston tool.
While doing so, make sure that the sealing lips and the piston in the
dosing cylinder are not damaged.

2 Couple the piston rod with the push rod.


When doing so, the hook profile of the piston rod must be carefully
aligned in the hook profile of the push rod.

3 Carefully push the cylinder unit downwards. The piston is pushed


into the dosing cylinder.
Screw the light protection of the cylinder unit securely into the
thread of the housing.

4 Now click on the [Continue] button.


The push rod moves the piston into the basic position.

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Make sure that the cylinder unit has been mounted correctly.
[Continue]

6 [Continue]

NOTICE

Make sure that the value for the cylinder volume in the System
menu is the same as the volume of the mounted cylinder unit.

7
NOTICE

Carry out the Prepare buret (PREP) command.

8.3 Displaying system data


The System ▶ About menu path shows detailed information on:
■ Program version
■ Instrument
■ Main board
■ Measuring interface

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Resetting the system ■■■■■■■■■■■■■■■■■■■■■■

Figure 59 System data

8.4 Resetting the system


In very rare instances, a faulty file system (e.g. because of a program
crash) may lead to an impairment of program functioning. The internal file
system must be initialized in such cases.

CAUTION

If the system is reset, all user data (methods, solutions, etc.) will be
deleted. The instrument will be reset to factory settings. The pass-
word for the Expert dialog type is: METROHM9100
We recommend creating a backup of the system at regular intervals
in order to avoid data losses.

The program version does not change when resetting the system.

Resetting the system

Prerequisite:
■ The instrument is switched off.

1 Switching on the instrument

Press the key.

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2 Resetting the system


Wait until the following text is displayed in the bottom line of the
screen:
Initializing, please wait...

Once the text shown above appears, press the 3 keys


simultaneously and hold for approx. 4 s.
The warning Factory reset appears: All information (including saved
methods, determination results etc.) is deleted. Do you want to con-
tinue?

3 Confirming the reset


Confirm the warning with [Continue].
The instrument deletes the user data and restarts.

NOTICE

Change the dialog language if needed: System ▶ Set-


tings ▶ Language (on page 2/2)

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9 Troubleshooting
Messages on malfunctions and errors are displayed in the control software
or in the embedded software (e.g. on the display of an instrument) and
contain the following information:
■ Descriptions of causes of malfunctions (e.g. jammed drive)
■ Descriptions of problems with the control (e.g. missing or invalid
parameter)
■ Information on how to solve the problem
System components with status display elements also indicate malfunc-
tions and errors with a red flashing LED.
Troubleshooting on the product is often only possible with the control
software or the embedded software (e.g. initializing, moving to a defined
position).
See also

Signals (chapter 3.1.1, page 11)

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10 Disposal
Properly dispose of chemicals and of the product to reduce negative
effects on the environment and public health. Local authorities, waste dis-
posal companies or dealers provide more detailed information on disposal.
Observe the WEEE EU directive (WEEE = Waste Electrical and Electronic
Equipment) for the proper disposal of waste electronic equipment within
the European Union.

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11 Technical specifications

11.1 Ambient conditions


Nominal function range +5 to +45 °C at
max. 80%
relative humidity, non-
condensing

Storage +5 to +45 °C

11.2 Energy supply


External power supply unit
Input
Nominal voltage range 100–240 VAC
Frequency range 50–60 Hz
Current max. 1.5 A
Output
Nominal voltage 24 VDC
Current max. 2.7 A
Power output 65 W

Instrument
Input
Nominal voltage 24 VDC
Power consumption max. 20 W
Output
Nominal voltage 24 VDC
Power output max. 45 W

USB connector
Nominal voltage 5V

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Current at the power supply unit 500 mA max. output current per
channel

Protection
Internal fuse 1.5 A

11.3 Dimensions
Measurements
Width 286 mm
Height
without cylinder unit 220 mm
with cylinder unit 358 mm
with support rod 508 mm
Depth 286 mm

Weight 3.6 kg without accessories and


power supply unit

11.4 Housing
Materials
Cover PP 20% filled with talc
Back panel 1.4301 stainless steel
Base PP 20% filled with talc
Front foils PET EBA 180, anti-glare

IP degree of protection IP 40

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11.5 Connectors specifications


Power IN
Socket round plug 4-pin

Power OUT
Socket round plug 4-pin

Remote
Socket D-Sub 9-pin

Ethernet
Type CAT 6
Socket RJ-45
Cable type min. FFTP shielded
Cable length max. 10 m from Metrohm acces-
sories

USB
Type 2.0
Socket type A
Cable type shielded
Cable length max. 5 m from Metrohm acces-
sories

Measuring inputs
Ind
Socket type F measuring input for
potentiometric electro-
des
Temp

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Socket 2 × 2 mm measuring input for


temperature sensors of
the Pt1000 or NTC type
for automatic tempera-
ture compensation
Pol
Socket type F measuring input for
polarizable electrodes
Ref
Socket 4 mm reference potential

11.6 Display specifications


Display
Type LCD VGA color display
Size approx. 4.3" diagonal
Resolution 480 × 272 pixels

Status display LED green

11.7 Operation specifications


Touch panel
Type resistive

Resistance to chemicals resistant to the following


chemicals (no visible
changes after 24 h of dura-
tion of action):
ethanol
methanol
water

Keys 5 keys

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11.8 Measurement specifications


Potentiometric
Measuring range –2,000 to +2,000 mV
Resolution 0.1 mV
Measuring accuracy ±0.5 mV in the measuring range
–2,000 mV to
+2,000 mV
Input resistance ≥ 1·1012Ω
Offset current ≤ ±1·10–12 A

Temperature
Pt1000
Measuring range –150 to +250 °C
Measuring resolution 0.1 °C
Measuring accuracy ±0.4 °C in the measuring range
–20.0 °C to +150.0 °C
NTC 30 kOhm
Measuring range –5 to +250 °C
Measuring resolution 0.1 °C
Measuring accuracy ±0.6 °C in the measuring range
+10.0 °C to +40.0 °C

Polarizer
Ipol DC
Polarization current 1, 20, 50, 100 µA can be selected
Measuring range 0–3,500 mV
Measuring resolution 0.1 mV

Reference conditions
Instrument status min. 30 minutes in operation
Adjusting interval annual

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Measuring accuracy applies to all measuring


ranges without sensor error,
under reference conditions,
measuring interval 100 ms,
room temperature
+25 °C (± 3 °C), relative
humidity ≤ 60%

11.9 Stirrer specifications


Variant magnetic

Adjustment range for rotational +1 to +15 120–1,800 rpm


speed

Rotational speed change per step 115–125 rpm

Maximum rotational speed 1,700–1,900 rpm

Stirring bar lengths 8, 12, 16, 25, 30 mm

11.10 Liquid handling specifications


Cylinder unit
Cylinder volume 5, 10, 20, 50 mL

Dosing drive
Dosing resolution 20,000 steps per cylinder vol-
ume
Dosing accuracy according to ISO/DIN 8655-3

Tubing
Tubing nipple outer thread M6
Inner diameter 2 mm
Material FEP fluorinated ethylene
propylene

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