Metrohm 848 Titrino plus User manual

848 Titrino plus
Manual
8.848.8008EN / 2015-01-19

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
848 Titrino plus
Manual
8.848.8008EN / 2015-01-19 jb/ebe

Technische Dokumentation
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
This document has been prepared with great care. However, errors can
never be entirely ruled out. Please send comments regarding possible
errors to the address above.
Documentation in additional languages can be found on
http://documents.metrohm.com.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
848 Titrino plus ￭￭￭￭￭￭￭￭ III
Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Titration and measuring modes ................................................ 1
1.1.2 Connectors .............................................................................. 2
1.1.3 Intended use ........................................................................... 2
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 3
1.3 Safety instructions ................................................................ 4
1.3.1 General notes on safety ........................................................... 4
1.3.2 Electrical safety ........................................................................ 4
1.3.3 Tubing and capillary connections ............................................. 5
1.3.4 Flammable solvents and chemicals ........................................... 5
1.3.5 Recycling and disposal ............................................................. 5
2 Overview of the instrument 7
3 Installation 9
3.1 Setting up the instrument .................................................... 9
3.1.1 Packaging ................................................................................ 9
3.1.2 Checks .................................................................................... 9
3.1.3 Location .................................................................................. 9
3.2 Connecting a sensor ............................................................. 9
3.3 Connecting a stirrer ............................................................ 11
3.4 Connecting a balance ......................................................... 12
3.5 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 12
3.6 Connecting instruments to the remote connector .......... 15
3.7 Attaching the exchange unit ............................................. 16
4 Titrations 17
4.1 Dynamic equivalence point titration (DET) ....................... 17
4.2 Monotonic equivalence point titration (MET) .................. 17
4.3 Endpoint titration (SET) ..................................................... 18
5 Operation 19
5.1 Switching the instrument on and off ............................... 19
5.2 Fundamentals of operation ............................................... 20
5.2.1 The keypad ............................................................................ 20
5.2.2 Structure of the dialog windows ............................................ 21

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 848 Titrino plus
5.2.3 Navigating in the dialog ......................................................... 21
5.2.4 Entering text and numbers ..................................................... 22
5.2.5 Selecting from a selection list ................................................. 23
5.3 Formula editor .................................................................... 23
5.4 Methods .............................................................................. 25
5.4.1 Creating a new method ......................................................... 25
5.4.2 Saving a method ................................................................... 26
5.4.3 Loading a method ................................................................. 27
5.4.4 Exporting a method ............................................................... 28
5.5 Control ................................................................................. 29
5.6 Sample data ........................................................................ 30
5.6.1 Entering sample data in the main dialog ................................ 30
5.6.2 Requesting sample data at the start of the determination ...... 31
5.7 Sample table ....................................................................... 32
5.7.1 General ................................................................................. 32
5.7.2 Editing the sample data ......................................................... 33
5.7.3 Sending the sample size from a balance ................................. 35
5.8 Carrying out a determination ............................................ 35
5.9 Live modifications .............................................................. 37
5.9.1 Editing the sample data of the running determination ............ 37
5.9.2 Editing the sample table while a determination is running ...... 38
5.9.3 Editing the live parameters ..................................................... 39
5.10 Results ................................................................................. 40
5.11 Statistics .............................................................................. 41
5.12 Printing a report manually ................................................. 43
5.13 Manual control ................................................................... 44
5.13.1 Dosing ................................................................................... 45
5.13.2 Measuring ............................................................................. 49
5.13.3 Stirring .................................................................................. 50
6 System settings 52
6.1 Basic settings ...................................................................... 52
6.2 Managing sensors .............................................................. 56
6.2.1 General ................................................................................. 56
6.2.2 Editing the sensor data .......................................................... 56
6.3 Managing solutions ............................................................ 58
6.3.1 General ................................................................................. 58
6.3.2 Editing the solution data ........................................................ 58
6.4 Managing common variables ............................................ 60
6.4.1 General ................................................................................. 60
6.4.2 Editing common variables ...................................................... 61
6.5 File management ................................................................ 62

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
848 Titrino plus ￭￭￭￭￭￭￭￭ V
6.6 Configuring external devices ............................................. 63
6.7 Instrument diagnosis .......................................................... 66
6.7.1 Loading program versions and language files ......................... 66
6.7.2 Diagnosis functions ............................................................... 67
7 Parameters 68
7.1 Dynamic equivalence point titrations (DET) ..................... 68
7.1.1 Start conditions ..................................................................... 68
7.1.2 Titration parameters .............................................................. 69
7.1.3 Stop conditions ..................................................................... 75
7.1.4 Evaluation ............................................................................. 76
7.1.5 Calculation ............................................................................ 79
7.1.6 Statistics ................................................................................ 81
7.1.7 Reports .................................................................................. 81
7.2 Monotonic equivalence point titrations (MET) ................ 83
7.2.1 Start conditions ..................................................................... 83
7.2.2 Titration parameters .............................................................. 84
7.2.3 Stop conditions ..................................................................... 89
7.2.4 Evaluation ............................................................................. 90
7.2.5 Calculation ............................................................................ 93
7.2.6 Statistics ................................................................................ 95
7.2.7 Reports .................................................................................. 95
7.3 Endpoint titrations (SET) .................................................... 97
7.3.1 Conditioning ......................................................................... 97
7.3.2 Start conditions ..................................................................... 98
7.3.3 Titration parameters ............................................................ 100
7.3.4 Control parameters EP1 ....................................................... 102
7.3.5 Control parameters EP2 ....................................................... 105
7.3.6 Stop conditions ................................................................... 105
7.3.7 Calculation .......................................................................... 106
7.3.8 Statistics .............................................................................. 108
7.3.9 Reports ................................................................................ 108
7.4 pH calibration (CAL) ......................................................... 110
7.4.1 Calibration parameters ........................................................ 110
7.4.2 Buffers ................................................................................. 112
7.4.3 Reports ................................................................................ 113
8 Operation and maintenance 114
8.1 Quality management and qualification with Metrohm 114
9 Troubleshooting 115
9.1 SET titration ...................................................................... 115
9.2 Miscellaneous ................................................................... 116

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VI ￭￭￭￭￭￭￭￭ 848 Titrino plus
10 Appendix 117
10.1 Exchange unit ................................................................... 117
10.1.1 Maximum dosing and filling rate .......................................... 117
10.1.2 Parameters for the preparing (PREP) ..................................... 117
10.2 Stirring rate ....................................................................... 118
10.3 Balance .............................................................................. 118
10.4 USB devices ....................................................................... 119
10.4.1 6.2147.000 numerical USB keypad ...................................... 119
10.4.2 Key assignment of a USB keyboard ...................................... 120
10.4.3 PC mouse ............................................................................ 120
10.4.4 Printer ................................................................................. 121
10.5 System initialization ......................................................... 121
10.6 Remote interface .............................................................. 122
10.6.1 Pin assignment of the remote interface ................................ 122
10.6.2 Status diagram of the remote interface ................................ 124
10.7 Remote control via an RS-232 connection ..................... 125
10.7.1 Commands and variables ..................................................... 126
10.8 Arithmetic algorithms in the 848 Titrino plus ............... 127
11 Technical specifications 130
11.1 Measuring inputs .............................................................. 130
11.1.1 Potentiometry ...................................................................... 130
11.1.2 Polarizer .............................................................................. 130
11.1.3 Temperature ........................................................................ 131
11.2 Dosing drive ...................................................................... 132
11.3 Interfaces .......................................................................... 132
11.4 Power connection ............................................................ 132
11.5 Safety specifications ........................................................ 132
11.6 Electromagnetic compatibility (EMC) ............................. 133
11.7 Ambient temperature ...................................................... 133
11.8 Reference conditions ........................................................ 134
11.9 Dimensions ........................................................................ 134
12 Accessories 135
Index 137

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures
848 Titrino plus ￭￭￭￭￭￭￭￭ VII
Table of figures
Figure 1 Front 848 Titrino plus ........................................................................ 7
Figure 2 Rear 848 Titrino plus ......................................................................... 8
Figure 3 Connecting pH or redox electrodes ................................................... 9
Figure 4 Connecting a reference electrode .................................................... 10
Figure 5 Connecting a temperature sensor .................................................... 10
Figure 6 Connecting a polarizable electrode .................................................. 11
Figure 7 Connecting a stirrer ......................................................................... 11
Figure 8 Connecting a balance ...................................................................... 12
Figure 9 Connecting USB devices .................................................................. 13
Figure 10 Connecting the USB stick ................................................................ 14
Figure 11 Connecting the 6.2147.000 USB keyboard with USB stick and
printer ............................................................................................. 14
Figure 12 Connecting the USB hub with USB stick, printer and the 6.2148.030
RS-232/USB Box (for connecting balances). ...................................... 15
Figure 13 Connecting a remote cable ............................................................. 15
Figure 14 Attaching the exchange unit ........................................................... 16
Figure 15 Reagent dosing for DET ................................................................... 17
Figure 16 Reagent dosing for MET .................................................................. 17
Figure 17 Reagent dosing for SET ................................................................... 18
Figure 18 Keypad 848 Titrino plus ................................................................... 20
Figure 19 Directory structure on the USB flash drive ........................................ 62
Figure 20 Tubbs method for determining the equivalence point ...................... 79
Figure 21 Rotational speed depending on stirring rate .................................. 118
Figure 22 Pin assignment of remote socket and remote plug ........................ 122
Figure 23 Remote status diagram DET/MET ................................................... 124
Figure 24 Remote status diagram SET ........................................................... 124
Figure 25 Remote status diagram CAL .......................................................... 125
Figure 26 Connecting the RS-232/USB Box to the PC .................................... 125

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
848 Titrino plus ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 848 Titrino plus is a titrator for volumetric titrations for universal appli-
cations. Methods can be created and saved under a new name. The meth-
ods can be exported to a connected USB flash drive. This function allows
you to copy methods quickly and easily from one device to another. The
remote connector makes it possible to integrate the device into a
Metrohm automation system.
1.1.1 Titration and measuring modes
The following titration and measuring modes are supported:
￭DET
Dynamic equivalence point titration. The reagent is added in variable
volume steps.
Measuring modes:
–pH (pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with selectable polarization cur-
rent)
–Upol (amperometric measurement with selectable polarization
voltage)
￭MET
Monotonic equivalence point titration. The reagent is added in con-
stant volume steps.
Measuring modes:
–pH (pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with selectable polarization cur-
rent)
–Upol (amperometric measurement with selectable polarization
voltage)
￭SET
Endpoint titration at one or two specified endpoints.
Measuring modes:
–pH (pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with selectable polarization cur-
rent)
–Upol (amperometric measurement with selectable polarization
voltage)

1.2 About the documentation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 848 Titrino plus
￭CAL
Electrode calibration.
Measuring mode:
–pH (calibration of pH electrodes)
1.1.2 Connectors
The instrument is equipped with the following connectors:
￭MSB connector (Metrohm Serial Bus)
For connecting a stirrer.
￭USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
￭Sensor connectors
Four connectors for the following sensor types:
– pH or redox electrodes
– Reference electrodes
– Polarizable electrodes
– Temperature sensors (Pt1000 or NTC)
￭Remote connector
For connecting a Dosimat or sample changer. The Dosimat enables
automatic addition of an auxiliary solution.
1.1.3 Intended use
The 848 Titrino plus is designed for usage as a titrator in analytical labora-
tories. Its main application field is volumetric titration.
This instrument is suitable for processing chemicals and flammable sam-
ples. Therefore, the use of the 848 Titrino plus requires the user to have
basic knowledge and experience in handling toxic and caustic substances.
Knowledge with respect to the application of the fire prevention measures
prescribed for laboratories is also mandatory.
1.2 About the documentation
CAUTION
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information
and warnings which the user must follow in order to ensure safe opera-
tion of the instrument.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
848 Titrino plus ￭￭￭￭￭￭￭￭ 3
1.2.1 Symbols and conventions
The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the sec-
ond to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threat-
ening hazard or risk of injury.
WARNING
This symbol draws attention to a possible hazard due
to electrical current.
WARNING
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
WARNING
This symbol draws attention to a possible biological
hazard.
CAUTION
This symbol draws attention to possible damage to
instruments or instrument parts.
NOTE
This symbol highlights additional information and
tips.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 848 Titrino plus
1.3 Safety instructions
1.3.1 General notes on safety
WARNING
This instrument may only be operated in accordance with the specifica-
tions in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
The electrical safety when working with the instrument is ensured as part
of the international standard IEC 61010.
WARNING
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
WARNING
Never open the housing of the instrument. The instrument could be
damaged by this. There is also a risk of serious injury if live components
are touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
Mains voltage
WARNING
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains voltage specified for it (see
rear panel of the instrument).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
848 Titrino plus ￭￭￭￭￭￭￭￭ 5
Protection against electrostatic charges
WARNING
Electronic components are sensitive to electrostatic charges and can be
destroyed by discharges.
Do not fail to pull the mains cable out of the mains connection socket
before you set up or disconnect electrical plug connections at the rear
of the instrument.
1.3.3 Tubing and capillary connections
CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate tools
can be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.
1.3.4 Flammable solvents and chemicals
WARNING
All relevant safety measures are to be observed when working with
flammable solvents and chemicals.
￭Set up the instrument in a well-ventilated location (e.g. fume cup-
board).
￭Keep all sources of flame far from the workplace.
￭Clean up spilled liquids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭ 848 Titrino plus
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument
848 Titrino plus ￭￭￭￭￭￭￭￭ 7
2 Overview of the instrument
2
5
4
3
1
Figure 1 Front 848 Titrino plus
1Piston rod
Of the dosing drive.
2Contact pins
For the data chip.
3Coupling
For switching the flat stopcock.
4Display
5Keypad

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ 848 Titrino plus
2
48
6
5
9
1
3
7
Figure 2 Rear 848 Titrino plus
1Electrode connector (Ind.)
For connecting pH or redox electrodes with
integrated or separate reference electrode.
Socket F.
2Type plate
Contains specifications concerning mains
voltage and serial number.
3Electrode connector (Ref.)
For connecting reference electrodes. Socket
B, 4 mm.
4Mains connection socket
5USB (OTG) connector
For connecting printers, USB sticks, USB
hubs, etc.
6MSB connector
Metrohm Serial Bus.
For connecting a stirrer. Mini DIN, 9-pin.
7Temperature sensor connector (Temp.)
For connecting temperature sensors of the
Pt1000 or NTC types. Two B sockets, 2 mm.
8Remote connector
For connecting instruments with a remote
interface. D-Sub, 9-pin.
9Electrode connector (Pol.)
For connecting polarizable electrodes, e.g.
double Pt electrodes. Socket F.

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848 Titrino plus ￭￭￭￭￭￭￭￭ 9
3 Installation
3.1 Setting up the instrument
3.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctu-
ations and direct sunlight.
3.2 Connecting a sensor
Connecting pH or redox electrodes
Figure 3 Connecting pH or redox electrodes

3.2 Connecting a sensor ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 848 Titrino plus
NOTE
The electrode cable is protected against accidental disconnection of the
cable by means of a pull-out protection feature. If you wish to remove
the plug, then you must first retract the outer plug sleeve.
Connecting a reference electrode
Figure 4 Connecting a reference electrode
Connecting a temperature sensor or an electrode with inte-
grated temperature sensor
Temperature sensors of the Pt1000 or NTC type can be connected to the
Temp. connector.
Figure 5 Connecting a temperature sensor
NOTE
The red plug must always be plugged into the red socket at the temper-
ature sensor for the purpose of shielding against disruptions.
If you use an electrode with an integrated NTC probe, then you must
plug the red plug into the red socket.